# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Diazoalkane reactivity of bis(phosphino)borate copper(I) complexes: Spectroscopic evidence for [Ph2BPtBu2]Cu=CPh2 ; _publ_contact_author_name 'Prof. Jonas Peters' _publ_contact_author_email JCPETERS@MIT.EDU loop_ _publ_author_name J.Peters N.P.Mankad # Attachment 'combined.cif' # Attachment 'Cu=CR2 Revision 2 combined cif.cif' data_npm08 _database_code_depnum_ccdc_archive 'CCDC 659790' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu(pyr) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H55 B Cu N P2' _chemical_formula_weight 626.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 16.5848(13) _cell_length_b 30.917(2) _cell_length_c 13.3863(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6863.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max .33 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8664 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2460 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following restraints were used to account for disorder in one of the tert-butyl groups: simu .04 .08 1.7 c3 c3a c4 c4a ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+7.9286P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(12) _refine_ls_number_reflns 2460 _refine_ls_number_parameters 210 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.0000 0.0000 0.00121(3) 0.01770(14) Uani 1 2 d S . . P P 0.10069(4) 0.02281(2) 0.10040(5) 0.01655(17) Uani 1 1 d . A . N N 0.0000 0.0000 -0.1469(3) 0.0205(8) Uani 1 2 d S . . B B 0.0000 0.0000 0.2926(4) 0.0189(10) Uani 1 2 d S . . C1 C 0.20339(19) 0.00088(10) 0.0608(3) 0.0279(8) Uani 1 1 d . . . C2 C 0.1920(2) -0.04698(11) 0.0449(3) 0.0436(9) Uani 1 1 d . A . H2A H 0.2418 -0.0595 0.0184 0.065 Uiso 1 1 calc R . . H2B H 0.1480 -0.0518 -0.0027 0.065 Uiso 1 1 calc R . . H2C H 0.1786 -0.0608 0.1087 0.065 Uiso 1 1 calc R . . C3 C 0.2656(5) -0.0003(4) 0.1550(12) 0.034(3) Uani 0.53(3) 1 d PU A 1 H3A H 0.3164 -0.0137 0.1342 0.085 Uiso 0.53(3) 1 calc PR A 1 H3B H 0.2418 -0.0171 0.2096 0.085 Uiso 0.53(3) 1 calc PR A 1 H3C H 0.2760 0.0293 0.1780 0.085 Uiso 0.53(3) 1 calc PR A 1 C3A C 0.2744(6) 0.0173(6) 0.1075(13) 0.046(4) Uani 0.47(3) 1 d PU A 2 H3A1 H 0.3205 -0.0011 0.0902 0.116 Uiso 0.47(3) 1 calc PR A 2 H3A2 H 0.2671 0.0174 0.1801 0.116 Uiso 0.47(3) 1 calc PR A 2 H3A3 H 0.2845 0.0469 0.0842 0.116 Uiso 0.47(3) 1 calc PR A 2 C4 C 0.2395(9) 0.0245(3) -0.0211(13) 0.043(3) Uani 0.53(3) 1 d PU A 1 H4A H 0.2603 0.0522 0.0035 0.107 Uiso 0.53(3) 1 calc PR A 1 H4B H 0.1988 0.0298 -0.0727 0.107 Uiso 0.53(3) 1 calc PR A 1 H4C H 0.2839 0.0076 -0.0494 0.107 Uiso 0.53(3) 1 calc PR A 1 C4A C 0.2098(9) 0.0123(7) -0.0591(10) 0.043(4) Uani 0.47(3) 1 d PU A 2 H4A1 H 0.2145 0.0437 -0.0678 0.108 Uiso 0.47(3) 1 calc PR A 2 H4A2 H 0.1613 0.0020 -0.0934 0.108 Uiso 0.47(3) 1 calc PR A 2 H4A3 H 0.2574 -0.0019 -0.0875 0.108 Uiso 0.47(3) 1 calc PR A 2 C5 C 0.10472(16) 0.08339(8) 0.1115(2) 0.0205(6) Uani 1 1 d . . . C6 C 0.01965(17) 0.09717(9) 0.1439(3) 0.0275(7) Uani 1 1 d . A . H6A H 0.0086 0.0860 0.2110 0.041 Uiso 1 1 calc R . . H6B H -0.0201 0.0854 0.0969 0.041 Uiso 1 1 calc R . . H6C H 0.0161 0.1288 0.1443 0.041 Uiso 1 1 calc R . . C7 C 0.12163(18) 0.10469(9) 0.0096(2) 0.0286(7) Uani 1 1 d . A . H7A H 0.1092 0.1356 0.0133 0.043 Uiso 1 1 calc R . . H7B H 0.0879 0.0911 -0.0417 0.043 Uiso 1 1 calc R . . H7C H 0.1786 0.1009 -0.0078 0.043 Uiso 1 1 calc R . . C8 C 0.16539(19) 0.09971(9) 0.1883(2) 0.0306(7) Uani 1 1 d . A . H8A H 0.1599 0.1311 0.1955 0.046 Uiso 1 1 calc R . . H8B H 0.2201 0.0928 0.1659 0.046 Uiso 1 1 calc R . . H8C H 0.1551 0.0857 0.2527 0.046 Uiso 1 1 calc R . . C9 C 0.08570(16) -0.00002(8) 0.2251(2) 0.0174(6) Uani 1 1 d . . . H9A H 0.1019 -0.0308 0.2197 0.021 Uiso 1 1 calc R A . H9B H 0.1267 0.0140 0.2680 0.021 Uiso 1 1 calc R . . C10 C -0.00326(15) 0.04257(9) 0.3686(2) 0.0190(6) Uani 1 1 d . . . C11 C -0.07280(18) 0.06622(9) 0.3896(2) 0.0238(6) Uani 1 1 d . A . H11 H -0.1221 0.0573 0.3599 0.029 Uiso 1 1 calc R . . C12 C -0.0735(2) 0.10229(10) 0.4521(2) 0.0288(7) Uani 1 1 d . . . H12 H -0.1225 0.1173 0.4640 0.035 Uiso 1 1 calc R A . C13 C -0.0031(2) 0.11621(8) 0.4966(3) 0.0291(6) Uani 1 1 d . A . H13 H -0.0027 0.1414 0.5374 0.035 Uiso 1 1 calc R . . C14 C 0.06692(19) 0.09292(10) 0.4808(2) 0.0281(7) Uani 1 1 d . . . H14 H 0.1157 0.1015 0.5123 0.034 Uiso 1 1 calc R A . C15 C 0.06583(18) 0.05709(9) 0.4190(2) 0.0222(6) Uani 1 1 d . A . H15 H 0.1146 0.0414 0.4102 0.027 Uiso 1 1 calc R . . C16 C -0.01423(19) 0.03601(11) -0.2004(2) 0.0289(7) Uani 1 1 d . . . H16 H -0.0245 0.0621 -0.1653 0.035 Uiso 1 1 calc R . . C17 C -0.0148(2) 0.03708(12) -0.3031(2) 0.0349(8) Uani 1 1 d . . . H17 H -0.0253 0.0634 -0.3372 0.042 Uiso 1 1 calc R . . C18 C 0.0000 0.0000 -0.3557(4) 0.0352(11) Uani 1 2 d S . . H18 H 0.0000 0.0000 -0.4267 0.042 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0215(2) 0.0182(2) 0.0134(2) 0.000 0.000 -0.0026(2) P 0.0159(3) 0.0176(3) 0.0162(3) -0.0011(3) 0.0016(3) -0.0028(3) N 0.0244(18) 0.0221(18) 0.0150(17) 0.000 0.000 -0.0020(13) B 0.018(2) 0.020(2) 0.018(2) 0.000 0.000 0.0006(18) C1 0.0203(17) 0.0255(17) 0.038(2) -0.0019(14) 0.0096(15) -0.0025(13) C2 0.0311(17) 0.0284(17) 0.071(3) -0.0102(18) 0.0216(17) -0.0013(15) C3 0.012(3) 0.028(5) 0.062(8) -0.023(4) -0.002(4) 0.000(3) C3A 0.016(4) 0.067(9) 0.056(8) -0.025(7) 0.006(5) 0.006(5) C4 0.041(6) 0.031(5) 0.056(8) -0.002(4) 0.024(6) 0.003(4) C4A 0.032(6) 0.072(9) 0.027(6) 0.006(5) 0.021(5) 0.018(6) C5 0.0226(13) 0.0177(13) 0.0212(14) 0.0013(12) 0.0015(12) -0.0020(11) C6 0.0284(15) 0.0203(15) 0.0337(17) 0.0008(14) 0.0069(13) 0.0013(12) C7 0.0374(16) 0.0235(15) 0.0249(16) 0.0051(13) 0.0017(14) -0.0042(13) C8 0.0392(17) 0.0181(15) 0.0346(18) -0.0032(14) -0.0100(15) -0.0031(13) C9 0.0176(13) 0.0161(14) 0.0185(15) -0.0010(11) -0.0025(12) -0.0004(10) C10 0.0255(15) 0.0158(14) 0.0156(15) 0.0048(12) 0.0008(11) 0.0004(11) C11 0.0265(15) 0.0241(15) 0.0208(15) -0.0026(12) -0.0005(12) 0.0019(12) C12 0.0382(17) 0.0240(15) 0.0241(16) -0.0027(13) 0.0025(13) 0.0102(13) C13 0.0509(17) 0.0177(12) 0.0188(14) -0.0043(16) 0.0048(13) -0.0003(16) C14 0.0339(16) 0.0293(16) 0.0211(17) -0.0034(13) 0.0021(13) -0.0094(13) C15 0.0260(15) 0.0220(15) 0.0186(14) -0.0014(11) 0.0010(12) 0.0025(12) C16 0.0399(18) 0.0240(16) 0.0227(17) -0.0002(14) 0.0000(13) 0.0038(13) C17 0.0435(18) 0.0389(19) 0.0223(18) 0.0133(16) -0.0003(15) -0.0016(15) C18 0.034(2) 0.056(3) 0.016(2) 0.000 0.000 -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.982(3) . ? Cu P 2.2470(7) . ? Cu P 2.2470(7) 2 ? P C9 1.829(3) . ? P C5 1.880(3) . ? P C1 1.908(3) . ? N C16 1.345(4) . ? N C16 1.345(4) 2 ? B C10 1.664(4) . ? B C10 1.664(4) 2 ? B C9 1.684(4) . ? B C9 1.684(4) 2 ? C1 C3A 1.427(10) . ? C1 C4 1.447(11) . ? C1 C2 1.507(4) . ? C1 C3 1.630(12) . ? C1 C4A 1.648(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5 C8 1.524(4) . ? C5 C6 1.536(4) . ? C5 C7 1.541(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.394(4) . ? C10 C15 1.403(4) . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(5) . ? C12 H12 0.9500 . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.368(5) . ? C17 H17 0.9500 . ? C18 C17 1.368(5) 2 ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu P 126.221(19) . . ? N Cu P 126.221(19) . 2 ? P Cu P 107.56(4) . 2 ? C9 P C5 108.49(13) . . ? C9 P C1 103.74(14) . . ? C5 P C1 110.13(12) . . ? C9 P Cu 108.49(9) . . ? C5 P Cu 112.68(9) . . ? C1 P Cu 112.82(12) . . ? C16 N C16 115.6(4) . 2 ? C16 N Cu 122.19(18) . . ? C16 N Cu 122.19(18) 2 . ? C10 B C10 104.6(3) . 2 ? C10 B C9 110.83(13) . . ? C10 B C9 107.47(12) 2 . ? C10 B C9 107.47(12) . 2 ? C10 B C9 110.83(13) 2 2 ? C9 B C9 115.1(3) . 2 ? C3A C1 C4 79.1(7) . . ? C3A C1 C2 121.0(8) . . ? C4 C1 C2 116.2(6) . . ? C3A C1 C3 31.4(6) . . ? C4 C1 C3 109.6(6) . . ? C2 C1 C3 99.6(4) . . ? C3A C1 C4A 107.3(7) . . ? C4 C1 C4A 29.1(4) . . ? C2 C1 C4A 94.7(8) . . ? C3 C1 C4A 135.9(6) . . ? C3A C1 P 119.2(4) . . ? C4 C1 P 113.6(5) . . ? C2 C1 P 106.0(2) . . ? C3 C1 P 111.0(4) . . ? C4A C1 P 104.6(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3A H3A1 109.5 . . ? C1 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? C1 C4A H4A1 109.5 . . ? C1 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C1 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C8 C5 C6 108.9(2) . . ? C8 C5 C7 109.6(2) . . ? C6 C5 C7 107.4(2) . . ? C8 C5 P 113.99(19) . . ? C6 C5 P 105.43(18) . . ? C7 C5 P 111.2(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? B C9 P 127.2(2) . . ? B C9 H9A 105.5 . . ? P C9 H9A 105.5 . . ? B C9 H9B 105.5 . . ? P C9 H9B 105.5 . . ? H9A C9 H9B 106.1 . . ? C11 C10 C15 114.2(3) . . ? C11 C10 B 124.4(2) . . ? C15 C10 B 121.4(2) . . ? C12 C11 C10 123.2(3) . . ? C12 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 118.8(3) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 123.7(3) . . ? C14 C15 H15 118.2 . . ? C10 C15 H15 118.2 . . ? N C16 C17 123.6(3) . . ? N C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C18 C17 C16 119.6(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C17 118.0(5) 2 . ? C17 C18 H18 121.0 2 . ? C17 C18 H18 121.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.316 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.048 #===END data_npm21 _database_code_depnum_ccdc_archive 'CCDC 659791' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((BP2)Cu(NHMes))(Li(12-C-4)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 B Cu Li N O8 P2' _chemical_formula_weight 1112.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9146(9) _cell_length_b 21.3858(16) _cell_length_c 24.4619(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.5560(10) _cell_angle_gamma 90.00 _cell_volume 6226.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72625 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 33.18 _reflns_number_total 14800 _reflns_number_gt 8871 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Only 14800 of a possible 23816 unique reflections were measured due to weak intensity at large values of 2-theta. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14800 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.725 _refine_ls_restrained_S_all 1.725 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.30379(3) 0.396884(15) 0.626762(14) 0.02089(10) Uani 1 1 d . . . P1 P 0.45659(6) 0.44506(3) 0.66728(3) 0.01795(18) Uani 1 1 d . . . P2 P 0.15406(6) 0.43834(3) 0.66782(3) 0.01920(18) Uani 1 1 d . . . N N 0.32206(18) 0.31945(10) 0.58507(9) 0.0257(6) Uani 1 1 d . . . H H 0.3267 0.2865 0.6066 0.031 Uiso 1 1 calc R . . B B 0.3110(3) 0.51518(14) 0.75025(13) 0.0180(7) Uani 1 1 d . . . C1 C 0.2654(2) 0.58752(12) 0.75390(11) 0.0193(7) Uani 1 1 d . . . C2 C 0.1788(2) 0.60212(14) 0.78881(11) 0.0265(7) Uani 1 1 d . . . H2 H 0.1477 0.5692 0.8093 0.032 Uiso 1 1 calc R . . C3 C 0.1360(2) 0.66184(14) 0.79509(12) 0.0310(8) Uani 1 1 d . . . H3 H 0.0768 0.6690 0.8191 0.037 Uiso 1 1 calc R . . C4 C 0.1801(3) 0.71085(14) 0.76628(12) 0.0332(8) Uani 1 1 d . . . H4 H 0.1513 0.7520 0.7700 0.040 Uiso 1 1 calc R . . C5 C 0.2664(3) 0.69936(14) 0.73209(12) 0.0315(8) Uani 1 1 d . . . H5 H 0.2980 0.7329 0.7125 0.038 Uiso 1 1 calc R . . C6 C 0.3074(2) 0.63929(13) 0.72606(11) 0.0241(7) Uani 1 1 d . . . H6 H 0.3667 0.6328 0.7020 0.029 Uiso 1 1 calc R . . C7 C 0.3577(2) 0.50039(12) 0.81389(11) 0.0186(7) Uani 1 1 d . . . C8 C 0.3172(2) 0.45477(13) 0.84807(11) 0.0224(7) Uani 1 1 d . . . H8 H 0.2580 0.4286 0.8343 0.027 Uiso 1 1 calc R . . C9 C 0.3588(2) 0.44538(14) 0.90142(12) 0.0287(7) Uani 1 1 d . . . H9 H 0.3275 0.4137 0.9233 0.034 Uiso 1 1 calc R . . C10 C 0.4454(3) 0.48198(15) 0.92245(12) 0.0313(8) Uani 1 1 d . . . H10 H 0.4758 0.4751 0.9585 0.038 Uiso 1 1 calc R . . C11 C 0.4872(2) 0.52860(15) 0.89044(13) 0.0307(8) Uani 1 1 d . . . H11 H 0.5460 0.5547 0.9047 0.037 Uiso 1 1 calc R . . C12 C 0.4441(2) 0.53761(13) 0.83770(12) 0.0252(7) Uani 1 1 d . . . H12 H 0.4741 0.5704 0.8166 0.030 Uiso 1 1 calc R . . C13 C 0.4163(2) 0.51296(12) 0.70720(11) 0.0191(7) Uani 1 1 d . . . H13A H 0.4846 0.5255 0.7290 0.023 Uiso 1 1 calc R . . H13B H 0.4010 0.5469 0.6804 0.023 Uiso 1 1 calc R . . C14 C 0.2056(2) 0.46577(12) 0.73547(10) 0.0185(7) Uani 1 1 d . . . H14A H 0.1393 0.4842 0.7524 0.022 Uiso 1 1 calc R . . H14B H 0.2241 0.4274 0.7566 0.022 Uiso 1 1 calc R . . C15 C 0.5358(2) 0.38970(12) 0.71532(11) 0.0217(7) Uani 1 1 d . . . C16 C 0.4449(2) 0.35447(13) 0.74571(11) 0.0263(7) Uani 1 1 d . . . H16A H 0.3945 0.3329 0.7191 0.040 Uiso 1 1 calc R . . H16B H 0.4016 0.3843 0.7668 0.040 Uiso 1 1 calc R . . H16C H 0.4806 0.3238 0.7706 0.040 Uiso 1 1 calc R . . C17 C 0.6152(2) 0.42064(13) 0.75830(11) 0.0303(8) Uani 1 1 d . . . H17A H 0.6523 0.3883 0.7810 0.046 Uiso 1 1 calc R . . H17B H 0.5721 0.4483 0.7815 0.046 Uiso 1 1 calc R . . H17C H 0.6720 0.4451 0.7399 0.046 Uiso 1 1 calc R . . C18 C 0.5993(2) 0.34122(13) 0.68292(11) 0.0287(8) Uani 1 1 d . . . H18A H 0.6648 0.3609 0.6672 0.043 Uiso 1 1 calc R . . H18B H 0.5497 0.3245 0.6534 0.043 Uiso 1 1 calc R . . H18C H 0.6243 0.3071 0.7073 0.043 Uiso 1 1 calc R . . C19 C 0.5575(2) 0.47831(13) 0.61669(11) 0.0211(7) Uani 1 1 d . . . C20 C 0.5808(2) 0.42907(13) 0.57228(11) 0.0274(7) Uani 1 1 d . . . H20A H 0.5096 0.4108 0.5585 0.041 Uiso 1 1 calc R . . H20B H 0.6292 0.3961 0.5881 0.041 Uiso 1 1 calc R . . H20C H 0.6184 0.4492 0.5421 0.041 Uiso 1 1 calc R . . C21 C 0.4971(2) 0.53347(12) 0.58754(11) 0.0250(7) Uani 1 1 d . . . H21A H 0.5393 0.5462 0.5559 0.037 Uiso 1 1 calc R . . H21B H 0.4925 0.5687 0.6130 0.037 Uiso 1 1 calc R . . H21C H 0.4212 0.5206 0.5752 0.037 Uiso 1 1 calc R . . C22 C 0.6695(2) 0.50209(13) 0.64220(11) 0.0288(8) Uani 1 1 d . . . H22A H 0.7121 0.5230 0.6141 0.043 Uiso 1 1 calc R . . H22B H 0.7131 0.4667 0.6573 0.043 Uiso 1 1 calc R . . H22C H 0.6549 0.5318 0.6716 0.043 Uiso 1 1 calc R . . C23 C 0.0502(2) 0.37498(13) 0.68625(11) 0.0235(7) Uani 1 1 d . . . C24 C 0.0076(3) 0.34056(15) 0.63484(12) 0.0514(10) Uani 1 1 d . . . H24A H 0.0715 0.3278 0.6136 0.077 Uiso 1 1 calc R . . H24B H -0.0415 0.3683 0.6126 0.077 Uiso 1 1 calc R . . H24C H -0.0347 0.3034 0.6452 0.077 Uiso 1 1 calc R . . C25 C -0.0484(2) 0.39730(14) 0.71945(12) 0.0347(8) Uani 1 1 d . . . H25A H -0.0918 0.3611 0.7310 0.052 Uiso 1 1 calc R . . H25B H -0.0969 0.4249 0.6968 0.052 Uiso 1 1 calc R . . H25C H -0.0195 0.4202 0.7518 0.052 Uiso 1 1 calc R . . C26 C 0.1171(2) 0.32578(13) 0.71969(12) 0.0335(8) Uani 1 1 d . . . H26A H 0.1397 0.3432 0.7556 0.050 Uiso 1 1 calc R . . H26B H 0.1841 0.3140 0.7003 0.050 Uiso 1 1 calc R . . H26C H 0.0701 0.2888 0.7246 0.050 Uiso 1 1 calc R . . C27 C 0.0771(2) 0.50552(12) 0.63314(11) 0.0206(7) Uani 1 1 d . . . C28 C 0.1702(2) 0.54688(13) 0.61080(11) 0.0277(7) Uani 1 1 d . . . H28A H 0.1366 0.5844 0.5939 0.042 Uiso 1 1 calc R . . H28B H 0.2105 0.5235 0.5834 0.042 Uiso 1 1 calc R . . H28C H 0.2228 0.5591 0.6409 0.042 Uiso 1 1 calc R . . C29 C 0.0018(2) 0.48412(14) 0.58454(11) 0.0323(8) Uani 1 1 d . . . H29A H -0.0197 0.5203 0.5619 0.048 Uiso 1 1 calc R . . H29B H -0.0658 0.4642 0.5979 0.048 Uiso 1 1 calc R . . H29C H 0.0426 0.4540 0.5626 0.048 Uiso 1 1 calc R . . C30 C 0.0078(2) 0.54508(13) 0.67098(11) 0.0295(8) Uani 1 1 d . . . H30A H 0.0569 0.5623 0.7005 0.044 Uiso 1 1 calc R . . H30B H -0.0502 0.5190 0.6867 0.044 Uiso 1 1 calc R . . H30C H -0.0279 0.5794 0.6501 0.044 Uiso 1 1 calc R . . C31 C 0.3294(2) 0.30375(13) 0.53198(12) 0.0238(7) Uani 1 1 d . . . C32 C 0.3613(2) 0.24278(13) 0.51439(13) 0.0274(7) Uani 1 1 d . . . C33 C 0.3602(2) 0.22889(14) 0.45859(14) 0.0345(8) Uani 1 1 d . . . H33 H 0.3808 0.1879 0.4480 0.041 Uiso 1 1 calc R . . C34 C 0.3309(2) 0.27146(15) 0.41777(13) 0.0345(8) Uani 1 1 d . . . C35 C 0.3028(2) 0.33082(14) 0.43520(12) 0.0293(8) Uani 1 1 d . . . H35 H 0.2839 0.3615 0.4083 0.035 Uiso 1 1 calc R . . C36 C 0.3009(2) 0.34782(13) 0.48995(12) 0.0243(7) Uani 1 1 d . . . C37 C 0.3940(2) 0.19454(13) 0.55601(13) 0.0383(9) Uani 1 1 d . . . H37A H 0.4165 0.1562 0.5375 0.057 Uiso 1 1 calc R . . H37B H 0.3300 0.1856 0.5786 0.057 Uiso 1 1 calc R . . H37C H 0.4570 0.2101 0.5793 0.057 Uiso 1 1 calc R . . C38 C 0.3315(3) 0.25378(16) 0.35812(13) 0.0540(11) Uani 1 1 d . . . H38A H 0.3931 0.2755 0.3409 0.081 Uiso 1 1 calc R . . H38B H 0.2599 0.2658 0.3399 0.081 Uiso 1 1 calc R . . H38C H 0.3420 0.2085 0.3548 0.081 Uiso 1 1 calc R . . C39 C 0.2621(2) 0.41164(12) 0.50588(11) 0.0275(7) Uani 1 1 d . . . H39A H 0.2430 0.4360 0.4728 0.041 Uiso 1 1 calc R . . H39B H 0.3223 0.4328 0.5273 0.041 Uiso 1 1 calc R . . H39C H 0.1957 0.4078 0.5279 0.041 Uiso 1 1 calc R . . Li Li 0.1337(3) 0.69137(18) 0.02843(16) 0.0070(9) Uani 1 1 d . . . O1 O 0.19246(16) 0.65050(9) -0.05386(8) 0.0329(5) Uani 1 1 d . . . O2 O 0.22282(15) 0.59719(9) 0.04708(8) 0.0334(5) Uani 1 1 d . . . O3 O 0.28582(16) 0.71193(10) 0.09133(8) 0.0346(5) Uani 1 1 d . . . O4 O 0.25072(16) 0.76631(9) -0.00966(8) 0.0339(5) Uani 1 1 d . . . O5 O 0.04622(16) 0.66073(9) 0.10644(8) 0.0346(5) Uani 1 1 d . . . O6 O -0.02271(16) 0.60965(10) 0.00555(9) 0.0374(5) Uani 1 1 d . . . O7 O 0.00202(15) 0.73290(9) -0.02568(8) 0.0305(5) Uani 1 1 d . . . O8 O 0.06948(16) 0.78450(9) 0.07574(8) 0.0323(5) Uani 1 1 d . . . C40 C 0.2110(3) 0.58458(13) -0.04902(12) 0.0341(8) Uani 1 1 d . . . H40A H 0.2516 0.5696 -0.0809 0.041 Uiso 1 1 calc R . . H40B H 0.1379 0.5627 -0.0489 0.041 Uiso 1 1 calc R . . C41 C 0.2787(3) 0.56960(14) 0.00295(12) 0.0343(8) Uani 1 1 d . . . H41A H 0.2841 0.5238 0.0080 0.041 Uiso 1 1 calc R . . H41B H 0.3557 0.5867 0.0012 0.041 Uiso 1 1 calc R . . C42 C 0.2909(2) 0.60249(14) 0.09652(12) 0.0315(8) Uani 1 1 d . . . H42A H 0.3402 0.5654 0.1006 0.038 Uiso 1 1 calc R . . H42B H 0.2422 0.6039 0.1282 0.038 Uiso 1 1 calc R . . C43 C 0.3616(2) 0.66072(14) 0.09563(12) 0.0314(8) Uani 1 1 d . . . H43A H 0.4096 0.6640 0.1296 0.038 Uiso 1 1 calc R . . H43B H 0.4106 0.6600 0.0640 0.038 Uiso 1 1 calc R . . C44 C 0.3355(3) 0.77068(14) 0.07921(12) 0.0350(8) Uani 1 1 d . . . H44A H 0.4079 0.7749 0.1004 0.042 Uiso 1 1 calc R . . H44B H 0.2855 0.8048 0.0905 0.042 Uiso 1 1 calc R . . C45 C 0.3554(2) 0.77689(15) 0.01926(13) 0.0394(9) Uani 1 1 d . . . H45A H 0.3838 0.8192 0.0112 0.047 Uiso 1 1 calc R . . H45B H 0.4116 0.7458 0.0082 0.047 Uiso 1 1 calc R . . C46 C 0.2617(3) 0.75185(15) -0.06619(12) 0.0346(8) Uani 1 1 d . . . H46A H 0.3239 0.7768 -0.0806 0.041 Uiso 1 1 calc R . . H46B H 0.1916 0.7636 -0.0870 0.041 Uiso 1 1 calc R . . C47 C 0.2847(2) 0.68342(15) -0.07463(12) 0.0351(8) Uani 1 1 d . . . H47A H 0.2915 0.6743 -0.1140 0.042 Uiso 1 1 calc R . . H47B H 0.3555 0.6711 -0.0548 0.042 Uiso 1 1 calc R . . C48 C -0.0580(3) 0.62920(15) 0.10136(13) 0.0399(9) Uani 1 1 d . . . H48A H -0.1193 0.6593 0.0925 0.048 Uiso 1 1 calc R . . H48B H -0.0740 0.6079 0.1361 0.048 Uiso 1 1 calc R . . C49 C -0.0496(3) 0.58187(14) 0.05588(13) 0.0402(9) Uani 1 1 d . . . H49A H 0.0089 0.5507 0.0665 0.048 Uiso 1 1 calc R . . H49B H -0.1221 0.5595 0.0510 0.048 Uiso 1 1 calc R . . C50 C -0.1138(2) 0.63997(14) -0.02278(13) 0.0380(9) Uani 1 1 d . . . H50A H -0.1645 0.6591 0.0035 0.046 Uiso 1 1 calc R . . H50B H -0.1574 0.6096 -0.0457 0.046 Uiso 1 1 calc R . . C51 C -0.0641(2) 0.68970(14) -0.05807(12) 0.0336(8) Uani 1 1 d . . . H51A H -0.0164 0.6698 -0.0853 0.040 Uiso 1 1 calc R . . H51B H -0.1253 0.7125 -0.0782 0.040 Uiso 1 1 calc R . . C52 C -0.0650(2) 0.77930(13) -0.00102(12) 0.0296(8) Uani 1 1 d . . . H52A H -0.1217 0.7593 0.0216 0.036 Uiso 1 1 calc R . . H52B H -0.1047 0.8048 -0.0296 0.036 Uiso 1 1 calc R . . C53 C 0.0115(2) 0.81958(13) 0.03381(12) 0.0293(8) Uani 1 1 d . . . H53A H 0.0668 0.8398 0.0106 0.035 Uiso 1 1 calc R . . H53B H -0.0330 0.8529 0.0507 0.035 Uiso 1 1 calc R . . C54 C 0.0037(3) 0.77017(14) 0.12113(12) 0.0351(8) Uani 1 1 d . . . H54A H -0.0762 0.7651 0.1090 0.042 Uiso 1 1 calc R . . H54B H 0.0093 0.8042 0.1485 0.042 Uiso 1 1 calc R . . C55 C 0.0486(3) 0.71054(14) 0.14540(12) 0.0342(8) Uani 1 1 d . . . H55A H 0.1269 0.7172 0.1594 0.041 Uiso 1 1 calc R . . H55B H 0.0033 0.6986 0.1767 0.041 Uiso 1 1 calc R . . C56 C 0.9019(5) 0.5288(3) 0.8486(2) 0.147(2) Uani 1 1 d . . . H56A H 0.9541 0.5574 0.8681 0.220 Uiso 1 1 calc R . . H56B H 0.9433 0.4924 0.8357 0.220 Uiso 1 1 calc R . . H56C H 0.8446 0.5148 0.8735 0.220 Uiso 1 1 calc R . . C57 C 0.8477(4) 0.5611(2) 0.8019(2) 0.0956(16) Uani 1 1 d . . . H57A H 0.8076 0.5309 0.7773 0.115 Uiso 1 1 calc R . . H57B H 0.9043 0.5834 0.7807 0.115 Uiso 1 1 calc R . . C58 C 0.7672(4) 0.6062(3) 0.8250(3) 0.160(3) Uani 1 1 d . . . H58A H 0.7072 0.5841 0.8440 0.192 Uiso 1 1 calc R . . H58B H 0.8061 0.6354 0.8509 0.192 Uiso 1 1 calc R . . C59 C 0.7255(7) 0.6363(4) 0.7810(5) 0.245(6) Uani 1 1 d . . . H59A H 0.7010 0.6042 0.7539 0.294 Uiso 1 1 calc R . . H59B H 0.7885 0.6593 0.7651 0.294 Uiso 1 1 calc R . . C60 C 0.6351(6) 0.6795(3) 0.7849(2) 0.191(4) Uani 1 1 d . . . H60A H 0.5797 0.6626 0.8094 0.287 Uiso 1 1 calc R . . H60B H 0.5994 0.6863 0.7485 0.287 Uiso 1 1 calc R . . H60C H 0.6640 0.7193 0.7995 0.287 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0239(2) 0.02166(19) 0.01720(19) -0.00117(17) 0.00221(15) -0.00232(17) P1 0.0185(4) 0.0193(4) 0.0163(4) 0.0010(3) 0.0032(3) -0.0003(3) P2 0.0192(4) 0.0216(4) 0.0167(4) -0.0019(3) 0.0009(3) -0.0026(3) N 0.0288(15) 0.0206(14) 0.0278(15) 0.0005(12) 0.0016(12) -0.0027(11) B 0.0177(18) 0.0176(18) 0.0187(19) -0.0020(14) 0.0013(15) -0.0003(14) C1 0.0165(16) 0.0262(17) 0.0145(16) -0.0033(13) -0.0057(13) -0.0020(13) C2 0.0257(17) 0.0281(18) 0.0255(18) -0.0034(15) -0.0026(14) -0.0021(15) C3 0.0296(19) 0.038(2) 0.0255(19) -0.0106(16) 0.0013(15) 0.0059(16) C4 0.043(2) 0.0231(18) 0.033(2) -0.0085(15) -0.0039(17) 0.0117(16) C5 0.037(2) 0.0213(18) 0.036(2) 0.0027(15) -0.0012(17) 0.0001(15) C6 0.0200(17) 0.0264(18) 0.0259(18) -0.0046(14) 0.0024(14) 0.0036(14) C7 0.0146(15) 0.0221(16) 0.0195(17) -0.0064(13) 0.0029(13) 0.0044(13) C8 0.0199(17) 0.0264(17) 0.0207(17) -0.0025(14) 0.0003(14) 0.0029(13) C9 0.0300(19) 0.0319(18) 0.0244(19) 0.0012(15) 0.0032(15) 0.0090(15) C10 0.033(2) 0.044(2) 0.0165(18) -0.0068(16) -0.0064(15) 0.0204(17) C11 0.0176(17) 0.044(2) 0.030(2) -0.0167(17) -0.0045(15) 0.0023(15) C12 0.0226(17) 0.0271(17) 0.0261(18) -0.0072(14) 0.0055(14) -0.0009(14) C13 0.0165(16) 0.0200(16) 0.0203(16) 0.0003(13) -0.0031(13) -0.0010(12) C14 0.0178(16) 0.0213(16) 0.0164(16) 0.0003(12) -0.0002(13) 0.0001(12) C15 0.0241(17) 0.0212(16) 0.0200(16) 0.0013(14) 0.0036(13) 0.0022(14) C16 0.0306(18) 0.0252(17) 0.0235(18) 0.0071(14) 0.0042(15) 0.0045(14) C17 0.0293(19) 0.0378(19) 0.0238(18) 0.0042(15) 0.0002(15) 0.0073(15) C18 0.0291(19) 0.0282(18) 0.0292(19) 0.0050(15) 0.0052(15) 0.0077(14) C19 0.0188(16) 0.0269(17) 0.0177(16) 0.0052(13) 0.0023(13) -0.0006(13) C20 0.0291(18) 0.0327(18) 0.0209(17) 0.0038(14) 0.0068(14) 0.0043(14) C21 0.0256(17) 0.0271(17) 0.0224(17) 0.0080(14) 0.0037(14) -0.0053(14) C22 0.0202(17) 0.0379(19) 0.0286(19) 0.0069(15) 0.0038(14) -0.0019(15) C23 0.0219(17) 0.0253(17) 0.0235(18) -0.0052(14) 0.0040(14) -0.0038(13) C24 0.060(3) 0.058(2) 0.036(2) -0.0055(19) -0.0010(19) -0.038(2) C25 0.0271(18) 0.0300(18) 0.048(2) 0.0054(17) 0.0096(16) -0.0054(15) C26 0.0276(19) 0.0244(18) 0.049(2) 0.0048(16) 0.0117(17) -0.0042(15) C27 0.0194(16) 0.0235(16) 0.0188(17) -0.0023(13) -0.0021(13) -0.0024(13) C28 0.0255(18) 0.0309(18) 0.0264(18) 0.0102(14) -0.0015(14) 0.0050(14) C29 0.0267(18) 0.038(2) 0.032(2) -0.0016(16) -0.0051(15) 0.0074(15) C30 0.0293(18) 0.0298(18) 0.0292(19) 0.0012(15) -0.0009(15) 0.0034(14) C31 0.0147(16) 0.0250(17) 0.032(2) -0.0063(15) 0.0087(14) -0.0037(13) C32 0.0140(16) 0.0266(18) 0.042(2) -0.0083(16) 0.0048(15) -0.0045(14) C33 0.0175(18) 0.0310(19) 0.056(2) -0.0247(18) 0.0103(17) -0.0064(15) C34 0.0269(19) 0.043(2) 0.035(2) -0.0136(18) 0.0117(16) -0.0066(16) C35 0.0268(18) 0.0350(19) 0.0266(19) -0.0046(15) 0.0078(15) -0.0103(15) C36 0.0190(17) 0.0258(17) 0.0288(19) -0.0043(15) 0.0085(14) -0.0086(14) C37 0.0256(19) 0.0256(18) 0.064(2) -0.0081(18) 0.0014(17) 0.0027(15) C38 0.048(2) 0.070(3) 0.045(2) -0.027(2) 0.0135(19) -0.010(2) C39 0.0314(18) 0.0276(18) 0.0239(18) 0.0008(14) 0.0057(14) -0.0039(14) Li 0.002(2) 0.013(2) 0.006(2) -0.0012(18) 0.0011(17) 0.0030(17) O1 0.0271(13) 0.0395(14) 0.0324(13) -0.0003(11) 0.0036(10) 0.0062(11) O2 0.0277(12) 0.0469(14) 0.0257(12) -0.0034(11) 0.0014(10) 0.0073(11) O3 0.0320(13) 0.0387(13) 0.0334(13) 0.0052(11) 0.0048(11) 0.0022(11) O4 0.0237(12) 0.0439(14) 0.0340(14) 0.0034(11) -0.0004(11) -0.0016(10) O5 0.0276(13) 0.0390(14) 0.0376(14) 0.0010(11) 0.0062(11) -0.0012(11) O6 0.0289(13) 0.0412(14) 0.0421(14) 0.0008(12) 0.0032(11) 0.0058(11) O7 0.0225(12) 0.0354(13) 0.0337(13) -0.0067(10) 0.0021(10) 0.0003(10) O8 0.0288(13) 0.0413(13) 0.0270(13) 0.0029(10) 0.0019(10) -0.0019(10) C40 0.032(2) 0.033(2) 0.038(2) -0.0059(16) 0.0016(16) 0.0088(15) C41 0.034(2) 0.037(2) 0.033(2) -0.0031(16) 0.0054(16) 0.0097(16) C42 0.0278(18) 0.043(2) 0.0243(18) 0.0056(16) 0.0033(15) 0.0068(16) C43 0.0279(19) 0.044(2) 0.0222(18) 0.0048(15) -0.0017(15) 0.0087(16) C44 0.0288(19) 0.038(2) 0.038(2) 0.0027(17) -0.0017(16) -0.0090(16) C45 0.0230(19) 0.049(2) 0.046(2) 0.0131(18) -0.0069(17) -0.0060(16) C46 0.0276(19) 0.051(2) 0.025(2) 0.0116(16) 0.0019(15) 0.0025(16) C47 0.0265(19) 0.054(2) 0.0245(19) 0.0051(16) 0.0036(15) 0.0048(17) C48 0.031(2) 0.039(2) 0.050(2) 0.0043(18) 0.0127(18) -0.0083(16) C49 0.037(2) 0.0294(19) 0.054(2) 0.0030(18) 0.0050(18) -0.0047(16) C50 0.0242(19) 0.038(2) 0.052(2) -0.0114(18) -0.0025(17) 0.0029(16) C51 0.0264(19) 0.039(2) 0.035(2) -0.0139(17) -0.0052(16) -0.0008(16) C52 0.0267(18) 0.0271(18) 0.035(2) 0.0010(15) 0.0047(16) 0.0040(15) C53 0.0299(19) 0.0272(18) 0.0313(19) 0.0016(15) 0.0048(16) 0.0015(15) C54 0.039(2) 0.039(2) 0.028(2) -0.0055(16) 0.0061(17) 0.0003(17) C55 0.034(2) 0.043(2) 0.0266(19) -0.0046(17) 0.0030(16) -0.0023(16) C56 0.199(7) 0.109(5) 0.134(6) -0.006(4) 0.025(5) -0.020(5) C57 0.090(4) 0.091(4) 0.104(4) 0.008(3) -0.009(3) 0.008(3) C58 0.063(4) 0.073(4) 0.339(11) 0.037(5) -0.052(5) 0.028(3) C59 0.186(9) 0.139(7) 0.419(17) 0.020(8) 0.121(10) 0.104(6) C60 0.261(9) 0.212(8) 0.095(5) 0.085(5) -0.061(5) -0.154(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.962(2) . ? Cu P2 2.2665(8) . ? Cu P1 2.2798(8) . ? P1 C13 1.826(3) . ? P1 C15 1.890(3) . ? P1 C19 1.901(3) . ? P2 C14 1.835(3) . ? P2 C27 1.885(3) . ? P2 C23 1.903(3) . ? N C31 1.348(3) . ? N H 0.8800 . ? B C1 1.644(4) . ? B C7 1.660(4) . ? B C14 1.669(4) . ? B C13 1.674(4) . ? C1 C2 1.403(3) . ? C1 C6 1.404(4) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.376(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.385(3) . ? C7 C12 1.407(3) . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C10 1.376(4) . ? C9 H9 0.9500 . ? C10 C11 1.375(4) . ? C10 H10 0.9500 . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.533(4) . ? C15 C18 1.526(3) . ? C15 C16 1.538(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.534(3) . ? C19 C21 1.540(3) . ? C19 C20 1.547(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.524(4) . ? C23 C25 1.533(4) . ? C23 C26 1.534(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.525(4) . ? C27 C29 1.527(3) . ? C27 C28 1.537(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.424(4) . ? C31 C32 1.430(4) . ? C32 C33 1.396(4) . ? C32 C37 1.489(4) . ? C33 C34 1.385(4) . ? C33 H33 0.9500 . ? C34 C35 1.385(4) . ? C34 C38 1.508(4) . ? C35 C36 1.389(4) . ? C35 H35 0.9500 . ? C36 C39 1.498(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Li O7 2.195(4) . ? Li O2 2.313(4) . ? Li O5 2.310(4) . ? Li O1 2.331(4) . ? Li O4 2.344(4) . ? Li O3 2.366(4) . ? Li O8 2.443(4) . ? Li O6 2.598(4) . ? O1 C47 1.418(3) . ? O1 C40 1.431(3) . ? O2 C41 1.422(3) . ? O2 C42 1.430(3) . ? O3 C43 1.421(3) . ? O3 C44 1.426(3) . ? O4 C45 1.424(3) . ? O4 C46 1.429(3) . ? O5 C48 1.414(3) . ? O5 C55 1.429(3) . ? O6 C49 1.416(3) . ? O6 C50 1.418(3) . ? O7 C52 1.424(3) . ? O7 C51 1.430(3) . ? O8 C54 1.421(3) . ? O8 C53 1.425(3) . ? C40 C41 1.509(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.505(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.502(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.505(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.511(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.508(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.493(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.496(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.462(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.490(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.332(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.425(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu P2 131.93(7) . . ? N Cu P1 120.16(7) . . ? P2 Cu P1 105.05(3) . . ? C13 P1 C15 107.54(12) . . ? C13 P1 C19 103.87(12) . . ? C15 P1 C19 109.04(12) . . ? C13 P1 Cu 111.58(9) . . ? C15 P1 Cu 110.73(9) . . ? C19 P1 Cu 113.70(9) . . ? C14 P2 C27 107.36(12) . . ? C14 P2 C23 102.06(12) . . ? C27 P2 C23 109.94(12) . . ? C14 P2 Cu 106.65(9) . . ? C27 P2 Cu 118.36(9) . . ? C23 P2 Cu 111.08(9) . . ? C31 N Cu 136.4(2) . . ? C31 N H 111.8 . . ? Cu N H 111.8 . . ? C1 B C7 103.1(2) . . ? C1 B C14 111.1(2) . . ? C7 B C14 107.4(2) . . ? C1 B C13 108.7(2) . . ? C7 B C13 110.8(2) . . ? C14 B C13 115.1(2) . . ? C2 C1 C6 114.0(3) . . ? C2 C1 B 119.8(2) . . ? C6 C1 B 126.2(2) . . ? C3 C2 C1 123.8(3) . . ? C3 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 123.0(3) . . ? C5 C6 H6 118.5 . . ? C1 C6 H6 118.5 . . ? C8 C7 C12 114.6(3) . . ? C8 C7 B 126.1(2) . . ? C12 C7 B 119.3(2) . . ? C7 C8 C9 123.3(3) . . ? C7 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 122.9(3) . . ? C11 C12 H12 118.6 . . ? C7 C12 H12 118.6 . . ? B C13 P1 125.54(18) . . ? B C13 H13A 105.9 . . ? P1 C13 H13A 105.9 . . ? B C13 H13B 105.9 . . ? P1 C13 H13B 105.9 . . ? H13A C13 H13B 106.3 . . ? B C14 P2 128.01(19) . . ? B C14 H14A 105.3 . . ? P2 C14 H14A 105.3 . . ? B C14 H14B 105.3 . . ? P2 C14 H14B 105.3 . . ? H14A C14 H14B 106.0 . . ? C17 C15 C18 110.1(2) . . ? C17 C15 C16 107.8(2) . . ? C18 C15 C16 107.1(2) . . ? C17 C15 P1 115.59(19) . . ? C18 C15 P1 110.35(18) . . ? C16 C15 P1 105.35(17) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C21 108.3(2) . . ? C22 C19 C20 109.3(2) . . ? C21 C19 C20 106.9(2) . . ? C22 C19 P1 115.02(18) . . ? C21 C19 P1 106.96(18) . . ? C20 C19 P1 109.94(18) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 110.6(2) . . ? C24 C23 C26 104.8(2) . . ? C25 C23 C26 108.8(2) . . ? C24 C23 P2 110.16(19) . . ? C25 C23 P2 115.17(19) . . ? C26 C23 P2 106.67(18) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C29 108.9(2) . . ? C30 C27 C28 108.4(2) . . ? C29 C27 C28 107.7(2) . . ? C30 C27 P2 114.54(19) . . ? C29 C27 P2 112.26(19) . . ? C28 C27 P2 104.76(17) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N C31 C36 120.5(3) . . ? N C31 C32 123.1(3) . . ? C36 C31 C32 116.4(3) . . ? C33 C32 C31 119.8(3) . . ? C33 C32 C37 120.8(3) . . ? C31 C32 C37 119.4(3) . . ? C34 C33 C32 123.8(3) . . ? C34 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? C35 C34 C33 115.9(3) . . ? C35 C34 C38 122.7(3) . . ? C33 C34 C38 121.4(3) . . ? C34 C35 C36 123.5(3) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C31 120.6(3) . . ? C35 C36 C39 120.5(3) . . ? C31 C36 C39 118.8(2) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 Li O2 141.3(2) . . ? O7 Li O5 106.04(16) . . ? O2 Li O5 79.05(14) . . ? O7 Li O1 82.25(14) . . ? O2 Li O1 71.98(13) . . ? O5 Li O1 140.46(19) . . ? O7 Li O4 84.58(15) . . ? O2 Li O4 113.44(17) . . ? O5 Li O4 145.14(19) . . ? O1 Li O4 72.92(13) . . ? O7 Li O3 145.4(2) . . ? O2 Li O3 72.65(13) . . ? O5 Li O3 82.89(14) . . ? O1 Li O3 112.36(16) . . ? O4 Li O3 71.31(13) . . ? O7 Li O8 74.06(13) . . ? O2 Li O8 140.09(19) . . ? O5 Li O8 71.19(13) . . ? O1 Li O8 145.82(19) . . ? O4 Li O8 80.53(14) . . ? O3 Li O8 77.73(13) . . ? O7 Li O6 69.86(13) . . ? O2 Li O6 77.01(13) . . ? O5 Li O6 68.98(12) . . ? O1 Li O6 78.57(13) . . ? O4 Li O6 143.90(18) . . ? O3 Li O6 141.87(18) . . ? O8 Li O6 114.44(16) . . ? C47 O1 C40 113.5(2) . . ? C47 O1 Li 113.00(19) . . ? C40 O1 Li 110.45(19) . . ? C41 O2 C42 114.1(2) . . ? C41 O2 Li 115.99(19) . . ? C42 O2 Li 109.63(19) . . ? C43 O3 C44 115.2(2) . . ? C43 O3 Li 111.78(19) . . ? C44 O3 Li 109.99(19) . . ? C45 O4 C46 113.5(2) . . ? C45 O4 Li 115.73(19) . . ? C46 O4 Li 108.57(19) . . ? C48 O5 C55 113.9(2) . . ? C48 O5 Li 119.3(2) . . ? C55 O5 Li 110.08(19) . . ? C49 O6 C50 114.8(2) . . ? C49 O6 Li 106.42(19) . . ? C50 O6 Li 108.88(18) . . ? C52 O7 C51 112.3(2) . . ? C52 O7 Li 115.19(19) . . ? C51 O7 Li 115.70(19) . . ? C54 O8 C53 114.2(2) . . ? C54 O8 Li 112.94(19) . . ? C53 O8 Li 103.90(18) . . ? O1 C40 C41 110.7(2) . . ? O1 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? O1 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? O2 C41 C40 107.5(2) . . ? O2 C41 H41A 110.2 . . ? C40 C41 H41A 110.2 . . ? O2 C41 H41B 110.2 . . ? C40 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? O2 C42 C43 110.5(2) . . ? O2 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? O2 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? O3 C43 C42 106.5(2) . . ? O3 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? O3 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? O3 C44 C45 111.5(2) . . ? O3 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? O3 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? O4 C45 C44 107.4(2) . . ? O4 C45 H45A 110.2 . . ? C44 C45 H45A 110.2 . . ? O4 C45 H45B 110.2 . . ? C44 C45 H45B 110.2 . . ? H45A C45 H45B 108.5 . . ? O4 C46 C47 111.6(2) . . ? O4 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? O4 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? O1 C47 C46 106.5(2) . . ? O1 C47 H47A 110.4 . . ? C46 C47 H47A 110.4 . . ? O1 C47 H47B 110.4 . . ? C46 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? O5 C48 C49 107.3(2) . . ? O5 C48 H48A 110.3 . . ? C49 C48 H48A 110.3 . . ? O5 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.5 . . ? O6 C49 C48 112.6(2) . . ? O6 C49 H49A 109.1 . . ? C48 C49 H49A 109.1 . . ? O6 C49 H49B 109.1 . . ? C48 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? O6 C50 C51 106.9(2) . . ? O6 C50 H50A 110.3 . . ? C51 C50 H50A 110.3 . . ? O6 C50 H50B 110.3 . . ? C51 C50 H50B 110.3 . . ? H50A C50 H50B 108.6 . . ? O7 C51 C50 111.0(2) . . ? O7 C51 H51A 109.4 . . ? C50 C51 H51A 109.4 . . ? O7 C51 H51B 109.4 . . ? C50 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? O7 C52 C53 107.7(2) . . ? O7 C52 H52A 110.2 . . ? C53 C52 H52A 110.2 . . ? O7 C52 H52B 110.2 . . ? C53 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? O8 C53 C52 111.8(2) . . ? O8 C53 H53A 109.3 . . ? C52 C53 H53A 109.3 . . ? O8 C53 H53B 109.3 . . ? C52 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? O8 C54 C55 107.1(2) . . ? O8 C54 H54A 110.3 . . ? C55 C54 H54A 110.3 . . ? O8 C54 H54B 110.3 . . ? C55 C54 H54B 110.3 . . ? H54A C54 H54B 108.6 . . ? O5 C55 C54 112.0(2) . . ? O5 C55 H55A 109.2 . . ? C54 C55 H55A 109.2 . . ? O5 C55 H55B 109.2 . . ? C54 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C56 C57 C58 106.2(5) . . ? C56 C57 H57A 110.5 . . ? C58 C57 H57A 110.5 . . ? C56 C57 H57B 110.5 . . ? C58 C57 H57B 110.5 . . ? H57A C57 H57B 108.7 . . ? C59 C58 C57 103.3(7) . . ? C59 C58 H58A 111.1 . . ? C57 C58 H58A 111.1 . . ? C59 C58 H58B 111.1 . . ? C57 C58 H58B 111.1 . . ? H58A C58 H58B 109.1 . . ? C58 C59 C60 121.0(9) . . ? C58 C59 H59A 107.1 . . ? C60 C59 H59A 107.1 . . ? C58 C59 H59B 107.1 . . ? C60 C59 H59B 107.1 . . ? H59A C59 H59B 106.8 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.621 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.621 _refine_diff_density_max 1.674 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.083 #===END data_npm36 _database_code_depnum_ccdc_archive 'CCDC 659792' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu(NH2Mes) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H63 B Cu N P2' _chemical_formula_weight 682.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.186(5) _cell_length_b 17.079(8) _cell_length_c 22.083(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.24(4) _cell_angle_gamma 90.00 _cell_volume 3802(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31590 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.1047 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.38 _reflns_number_total 7306 _reflns_number_gt 4330 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7306 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_restrained_S_all 1.288 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.86775(4) 0.23362(2) 0.903522(17) 0.01599(12) Uani 1 1 d . . . P1 P 0.89558(8) 0.19781(5) 0.80735(4) 0.0144(2) Uani 1 1 d . . . P2 P 1.06882(8) 0.23767(5) 0.96054(4) 0.0155(2) Uani 1 1 d . . . N N 0.6784(2) 0.24942(15) 0.92582(11) 0.0229(7) Uani 1 1 d . . . H0A H 0.6253 0.2641 0.8916 0.027 Uiso 1 1 calc R . . H0B H 0.6492 0.2026 0.9369 0.027 Uiso 1 1 calc R . . B B 1.2040(4) 0.1897(2) 0.84612(16) 0.0142(9) Uani 1 1 d . . . C1 C 1.3035(3) 0.11374(18) 0.86060(14) 0.0155(8) Uani 1 1 d . . . C2 C 1.2888(3) 0.04361(18) 0.82724(14) 0.0206(8) Uani 1 1 d . . . H2 H 1.2181 0.0393 0.7957 0.025 Uiso 1 1 calc R . . C3 C 1.3737(3) -0.0194(2) 0.83864(16) 0.0267(9) Uani 1 1 d . . . H3 H 1.3593 -0.0645 0.8150 0.032 Uiso 1 1 calc R . . C4 C 1.4793(3) -0.0158(2) 0.88478(16) 0.0270(9) Uani 1 1 d . . . H4 H 1.5362 -0.0582 0.8929 0.032 Uiso 1 1 calc R . . C5 C 1.4992(3) 0.0517(2) 0.91868(15) 0.0249(9) Uani 1 1 d . . . H5 H 1.5701 0.0553 0.9502 0.030 Uiso 1 1 calc R . . C6 C 1.4133(3) 0.11453(19) 0.90587(14) 0.0201(8) Uani 1 1 d . . . H6 H 1.4302 0.1599 0.9290 0.024 Uiso 1 1 calc R . . C7 C 1.2792(3) 0.24417(17) 0.79884(13) 0.0136(7) Uani 1 1 d . . . C8 C 1.3302(3) 0.31918(18) 0.81122(14) 0.0187(8) Uani 1 1 d . . . H8 H 1.3249 0.3408 0.8494 0.022 Uiso 1 1 calc R . . C9 C 1.3889(3) 0.36347(19) 0.76917(15) 0.0225(9) Uani 1 1 d . . . H9 H 1.4193 0.4138 0.7793 0.027 Uiso 1 1 calc R . . C10 C 1.4017(3) 0.3330(2) 0.71317(15) 0.0217(8) Uani 1 1 d . . . H10 H 1.4403 0.3623 0.6849 0.026 Uiso 1 1 calc R . . C11 C 1.3566(3) 0.25777(19) 0.69889(14) 0.0197(8) Uani 1 1 d . . . H11 H 1.3653 0.2362 0.6610 0.024 Uiso 1 1 calc R . . C12 C 1.2987(3) 0.21474(18) 0.74102(14) 0.0186(8) Uani 1 1 d . . . H12 H 1.2713 0.1639 0.7308 0.022 Uiso 1 1 calc R . . C13 C 1.1934(3) 0.24291(17) 0.90859(13) 0.0158(8) Uani 1 1 d . . . H13A H 1.1921 0.2969 0.8949 0.019 Uiso 1 1 calc R . . H13B H 1.2779 0.2358 0.9345 0.019 Uiso 1 1 calc R . . C14 C 1.0598(3) 0.15453(17) 0.81023(13) 0.0143(8) Uani 1 1 d . . . H14A H 1.0522 0.1022 0.8264 0.017 Uiso 1 1 calc R . . H14B H 1.0728 0.1478 0.7679 0.017 Uiso 1 1 calc R . . C15 C 0.8882(3) 0.28245(17) 0.75144(14) 0.0174(8) Uani 1 1 d . . . C16 C 0.9526(3) 0.26535(19) 0.69467(13) 0.0241(8) Uani 1 1 d . . . H16A H 0.9082 0.2220 0.6729 0.036 Uiso 1 1 calc R . . H16B H 1.0444 0.2526 0.7067 0.036 Uiso 1 1 calc R . . H16C H 0.9457 0.3107 0.6687 0.036 Uiso 1 1 calc R . . C17 C 0.7459(3) 0.31016(19) 0.73259(14) 0.0246(9) Uani 1 1 d . . . H17A H 0.7461 0.3581 0.7099 0.037 Uiso 1 1 calc R . . H17B H 0.7047 0.3188 0.7685 0.037 Uiso 1 1 calc R . . H17C H 0.6972 0.2710 0.7075 0.037 Uiso 1 1 calc R . . C18 C 0.9662(3) 0.34888(17) 0.78685(14) 0.0216(8) Uani 1 1 d . . . H18A H 1.0562 0.3325 0.7992 0.032 Uiso 1 1 calc R . . H18B H 0.9261 0.3615 0.8224 0.032 Uiso 1 1 calc R . . H18C H 0.9651 0.3942 0.7611 0.032 Uiso 1 1 calc R . . C19 C 0.7779(3) 0.11596(18) 0.77705(14) 0.0185(8) Uani 1 1 d . . . C20 C 0.8045(3) 0.04797(19) 0.82179(16) 0.0340(10) Uani 1 1 d . . . H20A H 0.8053 0.0668 0.8628 0.051 Uiso 1 1 calc R . . H20B H 0.8889 0.0250 0.8180 0.051 Uiso 1 1 calc R . . H20C H 0.7360 0.0093 0.8128 0.051 Uiso 1 1 calc R . . C21 C 0.7946(4) 0.0864(2) 0.71311(16) 0.0460(12) Uani 1 1 d . . . H21A H 0.7394 0.0413 0.7033 0.069 Uiso 1 1 calc R . . H21B H 0.8856 0.0724 0.7123 0.069 Uiso 1 1 calc R . . H21C H 0.7692 0.1269 0.6836 0.069 Uiso 1 1 calc R . . C22 C 0.6338(3) 0.1395(2) 0.77673(16) 0.0306(9) Uani 1 1 d . . . H22A H 0.5777 0.0947 0.7671 0.046 Uiso 1 1 calc R . . H22B H 0.6105 0.1795 0.7466 0.046 Uiso 1 1 calc R . . H22C H 0.6221 0.1591 0.8164 0.046 Uiso 1 1 calc R . . C23 C 1.1063(3) 0.32978(18) 1.00800(14) 0.0189(8) Uani 1 1 d . . . C24 C 1.2542(3) 0.34354(19) 1.02981(15) 0.0286(9) Uani 1 1 d . . . H24A H 1.3004 0.3481 0.9950 0.043 Uiso 1 1 calc R . . H24B H 1.2896 0.3002 1.0547 0.043 Uiso 1 1 calc R . . H24C H 1.2653 0.3909 1.0534 0.043 Uiso 1 1 calc R . . C25 C 1.0542(3) 0.39857(18) 0.96708(15) 0.0295(9) Uani 1 1 d . . . H25A H 1.0720 0.4467 0.9892 0.044 Uiso 1 1 calc R . . H25B H 0.9603 0.3930 0.9551 0.044 Uiso 1 1 calc R . . H25C H 1.0977 0.3992 0.9313 0.044 Uiso 1 1 calc R . . C26 C 1.0318(3) 0.33001(19) 1.06360(15) 0.0303(9) Uani 1 1 d . . . H26A H 1.0378 0.3810 1.0820 0.045 Uiso 1 1 calc R . . H26B H 1.0706 0.2920 1.0928 0.045 Uiso 1 1 calc R . . H26C H 0.9403 0.3172 1.0507 0.045 Uiso 1 1 calc R . . C27 C 1.1012(3) 0.14856(18) 1.01035(14) 0.0188(8) Uani 1 1 d . . . C28 C 1.1000(3) 0.07834(18) 0.96697(15) 0.0256(9) Uani 1 1 d . . . H28A H 1.1728 0.0826 0.9439 0.038 Uiso 1 1 calc R . . H28B H 1.0180 0.0777 0.9395 0.038 Uiso 1 1 calc R . . H28C H 1.1084 0.0308 0.9904 0.038 Uiso 1 1 calc R . . C29 C 1.2313(3) 0.1481(2) 1.05318(16) 0.0370(10) Uani 1 1 d . . . H29A H 1.2420 0.0987 1.0740 0.056 Uiso 1 1 calc R . . H29B H 1.2311 0.1895 1.0826 0.056 Uiso 1 1 calc R . . H29C H 1.3032 0.1559 1.0301 0.056 Uiso 1 1 calc R . . C30 C 0.9856(3) 0.13605(19) 1.04728(15) 0.0329(10) Uani 1 1 d . . . H30A H 0.9998 0.0886 1.0706 0.049 Uiso 1 1 calc R . . H30B H 0.9039 0.1323 1.0197 0.049 Uiso 1 1 calc R . . H30C H 0.9811 0.1795 1.0745 0.049 Uiso 1 1 calc R . . C31 C 0.6604(3) 0.3048(2) 0.97319(15) 0.0202(8) Uani 1 1 d . . . C32 C 0.6443(3) 0.27878(19) 1.03195(15) 0.0188(8) Uani 1 1 d . . . C33 C 0.6351(3) 0.3362(2) 1.07632(15) 0.0230(9) Uani 1 1 d . . . H33 H 0.6244 0.3202 1.1155 0.028 Uiso 1 1 calc R . . C34 C 0.6413(3) 0.4156(2) 1.06485(16) 0.0237(9) Uani 1 1 d . . . C35 C 0.6539(3) 0.43810(19) 1.00564(16) 0.0268(9) Uani 1 1 d . . . H35 H 0.6558 0.4912 0.9966 0.032 Uiso 1 1 calc R . . C36 C 0.6639(3) 0.3843(2) 0.95941(15) 0.0218(8) Uani 1 1 d . . . C37 C 0.6350(3) 0.19457(19) 1.04822(15) 0.0272(9) Uani 1 1 d . . . H37A H 0.6474 0.1891 1.0919 0.041 Uiso 1 1 calc R . . H37B H 0.7024 0.1655 1.0317 0.041 Uiso 1 1 calc R . . H37C H 0.5492 0.1748 1.0315 0.041 Uiso 1 1 calc R . . C38 C 0.6368(4) 0.4746(2) 1.11582(16) 0.0398(11) Uani 1 1 d . . . H38A H 0.5843 0.4541 1.1450 0.060 Uiso 1 1 calc R . . H38B H 0.5981 0.5225 1.0990 0.060 Uiso 1 1 calc R . . H38C H 0.7253 0.4846 1.1358 0.060 Uiso 1 1 calc R . . C39 C 0.6802(3) 0.4114(2) 0.89625(15) 0.0336(10) Uani 1 1 d . . . H39A H 0.6895 0.4674 0.8962 0.050 Uiso 1 1 calc R . . H39B H 0.6036 0.3966 0.8681 0.050 Uiso 1 1 calc R . . H39C H 0.7578 0.3877 0.8841 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0161(2) 0.0206(2) 0.0115(2) -0.00072(19) 0.00283(17) 0.00053(19) P1 0.0133(5) 0.0192(5) 0.0103(5) -0.0002(4) 0.0004(4) 0.0014(4) P2 0.0166(5) 0.0211(5) 0.0087(5) -0.0006(4) 0.0021(4) 0.0007(4) N 0.0168(15) 0.0325(19) 0.0189(16) -0.0012(13) 0.0013(12) -0.0023(13) B 0.016(2) 0.018(2) 0.009(2) -0.0007(17) 0.0035(17) 0.0023(17) C1 0.0147(19) 0.023(2) 0.010(2) 0.0027(15) 0.0048(15) -0.0043(15) C2 0.016(2) 0.025(2) 0.019(2) 0.0010(17) -0.0028(16) 0.0022(16) C3 0.026(2) 0.025(2) 0.030(3) -0.0043(17) 0.0076(19) 0.0013(17) C4 0.016(2) 0.022(2) 0.042(3) 0.0089(18) 0.0012(19) 0.0070(16) C5 0.016(2) 0.030(2) 0.026(2) 0.0013(18) -0.0045(16) -0.0018(17) C6 0.019(2) 0.023(2) 0.019(2) 0.0005(16) 0.0025(17) -0.0016(16) C7 0.0068(16) 0.021(2) 0.0119(19) -0.0021(15) -0.0021(14) 0.0037(14) C8 0.019(2) 0.029(2) 0.009(2) -0.0042(16) 0.0026(15) 0.0014(16) C9 0.022(2) 0.027(2) 0.018(2) -0.0016(17) 0.0023(17) -0.0045(16) C10 0.015(2) 0.037(2) 0.015(2) 0.0087(17) 0.0057(16) -0.0014(17) C11 0.0138(18) 0.037(2) 0.0090(19) -0.0017(16) 0.0033(14) 0.0041(17) C12 0.0153(19) 0.023(2) 0.017(2) -0.0019(15) 0.0008(15) 0.0036(15) C13 0.0146(17) 0.020(2) 0.0122(18) 0.0013(15) 0.0009(14) 0.0003(15) C14 0.0188(19) 0.0183(19) 0.0072(19) 0.0025(14) 0.0064(15) 0.0024(15) C15 0.0154(18) 0.024(2) 0.013(2) 0.0001(15) 0.0014(15) 0.0028(15) C16 0.0215(19) 0.036(2) 0.015(2) 0.0029(17) 0.0037(15) -0.0001(18) C17 0.020(2) 0.032(2) 0.021(2) 0.0036(17) 0.0017(16) 0.0028(17) C18 0.019(2) 0.025(2) 0.021(2) 0.0069(16) 0.0041(17) 0.0027(16) C19 0.0146(19) 0.024(2) 0.017(2) -0.0046(16) 0.0024(16) 0.0001(15) C20 0.025(2) 0.023(2) 0.053(3) 0.0014(19) 0.000(2) -0.0080(17) C21 0.041(3) 0.066(3) 0.033(3) -0.031(2) 0.012(2) -0.023(2) C22 0.016(2) 0.037(2) 0.037(3) -0.0023(18) -0.0018(18) -0.0039(17) C23 0.021(2) 0.025(2) 0.011(2) -0.0070(16) 0.0068(16) -0.0009(16) C24 0.035(2) 0.033(2) 0.017(2) -0.0056(17) 0.0011(18) -0.0053(18) C25 0.040(3) 0.023(2) 0.025(2) -0.0090(17) 0.0041(19) 0.0012(18) C26 0.033(2) 0.037(2) 0.021(2) -0.0111(18) 0.0085(18) -0.0038(19) C27 0.018(2) 0.026(2) 0.013(2) 0.0005(16) 0.0031(16) -0.0018(16) C28 0.029(2) 0.025(2) 0.024(2) 0.0115(17) 0.0074(18) 0.0007(16) C29 0.038(3) 0.038(2) 0.031(3) 0.0100(18) -0.009(2) -0.0012(19) C30 0.047(3) 0.033(2) 0.023(2) 0.0007(17) 0.0183(19) -0.0018(19) C31 0.0126(19) 0.028(2) 0.020(2) -0.0048(18) 0.0040(16) -0.0001(16) C32 0.0115(18) 0.024(2) 0.021(2) -0.0004(17) 0.0026(15) 0.0013(15) C33 0.022(2) 0.036(2) 0.012(2) 0.0031(17) 0.0034(16) -0.0041(17) C34 0.024(2) 0.028(2) 0.021(2) -0.0042(18) 0.0071(17) 0.0006(17) C35 0.032(2) 0.020(2) 0.029(2) -0.0009(18) 0.0075(18) -0.0001(17) C36 0.019(2) 0.030(2) 0.017(2) 0.0032(17) 0.0032(16) -0.0031(16) C37 0.025(2) 0.035(2) 0.022(2) 0.0006(18) 0.0016(17) -0.0046(18) C38 0.051(3) 0.036(2) 0.033(3) -0.0142(19) 0.011(2) -0.002(2) C39 0.037(2) 0.040(2) 0.025(2) 0.0039(18) 0.0072(19) 0.0002(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 2.076(2) . ? Cu P2 2.2464(14) . ? Cu P1 2.2667(11) . ? P1 C14 1.821(3) . ? P1 C15 1.896(3) . ? P1 C19 1.900(3) . ? P2 C13 1.831(3) . ? P2 C27 1.879(3) . ? P2 C23 1.898(3) . ? N C31 1.442(4) . ? N H0A 0.9000 . ? N H0B 0.9000 . ? B C1 1.649(5) . ? B C7 1.665(4) . ? B C13 1.669(4) . ? B C14 1.677(5) . ? C1 C6 1.389(4) . ? C1 C2 1.403(4) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.373(4) . ? C3 H3 0.9300 . ? C4 C5 1.374(4) . ? C4 H4 0.9300 . ? C5 C6 1.388(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.395(4) . ? C7 C12 1.413(4) . ? C8 C9 1.397(4) . ? C8 H8 0.9300 . ? C9 C10 1.365(4) . ? C9 H9 0.9300 . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.524(4) . ? C15 C17 1.526(4) . ? C15 C18 1.533(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C22 1.521(4) . ? C19 C20 1.524(4) . ? C19 C21 1.532(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C25 1.530(4) . ? C23 C24 1.533(4) . ? C23 C26 1.534(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C29 1.513(4) . ? C27 C28 1.534(4) . ? C27 C30 1.540(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C36 1.393(4) . ? C31 C32 1.403(4) . ? C32 C33 1.399(4) . ? C32 C37 1.489(4) . ? C33 C34 1.382(4) . ? C33 H33 0.9300 . ? C34 C35 1.387(4) . ? C34 C38 1.516(4) . ? C35 C36 1.388(4) . ? C35 H35 0.9300 . ? C36 C39 1.501(4) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu P2 131.81(8) . . ? N Cu P1 120.17(8) . . ? P2 Cu P1 107.89(5) . . ? C14 P1 C15 106.42(14) . . ? C14 P1 C19 104.09(14) . . ? C15 P1 C19 111.58(15) . . ? C14 P1 Cu 108.32(10) . . ? C15 P1 Cu 113.95(10) . . ? C19 P1 Cu 111.80(10) . . ? C13 P2 C27 109.08(14) . . ? C13 P2 C23 101.69(14) . . ? C27 P2 C23 110.09(15) . . ? C13 P2 Cu 107.97(11) . . ? C27 P2 Cu 111.89(11) . . ? C23 P2 Cu 115.47(11) . . ? C31 N Cu 118.46(19) . . ? C31 N H0A 107.7 . . ? Cu N H0A 107.7 . . ? C31 N H0B 107.7 . . ? Cu N H0B 107.7 . . ? H0A N H0B 107.1 . . ? C1 B C7 103.7(2) . . ? C1 B C13 112.3(3) . . ? C7 B C13 107.7(2) . . ? C1 B C14 106.4(2) . . ? C7 B C14 110.7(2) . . ? C13 B C14 115.4(2) . . ? C6 C1 C2 113.6(3) . . ? C6 C1 B 122.8(3) . . ? C2 C1 B 123.6(3) . . ? C3 C2 C1 123.6(3) . . ? C3 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 123.9(3) . . ? C5 C6 H6 118.0 . . ? C1 C6 H6 118.0 . . ? C8 C7 C12 114.0(3) . . ? C8 C7 B 125.6(3) . . ? C12 C7 B 120.3(3) . . ? C7 C8 C9 123.4(3) . . ? C7 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 123.2(3) . . ? C11 C12 H12 118.4 . . ? C7 C12 H12 118.4 . . ? B C13 P2 128.6(2) . . ? B C13 H13A 105.1 . . ? P2 C13 H13A 105.1 . . ? B C13 H13B 105.1 . . ? P2 C13 H13B 105.1 . . ? H13A C13 H13B 105.9 . . ? B C14 P1 127.5(2) . . ? B C14 H14A 105.4 . . ? P1 C14 H14A 105.4 . . ? B C14 H14B 105.4 . . ? P1 C14 H14B 105.4 . . ? H14A C14 H14B 106.0 . . ? C16 C15 C17 109.8(3) . . ? C16 C15 C18 108.0(2) . . ? C17 C15 C18 108.2(3) . . ? C16 C15 P1 114.1(2) . . ? C17 C15 P1 111.2(2) . . ? C18 C15 P1 105.2(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C20 106.6(3) . . ? C22 C19 C21 108.5(3) . . ? C20 C19 C21 108.3(3) . . ? C22 C19 P1 111.5(2) . . ? C20 C19 P1 106.7(2) . . ? C21 C19 P1 114.8(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 108.1(3) . . ? C25 C23 C26 107.5(3) . . ? C24 C23 C26 109.0(3) . . ? C25 C23 P2 106.6(2) . . ? C24 C23 P2 114.3(2) . . ? C26 C23 P2 111.1(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.3(3) . . ? C29 C27 C30 109.6(3) . . ? C28 C27 C30 106.5(3) . . ? C29 C27 P2 115.8(2) . . ? C28 C27 P2 106.4(2) . . ? C30 C27 P2 109.8(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 121.4(3) . . ? C36 C31 N 118.1(3) . . ? C32 C31 N 120.5(3) . . ? C33 C32 C31 117.0(3) . . ? C33 C32 C37 119.7(3) . . ? C31 C32 C37 123.3(3) . . ? C34 C33 C32 123.4(3) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C34 C35 117.2(3) . . ? C33 C34 C38 120.6(3) . . ? C35 C34 C38 122.2(3) . . ? C34 C35 C36 122.4(3) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 118.5(3) . . ? C35 C36 C39 120.6(3) . . ? C31 C36 C39 120.9(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.766 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.766 _refine_diff_density_max 0.640 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.088 #===END data_npm35 _database_code_depnum_ccdc_archive 'CCDC 659793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu(thf) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58 B Cu O P2' _chemical_formula_weight 619.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.548(3) _cell_length_b 30.333(5) _cell_length_c 12.818(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6823(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3639 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.45 _reflns_number_total 2005 _reflns_number_gt 1847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(14) _refine_ls_number_reflns 2005 _refine_ls_number_parameters 185 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu -0.7500 0.2500 0.52277(3) 0.01681(17) Uani 1 2 d S . . P P -0.65215(5) 0.22848(2) 0.62258(6) 0.0157(2) Uani 1 1 d . . . O O -0.7500 0.2500 0.3642(3) 0.0326(10) Uani 1 2 d S . . B B -0.7500 0.2500 0.8228(4) 0.0219(15) Uani 1 2 d S . . C1 C -0.7509(2) 0.20668(10) 0.9029(2) 0.0219(9) Uani 1 1 d . . . C2 C -0.8167(2) 0.18246(10) 0.9280(2) 0.0222(8) Uani 1 1 d . . . H2 H -0.8639 0.1909 0.8978 0.027 Uiso 1 1 calc R . . C3 C -0.8150(3) 0.14647(11) 0.9958(3) 0.0310(10) Uani 1 1 d . . . H3 H -0.8611 0.1315 1.0116 0.037 Uiso 1 1 calc R . . C4 C -0.7485(3) 0.13239(12) 1.0400(3) 0.0367(12) Uani 1 1 d . . . H4 H -0.7478 0.1073 1.0843 0.044 Uiso 1 1 calc R . . C5 C -0.6820(3) 0.15552(14) 1.0189(3) 0.0427(11) Uani 1 1 d . . . H5 H -0.6352 0.1466 1.0495 0.051 Uiso 1 1 calc R . . C6 C -0.6843(3) 0.19210(12) 0.9521(3) 0.0324(10) Uani 1 1 d . . . H6 H -0.6384 0.2078 0.9397 0.039 Uiso 1 1 calc R . . C7 C -0.6692(3) 0.25079(9) 0.7541(2) 0.0184(8) Uani 1 1 d . . . H7A H -0.6307 0.2364 0.7993 0.022 Uiso 1 1 calc R . . H7B H -0.6544 0.2822 0.7501 0.022 Uiso 1 1 calc R . . C8 C -0.5537(2) 0.25029(9) 0.5917(2) 0.0191(8) Uani 1 1 d . . . C9 C -0.4982(3) 0.25031(12) 0.6848(3) 0.0312(10) Uani 1 1 d . . . H9A H -0.4497 0.2635 0.6635 0.047 Uiso 1 1 calc R . . H9B H -0.4895 0.2199 0.7080 0.047 Uiso 1 1 calc R . . H9C H -0.5202 0.2675 0.7422 0.047 Uiso 1 1 calc R . . C10 C -0.5652(2) 0.29839(10) 0.5583(3) 0.0291(9) Uani 1 1 d . . . H10A H -0.5161 0.3110 0.5370 0.044 Uiso 1 1 calc R . . H10B H -0.5858 0.3153 0.6170 0.044 Uiso 1 1 calc R . . H10C H -0.6009 0.2996 0.4996 0.044 Uiso 1 1 calc R . . C11 C -0.5157(2) 0.22585(11) 0.5005(3) 0.0313(9) Uani 1 1 d . . . H11A H -0.5015 0.1961 0.5229 0.047 Uiso 1 1 calc R . . H11B H -0.4699 0.2419 0.4787 0.047 Uiso 1 1 calc R . . H11C H -0.5514 0.2240 0.4419 0.047 Uiso 1 1 calc R . . C12 C -0.6508(2) 0.16638(8) 0.6276(3) 0.0225(8) Uani 1 1 d . . . C13 C -0.5882(2) 0.14768(10) 0.6980(3) 0.0352(10) Uani 1 1 d . . . H13A H -0.5896 0.1154 0.6955 0.053 Uiso 1 1 calc R . . H13B H -0.5965 0.1576 0.7698 0.053 Uiso 1 1 calc R . . H13C H -0.5384 0.1581 0.6736 0.053 Uiso 1 1 calc R . . C14 C -0.7287(2) 0.15252(9) 0.6687(3) 0.0235(8) Uani 1 1 d . . . H14A H -0.7334 0.1612 0.7420 0.035 Uiso 1 1 calc R . . H14B H -0.7341 0.1205 0.6628 0.035 Uiso 1 1 calc R . . H14C H -0.7687 0.1670 0.6277 0.035 Uiso 1 1 calc R . . C15 C -0.6432(2) 0.14731(10) 0.5165(3) 0.0335(10) Uani 1 1 d . . . H15A H -0.6511 0.1153 0.5186 0.050 Uiso 1 1 calc R . . H15B H -0.5922 0.1537 0.4893 0.050 Uiso 1 1 calc R . . H15C H -0.6815 0.1608 0.4710 0.050 Uiso 1 1 calc R . . C16 C -0.8173(4) 0.25033(17) 0.2983(3) 0.0483(15) Uani 1 1 d . . . H16A H -0.8419 0.2797 0.2985 0.058 Uiso 1 1 calc R . . H16B H -0.8548 0.2280 0.3218 0.058 Uiso 1 1 calc R . . C17 C -0.7869(3) 0.2392(3) 0.1913(4) 0.084(2) Uani 1 1 d . . . H17A H -0.7817 0.2069 0.1820 0.185 Uiso 1 1 calc R . . H17B H -0.8203 0.2511 0.1357 0.185 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0165(4) 0.0210(2) 0.0130(2) 0.000 0.000 0.0034(2) P 0.0155(6) 0.0173(3) 0.0144(3) 0.0016(3) -0.0005(4) 0.0021(3) O 0.016(3) 0.067(3) 0.0149(16) 0.000 0.000 0.0084(17) B 0.025(5) 0.025(2) 0.016(2) 0.000 0.000 -0.003(2) C1 0.026(3) 0.0264(13) 0.0134(13) 0.0026(12) -0.0001(13) -0.0049(14) C2 0.015(3) 0.0340(14) 0.0182(14) 0.0023(13) -0.0004(15) -0.0023(13) C3 0.034(3) 0.0335(16) 0.0257(17) 0.0061(14) 0.0038(18) -0.0102(16) C4 0.041(4) 0.0385(16) 0.031(2) 0.0181(15) 0.005(2) -0.0021(18) C5 0.030(3) 0.062(2) 0.0358(19) 0.029(2) -0.003(2) 0.0050(19) C6 0.024(3) 0.0468(19) 0.0267(16) 0.0151(16) -0.0018(18) -0.0072(16) C7 0.022(3) 0.0212(13) 0.0123(14) 0.0013(11) -0.0043(15) -0.0017(11) C8 0.014(3) 0.0236(13) 0.0199(14) 0.0043(11) -0.0007(15) 0.0025(13) C9 0.025(3) 0.0348(16) 0.034(2) 0.0069(15) -0.0066(18) -0.0062(15) C10 0.023(3) 0.0269(14) 0.0371(18) 0.0086(14) 0.0058(18) 0.0023(14) C11 0.028(3) 0.0333(16) 0.0329(18) -0.0012(15) 0.0074(18) 0.0025(15) C12 0.025(3) 0.0155(11) 0.0266(14) 0.0012(12) -0.0001(17) 0.0004(12) C13 0.029(3) 0.0217(13) 0.055(2) 0.0125(16) -0.010(2) 0.0012(14) C14 0.023(3) 0.0195(12) 0.0279(15) -0.0004(13) -0.0005(17) -0.0013(12) C15 0.037(3) 0.0256(14) 0.0380(18) -0.0084(15) 0.011(2) 0.0001(14) C16 0.029(5) 0.089(4) 0.027(2) 0.001(2) 0.000(2) 0.002(2) C17 0.028(6) 0.201(7) 0.024(2) -0.027(3) 0.001(2) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O 2.032(4) . ? Cu P 2.2386(9) 14_355 ? Cu P 2.2386(9) . ? P C7 1.841(3) . ? P C12 1.885(3) . ? P C8 1.891(4) . ? O C16 1.453(6) . ? O C16 1.453(6) 14_355 ? B C1 1.668(4) 14_355 ? B C1 1.668(4) . ? B C7 1.669(5) 14_355 ? B C7 1.669(5) . ? C1 C6 1.399(5) . ? C1 C2 1.406(5) . ? C2 C3 1.396(4) . ? C2 H2 0.9500 . ? C3 C4 1.365(6) . ? C3 H3 0.9500 . ? C4 C5 1.389(6) . ? C4 H4 0.9500 . ? C5 C6 1.402(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.534(4) . ? C8 C11 1.537(5) . ? C8 C9 1.540(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.524(5) . ? C12 C13 1.531(5) . ? C12 C15 1.543(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.510(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C17 1.452(13) 14_355 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Cu P 124.86(2) . 14_355 ? O Cu P 124.86(2) . . ? P Cu P 110.29(5) 14_355 . ? C7 P C12 109.76(14) . . ? C7 P C8 102.18(16) . . ? C12 P C8 110.21(16) . . ? C7 P Cu 106.96(14) . . ? C12 P Cu 108.68(13) . . ? C8 P Cu 118.62(10) . . ? C16 O C16 108.8(5) . 14_355 ? C16 O Cu 125.6(2) . . ? C16 O Cu 125.6(2) 14_355 . ? C1 B C1 104.0(4) 14_355 . ? C1 B C7 110.11(16) 14_355 14_355 ? C1 B C7 107.78(15) . 14_355 ? C1 B C7 107.78(15) 14_355 . ? C1 B C7 110.11(16) . . ? C7 B C7 116.4(4) 14_355 . ? C6 C1 C2 114.7(3) . . ? C6 C1 B 121.3(3) . . ? C2 C1 B 124.1(3) . . ? C3 C2 C1 122.3(4) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 123.4(4) . . ? C1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? B C7 P 128.0(3) . . ? B C7 H7A 105.3 . . ? P C7 H7A 105.3 . . ? B C7 H7B 105.3 . . ? P C7 H7B 105.3 . . ? H7A C7 H7B 106.0 . . ? C10 C8 C11 107.7(3) . . ? C10 C8 C9 107.4(3) . . ? C11 C8 C9 108.3(3) . . ? C10 C8 P 105.8(3) . . ? C11 C8 P 112.8(2) . . ? C9 C8 P 114.6(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109.7(3) . . ? C14 C12 C15 107.1(3) . . ? C13 C12 C15 110.1(3) . . ? C14 C12 P 106.0(2) . . ? C13 C12 P 113.5(2) . . ? C15 C12 P 110.1(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O C16 C17 103.9(5) . . ? O C16 H16A 111.0 . . ? C17 C16 H16A 111.0 . . ? O C16 H16B 111.0 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C17 C17 C16 102.4(5) 14_355 . ? C17 C17 H17A 111.3 14_355 . ? C16 C17 H17A 111.3 . . ? C17 C17 H17B 111.3 14_355 . ? C16 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? _diffrn_measured_fraction_theta_max 0.707 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.707 _refine_diff_density_max 0.511 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.061 #===END data_npm37 _database_code_depnum_ccdc_archive 'CCDC 659794' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu(N2CTMS2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H68 B Cu N2 P2 Si2' _chemical_formula_weight 733.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 21.4508(13) _cell_length_b 21.4508(13) _cell_length_c 47.633(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 18981(2) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .41 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5535 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37738 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.33 _reflns_number_total 3067 _reflns_number_gt 2346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+152.8350P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3067 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.07422(3) 0.3333 0.5833 0.0300(2) Uani 1 2 d S . . P P 0.08990(5) 0.23785(5) 0.57816(2) 0.0250(3) Uani 1 1 d . . . N1 N -0.0153(4) 0.3333 0.5833 0.0751(19) Uani 1 2 d S . . N2 N -0.0712(3) 0.3333 0.5833 0.0613(17) Uani 1 2 d S A . Si Si -0.1440(2) 0.3580(2) 0.61697(8) 0.0631(11) Uani 0.50 1 d P A 1 SiA Si -0.1295(2) 0.4031(3) 0.60844(9) 0.0805(12) Uani 0.50 1 d P A 2 B B 0.2584(3) 0.3333 0.5833 0.0267(13) Uani 1 2 d S . . C1 C 0.2927(2) 0.3033(2) 0.60733(8) 0.0335(9) Uani 1 1 d . . . C2 C 0.3328(3) 0.3439(2) 0.63034(9) 0.0481(12) Uani 1 1 d . . . H2 H 0.3375 0.3899 0.6333 0.058 Uiso 1 1 calc R . . C3 C 0.3662(3) 0.3205(3) 0.64917(12) 0.0771(19) Uani 1 1 d . . . H3 H 0.3912 0.3494 0.6649 0.093 Uiso 1 1 calc R . . C4 C 0.3630(4) 0.2556(3) 0.64506(13) 0.088(2) Uani 1 1 d . . . H4 H 0.3864 0.2396 0.6576 0.105 Uiso 1 1 calc R . . C5 C 0.3250(3) 0.2140(3) 0.62225(12) 0.0709(18) Uani 1 1 d . . . H5 H 0.3222 0.1690 0.6191 0.085 Uiso 1 1 calc R . . C6 C 0.2912(3) 0.2376(2) 0.60409(10) 0.0498(12) Uani 1 1 d . . . H6 H 0.2657 0.2079 0.5886 0.060 Uiso 1 1 calc R . . C7 C 0.18319(19) 0.26616(19) 0.56890(7) 0.0255(8) Uani 1 1 d . . . H7A H 0.1875 0.2225 0.5709 0.031 Uiso 1 1 calc R . . H7B H 0.1872 0.2769 0.5485 0.031 Uiso 1 1 calc R . . C8 C 0.0671(2) 0.1854(2) 0.61195(8) 0.0311(9) Uani 1 1 d . . . C9 C 0.1206(2) 0.2380(2) 0.63353(8) 0.0384(10) Uani 1 1 d . . . H9A H 0.1098 0.2152 0.6521 0.058 Uiso 1 1 calc R . . H9B H 0.1167 0.2816 0.6342 0.058 Uiso 1 1 calc R . . H9C H 0.1697 0.2509 0.6281 0.058 Uiso 1 1 calc R . . C10 C 0.0740(2) 0.1180(2) 0.61070(9) 0.0421(11) Uani 1 1 d . . . H10A H 0.1217 0.1307 0.6035 0.063 Uiso 1 1 calc R . . H10B H 0.0369 0.0825 0.5983 0.063 Uiso 1 1 calc R . . H10C H 0.0680 0.0976 0.6296 0.063 Uiso 1 1 calc R . . C11 C -0.0084(2) 0.1656(2) 0.62225(9) 0.0406(11) Uani 1 1 d . . . H11A H -0.0447 0.1281 0.6101 0.061 Uiso 1 1 calc R . . H11B H -0.0138 0.2083 0.6216 0.061 Uiso 1 1 calc R . . H11C H -0.0149 0.1478 0.6416 0.061 Uiso 1 1 calc R . . C12 C 0.0364(2) 0.1779(2) 0.54767(8) 0.0298(9) Uani 1 1 d . . . C13 C 0.0603(2) 0.1248(2) 0.53804(8) 0.0348(9) Uani 1 1 d . . . H13A H 0.0520 0.0906 0.5532 0.052 Uiso 1 1 calc R . . H13B H 0.1116 0.1514 0.5333 0.052 Uiso 1 1 calc R . . H13C H 0.0325 0.0986 0.5215 0.052 Uiso 1 1 calc R . . C14 C -0.0444(2) 0.1359(2) 0.55460(9) 0.0419(11) Uani 1 1 d . . . H14A H -0.0720 0.1147 0.5374 0.063 Uiso 1 1 calc R . . H14B H -0.0588 0.1687 0.5628 0.063 Uiso 1 1 calc R . . H14C H -0.0540 0.0976 0.5681 0.063 Uiso 1 1 calc R . . C15 C 0.0472(2) 0.2294(2) 0.52332(8) 0.0402(10) Uani 1 1 d . . . H15A H 0.0982 0.2557 0.5180 0.060 Uiso 1 1 calc R . . H15B H 0.0322 0.2636 0.5292 0.060 Uiso 1 1 calc R . . H15C H 0.0183 0.2017 0.5072 0.060 Uiso 1 1 calc R . . C16 C -0.1288(4) 0.3333 0.5833 0.095(4) Uani 1 2 d S . . C25 C -0.0721(10) 0.4524(10) 0.6168(4) 0.146(10) Uani 0.50 1 d P A 1 H25A H -0.0277 0.4560 0.6240 0.219 Uiso 0.50 1 calc PR A 1 H25B H -0.0860 0.4807 0.6287 0.219 Uiso 0.50 1 calc PR A 1 H25C H -0.0642 0.4711 0.5976 0.219 Uiso 0.50 1 calc PR A 1 C26 C -0.2307(11) 0.3336(9) 0.6261(5) 0.163(11) Uani 0.50 1 d P A 1 H26A H -0.2558 0.2835 0.6325 0.244 Uiso 0.50 1 calc PR A 1 H26B H -0.2557 0.3384 0.6098 0.244 Uiso 0.50 1 calc PR A 1 H26C H -0.2299 0.3649 0.6412 0.244 Uiso 0.50 1 calc PR A 1 C27 C -0.1216(14) 0.3131(8) 0.6439(3) 0.165(10) Uani 0.50 1 d P A 1 H27A H -0.1333 0.2652 0.6373 0.247 Uiso 0.50 1 calc PR A 1 H27B H -0.1492 0.3085 0.6610 0.247 Uiso 0.50 1 calc PR A 1 H27C H -0.0700 0.3414 0.6481 0.247 Uiso 0.50 1 calc PR A 1 C28 C -0.1573(12) 0.4615(13) 0.5921(4) 0.182(11) Uani 0.50 1 d P A 2 H28A H -0.1796 0.4415 0.5739 0.273 Uiso 0.50 1 d PR A 2 H28B H -0.1160 0.5100 0.5895 0.273 Uiso 0.50 1 d PR A 2 H28C H -0.1926 0.4641 0.6045 0.273 Uiso 0.50 1 d PR A 2 C29 C -0.0403(5) 0.4495(10) 0.6273(3) 0.074(5) Uani 0.50 1 d P A 2 H29A H -0.0019 0.4784 0.6139 0.111 Uiso 0.50 1 calc PR A 2 H29B H -0.0311 0.4133 0.6359 0.111 Uiso 0.50 1 calc PR A 2 H29C H -0.0416 0.4809 0.6420 0.111 Uiso 0.50 1 calc PR A 2 C30 C -0.1942(9) 0.339(2) 0.6293(8) 0.40(4) Uani 0.50 1 d P A 2 H30A H -0.1891 0.3582 0.6484 0.607 Uiso 0.50 1 calc PR A 2 H30B H -0.1891 0.2964 0.6296 0.607 Uiso 0.50 1 calc PR A 2 H30C H -0.2418 0.3265 0.6220 0.607 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0288(3) 0.0247(4) 0.0351(4) -0.0030(3) -0.00150(15) 0.01234(19) P 0.0267(5) 0.0208(5) 0.0240(5) -0.0033(4) -0.0013(4) 0.0093(4) N1 0.080(4) 0.079(5) 0.065(4) 0.000(4) 0.0000(18) 0.040(2) N2 0.058(3) 0.110(6) 0.033(3) -0.002(3) -0.0011(16) 0.055(3) Si 0.068(2) 0.064(2) 0.045(2) -0.0086(17) 0.0091(16) 0.024(2) SiA 0.068(3) 0.128(4) 0.063(3) -0.028(3) -0.011(2) 0.063(3) B 0.031(3) 0.018(3) 0.027(3) -0.006(3) -0.0030(13) 0.0092(15) C1 0.031(2) 0.024(2) 0.043(2) -0.0070(18) -0.0095(19) 0.0119(18) C2 0.063(3) 0.033(2) 0.053(3) -0.016(2) -0.028(2) 0.028(2) C3 0.107(5) 0.051(3) 0.084(4) -0.030(3) -0.068(4) 0.048(3) C4 0.119(5) 0.051(3) 0.106(5) -0.028(3) -0.081(4) 0.053(4) C5 0.090(4) 0.036(3) 0.095(4) -0.019(3) -0.051(4) 0.038(3) C6 0.056(3) 0.036(3) 0.060(3) -0.014(2) -0.028(2) 0.024(2) C7 0.033(2) 0.023(2) 0.0208(19) -0.0011(15) 0.0026(16) 0.0149(17) C8 0.037(2) 0.023(2) 0.027(2) 0.0013(16) 0.0047(17) 0.0109(18) C9 0.049(3) 0.034(2) 0.026(2) 0.0045(17) 0.0036(19) 0.015(2) C10 0.059(3) 0.033(2) 0.034(2) 0.0061(19) 0.007(2) 0.024(2) C11 0.042(3) 0.032(2) 0.039(2) -0.0009(19) 0.014(2) 0.012(2) C12 0.026(2) 0.027(2) 0.032(2) -0.0085(17) -0.0075(17) 0.0099(18) C13 0.035(2) 0.032(2) 0.033(2) -0.0107(18) -0.0072(18) 0.0133(19) C14 0.036(2) 0.036(2) 0.046(3) -0.013(2) -0.010(2) 0.013(2) C15 0.047(3) 0.036(2) 0.032(2) -0.0048(19) -0.014(2) 0.017(2) C16 0.079(4) 0.204(11) 0.042(4) -0.059(6) -0.030(3) 0.102(6) C25 0.096(15) 0.098(14) 0.111(15) -0.045(12) 0.001(11) -0.052(13) C26 0.15(2) 0.082(11) 0.22(2) 0.000(13) 0.150(19) 0.029(12) C27 0.35(3) 0.085(11) 0.059(9) 0.003(8) 0.004(14) 0.113(17) C28 0.22(2) 0.33(3) 0.135(15) -0.112(19) -0.089(16) 0.24(2) C29 0.015(6) 0.137(13) 0.044(7) -0.039(7) -0.011(5) 0.017(7) C30 0.033(10) 0.49(6) 0.46(5) -0.41(5) 0.093(18) -0.044(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 1.921(8) . ? Cu P 2.2490(10) . ? Cu P 2.2490(11) 17 ? P C7 1.831(4) . ? P C8 1.883(4) . ? P C12 1.899(4) . ? N1 N2 1.199(8) . ? N2 C16 1.236(9) . ? Si C26 1.715(19) . ? Si C16 1.768(4) . ? Si C27 1.809(16) . ? Si C25 1.832(16) . ? SiA C30 1.70(4) . ? SiA C28 1.811(18) . ? SiA C29 1.886(10) . ? SiA C16 1.921(5) . ? B C1 1.654(6) . ? B C1 1.654(6) 17 ? B C7 1.682(5) 17 ? B C7 1.682(5) . ? C1 C2 1.397(6) . ? C1 C6 1.403(6) . ? C2 C3 1.389(6) . ? C2 H2 0.9500 . ? C3 C4 1.374(7) . ? C3 H3 0.9500 . ? C4 C5 1.383(7) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.527(5) . ? C8 C9 1.534(5) . ? C8 C11 1.535(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.533(5) . ? C12 C14 1.537(5) . ? C12 C15 1.537(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si 1.768(4) 17 ? C16 SiA 1.921(5) 17 ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C28 1.96(3) 16_455 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P 127.22(3) . . ? N1 Cu P 127.23(3) . 17 ? P Cu P 105.55(6) . 17 ? C7 P C8 108.57(17) . . ? C7 P C12 103.34(17) . . ? C8 P C12 111.14(17) . . ? C7 P Cu 111.15(12) . . ? C8 P Cu 109.74(12) . . ? C12 P Cu 112.69(12) . . ? N2 N1 Cu 180.000(2) . . ? N1 N2 C16 180.000(7) . . ? C26 Si C16 118.2(9) . . ? C26 Si C27 101.1(12) . . ? C16 Si C27 110.2(6) . . ? C26 Si C25 121.6(10) . . ? C16 Si C25 98.5(6) . . ? C27 Si C25 106.9(11) . . ? C30 SiA C28 112.9(16) . . ? C30 SiA C29 110.5(15) . . ? C28 SiA C29 116.0(10) . . ? C30 SiA C16 93.3(9) . . ? C28 SiA C16 114.0(6) . . ? C29 SiA C16 107.9(5) . . ? C1 B C1 100.6(4) . 17 ? C1 B C7 107.89(18) . 17 ? C1 B C7 111.82(18) 17 17 ? C1 B C7 111.82(18) . . ? C1 B C7 107.88(18) 17 . ? C7 B C7 115.8(4) 17 . ? C2 C1 C6 114.2(4) . . ? C2 C1 B 123.7(3) . . ? C6 C1 B 121.6(3) . . ? C3 C2 C1 123.3(4) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.3(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 123.3(4) . . ? C5 C6 H6 118.4 . . ? C1 C6 H6 118.4 . . ? B C7 P 127.4(3) . . ? B C7 H7A 105.5 . . ? P C7 H7A 105.5 . . ? B C7 H7B 105.5 . . ? P C7 H7B 105.5 . . ? H7A C7 H7B 106.0 . . ? C10 C8 C9 109.3(3) . . ? C10 C8 C11 109.8(3) . . ? C9 C8 C11 106.7(3) . . ? C10 C8 P 114.4(3) . . ? C9 C8 P 105.0(2) . . ? C11 C8 P 111.2(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 109.1(3) . . ? C13 C12 C15 108.7(3) . . ? C14 C12 C15 107.7(3) . . ? C13 C12 P 114.7(3) . . ? C14 C12 P 110.8(3) . . ? C15 C12 P 105.5(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 Si 109.5(3) . . ? N2 C16 Si 109.5(3) . 17 ? Si C16 Si 140.9(5) . 17 ? N2 C16 SiA 113.4(2) . . ? Si C16 SiA 29.35(16) . . ? Si C16 SiA 127.3(4) 17 . ? N2 C16 SiA 113.4(2) . 17 ? Si C16 SiA 127.3(4) . 17 ? Si C16 SiA 29.34(16) 17 17 ? SiA C16 SiA 133.2(5) . 17 ? SiA C28 C28 169.5(8) . 16_455 ? SiA C28 H28A 109.5 . . ? C28 C28 H28A 65.3 16_455 . ? SiA C28 H28B 110.7 . . ? C28 C28 H28B 79.8 16_455 . ? H28A C28 H28B 109.5 . . ? SiA C28 H28C 108.3 . . ? C28 C28 H28C 66.9 16_455 . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? SiA C29 H29A 109.5 . . ? SiA C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? SiA C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? SiA C30 H30A 109.5 . . ? SiA C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? SiA C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.573 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.067 #===END data_npm33 _database_code_depnum_ccdc_archive 'CCDC 659795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu(N2CMes2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H72 B Cu N2 P2' _chemical_formula_weight 825.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6975(16) _cell_length_b 17.955(2) _cell_length_c 23.035(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.707(4) _cell_angle_gamma 90.00 _cell_volume 4836.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blade _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22763 _diffrn_reflns_av_R_equivalents 0.1309 _diffrn_reflns_av_sigmaI/netI 0.1665 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.16 _reflns_number_total 6798 _reflns_number_gt 3549 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following restraints were used to approximate isotropic behavior of an anisotropically-refined tertiary carbon in a tert-butyl group; without the restraints a non-positive definite displacement parameter was inevitably obtained: isor c15 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6798 _refine_ls_number_parameters 514 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.69197(6) 0.24482(4) 0.15516(3) 0.0165(2) Uani 1 1 d . . . P1 P 0.62204(13) 0.33787(9) 0.09899(6) 0.0167(4) Uani 1 1 d . . . P2 P 0.59821(13) 0.14058(8) 0.12822(6) 0.0151(4) Uani 1 1 d . . . N1 N 0.8145(4) 0.2629(3) 0.2064(2) 0.0257(13) Uani 1 1 d . . . N2 N 0.8606(4) 0.2829(3) 0.2490(2) 0.0235(12) Uani 1 1 d . . . B B 0.4513(6) 0.2296(4) 0.0349(3) 0.0158(16) Uani 1 1 d . . . C1 C 0.4620(5) 0.2361(3) -0.0370(2) 0.0168(14) Uani 1 1 d . . . C2 C 0.4192(5) 0.2981(3) -0.0675(2) 0.0237(15) Uani 1 1 d . . . H2 H 0.3910 0.3386 -0.0456 0.028 Uiso 1 1 calc R . . C3 C 0.4151(5) 0.3043(3) -0.1276(2) 0.0259(16) Uani 1 1 d . . . H3 H 0.3841 0.3476 -0.1457 0.031 Uiso 1 1 calc R . . C4 C 0.4568(5) 0.2466(4) -0.1610(2) 0.0275(15) Uani 1 1 d . . . H4 H 0.4550 0.2500 -0.2022 0.033 Uiso 1 1 calc R . . C5 C 0.5007(5) 0.1848(4) -0.1336(2) 0.0267(16) Uani 1 1 d . . . H5 H 0.5295 0.1447 -0.1557 0.032 Uiso 1 1 calc R . . C6 C 0.5030(5) 0.1809(4) -0.0724(2) 0.0248(15) Uani 1 1 d . . . H6 H 0.5347 0.1376 -0.0545 0.030 Uiso 1 1 calc R . . C7 C 0.3145(5) 0.2157(3) 0.0410(2) 0.0205(15) Uani 1 1 d . . . C8 C 0.2632(5) 0.1484(3) 0.0209(2) 0.0228(15) Uani 1 1 d . . . H8 H 0.3120 0.1105 0.0070 0.027 Uiso 1 1 calc R . . C9 C 0.1467(6) 0.1344(4) 0.0201(2) 0.0327(17) Uani 1 1 d . . . H9 H 0.1175 0.0881 0.0063 0.039 Uiso 1 1 calc R . . C10 C 0.0731(5) 0.1889(4) 0.0399(3) 0.0356(18) Uani 1 1 d . . . H10 H -0.0072 0.1808 0.0390 0.043 Uiso 1 1 calc R . . C11 C 0.1182(5) 0.2550(4) 0.0608(2) 0.0342(17) Uani 1 1 d . . . H11 H 0.0688 0.2920 0.0754 0.041 Uiso 1 1 calc R . . C12 C 0.2344(5) 0.2676(3) 0.0606(2) 0.0238(16) Uani 1 1 d . . . H12 H 0.2619 0.3142 0.0746 0.029 Uiso 1 1 calc R . . C13 C 0.4829(5) 0.3093(3) 0.0682(2) 0.0189(14) Uani 1 1 d . . . H13A H 0.4292 0.3130 0.1005 0.023 Uiso 1 1 calc R . . H13B H 0.4602 0.3490 0.0403 0.023 Uiso 1 1 calc R . . C14 C 0.5322(4) 0.1563(3) 0.0566(2) 0.0135(13) Uani 1 1 d . . . H14A H 0.5956 0.1540 0.0291 0.016 Uiso 1 1 calc R . . H14B H 0.4844 0.1118 0.0485 0.016 Uiso 1 1 calc R . . C15 C 0.7188(4) 0.3629(3) 0.0385(2) 0.0149(14) Uani 1 1 d U . . C16 C 0.6751(5) 0.4274(3) 0.0009(2) 0.0311(16) Uani 1 1 d . . . H16A H 0.7269 0.4352 -0.0312 0.047 Uiso 1 1 calc R . . H16B H 0.6719 0.4727 0.0244 0.047 Uiso 1 1 calc R . . H16C H 0.5984 0.4156 -0.0148 0.047 Uiso 1 1 calc R . . C17 C 0.7297(5) 0.2931(3) 0.0013(2) 0.0225(15) Uani 1 1 d . . . H17A H 0.7826 0.3028 -0.0300 0.034 Uiso 1 1 calc R . . H17B H 0.6544 0.2797 -0.0154 0.034 Uiso 1 1 calc R . . H17C H 0.7590 0.2520 0.0255 0.034 Uiso 1 1 calc R . . C18 C 0.8393(5) 0.3809(3) 0.0622(2) 0.0241(15) Uani 1 1 d . . . H18A H 0.8696 0.3380 0.0841 0.036 Uiso 1 1 calc R . . H18B H 0.8362 0.4243 0.0879 0.036 Uiso 1 1 calc R . . H18C H 0.8892 0.3917 0.0298 0.036 Uiso 1 1 calc R . . C19 C 0.5850(5) 0.4217(3) 0.1456(2) 0.0200(14) Uani 1 1 d . . . C20 C 0.5008(5) 0.4755(3) 0.1157(2) 0.0302(17) Uani 1 1 d . . . H20A H 0.4856 0.5172 0.1418 0.045 Uiso 1 1 calc R . . H20B H 0.4291 0.4493 0.1062 0.045 Uiso 1 1 calc R . . H20C H 0.5337 0.4944 0.0800 0.045 Uiso 1 1 calc R . . C21 C 0.5312(6) 0.3900(3) 0.2004(2) 0.0303(17) Uani 1 1 d . . . H21A H 0.5868 0.3581 0.2210 0.045 Uiso 1 1 calc R . . H21B H 0.4633 0.3607 0.1893 0.045 Uiso 1 1 calc R . . H21C H 0.5091 0.4311 0.2258 0.045 Uiso 1 1 calc R . . C22 C 0.6914(5) 0.4644(3) 0.1648(3) 0.0310(17) Uani 1 1 d . . . H22A H 0.7230 0.4900 0.1313 0.047 Uiso 1 1 calc R . . H22B H 0.7484 0.4297 0.1811 0.047 Uiso 1 1 calc R . . H22C H 0.6717 0.5012 0.1943 0.047 Uiso 1 1 calc R . . C23 C 0.7046(5) 0.0636(3) 0.1157(2) 0.0190(14) Uani 1 1 d . . . C24 C 0.6606(6) 0.0005(4) 0.0773(3) 0.0363(18) Uani 1 1 d . . . H24A H 0.7228 -0.0348 0.0707 0.054 Uiso 1 1 calc R . . H24B H 0.6325 0.0207 0.0400 0.054 Uiso 1 1 calc R . . H24C H 0.5981 -0.0251 0.0965 0.054 Uiso 1 1 calc R . . C25 C 0.8053(5) 0.1011(4) 0.0852(3) 0.0322(17) Uani 1 1 d . . . H25A H 0.8658 0.0643 0.0792 0.048 Uiso 1 1 calc R . . H25B H 0.8356 0.1418 0.1094 0.048 Uiso 1 1 calc R . . H25C H 0.7786 0.1210 0.0475 0.048 Uiso 1 1 calc R . . C26 C 0.7522(5) 0.0313(4) 0.1729(2) 0.0288(16) Uani 1 1 d . . . H26A H 0.6942 -0.0004 0.1903 0.043 Uiso 1 1 calc R . . H26B H 0.7723 0.0720 0.1997 0.043 Uiso 1 1 calc R . . H26C H 0.8205 0.0016 0.1655 0.043 Uiso 1 1 calc R . . C27 C 0.4838(5) 0.1110(3) 0.1788(2) 0.0209(15) Uani 1 1 d . . . C28 C 0.4244(6) 0.0370(4) 0.1598(3) 0.0397(19) Uani 1 1 d . . . H28A H 0.3593 0.0274 0.1845 0.060 Uiso 1 1 calc R . . H28B H 0.4791 -0.0042 0.1635 0.060 Uiso 1 1 calc R . . H28C H 0.3973 0.0411 0.1192 0.060 Uiso 1 1 calc R . . C29 C 0.3972(5) 0.1738(4) 0.1797(2) 0.0293(17) Uani 1 1 d . . . H29A H 0.3419 0.1642 0.2099 0.044 Uiso 1 1 calc R . . H29B H 0.3570 0.1769 0.1418 0.044 Uiso 1 1 calc R . . H29C H 0.4367 0.2210 0.1878 0.044 Uiso 1 1 calc R . . C30 C 0.5332(5) 0.1004(3) 0.2412(2) 0.0231(15) Uani 1 1 d . . . H30A H 0.5757 0.1451 0.2531 0.035 Uiso 1 1 calc R . . H30B H 0.5847 0.0573 0.2423 0.035 Uiso 1 1 calc R . . H30C H 0.4705 0.0920 0.2677 0.035 Uiso 1 1 calc R . . C31 C 0.9160(5) 0.3089(3) 0.2956(2) 0.0210(15) Uani 1 1 d . . . C32 C 0.9254(5) 0.3917(3) 0.2959(2) 0.0221(15) Uani 1 1 d . . . C33 C 0.9736(5) 0.4300(4) 0.2486(2) 0.0246(15) Uani 1 1 d . . . C34 C 0.9739(5) 0.5069(4) 0.2486(3) 0.0269(16) Uani 1 1 d . . . H34 H 1.0041 0.5323 0.2163 0.032 Uiso 1 1 calc R . . C35 C 0.9318(5) 0.5487(3) 0.2942(3) 0.0280(16) Uani 1 1 d . . . C36 C 0.8878(5) 0.5110(4) 0.3410(3) 0.0270(16) Uani 1 1 d . . . H36 H 0.8600 0.5389 0.3727 0.032 Uiso 1 1 calc R . . C37 C 0.8829(5) 0.4329(3) 0.3431(2) 0.0209(15) Uani 1 1 d . . . C38 C 1.0277(5) 0.3876(4) 0.1992(2) 0.0316(17) Uani 1 1 d . . . H38A H 0.9675 0.3660 0.1740 0.047 Uiso 1 1 calc R . . H38B H 1.0764 0.3477 0.2152 0.047 Uiso 1 1 calc R . . H38C H 1.0742 0.4218 0.1766 0.047 Uiso 1 1 calc R . . C39 C 0.9332(6) 0.6323(3) 0.2929(3) 0.0426(19) Uani 1 1 d . . . H39A H 0.8854 0.6516 0.3237 0.064 Uiso 1 1 calc R . . H39B H 0.9034 0.6498 0.2551 0.064 Uiso 1 1 calc R . . H39C H 1.0119 0.6500 0.2991 0.064 Uiso 1 1 calc R . . C40 C 0.8322(6) 0.3956(4) 0.3947(3) 0.0364(18) Uani 1 1 d . . . H40A H 0.8927 0.3700 0.4173 0.055 Uiso 1 1 calc R . . H40B H 0.7745 0.3594 0.3815 0.055 Uiso 1 1 calc R . . H40C H 0.7964 0.4332 0.4191 0.055 Uiso 1 1 calc R . . C41 C 0.9591(5) 0.2542(4) 0.3386(2) 0.0209(14) Uani 1 1 d . . . C42 C 0.8938(5) 0.1910(3) 0.3521(2) 0.0238(15) Uani 1 1 d . . . C43 C 0.9402(5) 0.1371(3) 0.3899(2) 0.0256(16) Uani 1 1 d . . . H43 H 0.8970 0.0937 0.3978 0.031 Uiso 1 1 calc R . . C44 C 1.0491(5) 0.1455(3) 0.4163(2) 0.0253(15) Uani 1 1 d . . . C45 C 1.1091(5) 0.2101(3) 0.4047(2) 0.0238(15) Uani 1 1 d . . . H45 H 1.1811 0.2176 0.4240 0.029 Uiso 1 1 calc R . . C46 C 1.0686(5) 0.2647(3) 0.3658(2) 0.0238(15) Uani 1 1 d . . . C47 C 0.7729(5) 0.1798(4) 0.3292(2) 0.0342(17) Uani 1 1 d . . . H47A H 0.7741 0.1615 0.2892 0.051 Uiso 1 1 calc R . . H47B H 0.7316 0.2273 0.3302 0.051 Uiso 1 1 calc R . . H47C H 0.7343 0.1433 0.3535 0.051 Uiso 1 1 calc R . . C48 C 1.0987(5) 0.0881(3) 0.4569(3) 0.0328(17) Uani 1 1 d . . . H48A H 1.1729 0.0717 0.4430 0.049 Uiso 1 1 calc R . . H48B H 1.0468 0.0454 0.4586 0.049 Uiso 1 1 calc R . . H48C H 1.1091 0.1097 0.4958 0.049 Uiso 1 1 calc R . . C49 C 1.1426(5) 0.3308(3) 0.3544(3) 0.0304(16) Uani 1 1 d . . . H49A H 1.1104 0.3749 0.3728 0.046 Uiso 1 1 calc R . . H49B H 1.1459 0.3389 0.3124 0.046 Uiso 1 1 calc R . . H49C H 1.2199 0.3217 0.3704 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0140(4) 0.0181(4) 0.0171(3) -0.0004(3) -0.0028(3) -0.0014(4) P1 0.0168(9) 0.0153(9) 0.0179(8) -0.0008(7) -0.0023(6) 0.0001(7) P2 0.0129(9) 0.0157(9) 0.0168(8) 0.0006(7) -0.0014(6) 0.0001(7) N1 0.033(3) 0.016(3) 0.027(3) -0.002(3) -0.014(2) 0.003(3) N2 0.016(3) 0.022(3) 0.033(3) 0.003(3) 0.003(3) 0.003(2) B 0.018(4) 0.016(4) 0.013(3) 0.006(3) -0.001(3) -0.007(3) C1 0.018(3) 0.011(4) 0.021(3) 0.001(3) -0.001(3) -0.006(3) C2 0.018(4) 0.031(4) 0.022(4) -0.003(3) -0.001(3) -0.001(3) C3 0.028(4) 0.026(4) 0.023(4) 0.002(3) -0.004(3) -0.002(3) C4 0.037(4) 0.027(4) 0.018(3) 0.009(3) 0.001(3) -0.007(4) C5 0.037(4) 0.024(4) 0.019(3) -0.008(3) 0.004(3) -0.007(3) C6 0.024(4) 0.028(4) 0.023(3) 0.005(3) -0.004(3) -0.002(3) C7 0.019(4) 0.027(4) 0.016(3) 0.004(3) 0.000(3) 0.004(3) C8 0.014(4) 0.030(4) 0.024(3) 0.005(3) -0.002(3) 0.002(3) C9 0.029(5) 0.039(5) 0.029(4) 0.002(3) -0.008(3) -0.010(4) C10 0.008(4) 0.067(6) 0.031(4) 0.009(4) -0.003(3) -0.015(4) C11 0.017(4) 0.052(5) 0.034(4) 0.003(4) 0.007(3) 0.011(4) C12 0.016(4) 0.033(4) 0.022(3) 0.003(3) 0.006(3) 0.004(3) C13 0.019(4) 0.019(4) 0.019(3) 0.003(3) 0.000(3) -0.001(3) C14 0.008(3) 0.015(3) 0.017(3) -0.002(3) 0.003(2) -0.007(3) C15 0.008(3) 0.021(4) 0.015(3) -0.001(3) -0.007(2) -0.006(3) C16 0.032(4) 0.030(4) 0.031(4) 0.010(3) 0.004(3) -0.002(3) C17 0.022(4) 0.023(4) 0.022(3) -0.003(3) 0.007(3) -0.009(3) C18 0.016(4) 0.025(4) 0.032(4) 0.002(3) 0.006(3) 0.004(3) C19 0.024(4) 0.012(3) 0.024(3) -0.007(3) -0.001(3) 0.001(3) C20 0.039(4) 0.023(4) 0.029(4) -0.007(3) -0.004(3) 0.009(3) C21 0.044(5) 0.028(4) 0.019(3) -0.006(3) -0.002(3) 0.001(3) C22 0.032(4) 0.023(4) 0.038(4) -0.010(3) -0.004(3) 0.004(3) C23 0.020(4) 0.020(4) 0.017(3) -0.005(3) -0.003(3) -0.001(3) C24 0.029(4) 0.031(4) 0.049(4) -0.012(3) -0.005(3) 0.004(3) C25 0.026(4) 0.040(4) 0.031(4) 0.003(3) 0.006(3) 0.013(4) C26 0.015(4) 0.038(4) 0.033(4) 0.004(3) -0.005(3) 0.007(3) C27 0.022(4) 0.024(4) 0.017(3) -0.003(3) -0.003(3) -0.003(3) C28 0.036(5) 0.050(5) 0.034(4) -0.003(4) 0.009(3) -0.022(4) C29 0.012(4) 0.058(5) 0.019(3) 0.010(3) 0.006(3) 0.008(3) C30 0.018(4) 0.030(4) 0.022(3) 0.007(3) 0.002(3) 0.005(3) C31 0.012(3) 0.033(4) 0.019(3) -0.006(3) -0.005(3) -0.003(3) C32 0.010(3) 0.032(4) 0.024(3) -0.001(3) -0.005(3) 0.000(3) C33 0.014(4) 0.029(4) 0.031(4) -0.004(3) -0.006(3) -0.007(3) C34 0.014(4) 0.035(5) 0.031(4) 0.005(3) -0.009(3) -0.009(3) C35 0.022(4) 0.023(4) 0.039(4) 0.004(3) 0.000(3) -0.002(3) C36 0.015(4) 0.033(5) 0.032(4) -0.012(3) -0.005(3) 0.000(3) C37 0.015(4) 0.028(4) 0.020(3) -0.005(3) -0.003(3) -0.003(3) C38 0.027(4) 0.040(5) 0.027(4) 0.000(3) -0.002(3) -0.008(3) C39 0.031(5) 0.029(5) 0.067(5) 0.003(4) -0.007(4) 0.002(4) C40 0.038(5) 0.033(4) 0.038(4) -0.009(3) 0.009(3) 0.002(4) C41 0.020(3) 0.023(4) 0.019(3) -0.005(3) -0.002(3) 0.006(3) C42 0.023(4) 0.027(4) 0.021(3) -0.006(3) 0.002(3) -0.008(3) C43 0.029(4) 0.026(4) 0.023(3) -0.004(3) 0.004(3) -0.009(3) C44 0.032(4) 0.021(4) 0.022(3) -0.006(3) -0.001(3) 0.004(3) C45 0.017(4) 0.028(4) 0.025(3) -0.003(3) -0.005(3) 0.004(3) C46 0.022(4) 0.029(4) 0.019(3) -0.001(3) -0.005(3) 0.003(3) C47 0.026(4) 0.047(5) 0.030(4) 0.003(3) -0.003(3) -0.014(4) C48 0.034(4) 0.027(4) 0.037(4) 0.005(3) 0.003(3) 0.013(3) C49 0.019(4) 0.029(4) 0.042(4) -0.002(3) -0.016(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 1.858(5) . ? Cu P2 2.2473(17) . ? Cu P1 2.2521(17) . ? P1 C13 1.829(6) . ? P1 C15 1.876(5) . ? P1 C19 1.907(6) . ? P2 C14 1.823(5) . ? P2 C27 1.878(6) . ? P2 C23 1.888(6) . ? N1 N2 1.163(6) . ? N2 C31 1.321(7) . ? B C7 1.630(9) . ? B C13 1.660(8) . ? B C1 1.670(8) . ? B C14 1.688(8) . ? C1 C6 1.380(8) . ? C1 C2 1.400(8) . ? C2 C3 1.389(7) . ? C2 H2 0.9500 . ? C3 C4 1.386(8) . ? C3 H3 0.9500 . ? C4 C5 1.369(8) . ? C4 H4 0.9500 . ? C5 C6 1.410(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.406(8) . ? C7 C8 1.421(8) . ? C8 C9 1.385(8) . ? C8 H8 0.9500 . ? C9 C10 1.389(9) . ? C9 H9 0.9500 . ? C10 C11 1.379(9) . ? C10 H10 0.9500 . ? C11 C12 1.378(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.524(7) . ? C15 C16 1.525(8) . ? C15 C18 1.531(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.517(8) . ? C19 C20 1.528(8) . ? C19 C21 1.536(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.517(8) . ? C23 C26 1.531(7) . ? C23 C25 1.545(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.517(8) . ? C27 C30 1.544(7) . ? C27 C28 1.556(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C41 1.473(8) . ? C31 C32 1.492(8) . ? C32 C37 1.417(8) . ? C32 C33 1.418(8) . ? C33 C34 1.382(8) . ? C33 C38 1.524(8) . ? C34 C35 1.392(8) . ? C34 H34 0.9500 . ? C35 C36 1.386(8) . ? C35 C39 1.501(8) . ? C36 C37 1.405(8) . ? C36 H36 0.9500 . ? C37 C40 1.502(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.407(8) . ? C41 C46 1.422(8) . ? C42 C43 1.400(8) . ? C42 C47 1.509(8) . ? C43 C44 1.403(8) . ? C43 H43 0.9500 . ? C44 C45 1.385(8) . ? C44 C48 1.498(8) . ? C45 C46 1.401(8) . ? C45 H45 0.9500 . ? C46 C49 1.497(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P2 133.01(15) . . ? N1 Cu P1 119.67(15) . . ? P2 Cu P1 107.06(6) . . ? C13 P1 C15 109.2(2) . . ? C13 P1 C19 103.0(3) . . ? C15 P1 C19 112.4(3) . . ? C13 P1 Cu 108.56(19) . . ? C15 P1 Cu 112.81(18) . . ? C19 P1 Cu 110.30(18) . . ? C14 P2 C27 108.4(2) . . ? C14 P2 C23 103.8(2) . . ? C27 P2 C23 111.9(3) . . ? C14 P2 Cu 108.12(19) . . ? C27 P2 Cu 114.55(18) . . ? C23 P2 Cu 109.50(18) . . ? N2 N1 Cu 156.9(5) . . ? N1 N2 C31 176.4(6) . . ? C7 B C13 107.3(5) . . ? C7 B C1 101.5(4) . . ? C13 B C1 112.1(4) . . ? C7 B C14 113.4(4) . . ? C13 B C14 114.9(4) . . ? C1 B C14 106.9(4) . . ? C6 C1 C2 113.6(5) . . ? C6 C1 B 125.0(5) . . ? C2 C1 B 121.1(5) . . ? C3 C2 C1 124.3(6) . . ? C3 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 118.9(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 123.9(6) . . ? C1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C12 C7 C8 112.9(5) . . ? C12 C7 B 126.3(5) . . ? C8 C7 B 120.6(5) . . ? C9 C8 C7 124.4(6) . . ? C9 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? C8 C9 C10 119.2(6) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 119.1(6) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 120.5(6) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 124.0(6) . . ? C11 C12 H12 118.0 . . ? C7 C12 H12 118.0 . . ? B C13 P1 127.1(4) . . ? B C13 H13A 105.5 . . ? P1 C13 H13A 105.5 . . ? B C13 H13B 105.5 . . ? P1 C13 H13B 105.5 . . ? H13A C13 H13B 106.1 . . ? B C14 P2 127.4(4) . . ? B C14 H14A 105.5 . . ? P2 C14 H14A 105.5 . . ? B C14 H14B 105.5 . . ? P2 C14 H14B 105.5 . . ? H14A C14 H14B 106.0 . . ? C17 C15 C16 109.7(4) . . ? C17 C15 C18 106.4(5) . . ? C16 C15 C18 109.4(5) . . ? C17 C15 P1 106.4(4) . . ? C16 C15 P1 113.9(4) . . ? C18 C15 P1 110.8(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C20 108.9(5) . . ? C22 C19 C21 107.5(5) . . ? C20 C19 C21 109.3(5) . . ? C22 C19 P1 111.4(4) . . ? C20 C19 P1 113.5(4) . . ? C21 C19 P1 106.0(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C26 109.1(5) . . ? C24 C23 C25 108.1(5) . . ? C26 C23 C25 107.1(5) . . ? C24 C23 P2 115.0(4) . . ? C26 C23 P2 111.7(4) . . ? C25 C23 P2 105.4(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 108.1(5) . . ? C29 C27 C28 110.2(5) . . ? C30 C27 C28 108.0(5) . . ? C29 C27 P2 106.6(4) . . ? C30 C27 P2 111.0(4) . . ? C28 C27 P2 112.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 C41 117.5(5) . . ? N2 C31 C32 112.9(5) . . ? C41 C31 C32 129.6(5) . . ? C37 C32 C33 119.5(6) . . ? C37 C32 C31 119.8(5) . . ? C33 C32 C31 120.7(5) . . ? C34 C33 C32 119.1(6) . . ? C34 C33 C38 119.9(6) . . ? C32 C33 C38 121.0(6) . . ? C33 C34 C35 122.6(6) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C36 C35 C34 118.1(6) . . ? C36 C35 C39 120.5(6) . . ? C34 C35 C39 121.3(6) . . ? C35 C36 C37 122.0(6) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C36 C37 C32 118.7(5) . . ? C36 C37 C40 119.2(5) . . ? C32 C37 C40 122.0(5) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 119.8(5) . . ? C42 C41 C31 120.6(5) . . ? C46 C41 C31 119.6(5) . . ? C43 C42 C41 119.5(5) . . ? C43 C42 C47 117.8(5) . . ? C41 C42 C47 122.6(6) . . ? C42 C43 C44 121.6(6) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C45 C44 C43 117.7(6) . . ? C45 C44 C48 120.5(6) . . ? C43 C44 C48 121.8(6) . . ? C44 C45 C46 123.0(6) . . ? C44 C45 H45 118.5 . . ? C46 C45 H45 118.5 . . ? C45 C46 C41 118.2(6) . . ? C45 C46 C49 118.8(5) . . ? C41 C46 C49 123.0(5) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.505 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.085 #===END data_npm29 _database_code_depnum_ccdc_archive 'CCDC 659796' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (BP2)Cu-N(=CPh2)(NCPh2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H70 B Cu N2 P2' _chemical_formula_weight 907.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0749(11) _cell_length_b 22.347(2) _cell_length_c 19.2412(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.625(2) _cell_angle_gamma 90.00 _cell_volume 5023.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42567 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.46 _reflns_number_total 11402 _reflns_number_gt 7627 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+3.8260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11402 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.15187(3) 0.379589(15) 0.801043(17) 0.01953(10) Uani 1 1 d . . . P1 P 0.24163(6) 0.33294(3) 0.72650(4) 0.02136(17) Uani 1 1 d . . . P2 P 0.19226(6) 0.47902(3) 0.79935(4) 0.01779(16) Uani 1 1 d . . . N1 N 0.01997(19) 0.35125(10) 0.83909(12) 0.0218(5) Uani 1 1 d . . . N2 N -0.0761(2) 0.34724(13) 0.78052(14) 0.0350(6) Uani 1 1 d . . . B B 0.3176(3) 0.45632(14) 0.67811(17) 0.0200(6) Uani 1 1 d . . . C1 C 0.4409(2) 0.49326(12) 0.69868(14) 0.0200(6) Uani 1 1 d . . . C2 C 0.4397(2) 0.55353(14) 0.67876(16) 0.0291(7) Uani 1 1 d . . . H2 H 0.3683 0.5716 0.6566 0.035 Uiso 1 1 calc R . . C3 C 0.5376(3) 0.58776(14) 0.68991(17) 0.0297(7) Uani 1 1 d . . . H3 H 0.5326 0.6285 0.6752 0.036 Uiso 1 1 calc R . . C4 C 0.6434(3) 0.56308(14) 0.72252(16) 0.0288(7) Uani 1 1 d . . . H4 H 0.7109 0.5867 0.7315 0.035 Uiso 1 1 calc R . . C5 C 0.6480(2) 0.50379(14) 0.74158(16) 0.0290(7) Uani 1 1 d . . . H5 H 0.7199 0.4859 0.7632 0.035 Uiso 1 1 calc R . . C6 C 0.5488(2) 0.46945(13) 0.72962(15) 0.0235(6) Uani 1 1 d . . . H6 H 0.5548 0.4284 0.7430 0.028 Uiso 1 1 calc R . . C7 C 0.2800(2) 0.46167(13) 0.58962(15) 0.0244(6) Uani 1 1 d . . . C8 C 0.1817(2) 0.49040(14) 0.54830(16) 0.0289(7) Uani 1 1 d . . . H8 H 0.1266 0.5051 0.5717 0.035 Uiso 1 1 calc R . . C9 C 0.1620(3) 0.49814(18) 0.47476(17) 0.0401(9) Uani 1 1 d . . . H9 H 0.0950 0.5183 0.4489 0.048 Uiso 1 1 calc R . . C10 C 0.2401(3) 0.47652(19) 0.43868(17) 0.0444(9) Uani 1 1 d . . . H10 H 0.2265 0.4815 0.3882 0.053 Uiso 1 1 calc R . . C11 C 0.3370(3) 0.44791(18) 0.47692(17) 0.0431(9) Uani 1 1 d . . . H11 H 0.3914 0.4331 0.4531 0.052 Uiso 1 1 calc R . . C12 C 0.3553(3) 0.44065(16) 0.55077(16) 0.0346(8) Uani 1 1 d . . . H12 H 0.4224 0.4203 0.5761 0.042 Uiso 1 1 calc R . . C13 C 0.3432(2) 0.38489(12) 0.70331(15) 0.0214(6) Uani 1 1 d . . . H13A H 0.4101 0.3858 0.7455 0.026 Uiso 1 1 calc R . . H13B H 0.3697 0.3654 0.6642 0.026 Uiso 1 1 calc R . . C14 C 0.2207(2) 0.49232(13) 0.71161(14) 0.0210(6) Uani 1 1 d . . . H14A H 0.1465 0.4869 0.6759 0.025 Uiso 1 1 calc R . . H14B H 0.2397 0.5354 0.7107 0.025 Uiso 1 1 calc R . . C15 C 0.3344(3) 0.26642(13) 0.76505(17) 0.0288(7) Uani 1 1 d . . . C16 C 0.3863(3) 0.23471(16) 0.71036(19) 0.0426(9) Uani 1 1 d . . . H16A H 0.4226 0.2643 0.6856 0.064 Uiso 1 1 calc R . . H16B H 0.3258 0.2138 0.6752 0.064 Uiso 1 1 calc R . . H16C H 0.4437 0.2058 0.7352 0.064 Uiso 1 1 calc R . . C17 C 0.4323(3) 0.28940(15) 0.82668(18) 0.0348(7) Uani 1 1 d . . . H17A H 0.4720 0.2554 0.8542 0.052 Uiso 1 1 calc R . . H17B H 0.4009 0.3151 0.8583 0.052 Uiso 1 1 calc R . . H17C H 0.4863 0.3124 0.8069 0.052 Uiso 1 1 calc R . . C18 C 0.2658(3) 0.22130(14) 0.79855(19) 0.0358(8) Uani 1 1 d . . . H18A H 0.2082 0.2016 0.7603 0.054 Uiso 1 1 calc R . . H18B H 0.2276 0.2425 0.8306 0.054 Uiso 1 1 calc R . . H18C H 0.3179 0.1912 0.8260 0.054 Uiso 1 1 calc R . . C19 C 0.1337(3) 0.31117(14) 0.64109(16) 0.0285(7) Uani 1 1 d . . . C20 C 0.1843(3) 0.30108(16) 0.57676(17) 0.0389(8) Uani 1 1 d . . . H20A H 0.2381 0.2674 0.5868 0.058 Uiso 1 1 calc R . . H20B H 0.2247 0.3373 0.5681 0.058 Uiso 1 1 calc R . . H20C H 0.1226 0.2921 0.5341 0.058 Uiso 1 1 calc R . . C21 C 0.0501(3) 0.36444(15) 0.62327(16) 0.0321(7) Uani 1 1 d . . . H21A H 0.0921 0.4006 0.6164 0.048 Uiso 1 1 calc R . . H21B H 0.0139 0.3707 0.6629 0.048 Uiso 1 1 calc R . . H21C H -0.0089 0.3558 0.5791 0.048 Uiso 1 1 calc R . . C22 C 0.0659(3) 0.25594(16) 0.65316(19) 0.0422(9) Uani 1 1 d . . . H22A H -0.0028 0.2520 0.6134 0.063 Uiso 1 1 calc R . . H22B H 0.0436 0.2603 0.6985 0.063 Uiso 1 1 calc R . . H22C H 0.1136 0.2202 0.6553 0.063 Uiso 1 1 calc R . . C23 C 0.3185(2) 0.50563(13) 0.87168(14) 0.0222(6) Uani 1 1 d . . . C24 C 0.3699(3) 0.56485(14) 0.85469(17) 0.0327(7) Uani 1 1 d . . . H24A H 0.4375 0.5745 0.8934 0.049 Uiso 1 1 calc R . . H24B H 0.3130 0.5968 0.8505 0.049 Uiso 1 1 calc R . . H24C H 0.3921 0.5611 0.8093 0.049 Uiso 1 1 calc R . . C25 C 0.4099(2) 0.45716(14) 0.87942(15) 0.0261(6) Uani 1 1 d . . . H25A H 0.4315 0.4527 0.8339 0.039 Uiso 1 1 calc R . . H25B H 0.3796 0.4191 0.8920 0.039 Uiso 1 1 calc R . . H25C H 0.4774 0.4685 0.9174 0.039 Uiso 1 1 calc R . . C26 C 0.2863(3) 0.51054(14) 0.94397(15) 0.0287(7) Uani 1 1 d . . . H26A H 0.2460 0.4742 0.9521 0.043 Uiso 1 1 calc R . . H26B H 0.2365 0.5453 0.9430 0.043 Uiso 1 1 calc R . . H26C H 0.3560 0.5153 0.9828 0.043 Uiso 1 1 calc R . . C27 C 0.0641(2) 0.52840(13) 0.79844(15) 0.0235(6) Uani 1 1 d . . . C28 C 0.0869(3) 0.59572(14) 0.80118(18) 0.0343(7) Uani 1 1 d . . . H28A H 0.1280 0.6063 0.7650 0.051 Uiso 1 1 calc R . . H28B H 0.1334 0.6066 0.8490 0.051 Uiso 1 1 calc R . . H28C H 0.0140 0.6173 0.7913 0.051 Uiso 1 1 calc R . . C29 C -0.0260(2) 0.51473(16) 0.72885(16) 0.0331(7) Uani 1 1 d . . . H29A H -0.0369 0.4713 0.7238 0.050 Uiso 1 1 calc R . . H29B H -0.0003 0.5303 0.6880 0.050 Uiso 1 1 calc R . . H29C H -0.0985 0.5337 0.7302 0.050 Uiso 1 1 calc R . . C30 C 0.0116(3) 0.51087(15) 0.86019(17) 0.0307(7) Uani 1 1 d . . . H30A H -0.0595 0.5333 0.8561 0.046 Uiso 1 1 calc R . . H30B H 0.0657 0.5202 0.9061 0.046 Uiso 1 1 calc R . . H30C H -0.0049 0.4679 0.8578 0.046 Uiso 1 1 calc R . . C31 C 0.0086(2) 0.35376(12) 0.90458(15) 0.0221(6) Uani 1 1 d . . . C32 C 0.1155(2) 0.36015(13) 0.96251(15) 0.0226(6) Uani 1 1 d . . . C33 C 0.2179(2) 0.33488(14) 0.95482(16) 0.0267(6) Uani 1 1 d . . . H33 H 0.2184 0.3128 0.9127 0.032 Uiso 1 1 calc R . . C34 C 0.3186(3) 0.34170(15) 1.00800(17) 0.0321(7) Uani 1 1 d . . . H34 H 0.3874 0.3241 1.0024 0.039 Uiso 1 1 calc R . . C35 C 0.3189(3) 0.37419(15) 1.06919(16) 0.0329(7) Uani 1 1 d . . . H35 H 0.3879 0.3791 1.1056 0.039 Uiso 1 1 calc R . . C36 C 0.2189(3) 0.39936(16) 1.07709(17) 0.0348(8) Uani 1 1 d . . . H36 H 0.2191 0.4219 1.1190 0.042 Uiso 1 1 calc R . . C37 C 0.1173(3) 0.39205(15) 1.02421(16) 0.0308(7) Uani 1 1 d . . . H37 H 0.0485 0.4092 1.0306 0.037 Uiso 1 1 calc R . . C38 C -0.1026(2) 0.35201(13) 0.92426(15) 0.0234(6) Uani 1 1 d . . . C39 C -0.1972(2) 0.38531(14) 0.88689(16) 0.0279(7) Uani 1 1 d . . . H39 H -0.1911 0.4102 0.8480 0.033 Uiso 1 1 calc R . . C40 C -0.2994(3) 0.38191(15) 0.90651(17) 0.0335(7) Uani 1 1 d . . . H40 H -0.3633 0.4048 0.8814 0.040 Uiso 1 1 calc R . . C41 C -0.3089(3) 0.34550(16) 0.96223(17) 0.0362(8) Uani 1 1 d . . . H41 H -0.3798 0.3431 0.9751 0.043 Uiso 1 1 calc R . . C42 C -0.2167(3) 0.31236(17) 0.99969(17) 0.0372(8) Uani 1 1 d . . . H42 H -0.2238 0.2872 1.0381 0.045 Uiso 1 1 calc R . . C43 C -0.1136(3) 0.31608(15) 0.98078(16) 0.0308(7) Uani 1 1 d . . . H43 H -0.0496 0.2937 1.0069 0.037 Uiso 1 1 calc R . . C44 C -0.1402(3) 0.29960(16) 0.76799(18) 0.0363(8) Uani 1 1 d . . . C45 C -0.2353(3) 0.30168(17) 0.70159(18) 0.0382(8) Uani 1 1 d . . . C46 C -0.2627(3) 0.3547(2) 0.6643(2) 0.0522(10) Uani 1 1 d . . . H46 H -0.2219 0.3901 0.6823 0.063 Uiso 1 1 calc R . . C47 C -0.3493(4) 0.3574(2) 0.6006(2) 0.0650(13) Uani 1 1 d . . . H47 H -0.3655 0.3938 0.5746 0.078 Uiso 1 1 calc R . . C48 C -0.4117(3) 0.3056(2) 0.5757(2) 0.0659(14) Uani 1 1 d . . . H48 H -0.4733 0.3070 0.5338 0.079 Uiso 1 1 calc R . . C49 C -0.3834(3) 0.2518(2) 0.6126(2) 0.0600(12) Uani 1 1 d . . . H49 H -0.4248 0.2165 0.5949 0.072 Uiso 1 1 calc R . . C50 C -0.2942(3) 0.24932(19) 0.6756(2) 0.0492(10) Uani 1 1 d . . . H50 H -0.2744 0.2125 0.7002 0.059 Uiso 1 1 calc R . . C51 C -0.1251(3) 0.24605(17) 0.81605(19) 0.0447(9) Uani 1 1 d . . . C52 C -0.0191(4) 0.21732(18) 0.8390(2) 0.0561(11) Uani 1 1 d . . . H52 H 0.0438 0.2322 0.8228 0.067 Uiso 1 1 calc R . . C53 C -0.0019(7) 0.1683(2) 0.8843(2) 0.100(2) Uani 1 1 d . . . H53 H 0.0704 0.1489 0.8974 0.120 Uiso 1 1 calc R . . C54 C -0.2016(8) 0.1763(3) 0.8878(3) 0.119(3) Uani 1 1 d . . . H54 H -0.2634 0.1620 0.9054 0.143 Uiso 1 1 calc R . . C55 C -0.0913(9) 0.1482(3) 0.9099(3) 0.125(4) Uani 1 1 d . . . H55 H -0.0803 0.1156 0.9425 0.150 Uiso 1 1 calc R . . C56 C -0.2178(4) 0.2245(2) 0.8405(2) 0.0690(14) Uani 1 1 d . . . H56 H -0.2909 0.2427 0.8249 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.01623(17) 0.02208(18) 0.01926(17) -0.00392(14) 0.00259(13) -0.00170(13) P1 0.0182(3) 0.0220(4) 0.0231(4) -0.0064(3) 0.0035(3) -0.0004(3) P2 0.0154(3) 0.0199(4) 0.0167(3) -0.0032(3) 0.0014(3) 0.0007(3) N1 0.0176(11) 0.0231(12) 0.0225(12) -0.0035(10) 0.0010(9) -0.0028(9) N2 0.0291(14) 0.0431(17) 0.0323(15) -0.0054(13) 0.0064(12) -0.0045(12) B 0.0172(15) 0.0232(16) 0.0186(15) 0.0001(13) 0.0025(12) 0.0014(12) C1 0.0204(14) 0.0230(14) 0.0165(13) -0.0014(11) 0.0044(11) 0.0021(11) C2 0.0196(15) 0.0330(17) 0.0337(17) 0.0054(14) 0.0051(13) 0.0034(13) C3 0.0318(17) 0.0220(15) 0.0369(18) 0.0049(13) 0.0114(14) 0.0000(13) C4 0.0229(15) 0.0346(18) 0.0291(16) 0.0000(13) 0.0069(13) -0.0052(13) C5 0.0206(15) 0.0365(18) 0.0270(16) 0.0044(13) 0.0005(12) 0.0013(13) C6 0.0214(14) 0.0264(15) 0.0222(14) 0.0032(12) 0.0045(11) 0.0005(12) C7 0.0204(14) 0.0321(16) 0.0195(14) -0.0031(12) 0.0028(11) -0.0008(12) C8 0.0203(14) 0.0423(19) 0.0236(15) -0.0002(13) 0.0045(12) 0.0058(13) C9 0.0270(17) 0.068(3) 0.0225(16) 0.0075(16) 0.0008(13) 0.0091(16) C10 0.0334(19) 0.080(3) 0.0179(15) 0.0015(17) 0.0037(13) 0.0033(18) C11 0.0320(18) 0.074(3) 0.0258(17) -0.0027(17) 0.0110(14) 0.0098(18) C12 0.0251(16) 0.053(2) 0.0248(16) -0.0023(15) 0.0046(13) 0.0109(15) C13 0.0178(13) 0.0248(15) 0.0218(14) -0.0040(12) 0.0051(11) -0.0016(11) C14 0.0174(13) 0.0262(15) 0.0174(13) 0.0005(11) 0.0011(11) 0.0012(11) C15 0.0306(16) 0.0234(15) 0.0333(17) -0.0026(13) 0.0100(13) 0.0055(13) C16 0.050(2) 0.036(2) 0.046(2) 0.0006(16) 0.0194(17) 0.0175(16) C17 0.0302(17) 0.0312(17) 0.0392(19) 0.0073(15) 0.0019(14) 0.0056(14) C18 0.0383(18) 0.0245(17) 0.048(2) -0.0011(15) 0.0169(16) 0.0032(14) C19 0.0266(15) 0.0327(17) 0.0240(15) -0.0113(13) 0.0023(12) -0.0045(13) C20 0.0402(19) 0.046(2) 0.0277(17) -0.0139(15) 0.0040(15) 0.0031(16) C21 0.0231(15) 0.0439(19) 0.0252(15) -0.0117(14) -0.0018(12) 0.0000(13) C22 0.042(2) 0.045(2) 0.0351(19) -0.0142(16) 0.0028(16) -0.0168(17) C23 0.0209(14) 0.0260(15) 0.0167(13) -0.0050(11) -0.0007(11) -0.0028(11) C24 0.0282(16) 0.0312(17) 0.0335(17) -0.0064(14) -0.0017(14) -0.0097(13) C25 0.0184(14) 0.0355(17) 0.0208(14) -0.0018(13) -0.0019(11) 0.0003(12) C26 0.0263(15) 0.0353(17) 0.0204(14) -0.0089(13) -0.0021(12) -0.0007(13) C27 0.0198(14) 0.0267(15) 0.0226(14) -0.0041(12) 0.0028(11) 0.0051(12) C28 0.0345(18) 0.0278(17) 0.0394(19) -0.0021(14) 0.0070(15) 0.0096(14) C29 0.0183(15) 0.050(2) 0.0294(17) -0.0077(15) 0.0025(12) 0.0099(14) C30 0.0271(16) 0.0354(18) 0.0320(17) -0.0039(14) 0.0116(13) 0.0080(13) C31 0.0207(14) 0.0207(14) 0.0236(14) -0.0012(12) 0.0032(11) -0.0004(11) C32 0.0200(14) 0.0257(15) 0.0208(14) 0.0024(12) 0.0027(11) -0.0029(11) C33 0.0255(15) 0.0298(16) 0.0250(15) 0.0034(13) 0.0065(12) 0.0018(12) C34 0.0200(15) 0.0426(19) 0.0328(17) 0.0099(15) 0.0046(13) 0.0040(13) C35 0.0242(16) 0.047(2) 0.0235(15) 0.0105(14) -0.0017(12) -0.0075(14) C36 0.0284(17) 0.049(2) 0.0234(16) -0.0069(14) 0.0002(13) -0.0061(15) C37 0.0207(15) 0.044(2) 0.0264(16) -0.0081(14) 0.0029(12) 0.0002(13) C38 0.0190(14) 0.0295(16) 0.0197(14) -0.0054(12) 0.0014(11) -0.0040(12) C39 0.0236(15) 0.0344(17) 0.0235(15) -0.0041(13) 0.0020(12) -0.0018(13) C40 0.0194(15) 0.047(2) 0.0307(17) -0.0091(15) -0.0003(13) 0.0025(14) C41 0.0220(16) 0.056(2) 0.0313(17) -0.0150(16) 0.0078(13) -0.0084(15) C42 0.0330(18) 0.053(2) 0.0263(17) -0.0014(15) 0.0095(14) -0.0089(16) C43 0.0253(16) 0.0418(19) 0.0236(15) 0.0007(14) 0.0029(12) -0.0020(14) C44 0.0313(17) 0.044(2) 0.0355(18) -0.0119(16) 0.0123(14) -0.0084(15) C45 0.0297(17) 0.052(2) 0.0338(18) -0.0138(16) 0.0104(14) 0.0018(16) C46 0.035(2) 0.064(3) 0.052(2) -0.018(2) 0.0001(17) 0.0067(18) C47 0.045(2) 0.075(3) 0.062(3) -0.014(2) -0.012(2) 0.015(2) C48 0.033(2) 0.100(4) 0.058(3) -0.030(3) -0.0019(19) 0.013(2) C49 0.034(2) 0.089(3) 0.054(3) -0.039(2) 0.0073(19) -0.004(2) C50 0.037(2) 0.064(3) 0.049(2) -0.025(2) 0.0141(17) -0.0089(18) C51 0.055(2) 0.042(2) 0.0361(19) -0.0104(16) 0.0092(17) -0.0152(18) C52 0.079(3) 0.041(2) 0.041(2) -0.0099(18) 0.002(2) -0.004(2) C53 0.207(7) 0.030(2) 0.037(3) -0.009(2) -0.019(3) -0.002(3) C54 0.236(9) 0.079(4) 0.042(3) -0.019(3) 0.034(4) -0.104(5) C55 0.260(11) 0.057(4) 0.034(3) 0.003(3) -0.005(4) -0.072(5) C56 0.082(3) 0.082(3) 0.048(2) -0.022(2) 0.025(2) -0.050(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 2.016(2) . ? Cu P1 2.2592(8) . ? Cu P2 2.2769(8) . ? P1 C13 1.824(3) . ? P1 C19 1.885(3) . ? P1 C15 1.896(3) . ? P2 C14 1.830(3) . ? P2 C23 1.882(3) . ? P2 C27 1.898(3) . ? N1 C31 1.303(4) . ? N1 N2 1.401(3) . ? N2 C44 1.302(4) . ? B C7 1.652(4) . ? B C1 1.661(4) . ? B C13 1.674(4) . ? B C14 1.676(4) . ? C1 C6 1.394(4) . ? C1 C2 1.400(4) . ? C2 C3 1.379(4) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.372(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.396(4) . ? C7 C8 1.406(4) . ? C8 C9 1.385(4) . ? C8 H8 0.9500 . ? C9 C10 1.391(5) . ? C9 H9 0.9500 . ? C10 C11 1.373(5) . ? C10 H10 0.9500 . ? C11 C12 1.391(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.528(4) . ? C15 C17 1.536(4) . ? C15 C18 1.546(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.529(4) . ? C19 C22 1.531(5) . ? C19 C21 1.543(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.527(4) . ? C23 C24 1.532(4) . ? C23 C26 1.540(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.528(4) . ? C27 C29 1.527(4) . ? C27 C30 1.532(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.485(4) . ? C31 C38 1.484(4) . ? C32 C37 1.381(4) . ? C32 C33 1.401(4) . ? C33 C34 1.386(4) . ? C33 H33 0.9500 . ? C34 C35 1.383(5) . ? C34 H34 0.9500 . ? C35 C36 1.375(5) . ? C35 H35 0.9500 . ? C36 C37 1.392(4) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.385(4) . ? C38 C39 1.401(4) . ? C39 C40 1.380(4) . ? C39 H39 0.9500 . ? C40 C41 1.374(5) . ? C40 H40 0.9500 . ? C41 C42 1.380(5) . ? C41 H41 0.9500 . ? C42 C43 1.385(4) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.487(5) . ? C44 C51 1.495(5) . ? C45 C46 1.382(6) . ? C45 C50 1.395(5) . ? C46 C47 1.396(5) . ? C46 H46 0.9500 . ? C47 C48 1.398(6) . ? C47 H47 0.9500 . ? C48 C49 1.393(7) . ? C48 H48 0.9500 . ? C49 C50 1.405(6) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.400(6) . ? C51 C56 1.404(6) . ? C52 C53 1.383(6) . ? C52 H52 0.9500 . ? C53 C55 1.370(10) . ? C53 H53 0.9500 . ? C54 C55 1.435(11) . ? C54 C56 1.391(8) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P1 129.45(7) . . ? N1 Cu P2 120.24(7) . . ? P1 Cu P2 107.60(3) . . ? C13 P1 C19 108.08(14) . . ? C13 P1 C15 103.13(13) . . ? C19 P1 C15 110.41(14) . . ? C13 P1 Cu 108.76(9) . . ? C19 P1 Cu 109.62(10) . . ? C15 P1 Cu 116.37(10) . . ? C14 P2 C23 108.97(13) . . ? C14 P2 C27 103.89(13) . . ? C23 P2 C27 109.24(13) . . ? C14 P2 Cu 105.22(10) . . ? C23 P2 Cu 115.73(9) . . ? C27 P2 Cu 112.98(10) . . ? C31 N1 N2 120.8(2) . . ? C31 N1 Cu 128.61(19) . . ? N2 N1 Cu 107.31(17) . . ? C44 N2 N1 122.3(3) . . ? C7 B C1 101.9(2) . . ? C7 B C13 110.5(2) . . ? C1 B C13 108.4(2) . . ? C7 B C14 109.0(2) . . ? C1 B C14 109.9(2) . . ? C13 B C14 116.2(2) . . ? C6 C1 C2 115.4(3) . . ? C6 C1 B 126.7(3) . . ? C2 C1 B 117.8(2) . . ? C3 C2 C1 122.8(3) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 118.4(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 122.2(3) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? C12 C7 C8 114.9(3) . . ? C12 C7 B 118.8(3) . . ? C8 C7 B 126.1(3) . . ? C9 C8 C7 122.5(3) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.2(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 119.7(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C7 123.5(3) . . ? C11 C12 H12 118.3 . . ? C7 C12 H12 118.3 . . ? B C13 P1 126.23(19) . . ? B C13 H13A 105.8 . . ? P1 C13 H13A 105.8 . . ? B C13 H13B 105.8 . . ? P1 C13 H13B 105.8 . . ? H13A C13 H13B 106.2 . . ? B C14 P2 126.05(19) . . ? B C14 H14A 105.8 . . ? P2 C14 H14A 105.8 . . ? B C14 H14B 105.8 . . ? P2 C14 H14B 105.8 . . ? H14A C14 H14B 106.2 . . ? C16 C15 C17 108.5(3) . . ? C16 C15 C18 109.9(3) . . ? C17 C15 C18 106.6(3) . . ? C16 C15 P1 113.5(2) . . ? C17 C15 P1 107.7(2) . . ? C18 C15 P1 110.4(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 110.0(3) . . ? C20 C19 C21 107.9(3) . . ? C22 C19 C21 108.1(3) . . ? C20 C19 P1 114.5(2) . . ? C22 C19 P1 110.7(2) . . ? C21 C19 P1 105.32(19) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 108.2(2) . . ? C25 C23 C26 107.7(2) . . ? C24 C23 C26 109.8(2) . . ? C25 C23 P2 106.18(18) . . ? C24 C23 P2 114.3(2) . . ? C26 C23 P2 110.40(19) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 108.0(3) . . ? C28 C27 C30 109.4(2) . . ? C29 C27 C30 106.7(2) . . ? C28 C27 P2 115.6(2) . . ? C29 C27 P2 106.86(19) . . ? C30 C27 P2 109.9(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 C32 116.5(2) . . ? N1 C31 C38 124.7(2) . . ? C32 C31 C38 118.8(2) . . ? C37 C32 C33 118.5(3) . . ? C37 C32 C31 121.1(3) . . ? C33 C32 C31 120.4(3) . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.5(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C32 C37 C36 120.6(3) . . ? C32 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C43 C38 C39 118.9(3) . . ? C43 C38 C31 119.2(3) . . ? C39 C38 C31 121.9(3) . . ? C40 C39 C38 120.0(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.6(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C43 119.4(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C38 C43 C42 120.8(3) . . ? C38 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? N2 C44 C45 115.3(3) . . ? N2 C44 C51 124.5(3) . . ? C45 C44 C51 120.2(3) . . ? C46 C45 C50 120.0(3) . . ? C46 C45 C44 120.3(3) . . ? C50 C45 C44 119.7(4) . . ? C45 C46 C47 121.3(4) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 119.0(5) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C49 C48 C47 119.9(4) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C50 120.7(4) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C45 C50 C49 119.1(4) . . ? C45 C50 H50 120.4 . . ? C49 C50 H50 120.5 . . ? C52 C51 C56 118.7(4) . . ? C52 C51 C44 121.4(4) . . ? C56 C51 C44 119.9(4) . . ? C51 C52 C53 122.8(5) . . ? C51 C52 H52 118.6 . . ? C53 C52 H52 118.6 . . ? C55 C53 C52 118.6(7) . . ? C55 C53 H53 120.7 . . ? C52 C53 H53 120.7 . . ? C55 C54 C56 119.9(7) . . ? C55 C54 H54 120.0 . . ? C56 C54 H54 120.0 . . ? C54 C55 C53 120.4(6) . . ? C54 C55 H55 119.8 . . ? C53 C55 H55 119.8 . . ? C51 C56 C54 119.5(6) . . ? C51 C56 H56 120.3 . . ? C54 C56 H56 120.3 . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.694 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.078 #===END