#============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Michael W. Day Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; _publ_contact_author_phone '(818) 395 2734' _publ_contact_author_fax '(818) 449 4159' _publ_contact_author_email mikeday@caltech.edu _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition in the Cambridge Structural Database. ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Day, Michael W.' #<--'Last name, first name' ; Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; 'Klamo, Sara B.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; 'Bercaw, John E.' ; Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, CA 91125 USA ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== # 5. CHEMICAL DATA data_sbk03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H42 Zr' _chemical_formula_weight 433.81 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.7467(4) _cell_length_b 25.9839(12) _cell_length_c 10.2031(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.6710(10) _cell_angle_gamma 90.00 _cell_volume 2309.07(18) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 27315 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.81 _exptl_crystal_description Chunks _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.9140 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 7 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46222 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.37 _reflns_number_total 5440 _reflns_number_gt 4770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v.5054' _computing_cell_refinement 'Bruker SAINT v6.022' _computing_data_reduction 'Bruker SAINT v6.022' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5440 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0475 _refine_ls_goodness_of_fit_ref 2.059 _refine_ls_restrained_S_all 2.059 _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 Zr Zr 0.329967(14) 0.142554(5) 0.623210(14) 0.00987(5) Uani 1 1 d . . . C1 C 0.44698(17) 0.23048(5) 0.66724(16) 0.0171(3) Uani 1 1 d . . . C2 C 0.29435(17) 0.23901(5) 0.64160(16) 0.0171(3) Uani 1 1 d . . . C3 C 0.27477(17) 0.21732(5) 0.75742(16) 0.0166(3) Uani 1 1 d . . . C4 C 0.41652(17) 0.19575(5) 0.85716(16) 0.0155(3) Uani 1 1 d . . . C5 C 0.52277(17) 0.20450(5) 0.80258(16) 0.0154(3) Uani 1 1 d . . . C6 C 0.58024(15) 0.11992(5) 0.61369(15) 0.0136(3) Uani 1 1 d . . . C7 C 0.46145(15) 0.11246(5) 0.47015(15) 0.0131(3) Uani 1 1 d . . . C8 C 0.37235(15) 0.06972(5) 0.47432(15) 0.0127(3) Uani 1 1 d . . . C9 C 0.43508(15) 0.05147(5) 0.62019(15) 0.0133(3) Uani 1 1 d . . . C10 C 0.56238(15) 0.08314(5) 0.70788(15) 0.0134(3) Uani 1 1 d . . . C11 C 0.71599(18) 0.15453(7) 0.65117(19) 0.0204(3) Uani 1 1 d . . . C12 C 0.44555(18) 0.14159(7) 0.33705(17) 0.0182(3) Uani 1 1 d . . . C13 C 0.24751(18) 0.04284(6) 0.34667(18) 0.0191(3) Uani 1 1 d . . . C14 C 0.3893(2) 0.00168(6) 0.6637(2) 0.0195(3) Uani 1 1 d . . . C15 C 0.67007(19) 0.07475(7) 0.86733(17) 0.0179(3) Uani 1 1 d . . . C16 C 0.19417(16) 0.09805(6) 0.71665(16) 0.0135(3) Uani 1 1 d . . . C17 C 0.18607(15) 0.08400(5) 0.85965(15) 0.0150(3) Uani 1 1 d . . . C18 C 0.33933(18) 0.06252(6) 0.97441(18) 0.0196(3) Uani 1 1 d . . . C19 C 0.14287(18) 0.13043(6) 0.92590(17) 0.0174(3) Uani 1 1 d . . . C20 C 0.0631(2) 0.04244(6) 0.8273(2) 0.0229(4) Uani 1 1 d . . . C21 C 0.13183(16) 0.16195(6) 0.38956(15) 0.0134(3) Uani 1 1 d . . . C22 C -0.04377(16) 0.16839(6) 0.33403(15) 0.0150(3) Uani 1 1 d . . . C23 C -0.11788(18) 0.11610(6) 0.32960(19) 0.0208(3) Uani 1 1 d . . . C24 C -0.08430(18) 0.20567(6) 0.42724(18) 0.0193(3) Uani 1 1 d . . . C25 C -0.11471(19) 0.18972(7) 0.17714(17) 0.0221(4) Uani 1 1 d . . . H1 H 0.4906(16) 0.2399(6) 0.6070(15) 0.014(4) Uiso 1 1 d . . . H2 H 0.2199(17) 0.2562(6) 0.5622(17) 0.023(4) Uiso 1 1 d . . . H3 H 0.1841(16) 0.2181(5) 0.7656(15) 0.013(4) Uiso 1 1 d . . . H4 H 0.4356(16) 0.1804(5) 0.9417(16) 0.013(4) Uiso 1 1 d . . . H5 H 0.6244(17) 0.1968(5) 0.8440(15) 0.014(4) Uiso 1 1 d . . . H11A H 0.784(2) 0.1392(6) 0.6177(17) 0.028(5) Uiso 1 1 d . . . H11B H 0.6922(19) 0.1870(7) 0.6099(19) 0.033(5) Uiso 1 1 d . . . H11C H 0.7711(19) 0.1596(6) 0.7528(19) 0.028(5) Uiso 1 1 d . . . H12A H 0.5047(19) 0.1257(6) 0.2958(18) 0.030(5) Uiso 1 1 d . . . H12B H 0.341(2) 0.1431(6) 0.2625(19) 0.031(5) Uiso 1 1 d . . . H12C H 0.4758(19) 0.1748(7) 0.3566(18) 0.034(5) Uiso 1 1 d . . . H13A H 0.2796(19) 0.0106(7) 0.3335(18) 0.036(5) Uiso 1 1 d . . . H13B H 0.1590(18) 0.0374(6) 0.3618(17) 0.026(5) Uiso 1 1 d . . . H13C H 0.2185(17) 0.0604(6) 0.2552(18) 0.026(4) Uiso 1 1 d . . . H14A H 0.4255(18) -0.0272(7) 0.6245(18) 0.031(5) Uiso 1 1 d . . . H14B H 0.4282(17) -0.0018(6) 0.7637(19) 0.027(5) Uiso 1 1 d . . . H14C H 0.283(2) -0.0029(6) 0.6269(17) 0.032(5) Uiso 1 1 d . . . H15A H 0.753(2) 0.0529(7) 0.8814(19) 0.044(5) Uiso 1 1 d . . . H15B H 0.710(2) 0.1021(8) 0.912(2) 0.047(6) Uiso 1 1 d . . . H15C H 0.627(2) 0.0588(7) 0.919(2) 0.045(6) Uiso 1 1 d . . . H16A H 0.1736(16) 0.0682(6) 0.6582(16) 0.016(4) Uiso 1 1 d . . . H16B H 0.1139(18) 0.1205(6) 0.6624(17) 0.025(4) Uiso 1 1 d . . . H18A H 0.3654(16) 0.0319(6) 0.9385(16) 0.017(4) Uiso 1 1 d . . . H18B H 0.4219(16) 0.0871(6) 1.0005(15) 0.014(4) Uiso 1 1 d . . . H18C H 0.3299(16) 0.0541(6) 1.0634(18) 0.024(4) Uiso 1 1 d . . . H19A H 0.1278(16) 0.1205(6) 1.0103(17) 0.019(4) Uiso 1 1 d . . . H19B H 0.0494(18) 0.1475(6) 0.8557(17) 0.022(4) Uiso 1 1 d . . . H19C H 0.2240(18) 0.1565(6) 0.9671(17) 0.018(4) Uiso 1 1 d . . . H20A H -0.0332(17) 0.0545(6) 0.7608(17) 0.019(4) Uiso 1 1 d . . . H20B H 0.0841(16) 0.0113(6) 0.7852(16) 0.017(4) Uiso 1 1 d . . . H20C H 0.0560(17) 0.0325(6) 0.9140(18) 0.022(4) Uiso 1 1 d . . . H21A H 0.1395(16) 0.1348(6) 0.3257(17) 0.018(4) Uiso 1 1 d . . . H21B H 0.1707(16) 0.1934(6) 0.3672(15) 0.018(4) Uiso 1 1 d . . . H23A H -0.2274(18) 0.1201(6) 0.2933(16) 0.020(4) Uiso 1 1 d . . . H23B H -0.0810(17) 0.1001(6) 0.4270(18) 0.023(4) Uiso 1 1 d . . . H23C H -0.1009(17) 0.0931(6) 0.2683(16) 0.017(4) Uiso 1 1 d . . . H24A H -0.0467(17) 0.1946(6) 0.5250(18) 0.018(4) Uiso 1 1 d . . . H24B H -0.1947(18) 0.2080(6) 0.3898(17) 0.023(4) Uiso 1 1 d . . . H24C H -0.0450(16) 0.2391(6) 0.4246(15) 0.016(4) Uiso 1 1 d . . . H25A H -0.2263(18) 0.1915(5) 0.1385(16) 0.017(4) Uiso 1 1 d . . . H25B H -0.0762(17) 0.2245(6) 0.1753(16) 0.024(4) Uiso 1 1 d . . . H25C H -0.0909(16) 0.1683(6) 0.1119(16) 0.015(4) Uiso 1 1 d . . . 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 Zr 0.01084(7) 0.00813(7) 0.00944(7) -0.00024(6) 0.00349(5) -0.00002(6) C1 0.0230(8) 0.0107(7) 0.0171(8) -0.0023(6) 0.0086(7) -0.0060(6) C2 0.0226(8) 0.0060(7) 0.0169(8) -0.0004(6) 0.0037(6) 0.0011(6) C3 0.0182(8) 0.0102(7) 0.0205(8) -0.0062(6) 0.0078(7) -0.0005(6) C4 0.0226(8) 0.0107(7) 0.0105(7) -0.0032(6) 0.0049(6) -0.0018(6) C5 0.0151(8) 0.0114(7) 0.0155(7) -0.0049(6) 0.0031(6) -0.0030(6) C6 0.0119(7) 0.0120(7) 0.0170(7) -0.0012(6) 0.0066(6) 0.0008(6) C7 0.0130(7) 0.0132(7) 0.0147(7) 0.0003(6) 0.0076(6) 0.0032(6) C8 0.0126(7) 0.0113(7) 0.0149(7) -0.0034(6) 0.0069(6) 0.0019(6) C9 0.0147(7) 0.0087(7) 0.0184(7) 0.0002(6) 0.0091(6) 0.0036(5) C10 0.0121(7) 0.0128(7) 0.0149(7) 0.0006(6) 0.0057(6) 0.0044(6) C11 0.0140(8) 0.0220(9) 0.0248(9) -0.0016(7) 0.0083(7) -0.0028(6) C12 0.0195(8) 0.0201(8) 0.0174(8) 0.0024(7) 0.0104(7) 0.0031(7) C13 0.0177(8) 0.0168(8) 0.0212(9) -0.0068(7) 0.0073(7) -0.0002(6) C14 0.0249(9) 0.0117(8) 0.0264(9) 0.0014(7) 0.0153(7) 0.0028(7) C15 0.0161(8) 0.0190(8) 0.0141(8) 0.0018(7) 0.0029(6) 0.0042(7) C16 0.0153(7) 0.0098(7) 0.0133(7) -0.0003(6) 0.0046(6) 0.0016(6) C17 0.0160(7) 0.0140(7) 0.0163(8) 0.0015(6) 0.0085(6) 0.0007(6) C18 0.0223(8) 0.0200(9) 0.0175(8) 0.0055(7) 0.0098(7) 0.0052(7) C19 0.0185(8) 0.0206(9) 0.0143(8) 0.0006(6) 0.0085(7) 0.0020(6) C20 0.0259(9) 0.0208(9) 0.0262(9) 0.0004(7) 0.0155(8) -0.0046(7) C21 0.0148(7) 0.0126(7) 0.0131(7) -0.0008(6) 0.0064(6) -0.0010(6) C22 0.0135(7) 0.0160(8) 0.0133(7) 0.0014(6) 0.0039(6) 0.0018(6) C23 0.0146(8) 0.0221(9) 0.0217(9) -0.0009(7) 0.0045(7) -0.0017(7) C24 0.0156(8) 0.0214(9) 0.0193(9) 0.0006(7) 0.0064(7) 0.0037(7) C25 0.0152(8) 0.0305(10) 0.0155(8) 0.0041(7) 0.0022(6) 0.0028(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 Zr Cent1 2.241(1) . yes Zr Cent2 2.260(1) . yes Zr Pln1 2.239(1) . yes Zr Pln2 2.260(1) . yes Zr C16 2.2651(14) . yes Zr C21 2.3524(14) . yes Zr C1 2.5024(14) . ? Zr C5 2.5266(14) . ? Zr C10 2.5503(13) . ? Zr C6 2.5531(14) . ? Zr C7 2.5473(14) . ? Zr C2 2.5488(14) . ? Zr C4 2.5519(14) . ? Zr C8 2.5736(13) . ? Zr C3 2.5691(14) . ? Zr C9 2.5845(13) . ? C1 C2 1.408(2) . ? C1 C5 1.412(2) . ? C1 H1 0.923(14) . ? C2 C3 1.398(2) . ? C2 H2 0.924(15) . ? C3 C4 1.413(2) . ? C3 H3 0.924(14) . ? C4 C5 1.397(2) . ? C4 H4 0.890(15) . ? C5 H5 0.907(15) . ? C6 C7 1.4145(19) . ? C6 C10 1.4202(19) . ? C6 C11 1.501(2) . ? C7 C8 1.4222(19) . ? C7 C12 1.501(2) . ? C8 C9 1.4130(19) . ? C8 C13 1.4973(19) . ? C9 C10 1.4215(19) . ? C9 C14 1.499(2) . ? C10 C15 1.504(2) . ? C11 H11A 0.955(17) . ? C11 H11B 0.926(18) . ? C11 H11C 0.939(17) . ? C12 H12A 0.947(17) . ? C12 H12B 0.959(17) . ? C12 H12C 0.904(19) . ? C13 H13A 0.925(18) . ? C13 H13B 0.953(16) . ? C13 H13C 0.959(17) . ? C14 H14A 0.988(17) . ? C14 H14B 0.920(17) . ? C14 H14C 0.937(17) . ? C15 H15A 0.947(19) . ? C15 H15B 0.84(2) . ? C15 H15C 0.91(2) . ? C16 C17 1.5401(19) . ? C16 H16A 0.944(15) . ? C16 H16B 0.933(16) . ? C17 C19 1.531(2) . ? C17 C18 1.531(2) . ? C17 C20 1.535(2) . ? C18 H18A 0.958(15) . ? C18 H18B 0.966(15) . ? C18 H18C 0.977(17) . ? C19 H19A 0.971(16) . ? C19 H19B 0.976(16) . ? C19 H19C 0.980(16) . ? C20 H20A 0.932(15) . ? C20 H20B 0.979(15) . ? C20 H20C 0.953(16) . ? C21 C22 1.5517(19) . ? C21 H21A 0.985(15) . ? C21 H21B 0.970(15) . ? C22 C25 1.534(2) . ? C22 C23 1.530(2) . ? C22 C24 1.528(2) . ? C23 H23A 0.966(16) . ? C23 H23B 0.984(16) . ? C23 H23C 0.932(15) . ? C24 H24A 0.939(16) . ? C24 H24B 0.968(16) . ? C24 H24C 0.954(15) . ? C25 H25A 0.977(15) . ? C25 H25B 0.981(16) . ? C25 H25C 0.972(16) . ? 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 Cent1 Zr Cent2 129.1(1) . . yes Pln1 Zr Pln2 126.7(1) . . yes C16 Zr C21 99.61(5) . . yes C16 Zr C1 134.09(5) . . ? C21 Zr C1 95.00(5) . . ? C16 Zr C5 113.92(5) . . ? C21 Zr C5 127.08(5) . . ? C1 Zr C5 32.60(5) . . ? C16 Zr C10 98.42(5) . . ? C21 Zr C10 132.32(5) . . ? C1 Zr C10 103.17(5) . . ? C5 Zr C10 83.19(5) . . ? C16 Zr C6 130.33(5) . . ? C21 Zr C6 112.00(5) . . ? C1 Zr C6 81.43(5) . . ? C5 Zr C6 76.21(5) . . ? C10 Zr C6 32.32(4) . . ? C16 Zr C7 130.63(5) . . ? C21 Zr C7 81.63(5) . . ? C1 Zr C7 94.37(5) . . ? C5 Zr C7 102.96(5) . . ? C10 Zr C7 53.64(4) . . ? C6 Zr C7 32.20(4) . . ? C16 Zr C2 110.27(5) . . ? C21 Zr C2 77.70(5) . . ? C1 Zr C2 32.35(5) . . ? C5 Zr C2 53.26(5) . . ? C10 Zr C2 134.42(5) . . ? C6 Zr C2 113.17(5) . . ? C7 Zr C2 118.01(5) . . ? C16 Zr C4 83.86(5) . . ? C21 Zr C4 127.46(5) . . ? C1 Zr C4 53.48(5) . . ? C5 Zr C4 31.93(5) . . ? C10 Zr C4 98.08(5) . . ? C6 Zr C4 103.89(5) . . ? C7 Zr C4 133.92(5) . . ? C2 Zr C4 52.94(5) . . ? C16 Zr C8 98.74(5) . . ? C21 Zr C8 80.54(5) . . ? C1 Zr C8 126.61(5) . . ? C5 Zr C8 129.18(5) . . ? C10 Zr C8 53.22(4) . . ? C6 Zr C8 53.05(4) . . ? C7 Zr C8 32.24(4) . . ? C2 Zr C8 146.08(5) . . ? C4 Zr C8 151.30(4) . . ? C16 Zr C3 81.95(5) . . ? C21 Zr C3 96.04(5) . . ? C1 Zr C3 53.24(5) . . ? C5 Zr C3 52.97(5) . . ? C10 Zr C3 130.08(4) . . ? C6 Zr C3 128.81(5) . . ? C7 Zr C3 147.37(5) . . ? C2 Zr C3 31.69(5) . . ? C4 Zr C3 32.03(4) . . ? C8 Zr C3 176.57(4) . . ? C16 Zr C9 81.21(5) . . ? C21 Zr C9 109.48(5) . . ? C1 Zr C9 133.39(5) . . ? C5 Zr C9 114.96(5) . . ? C10 Zr C9 32.13(4) . . ? C6 Zr C9 52.99(4) . . ? C7 Zr C9 53.16(4) . . ? C2 Zr C9 165.73(5) . . ? C4 Zr C9 122.74(5) . . ? C8 Zr C9 31.80(4) . . ? C3 Zr C9 151.38(5) . . ? C2 C1 C5 107.61(14) . . ? C2 C1 Zr 75.64(8) . . ? C5 C1 Zr 74.65(8) . . ? C2 C1 H1 126.8(9) . . ? C5 C1 H1 125.6(9) . . ? Zr C1 H1 115.5(9) . . ? C3 C2 C1 108.26(14) . . ? C3 C2 Zr 74.96(8) . . ? C1 C2 Zr 72.01(8) . . ? C3 C2 H2 125.8(10) . . ? C1 C2 H2 126.0(10) . . ? Zr C2 H2 119.3(10) . . ? C2 C3 C4 107.97(14) . . ? C2 C3 Zr 73.35(8) . . ? C4 C3 Zr 73.32(8) . . ? C2 C3 H3 124.5(9) . . ? C4 C3 H3 127.5(9) . . ? Zr C3 H3 120.1(9) . . ? C5 C4 C3 107.97(13) . . ? C5 C4 Zr 73.04(8) . . ? C3 C4 Zr 74.65(8) . . ? C5 C4 H4 126.1(9) . . ? C3 C4 H4 125.9(9) . . ? Zr C4 H4 120.1(9) . . ? C4 C5 C1 108.16(13) . . ? C4 C5 Zr 75.03(8) . . ? C1 C5 Zr 72.76(8) . . ? C4 C5 H5 128.9(9) . . ? C1 C5 H5 122.9(9) . . ? Zr C5 H5 119.9(9) . . ? C7 C6 C10 108.45(12) . . ? C7 C6 C11 124.35(13) . . ? C10 C6 C11 126.35(13) . . ? C7 C6 Zr 73.67(8) . . ? C10 C6 Zr 73.73(8) . . ? C11 C6 Zr 126.90(10) . . ? C6 C7 C8 107.64(12) . . ? C6 C7 C12 124.89(13) . . ? C8 C7 C12 127.19(13) . . ? C6 C7 Zr 74.12(8) . . ? C8 C7 Zr 74.90(8) . . ? C12 C7 Zr 121.60(10) . . ? C9 C8 C7 108.19(12) . . ? C9 C8 C13 123.93(13) . . ? C7 C8 C13 127.37(13) . . ? C9 C8 Zr 74.53(8) . . ? C7 C8 Zr 72.86(8) . . ? C13 C8 Zr 124.98(9) . . ? C8 C9 C10 108.15(12) . . ? C8 C9 C14 123.76(13) . . ? C10 C9 C14 127.23(13) . . ? C8 C9 Zr 73.68(8) . . ? C10 C9 Zr 72.61(8) . . ? C14 C9 Zr 127.91(10) . . ? C9 C10 C6 107.52(12) . . ? C9 C10 C15 125.80(13) . . ? C6 C10 C15 126.25(13) . . ? C9 C10 Zr 75.26(8) . . ? C6 C10 Zr 73.95(8) . . ? C15 C10 Zr 122.45(10) . . ? C6 C11 H11A 109.3(10) . . ? C6 C11 H11B 114.8(10) . . ? H11A C11 H11B 106.8(14) . . ? C6 C11 H11C 111.6(10) . . ? H11A C11 H11C 108.0(13) . . ? H11B C11 H11C 106.0(14) . . ? C7 C12 H12A 110.2(10) . . ? C7 C12 H12B 112.4(10) . . ? H12A C12 H12B 107.8(14) . . ? C7 C12 H12C 113.0(11) . . ? H12A C12 H12C 108.1(15) . . ? H12B C12 H12C 105.1(14) . . ? C8 C13 H13A 110.7(10) . . ? C8 C13 H13B 111.7(9) . . ? H13A C13 H13B 106.2(14) . . ? C8 C13 H13C 113.2(10) . . ? H13A C13 H13C 105.1(14) . . ? H13B C13 H13C 109.5(13) . . ? C9 C14 H14A 109.2(9) . . ? C9 C14 H14B 112.6(10) . . ? H14A C14 H14B 109.3(14) . . ? C9 C14 H14C 114.4(10) . . ? H14A C14 H14C 105.8(14) . . ? H14B C14 H14C 105.2(14) . . ? C10 C15 H15A 112.6(11) . . ? C10 C15 H15B 113.1(13) . . ? H15A C15 H15B 105.5(16) . . ? C10 C15 H15C 114.2(12) . . ? H15A C15 H15C 103.2(15) . . ? H15B C15 H15C 107.3(17) . . ? C17 C16 Zr 143.89(10) . . ? C17 C16 H16A 108.5(9) . . ? Zr C16 H16A 98.7(9) . . ? C17 C16 H16B 108.9(10) . . ? Zr C16 H16B 85.7(10) . . ? H16A C16 H16B 104.9(13) . . ? C19 C17 C18 108.47(12) . . ? C19 C17 C16 111.88(12) . . ? C18 C17 C16 111.32(12) . . ? C19 C17 C20 107.83(12) . . ? C18 C17 C20 107.92(13) . . ? C16 C17 C20 109.27(12) . . ? C17 C18 H18A 110.3(9) . . ? C17 C18 H18B 112.1(9) . . ? H18A C18 H18B 108.9(12) . . ? C17 C18 H18C 109.0(9) . . ? H18A C18 H18C 108.8(12) . . ? H18B C18 H18C 107.8(12) . . ? C17 C19 H19A 111.2(9) . . ? C17 C19 H19B 112.6(9) . . ? H19A C19 H19B 108.0(12) . . ? C17 C19 H19C 113.8(9) . . ? H19A C19 H19C 102.6(13) . . ? H19B C19 H19C 108.0(12) . . ? C17 C20 H20A 110.7(9) . . ? C17 C20 H20B 112.2(8) . . ? H20A C20 H20B 107.4(13) . . ? C17 C20 H20C 111.4(9) . . ? H20A C20 H20C 107.4(13) . . ? H20B C20 H20C 107.5(13) . . ? C22 C21 Zr 131.47(10) . . ? C22 C21 H21A 103.6(9) . . ? Zr C21 H21A 104.2(9) . . ? C22 C21 H21B 107.9(8) . . ? Zr C21 H21B 100.9(8) . . ? H21A C21 H21B 107.0(12) . . ? C25 C22 C23 107.71(12) . . ? C25 C22 C24 107.39(12) . . ? C23 C22 C24 109.31(13) . . ? C25 C22 C21 109.06(12) . . ? C23 C22 C21 110.11(12) . . ? C24 C22 C21 113.08(12) . . ? C22 C23 H23A 109.9(9) . . ? C22 C23 H23B 113.1(9) . . ? H23A C23 H23B 105.9(13) . . ? C22 C23 H23C 111.4(9) . . ? H23A C23 H23C 108.1(13) . . ? H23B C23 H23C 108.2(13) . . ? C22 C24 H24A 112.3(9) . . ? C22 C24 H24B 110.3(9) . . ? H24A C24 H24B 105.8(13) . . ? C22 C24 H24C 109.9(9) . . ? H24A C24 H24C 109.7(12) . . ? H24B C24 H24C 108.7(13) . . ? C22 C25 H25A 109.7(9) . . ? C22 C25 H25B 110.8(9) . . ? H25A C25 H25B 108.3(12) . . ? C22 C25 H25C 111.9(9) . . ? H25A C25 H25C 108.4(12) . . ? H25B C25 H25C 107.6(13) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.473 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.055