data_renophet _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 F6 N4 O5 P Re' _chemical_formula_weight 747.56 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' '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' 'Re' 'Re' -1.0185 7.2310 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 17.139(8) _cell_length_b 11.904(6) _cell_length_c 12.566(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.43(8) _cell_angle_gamma 90.00 _cell_volume 2418(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 5.182 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2310 _exptl_absorpt_correction_T_max 0.4238 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 4576 _diffrn_reflns_av_R_equivalents 0.0118 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4229 _reflns_number_gt 3020 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0812P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4229 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _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 Re1 Re 0.239293(18) 0.06707(2) 0.37264(2) 0.01625(11) Uani 1 1 d . . . P1 P 0.69440(14) 0.05233(17) 0.11019(18) 0.0271(5) Uani 1 1 d . . . F1 F 0.6417(4) 0.1611(5) 0.0625(6) 0.074(2) Uani 1 1 d . . . F2 F 0.7018(5) 0.0272(7) -0.0100(5) 0.078(2) Uani 1 1 d . . . F3 F 0.7777(3) 0.1273(4) 0.1425(4) 0.0323(12) Uani 1 1 d . . . F4 F 0.7496(4) -0.0550(4) 0.1614(6) 0.0549(16) Uani 1 1 d . . . F5 F 0.6884(3) 0.0775(5) 0.2313(4) 0.0446(14) Uani 1 1 d . . . F6 F 0.6129(3) -0.0224(5) 0.0785(5) 0.0438(13) Uani 1 1 d . . . N1 N 0.3365(4) 0.1331(5) 0.5215(5) 0.0181(13) Uani 1 1 d . . . N2 N 0.1602(4) 0.1601(5) 0.4461(5) 0.0188(14) Uani 1 1 d . . . N3 N 0.2087(4) -0.0536(5) 0.4811(5) 0.0193(14) Uani 1 1 d . . . N4 N 0.0505(4) -0.0957(6) 0.7444(6) 0.0286(16) Uani 1 1 d . . . O1 O 0.2649(3) 0.2454(4) 0.2107(5) 0.0290(13) Uani 1 1 d . . . O2 O 0.3613(4) -0.0811(5) 0.3049(6) 0.0404(16) Uani 1 1 d . . . O3 O 0.1078(4) -0.0358(5) 0.1667(5) 0.0368(15) Uani 1 1 d . . . O4 O 0.0313(4) -0.1950(5) 0.7241(5) 0.0395(15) Uani 1 1 d . . . O5 O 0.0488(4) -0.0470(5) 0.8288(5) 0.0412(16) Uani 1 1 d . . . C1 C 0.2558(5) 0.1811(6) 0.2738(6) 0.0222(17) Uani 1 1 d . . . C2 C 0.3165(5) -0.0262(7) 0.3304(7) 0.0270(18) Uani 1 1 d . . . C3 C 0.1550(5) 0.0057(6) 0.2450(7) 0.0250(18) Uani 1 1 d . . . C4 C 0.3609(5) 0.2417(6) 0.5288(7) 0.0262(18) Uani 1 1 d . . . H4 H 0.3314 0.2908 0.4694 0.031 Uiso 1 1 calc R . . C5 C 0.4243(5) 0.2859(6) 0.6147(7) 0.0270(18) Uani 1 1 d . . . H5 H 0.4385 0.3629 0.6131 0.032 Uiso 1 1 calc R . . C6 C 0.4684(5) 0.2188(7) 0.7045(7) 0.0235(18) Uani 1 1 d . . . C7 C 0.4423(5) 0.1076(7) 0.7011(7) 0.0272(19) Uani 1 1 d . . . H7 H 0.4686 0.0586 0.7621 0.033 Uiso 1 1 calc R . . C8 C 0.3784(5) 0.0685(7) 0.6099(7) 0.0272(17) Uani 1 1 d . . . H8 H 0.3630 -0.0082 0.6093 0.033 Uiso 1 1 calc R . . C9 C 0.5368(5) 0.2649(7) 0.8023(7) 0.0279(19) Uani 1 1 d . . . H9A H 0.5668 0.3232 0.7751 0.034 Uiso 1 1 calc R . . H9B H 0.5764 0.2040 0.8371 0.034 Uiso 1 1 calc R . . C10 C 0.5052(6) 0.3152(9) 0.8900(8) 0.042(2) Uani 1 1 d . . . H10A H 0.4680 0.3778 0.8567 0.063 Uiso 1 1 calc R . . H10B H 0.5520 0.3428 0.9534 0.063 Uiso 1 1 calc R . . H10C H 0.4752 0.2579 0.9168 0.063 Uiso 1 1 calc R . . C11 C 0.1406(4) 0.2701(6) 0.4334(6) 0.0200(16) Uani 1 1 d . . . H11 H 0.1607 0.3140 0.3849 0.024 Uiso 1 1 calc R . . C12 C 0.0924(5) 0.3213(6) 0.4881(7) 0.0263(18) Uani 1 1 d . . . H12 H 0.0800 0.3991 0.4765 0.032 Uiso 1 1 calc R . . C13 C 0.0624(5) 0.2616(7) 0.5582(7) 0.0258(18) Uani 1 1 d . . . H13 H 0.0280 0.2965 0.5942 0.031 Uiso 1 1 calc R . . C14 C 0.0830(4) 0.1482(6) 0.5764(6) 0.0193(16) Uani 1 1 d . . . C15 C 0.1329(5) 0.1004(6) 0.5202(6) 0.0174(16) Uani 1 1 d . . . C16 C 0.1560(4) -0.0149(6) 0.5374(6) 0.0166(15) Uani 1 1 d . . . C17 C 0.1284(4) -0.0853(6) 0.6065(6) 0.0194(16) Uani 1 1 d . . . C18 C 0.0789(4) -0.0314(6) 0.6644(6) 0.0170(16) Uani 1 1 d . . . C19 C 0.0575(5) 0.0775(7) 0.6519(6) 0.0230(17) Uani 1 1 d . . . H19 H 0.0252 0.1083 0.6932 0.028 Uiso 1 1 calc R . . C20 C 0.2317(5) -0.1613(6) 0.4947(7) 0.0227(17) Uani 1 1 d . . . H20 H 0.2684 -0.1882 0.4581 0.027 Uiso 1 1 calc R . . C21 C 0.2044(5) -0.2359(6) 0.5599(7) 0.0266(18) Uani 1 1 d . . . H21 H 0.2214 -0.3123 0.5660 0.032 Uiso 1 1 calc R . . C22 C 0.1527(5) -0.1981(6) 0.6153(6) 0.0243(17) Uani 1 1 d . . . H22 H 0.1334 -0.2485 0.6597 0.029 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 Re1 0.01902(16) 0.01480(16) 0.01822(16) 0.00012(14) 0.01059(11) 0.00020(14) P1 0.0332(12) 0.0222(11) 0.0237(11) 0.0017(9) 0.0067(9) -0.0038(9) F1 0.056(4) 0.033(3) 0.102(6) 0.027(3) -0.017(4) 0.002(3) F2 0.100(6) 0.108(6) 0.036(4) -0.024(4) 0.035(4) -0.060(5) F3 0.039(3) 0.028(3) 0.029(3) 0.008(2) 0.011(2) -0.010(2) F4 0.047(3) 0.024(3) 0.100(5) 0.002(3) 0.032(3) 0.009(2) F5 0.044(3) 0.058(4) 0.040(3) -0.017(3) 0.025(3) -0.009(3) F6 0.039(3) 0.042(3) 0.051(3) -0.009(3) 0.016(3) -0.018(3) N1 0.020(3) 0.019(3) 0.020(3) 0.003(3) 0.013(3) -0.001(3) N2 0.026(4) 0.018(3) 0.016(3) -0.001(3) 0.012(3) 0.000(3) N3 0.029(3) 0.014(3) 0.018(3) -0.004(3) 0.011(3) 0.000(3) N4 0.027(4) 0.029(4) 0.031(4) -0.001(3) 0.011(3) -0.001(3) O1 0.036(3) 0.030(3) 0.021(3) 0.008(2) 0.011(3) -0.006(3) O2 0.042(4) 0.041(4) 0.047(4) -0.004(3) 0.026(3) 0.017(3) O3 0.039(4) 0.028(3) 0.036(4) -0.007(3) 0.002(3) -0.004(3) O4 0.048(4) 0.036(4) 0.041(4) -0.007(3) 0.023(3) -0.022(3) O5 0.057(4) 0.043(4) 0.038(4) -0.008(3) 0.036(3) -0.004(3) C1 0.020(4) 0.025(4) 0.021(4) -0.009(3) 0.006(3) -0.004(3) C2 0.029(5) 0.023(4) 0.028(5) 0.004(4) 0.010(4) 0.001(4) C3 0.022(4) 0.021(4) 0.034(5) 0.006(4) 0.012(4) 0.002(3) C4 0.029(4) 0.021(4) 0.029(5) 0.001(3) 0.009(4) 0.001(4) C5 0.036(5) 0.016(4) 0.027(4) -0.002(3) 0.008(4) -0.001(3) C6 0.020(4) 0.032(5) 0.028(4) -0.005(4) 0.021(4) -0.003(3) C7 0.030(5) 0.031(4) 0.017(4) 0.012(4) 0.003(4) 0.005(4) C8 0.027(4) 0.025(4) 0.031(4) 0.002(4) 0.012(4) -0.003(4) C9 0.021(4) 0.036(5) 0.026(5) 0.001(4) 0.006(3) 0.001(4) C10 0.041(5) 0.059(6) 0.029(5) -0.007(5) 0.016(4) -0.002(5) C11 0.019(4) 0.014(4) 0.020(4) 0.007(3) -0.003(3) 0.005(3) C12 0.034(5) 0.019(4) 0.030(5) 0.001(3) 0.016(4) 0.003(3) C13 0.025(4) 0.027(4) 0.028(5) -0.005(3) 0.013(3) 0.014(4) C14 0.014(4) 0.023(4) 0.018(4) -0.006(3) 0.001(3) -0.003(3) C15 0.020(4) 0.015(4) 0.020(4) -0.007(3) 0.009(3) -0.005(3) C16 0.015(4) 0.019(4) 0.019(4) -0.006(3) 0.009(3) -0.006(3) C17 0.018(4) 0.022(4) 0.021(4) -0.004(3) 0.009(3) -0.004(3) C18 0.017(4) 0.018(4) 0.021(4) -0.001(3) 0.013(3) -0.007(3) C19 0.017(4) 0.033(5) 0.021(4) -0.003(4) 0.009(3) 0.000(3) C20 0.029(4) 0.016(4) 0.024(4) -0.003(3) 0.011(4) 0.006(3) C21 0.046(5) 0.007(3) 0.031(5) -0.008(3) 0.018(4) -0.005(3) C22 0.037(5) 0.017(4) 0.026(4) 0.001(3) 0.019(4) -0.009(4) _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 Re1 C3 1.912(9) . ? Re1 C1 1.924(8) . ? Re1 C2 1.932(9) . ? Re1 N3 2.161(6) . ? Re1 N2 2.180(6) . ? Re1 N1 2.196(7) . ? P1 F1 1.578(6) . ? P1 F2 1.585(6) . ? P1 F5 1.588(5) . ? P1 F6 1.590(5) . ? P1 F4 1.593(6) . ? P1 F3 1.617(5) . ? N1 C8 1.344(10) . ? N1 C4 1.353(9) . ? N2 C11 1.348(9) . ? N2 C15 1.371(9) . ? N3 C20 1.335(9) . ? N3 C16 1.399(9) . ? N4 O5 1.218(9) . ? N4 O4 1.231(8) . ? N4 C18 1.469(10) . ? O1 C1 1.148(9) . ? O2 C2 1.132(10) . ? O3 C3 1.156(10) . ? C4 C5 1.358(11) . ? C4 H4 0.9500 . ? C5 C6 1.384(11) . ? C5 H5 0.9500 . ? C6 C7 1.393(11) . ? C6 C9 1.493(11) . ? C7 C8 1.376(12) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.504(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.380(11) . ? C11 H11 0.9500 . ? C12 C13 1.359(11) . ? C12 H12 0.9500 . ? C13 C14 1.395(10) . ? C13 H13 0.9500 . ? C14 C15 1.398(10) . ? C14 C19 1.440(10) . ? C15 C16 1.426(10) . ? C16 C17 1.398(10) . ? C17 C22 1.399(10) . ? C17 C18 1.440(10) . ? C18 C19 1.342(10) . ? C19 H19 0.9500 . ? C20 C21 1.390(11) . ? C20 H20 0.9500 . ? C21 C22 1.373(11) . ? C21 H21 0.9500 . ? C22 H22 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 C3 Re1 C1 87.7(3) . . ? C3 Re1 C2 86.9(3) . . ? C1 Re1 C2 88.1(3) . . ? C3 Re1 N3 90.1(3) . . ? C1 Re1 N3 174.3(3) . . ? C2 Re1 N3 97.1(3) . . ? C3 Re1 N2 98.4(3) . . ? C1 Re1 N2 99.3(3) . . ? C2 Re1 N2 171.1(3) . . ? N3 Re1 N2 75.8(2) . . ? C3 Re1 N1 178.4(3) . . ? C1 Re1 N1 93.7(3) . . ? C2 Re1 N1 92.6(3) . . ? N3 Re1 N1 88.6(2) . . ? N2 Re1 N1 81.9(2) . . ? F1 P1 F2 90.6(4) . . ? F1 P1 F5 89.9(4) . . ? F2 P1 F5 179.2(4) . . ? F1 P1 F6 91.2(3) . . ? F2 P1 F6 89.9(3) . . ? F5 P1 F6 90.8(3) . . ? F1 P1 F4 178.1(4) . . ? F2 P1 F4 90.5(4) . . ? F5 P1 F4 89.1(4) . . ? F6 P1 F4 90.4(3) . . ? F1 P1 F3 89.3(3) . . ? F2 P1 F3 89.9(3) . . ? F5 P1 F3 89.4(3) . . ? F6 P1 F3 179.5(3) . . ? F4 P1 F3 89.1(3) . . ? C8 N1 C4 115.0(7) . . ? C8 N1 Re1 123.0(5) . . ? C4 N1 Re1 121.9(5) . . ? C11 N2 C15 117.1(6) . . ? C11 N2 Re1 127.5(5) . . ? C15 N2 Re1 115.2(5) . . ? C20 N3 C16 117.6(6) . . ? C20 N3 Re1 126.6(5) . . ? C16 N3 Re1 115.7(5) . . ? O5 N4 O4 123.7(7) . . ? O5 N4 C18 117.2(7) . . ? O4 N4 C18 119.1(7) . . ? O1 C1 Re1 176.7(6) . . ? O2 C2 Re1 179.5(9) . . ? O3 C3 Re1 175.7(7) . . ? N1 C4 C5 124.8(8) . . ? N1 C4 H4 117.6 . . ? C5 C4 H4 117.6 . . ? C4 C5 C6 120.0(7) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 116.2(7) . . ? C5 C6 C9 121.7(7) . . ? C7 C6 C9 122.1(7) . . ? C8 C7 C6 120.3(7) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N1 C8 C7 123.6(8) . . ? N1 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? C6 C9 C10 112.0(7) . . ? C6 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C6 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 122.5(7) . . ? N2 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 120.7(7) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 118.9(7) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C15 118.4(7) . . ? C13 C14 C19 123.9(7) . . ? C15 C14 C19 117.7(7) . . ? N2 C15 C14 122.4(7) . . ? N2 C15 C16 117.5(6) . . ? C14 C15 C16 120.1(7) . . ? C17 C16 N3 121.8(7) . . ? C17 C16 C15 122.5(7) . . ? N3 C16 C15 115.7(6) . . ? C16 C17 C22 118.1(7) . . ? C16 C17 C18 115.1(6) . . ? C22 C17 C18 126.7(7) . . ? C19 C18 C17 123.7(7) . . ? C19 C18 N4 116.4(7) . . ? C17 C18 N4 119.9(6) . . ? C18 C19 C14 120.7(7) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? N3 C20 C21 123.2(7) . . ? N3 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C22 C21 C20 119.3(7) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C17 120.0(7) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.590 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.154