# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2145 data_Complex2a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H56 N2 O2 P4 Re' _chemical_formula_weight 1099.22 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.5980 7.2320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0020 0.0020 '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' 'O' 'O' 0.0080 0.0060 '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 10.185(6) _cell_length_b 18.738(6) _cell_length_c 13.507(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.80(4) _cell_angle_gamma 90.00 _cell_volume 2454.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method ? _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 2.511 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4493 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.1863 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4298 _reflns_number_observed 1752 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1409P)^2^+91.8115P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4298 _refine_ls_number_parameters 285 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.2710 _refine_ls_R_factor_obs 0.1391 _refine_ls_wR_factor_all 0.4059 _refine_ls_wR_factor_obs 0.2992 _refine_ls_goodness_of_fit_all 1.085 _refine_ls_goodness_of_fit_obs 1.271 _refine_ls_restrained_S_all 1.071 _refine_ls_restrained_S_obs 1.221 _refine_ls_shift/esd_max 0.119 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.0000 0.0000 0.0000 0.0679(8) Uani 1 d S . P1 P -0.0472(7) -0.0099(4) 0.1672(9) 0.079(3) Uani 1 d . . P2 P -0.2136(7) -0.0669(4) -0.0592(8) 0.068(3) Uani 1 d . . C21 C -0.2081(31) -0.1672(14) -0.0678(28) 0.071(9) Uani 1 d U . C11 C 0.0595(30) -0.0542(11) 0.2849(27) 0.065(9) Uani 1 d U . C224 C -0.5344(34) -0.0050(21) -0.3733(29) 0.084(10) Uani 1 d U . H224 H -0.5883(34) 0.0121(21) -0.4375(29) 0.100 Uiso 1 calc R . C226 C -0.4175(30) 0.0174(13) -0.1930(26) 0.066(9) Uani 1 d U . H226 H -0.4004(30) 0.0474(13) -0.1356(26) 0.080 Uiso 1 calc R . C213 C -0.1183(32) -0.2756(15) -0.1104(27) 0.070(9) Uani 1 d U . H213 H -0.0483(32) -0.2996(15) -0.1275(27) 0.084 Uiso 1 calc R . C212 C -0.1069(29) -0.2007(15) -0.0977(24) 0.061(8) Uani 1 d U . H212 H -0.0342(29) -0.1755(15) -0.1092(24) 0.074 Uiso 1 calc R . C214 C -0.2186(31) -0.3120(16) -0.0999(27) 0.073(9) Uani 1 d U . H214 H -0.2201(31) -0.3609(16) -0.1117(27) 0.088 Uiso 1 calc R . C215 C -0.3234(37) -0.2822(18) -0.0720(30) 0.086(11) Uani 1 d U . H215 H -0.3958(37) -0.3095(18) -0.0641(30) 0.103 Uiso 1 calc R . C222 C -0.3687(31) -0.0928(18) -0.2721(29) 0.075(9) Uani 1 d U . H222 H -0.3212(31) -0.1356(18) -0.2688(29) 0.089 Uiso 1 calc R . C22 C -0.3426(25) -0.0473(15) -0.1874(27) 0.067(9) Uani 1 d U . C216 C -0.3171(28) -0.2076(16) -0.0556(27) 0.073(9) Uani 1 d U . H216 H -0.3869(28) -0.1851(16) -0.0364(27) 0.087 Uiso 1 calc R . C223 C -0.4720(36) -0.0707(19) -0.3647(31) 0.087(11) Uani 1 d U . H223 H -0.4979(36) -0.1018(19) -0.4210(31) 0.104 Uiso 1 calc R . C116 C 0.1579(31) -0.1010(18) 0.2683(28) 0.079(10) Uani 1 d U . H116 H 0.1700(31) -0.1078(18) 0.2034(28) 0.095 Uiso 1 calc R . C112 C 0.0320(38) -0.0441(19) 0.3815(29) 0.084(11) Uani 1 d U . H112 H -0.0359(38) -0.0138(19) 0.3903(29) 0.101 Uiso 1 calc R . C114 C 0.2160(33) -0.1319(18) 0.4515(26) 0.074(10) Uani 1 d U . H114 H 0.2654(33) -0.1590(18) 0.5084(26) 0.088 Uiso 1 calc R . C115 C 0.2367(33) -0.1368(19) 0.3585(29) 0.079(10) Uani 1 d U . H115 H 0.3081(33) -0.1660(19) 0.3531(29) 0.095 Uiso 1 calc R . C113 C 0.1143(43) -0.0829(22) 0.4567(38) 0.108(13) Uani 1 d U . H113 H 0.1032(43) -0.0770(22) 0.5220(38) 0.130 Uiso 1 calc R . C225 C -0.5150(35) 0.0346(20) -0.2842(32) 0.085(11) Uani 1 d U . H225 H -0.5702(35) 0.0745(20) -0.2863(32) 0.102 Uiso 1 calc R . C126 C 0.0226(36) 0.1111(18) 0.2825(29) 0.082(10) Uani 1 d U . H126 H 0.1119(36) 0.0937(18) 0.2958(29) 0.099 Uiso 1 calc R . C125 C -0.0034(43) 0.1763(19) 0.3200(31) 0.097(12) Uani 1 d U . H125 H 0.0703(43) 0.2053(19) 0.3552(31) 0.117 Uiso 1 calc R . C12 C -0.0903(29) 0.0731(14) 0.2241(28) 0.068(9) Uani 1 d U . C122 C -0.2247(36) 0.0944(18) 0.2008(28) 0.079(10) Uani 1 d U . H122 H -0.2957(36) 0.0667(18) 0.1587(28) 0.095 Uiso 1 calc R . C123 C -0.2520(39) 0.1582(19) 0.2415(33) 0.095(12) Uani 1 d U . H123 H -0.3428(39) 0.1735(19) 0.2265(33) 0.114 Uiso 1 calc R . C124 C -0.1444(43) 0.2012(21) 0.3059(32) 0.099(12) Uani 1 d U . H124 H -0.1626(43) 0.2427(21) 0.3372(32) 0.119 Uiso 1 calc R . C1 C -0.1329(32) 0.0882(15) -0.0256(22) 0.055(8) Uani 1 d U . N1 N -0.2082(28) 0.1374(12) -0.0359(27) 0.096(11) Uani 1 d . . C2 C -0.2101(27) -0.0616(14) 0.1458(24) 0.057(8) Uani 1 d U . H2A H -0.1895(27) -0.1120(14) 0.1577(24) 0.069 Uiso 1 calc R . H2B H -0.2579(27) -0.0457(14) 0.1939(24) 0.069 Uiso 1 calc R . C3 C -0.3010(34) -0.0495(18) 0.0336(26) 0.077(10) Uani 1 d U . H3A H -0.3330(34) -0.0004(18) 0.0261(26) 0.092 Uiso 1 calc R . H3B H -0.3813(34) -0.0802(18) 0.0194(26) 0.092 Uiso 1 calc R . O O 0.5650(37) 0.2207(21) -0.0380(30) 0.165(14) Uiso 1 d . . H H 0.5614(37) 0.1804(21) -0.0154(30) 0.198 Uiso 1 calc R . CM C 0.5050(44) 0.2208(24) -0.1461(34) 0.120(15) Uiso 1 d . . HMA H 0.4496(44) 0.1787(24) -0.1668(34) 0.144 Uiso 1 calc R . HMB H 0.5762(44) 0.2213(24) -0.1791(34) 0.144 Uiso 1 calc R . HMC H 0.4481(44) 0.2624(24) -0.1665(34) 0.144 Uiso 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 Re 0.0309(7) 0.0243(7) 0.135(2) -0.0010(12) 0.0056(8) 0.0004(8) P1 0.036(3) 0.041(4) 0.158(9) -0.003(5) 0.027(4) -0.002(3) P2 0.034(4) 0.037(4) 0.118(8) -0.001(4) 0.003(4) 0.005(3) C21 0.064(16) 0.032(13) 0.099(22) 0.003(14) 0.000(15) 0.002(13) C11 0.076(16) 0.006(9) 0.087(21) 0.006(12) -0.013(15) 0.016(10) C224 0.084(18) 0.093(20) 0.070(20) 0.004(19) 0.018(15) 0.016(19) C226 0.065(16) 0.037(15) 0.081(20) -0.016(13) -0.002(14) -0.008(11) C213 0.066(16) 0.044(14) 0.101(22) -0.016(15) 0.026(15) 0.004(13) C212 0.056(15) 0.051(15) 0.082(20) -0.023(14) 0.029(14) -0.003(12) C214 0.058(16) 0.045(14) 0.102(22) -0.001(15) 0.004(15) -0.019(13) C215 0.079(19) 0.062(17) 0.119(24) -0.008(17) 0.034(18) -0.021(15) C222 0.058(16) 0.063(17) 0.099(22) -0.004(17) 0.020(16) -0.006(14) C22 0.027(12) 0.055(15) 0.102(22) 0.012(15) -0.003(13) 0.004(11) C216 0.036(13) 0.066(17) 0.108(22) -0.001(16) 0.009(14) -0.014(13) C223 0.086(20) 0.069(18) 0.099(23) -0.011(17) 0.019(18) -0.005(16) C116 0.063(17) 0.084(19) 0.074(20) 0.006(17) -0.003(15) -0.007(15) C112 0.095(20) 0.074(18) 0.074(21) 0.044(17) 0.010(17) -0.032(16) C114 0.075(18) 0.081(19) 0.043(18) 0.013(16) -0.016(14) 0.010(16) C115 0.070(18) 0.088(20) 0.063(20) 0.013(17) -0.005(16) -0.008(16) C113 0.107(23) 0.087(22) 0.121(26) -0.003(20) 0.021(20) -0.013(19) C225 0.069(18) 0.079(19) 0.102(24) 0.017(18) 0.020(17) 0.019(15) C126 0.072(18) 0.072(19) 0.112(24) -0.010(18) 0.042(17) -0.002(15) C125 0.116(23) 0.060(18) 0.103(24) -0.021(17) 0.014(19) -0.009(17) C12 0.050(15) 0.035(13) 0.114(22) 0.006(14) 0.017(15) -0.018(12) C122 0.081(19) 0.065(18) 0.084(21) -0.007(16) 0.013(16) -0.008(15) C123 0.082(20) 0.074(19) 0.132(26) -0.025(19) 0.039(19) 0.017(16) C124 0.116(23) 0.076(20) 0.106(24) -0.007(19) 0.037(20) 0.015(19) C1 0.083(18) 0.053(15) 0.043(17) 0.006(13) 0.037(14) -0.001(14) N1 0.072(18) 0.024(12) 0.169(32) 0.015(16) 0.004(18) 0.011(12) C2 0.063(15) 0.034(13) 0.075(19) 0.003(13) 0.023(14) 0.009(12) C3 0.082(19) 0.072(18) 0.075(21) 0.000(16) 0.020(16) -0.006(16) _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 Re C1 2.10(3) . ? Re C1 2.10(3) 3 ? Re P2 2.425(7) . ? Re P2 2.425(7) 3 ? Re P1 2.456(11) 3 ? Re P1 2.456(11) . ? P1 C11 1.83(3) . ? P1 C12 1.85(3) . ? P1 C2 1.86(3) . ? P2 C3 1.78(3) . ? P2 C22 1.86(3) . ? P2 C21 1.89(3) . ? C21 C212 1.37(4) . ? C21 C216 1.39(4) . ? C11 C116 1.40(4) . ? C11 C112 1.43(5) . ? C224 C223 1.37(4) . ? C224 C225 1.38(5) . ? C226 C225 1.36(4) . ? C226 C22 1.42(4) . ? C213 C214 1.27(4) . ? C213 C212 1.41(4) . ? C214 C215 1.36(4) . ? C215 C216 1.41(4) . ? C222 C22 1.39(4) . ? C222 C223 1.43(5) . ? C116 C115 1.41(4) . ? C112 C113 1.32(5) . ? C114 C115 1.34(4) . ? C114 C113 1.40(5) . ? C126 C125 1.38(4) . ? C126 C12 1.38(4) . ? C125 C124 1.47(5) . ? C12 C122 1.37(4) . ? C122 C123 1.38(4) . ? C123 C124 1.42(5) . ? C1 N1 1.18(3) . ? C2 C3 1.53(4) . ? O CM 1.40(5) . ? 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 C1 Re C1 180.000(2) . 3 ? C1 Re P2 83.3(8) . . ? C1 Re P2 96.7(8) 3 . ? C1 Re P2 96.7(8) . 3 ? C1 Re P2 83.3(8) 3 3 ? P2 Re P2 180.0 . 3 ? C1 Re P1 95.0(8) . 3 ? C1 Re P1 85.0(8) 3 3 ? P2 Re P1 98.3(3) . 3 ? P2 Re P1 81.7(3) 3 3 ? C1 Re P1 85.0(8) . . ? C1 Re P1 95.0(8) 3 . ? P2 Re P1 81.7(3) . . ? P2 Re P1 98.3(3) 3 . ? P1 Re P1 180.0 3 . ? C11 P1 C12 100.0(15) . . ? C11 P1 C2 99.4(14) . . ? C12 P1 C2 100.8(12) . . ? C11 P1 Re 127.1(12) . . ? C12 P1 Re 117.2(11) . . ? C2 P1 Re 108.2(11) . . ? C3 P2 C22 104.9(15) . . ? C3 P2 C21 104.9(17) . . ? C22 P2 C21 99.5(14) . . ? C3 P2 Re 105.4(11) . . ? C22 P2 Re 120.8(10) . . ? C21 P2 Re 119.7(10) . . ? C212 C21 C216 119.0(27) . . ? C212 C21 P2 120.9(24) . . ? C216 C21 P2 119.6(25) . . ? C116 C11 C112 125.4(30) . . ? C116 C11 P1 114.1(28) . . ? C112 C11 P1 120.3(23) . . ? C223 C224 C225 118.1(35) . . ? C225 C226 C22 118.7(31) . . ? C214 C213 C212 123.9(31) . . ? C21 C212 C213 116.7(28) . . ? C213 C214 C215 122.5(31) . . ? C214 C215 C216 116.7(31) . . ? C22 C222 C223 116.6(31) . . ? C222 C22 C226 121.1(28) . . ? C222 C22 P2 123.3(23) . . ? C226 C22 P2 115.6(25) . . ? C21 C216 C215 121.1(32) . . ? C224 C223 C222 122.2(35) . . ? C115 C116 C11 114.0(35) . . ? C113 C112 C11 112.0(42) . . ? C115 C114 C113 115.0(33) . . ? C114 C115 C116 124.6(36) . . ? C112 C113 C114 128.8(47) . . ? C226 C225 C224 122.2(33) . . ? C125 C126 C12 116.6(33) . . ? C126 C125 C124 121.6(35) . . ? C122 C12 C126 125.7(31) . . ? C122 C12 P1 119.9(24) . . ? C126 C12 P1 114.2(24) . . ? C12 C122 C123 118.1(33) . . ? C122 C123 C124 121.6(34) . . ? C123 C124 C125 116.2(33) . . ? N1 C1 Re 177.2(28) . . ? C3 C2 P1 108.4(21) . . ? C2 C3 P2 112.9(23) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Re P1 C11 -157.7(14) . . . . ? C1 Re P1 C11 22.3(14) 3 . . . ? P2 Re P1 C11 118.3(11) . . . . ? P2 Re P1 C11 -61.7(11) 3 . . . ? P1 Re P1 C11 -97.8(1000) 3 . . . ? C1 Re P1 C12 -28.4(13) . . . . ? C1 Re P1 C12 151.6(13) 3 . . . ? P2 Re P1 C12 -112.4(10) . . . . ? P2 Re P1 C12 67.6(10) 3 . . . ? P1 Re P1 C12 31.5(1000) 3 . . . ? C1 Re P1 C2 84.6(12) . . . . ? C1 Re P1 C2 -95.4(12) 3 . . . ? P2 Re P1 C2 0.7(9) . . . . ? P2 Re P1 C2 -179.3(9) 3 . . . ? P1 Re P1 C2 144.5(1000) 3 . . . ? C1 Re P2 C3 -63.0(14) . . . . ? C1 Re P2 C3 117.0(14) 3 . . . ? P2 Re P2 C3 -125.3(1000) 3 . . . ? P1 Re P2 C3 -157.0(12) 3 . . . ? P1 Re P2 C3 23.0(12) . . . . ? C1 Re P2 C22 55.3(15) . . . . ? C1 Re P2 C22 -124.7(15) 3 . . . ? P2 Re P2 C22 -7.1(1000) 3 . . . ? P1 Re P2 C22 -38.8(13) 3 . . . ? P1 Re P2 C22 141.2(13) . . . . ? C1 Re P2 C21 179.4(16) . . . . ? C1 Re P2 C21 -0.6(16) 3 . . . ? P2 Re P2 C21 117.0(1000) 3 . . . ? P1 Re P2 C21 85.3(14) 3 . . . ? P1 Re P2 C21 -94.7(14) . . . . ? C3 P2 C21 C212 -154.1(28) . . . . ? C22 P2 C21 C212 97.6(29) . . . . ? Re P2 C21 C212 -36.3(33) . . . . ? C3 P2 C21 C216 33.6(32) . . . . ? C22 P2 C21 C216 -74.7(31) . . . . ? Re P2 C21 C216 151.4(23) . . . . ? C12 P1 C11 C116 -152.4(22) . . . . ? C2 P1 C11 C116 104.7(24) . . . . ? Re P1 C11 C116 -16.7(26) . . . . ? C12 P1 C11 C112 32.6(25) . . . . ? C2 P1 C11 C112 -70.3(24) . . . . ? Re P1 C11 C112 168.2(19) . . . . ? C216 C21 C212 C213 -2.4(49) . . . . ? P2 C21 C212 C213 -174.7(25) . . . . ? C214 C213 C212 C21 3.0(54) . . . . ? C212 C213 C214 C215 -2.0(60) . . . . ? C213 C214 C215 C216 0.4(59) . . . . ? C223 C222 C22 C226 1.1(46) . . . . ? C223 C222 C22 P2 179.2(23) . . . . ? C225 C226 C22 C222 -0.9(48) . . . . ? C225 C226 C22 P2 -179.1(26) . . . . ? C3 P2 C22 C222 -132.3(28) . . . . ? C21 P2 C22 C222 -24.0(30) . . . . ? Re P2 C22 C222 109.2(25) . . . . ? C3 P2 C22 C226 45.9(26) . . . . ? C21 P2 C22 C226 154.2(24) . . . . ? Re P2 C22 C226 -72.6(25) . . . . ? C212 C21 C216 C215 1.0(53) . . . . ? P2 C21 C216 C215 173.5(28) . . . . ? C214 C215 C216 C21 0.0(57) . . . . ? C225 C224 C223 C222 -12.2(55) . . . . ? C22 C222 C223 C224 5.6(52) . . . . ? C112 C11 C116 C115 -3.1(45) . . . . ? P1 C11 C116 C115 -177.9(22) . . . . ? C116 C11 C112 C113 2.1(45) . . . . ? P1 C11 C112 C113 176.6(25) . . . . ? C113 C114 C115 C116 -4.8(52) . . . . ? C11 C116 C115 C114 4.6(48) . . . . ? C11 C112 C113 C114 -2.5(55) . . . . ? C115 C114 C113 C112 3.9(59) . . . . ? C22 C226 C225 C224 -6.0(53) . . . . ? C223 C224 C225 C226 12.4(56) . . . . ? C12 C126 C125 C124 4.9(58) . . . . ? C125 C126 C12 C122 -0.1(57) . . . . ? C125 C126 C12 P1 175.1(29) . . . . ? C11 P1 C12 C122 -128.7(29) . . . . ? C2 P1 C12 C122 -27.0(31) . . . . ? Re P1 C12 C122 90.1(28) . . . . ? C11 P1 C12 C126 55.8(29) . . . . ? C2 P1 C12 C126 157.5(27) . . . . ? Re P1 C12 C126 -85.4(27) . . . . ? C126 C12 C122 C123 -2.4(58) . . . . ? P1 C12 C122 C123 -177.4(29) . . . . ? C12 C122 C123 C124 0.1(61) . . . . ? C122 C123 C124 C125 4.3(61) . . . . ? C126 C125 C124 C123 -6.9(60) . . . . ? C1 Re C1 N1 -164.5(1000) 3 . . . ? P2 Re C1 N1 84.6(538) . . . . ? P2 Re C1 N1 -95.4(538) 3 . . . ? P1 Re C1 N1 -177.6(1000) 3 . . . ? P1 Re C1 N1 2.4(537) . . . . ? C11 P1 C2 C3 -163.0(21) . . . . ? C12 P1 C2 C3 94.9(23) . . . . ? Re P1 C2 C3 -28.7(21) . . . . ? P1 C2 C3 P2 52.5(25) . . . . ? C22 P2 C3 C2 -179.1(21) . . . . ? C21 P2 C3 C2 76.5(24) . . . . ? Re P2 C3 C2 -50.7(23) . . . . ? _refine_diff_density_max 4.582 _refine_diff_density_min -2.807 _refine_diff_density_rms 0.271 data_Complex2b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H60 N2 O2 P4 Re' _chemical_formula_weight 1151.30 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -5.7900 5.8910 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2830 0.4340 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0170 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0290 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0470 0.0320 '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' _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 11.713 _cell_length_b 13.432 _cell_length_c 17.179 _cell_angle_alpha 90.00 _cell_angle_beta 96.48 _cell_angle_gamma 90.00 _cell_volume 2685.5 _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method ? _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 5.344 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54247 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5303 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 70.00 _reflns_number_total 5085 _reflns_number_observed 3214 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1341P)^2^+19.9523P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5085 _refine_ls_number_parameters 199 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_obs 0.0810 _refine_ls_wR_factor_all 0.2645 _refine_ls_wR_factor_obs 0.1999 _refine_ls_goodness_of_fit_all 1.090 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max 0.093 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 1.0000 1.0000 0.0000 0.0461(3) Uani 1 d S . P1 P 0.8941(3) 0.8912(2) -0.0940(2) 0.0546(7) Uani 1 d . . P2 P 1.0262(3) 0.8908(3) 0.1125(2) 0.0567(8) Uani 1 d . . C13 C 0.7390(10) 0.9060(10) -0.1043(7) 0.061(3) Uani 1 d . . C132 C 0.6820(11) 0.8899(11) -0.0387(9) 0.073(4) Uani 1 d . . H132 H 0.7241(11) 0.8730(11) 0.0086(9) 0.087 Uiso 1 calc R . N1 N 0.7841(10) 1.0764(12) 0.0869(8) 0.090(4) Uani 1 d . . C236 C 0.8830(13) 0.7240(11) 0.0979(8) 0.073(4) Uiso 1 d . . H236 H 0.9396(13) 0.6949(11) 0.0715(8) 0.087 Uiso 1 calc R . C1 C 0.8542(11) 1.0475(10) 0.0535(8) 0.063(3) Uani 1 d . . C12 C 0.9123(12) 0.7578(11) -0.0948(7) 0.065(3) Uani 1 d . . C126 C 1.0240(14) 0.7194(13) -0.0815(9) 0.084(4) Uiso 1 d . . H126 H 1.0869(14) 0.7619(13) -0.0733(9) 0.101 Uiso 1 calc R . C22 C 1.1399(12) 0.8003(13) 0.1270(8) 0.075(4) Uani 1 d . . C232 C 0.8150(14) 0.8580(12) 0.1733(9) 0.082(4) Uiso 1 d . . H232 H 0.8272(14) 0.9200(12) 0.1970(9) 0.098 Uiso 1 calc R . C133 C 0.5607(15) 0.8987(13) -0.0428(10) 0.089(4) Uiso 1 d . . H133 H 0.5222(15) 0.8840(13) 0.0002(10) 0.107 Uiso 1 calc R . C23 C 0.8985(12) 0.8177(12) 0.1306(8) 0.070(4) Uani 1 d . . C122 C 0.8245(15) 0.6931(13) -0.1103(9) 0.087(4) Uiso 1 d . . H122 H 0.7505(15) 0.7180(13) -0.1221(9) 0.105 Uiso 1 calc R . C222 C 1.1366(16) 0.7277(13) 0.1864(10) 0.094(5) Uiso 1 d . . H222 H 1.0724(16) 0.7229(13) 0.2134(10) 0.112 Uiso 1 calc R . C136 C 0.6756(13) 0.9313(11) -0.1730(9) 0.077(4) Uiso 1 d . . H136 H 0.7123(13) 0.9403(11) -0.2177(9) 0.092 Uiso 1 calc R . C135 C 0.5568(16) 0.9441(14) -0.1774(11) 0.094(5) Uiso 1 d . . H135 H 0.5155(16) 0.9622(14) -0.2247(11) 0.113 Uiso 1 calc R . C233 C 0.7127(16) 0.8059(14) 0.1810(10) 0.095(5) Uiso 1 d . . H233 H 0.6563(16) 0.8325(14) 0.2089(10) 0.114 Uiso 1 calc R . C134 C 0.5014(17) 0.9302(14) -0.1133(11) 0.096(5) Uiso 1 d . . H134 H 0.4228(17) 0.9419(14) -0.1163(11) 0.116 Uiso 1 calc R . C234 C 0.6998(16) 0.7176(14) 0.1470(10) 0.095(5) Uiso 1 d . . H234 H 0.6320(16) 0.6832(14) 0.1516(10) 0.114 Uiso 1 calc R . C124 C 0.9476(18) 0.5535(17) -0.0963(11) 0.102(5) Uiso 1 d . . H124 H 0.9599(18) 0.4852(17) -0.0978(11) 0.123 Uiso 1 calc R . C123 C 0.8414(17) 0.5870(15) -0.1094(11) 0.100(5) Uiso 1 d . . H123 H 0.7794(17) 0.5435(15) -0.1177(11) 0.120 Uiso 1 calc R . C235 C 0.7788(14) 0.6734(13) 0.1055(9) 0.087(4) Uiso 1 d . . H235 H 0.7644(14) 0.6112(13) 0.0828(9) 0.104 Uiso 1 calc R . C125 C 1.0396(18) 0.6144(15) -0.0807(11) 0.103(5) Uiso 1 d . . H125 H 1.1128(18) 0.5876(15) -0.0696(11) 0.124 Uiso 1 calc R . C226 C 1.2369(16) 0.8054(15) 0.0906(11) 0.100(5) Uiso 1 d . . H226 H 1.2439(16) 0.8534(15) 0.0524(11) 0.120 Uiso 1 calc R . C223 C 1.2305(17) 0.6619(15) 0.2051(11) 0.102(5) Uiso 1 d . . H223 H 1.2278(17) 0.6155(15) 0.2450(11) 0.122 Uiso 1 calc R . C225 C 1.3277(20) 0.7366(17) 0.1115(13) 0.120(7) Uiso 1 d . . H225 H 1.3937(20) 0.7406(17) 0.0861(13) 0.145 Uiso 1 calc R . C224 C 1.3218(19) 0.6660(16) 0.1665(12) 0.112(6) Uiso 1 d . . H224 H 1.3814(19) 0.6205(16) 0.1772(12) 0.135 Uiso 1 calc R . C1A C 0.5732(66) 0.4003(70) 0.1174(42) 0.304(30) Uiso 1 d D . O1A O 0.5962(53) 0.4787(36) 0.1292(34) 0.346(30) Uiso 1 d D . C2A C 0.6353(51) 0.3349(48) 0.1529(33) 0.353(36) Uiso 1 d D . H2A H 0.6531(51) 0.2845(48) 0.1165(33) 0.424 Uiso 1 calc R . H2A H 0.5951(51) 0.3053(48) 0.1928(33) 0.424 Uiso 1 calc R . H2A H 0.7052(51) 0.3647(48) 0.1766(33) 0.424 Uiso 1 calc R . C3A C 0.4945(59) 0.3819(62) 0.0665(40) 0.439(53) Uiso 1 d D . H3AA H 0.4232(59) 0.3810(62) 0.0891(40) 0.527 Uiso 1 calc R . H3AB H 0.5070(59) 0.3181(62) 0.0437(40) 0.527 Uiso 1 calc R . H3AC H 0.4914(59) 0.4322(62) 0.0266(40) 0.527 Uiso 1 calc R . C11 C 0.9380(11) 0.9240(11) -0.1886(7) 0.065(3) Uani 1 d . . H11A H 1.0152(11) 0.8994(11) -0.1918(7) 0.078 Uiso 1 calc R . H11B H 0.8872(11) 0.8918(11) -0.2295(7) 0.078 Uiso 1 calc R . C21 C 1.0643(14) 0.9648(13) 0.2025(8) 0.078(4) Uani 1 d . . H11A H 1.0111(14) 0.9488(13) 0.2400(8) 0.094 Uiso 1 calc R . H11B H 1.1407(14) 0.9459(13) 0.2254(8) 0.094 Uiso 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 0.0389(4) 0.0552(5) 0.0449(4) 0.0008(3) 0.0086(3) 0.0004(3) P1 0.049(2) 0.062(2) 0.053(2) -0.0074(14) 0.0071(12) -0.0009(13) P2 0.055(2) 0.065(2) 0.050(2) 0.0100(14) 0.0079(13) -0.0015(14) C13 0.052(6) 0.068(8) 0.062(7) -0.008(6) 0.009(5) -0.007(6) C132 0.054(7) 0.081(9) 0.085(9) -0.006(8) 0.014(6) -0.008(7) N1 0.054(6) 0.134(12) 0.089(9) -0.009(8) 0.031(6) 0.012(7) C1 0.059(7) 0.062(7) 0.067(8) -0.002(6) 0.010(6) -0.007(6) C12 0.066(8) 0.073(8) 0.058(7) -0.001(6) 0.015(6) -0.005(7) C22 0.058(7) 0.103(11) 0.064(8) 0.007(8) 0.004(6) -0.012(8) C23 0.069(8) 0.086(10) 0.057(7) 0.013(7) 0.014(6) 0.004(7) C11 0.059(7) 0.086(9) 0.050(6) -0.016(6) 0.008(5) 0.006(6) C21 0.077(9) 0.111(12) 0.047(7) 0.017(7) 0.010(6) -0.012(9) _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 C1 2.127(14) . ? Re1 C1 2.127(14) 3_775 ? Re1 P1 2.415(3) 3_775 ? Re1 P1 2.415(3) . ? Re1 P2 2.417(3) . ? Re1 P2 2.417(3) 3_775 ? P1 C12 1.804(14) . ? P1 C11 1.813(13) . ? P1 C13 1.816(12) . ? P2 C22 1.80(2) . ? P2 C23 1.845(15) . ? P2 C21 1.85(2) . ? C13 C136 1.36(2) . ? C13 C132 1.39(2) . ? C132 C133 1.42(2) . ? N1 C1 1.12(2) . ? C236 C23 1.38(2) . ? C236 C235 1.42(2) . ? C12 C122 1.35(2) . ? C12 C126 1.40(2) . ? C126 C125 1.42(2) . ? C22 C226 1.36(2) . ? C22 C222 1.42(2) . ? C232 C23 1.40(2) . ? C232 C233 1.41(2) . ? C133 C134 1.39(2) . ? C122 C123 1.44(2) . ? C222 C223 1.42(2) . ? C136 C135 1.39(2) . ? C135 C134 1.35(2) . ? C233 C234 1.32(2) . ? C234 C235 1.37(2) . ? C124 C123 1.32(2) . ? C124 C125 1.36(3) . ? C226 C225 1.42(3) . ? C223 C224 1.32(3) . ? C225 C224 1.35(3) . ? C1A O1A 1.10(9) . ? C1A C3A 1.22(9) . ? C1A C2A 1.25(8) . ? C11 C21 1.51(2) 3_775 ? C21 C11 1.51(2) 3_775 ? 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 C1 Re1 C1 180.000(1) . 3_775 ? C1 Re1 P1 84.6(4) . 3_775 ? C1 Re1 P1 95.4(4) 3_775 3_775 ? C1 Re1 P1 95.4(4) . . ? C1 Re1 P1 84.6(4) 3_775 . ? P1 Re1 P1 180.0 3_775 . ? C1 Re1 P2 82.6(4) . . ? C1 Re1 P2 97.4(4) 3_775 . ? P1 Re1 P2 79.82(11) 3_775 . ? P1 Re1 P2 100.18(11) . . ? C1 Re1 P2 97.4(4) . 3_775 ? C1 Re1 P2 82.6(4) 3_775 3_775 ? P1 Re1 P2 100.18(11) 3_775 3_775 ? P1 Re1 P2 79.82(11) . 3_775 ? P2 Re1 P2 180.0 . 3_775 ? C12 P1 C11 100.9(6) . . ? C12 P1 C13 103.0(6) . . ? C11 P1 C13 105.6(6) . . ? C12 P1 Re1 123.6(5) . . ? C11 P1 Re1 106.0(5) . . ? C13 P1 Re1 115.5(4) . . ? C22 P2 C23 102.6(7) . . ? C22 P2 C21 98.1(7) . . ? C23 P2 C21 105.6(6) . . ? C22 P2 Re1 123.1(5) . . ? C23 P2 Re1 115.2(4) . . ? C21 P2 Re1 109.8(5) . . ? C136 C13 C132 118.4(13) . . ? C136 C13 P1 123.5(11) . . ? C132 C13 P1 118.1(10) . . ? C13 C132 C133 121.1(15) . . ? C23 C236 C235 118.3(15) . . ? N1 C1 Re1 173.6(13) . . ? C122 C12 C126 118.2(15) . . ? C122 C12 P1 123.6(12) . . ? C126 C12 P1 118.2(11) . . ? C12 C126 C125 118.9(16) . . ? C226 C22 C222 117.2(16) . . ? C226 C22 P2 123.1(14) . . ? C222 C22 P2 119.1(12) . . ? C23 C232 C233 120.7(16) . . ? C134 C133 C132 117.9(17) . . ? C236 C23 C232 119.9(14) . . ? C236 C23 P2 119.2(11) . . ? C232 C23 P2 120.8(12) . . ? C12 C122 C123 122.3(17) . . ? C22 C222 C223 120.6(17) . . ? C13 C136 C135 121.3(15) . . ? C134 C135 C136 120.3(18) . . ? C234 C233 C232 117.5(18) . . ? C135 C134 C133 120.8(19) . . ? C233 C234 C235 124.7(19) . . ? C123 C124 C125 122.8(22) . . ? C124 C123 C122 117.7(20) . . ? C234 C235 C236 118.8(17) . . ? C124 C125 C126 119.9(20) . . ? C22 C226 C225 119.4(19) . . ? C224 C223 C222 120.7(20) . . ? C224 C225 C226 122.5(22) . . ? C223 C224 C225 119.4(23) . . ? O1A C1A C3A 118.3(100) . . ? O1A C1A C2A 117.7(100) . . ? C3A C1A C2A 123.8(100) . . ? C21 C11 P1 112.3(9) 3_775 . ? C11 C21 P2 113.6(9) 3_775 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Re1 P1 C12 -115.0(6) . . . . ? C1 Re1 P1 C12 65.0(6) 3_775 . . . ? P1 Re1 P1 C12 -162.6(575) 3_775 . . . ? P2 Re1 P1 C12 -31.5(5) . . . . ? P2 Re1 P1 C12 148.5(5) 3_775 . . . ? C1 Re1 P1 C11 129.7(6) . . . . ? C1 Re1 P1 C11 -50.3(6) 3_775 . . . ? P1 Re1 P1 C11 82.1(554) 3_775 . . . ? P2 Re1 P1 C11 -146.8(5) . . . . ? P2 Re1 P1 C11 33.2(5) 3_775 . . . ? C1 Re1 P1 C13 13.2(6) . . . . ? C1 Re1 P1 C13 -166.8(6) 3_775 . . . ? P1 Re1 P1 C13 -34.5(502) 3_775 . . . ? P2 Re1 P1 C13 96.6(5) . . . . ? P2 Re1 P1 C13 -83.4(5) 3_775 . . . ? C1 Re1 P2 C22 177.5(7) . . . . ? C1 Re1 P2 C22 -2.5(7) 3_775 . . . ? P1 Re1 P2 C22 -96.7(6) 3_775 . . . ? P1 Re1 P2 C22 83.3(6) . . . . ? P2 Re1 P2 C22 103.7(1000) 3_775 . . . ? C1 Re1 P2 C23 51.0(7) . . . . ? C1 Re1 P2 C23 -129.0(7) 3_775 . . . ? P1 Re1 P2 C23 136.8(6) 3_775 . . . ? P1 Re1 P2 C23 -43.2(6) . . . . ? P2 Re1 P2 C23 -22.8(1000) 3_775 . . . ? C1 Re1 P2 C21 -68.1(7) . . . . ? C1 Re1 P2 C21 111.9(7) 3_775 . . . ? P1 Re1 P2 C21 17.8(6) 3_775 . . . ? P1 Re1 P2 C21 -162.2(6) . . . . ? P2 Re1 P2 C21 -141.9(1000) 3_775 . . . ? C12 P1 C13 C136 -102.1(13) . . . . ? C11 P1 C13 C136 3.4(14) . . . . ? Re1 P1 C13 C136 120.1(12) . . . . ? C12 P1 C13 C132 77.4(12) . . . . ? C11 P1 C13 C132 -177.1(11) . . . . ? Re1 P1 C13 C132 -60.4(12) . . . . ? C136 C13 C132 C133 0.4(22) . . . . ? P1 C13 C132 C133 -179.1(12) . . . . ? C1 Re1 C1 N1 -134.7(119) 3_775 . . . ? P1 Re1 C1 N1 -10.3(123) 3_775 . . . ? P1 Re1 C1 N1 169.7(123) . . . . ? P2 Re1 C1 N1 70.1(124) . . . . ? P2 Re1 C1 N1 -109.9(124) 3_775 . . . ? C11 P1 C12 C122 -101.4(13) . . . . ? C13 P1 C12 C122 7.6(14) . . . . ? Re1 P1 C12 C122 140.9(11) . . . . ? C11 P1 C12 C126 76.0(12) . . . . ? C13 P1 C12 C126 -175.0(11) . . . . ? Re1 P1 C12 C126 -41.7(13) . . . . ? C122 C12 C126 C125 -3.4(23) . . . . ? P1 C12 C126 C125 179.1(13) . . . . ? C23 P2 C22 C226 151.9(14) . . . . ? C21 P2 C22 C226 -100.0(15) . . . . ? Re1 P2 C22 C226 20.1(17) . . . . ? C23 P2 C22 C222 -36.8(14) . . . . ? C21 P2 C22 C222 71.3(14) . . . . ? Re1 P2 C22 C222 -168.6(10) . . . . ? C13 C132 C133 C134 -4.0(24) . . . . ? C235 C236 C23 C232 3.2(21) . . . . ? C235 C236 C23 P2 -173.4(11) . . . . ? C233 C232 C23 C236 -2.5(23) . . . . ? C233 C232 C23 P2 174.0(12) . . . . ? C22 P2 C23 C236 -44.9(12) . . . . ? C21 P2 C23 C236 -147.2(12) . . . . ? Re1 P2 C23 C236 91.5(11) . . . . ? C22 P2 C23 C232 138.5(12) . . . . ? C21 P2 C23 C232 36.2(14) . . . . ? Re1 P2 C23 C232 -85.1(12) . . . . ? C126 C12 C122 C123 3.5(23) . . . . ? P1 C12 C122 C123 -179.1(13) . . . . ? C226 C22 C222 C223 -1.4(25) . . . . ? P2 C22 C222 C223 -173.3(13) . . . . ? C132 C13 C136 C135 2.0(23) . . . . ? P1 C13 C136 C135 -178.5(13) . . . . ? C13 C136 C135 C134 -0.8(27) . . . . ? C23 C232 C233 C234 0.7(25) . . . . ? C136 C135 C134 C133 -2.9(29) . . . . ? C132 C133 C134 C135 5.2(27) . . . . ? C232 C233 C234 C235 0.4(28) . . . . ? C125 C124 C123 C122 2.8(30) . . . . ? C12 C122 C123 C124 -3.2(27) . . . . ? C233 C234 C235 C236 0.3(27) . . . . ? C23 C236 C235 C234 -2.1(23) . . . . ? C123 C124 C125 C126 -2.9(32) . . . . ? C12 C126 C125 C124 3.1(27) . . . . ? C222 C22 C226 C225 2.1(26) . . . . ? P2 C22 C226 C225 173.6(14) . . . . ? C22 C222 C223 C224 -1.3(29) . . . . ? C22 C226 C225 C224 -0.2(31) . . . . ? C222 C223 C224 C225 3.3(31) . . . . ? C226 C225 C224 C223 -2.6(33) . . . . ? C12 P1 C11 C21 -177.6(10) . . . 3_775 ? C13 P1 C11 C21 75.4(11) . . . 3_775 ? Re1 P1 C11 C21 -47.7(10) . . . 3_775 ? C22 P2 C21 C11 134.2(11) . . . 3_775 ? C23 P2 C21 C11 -120.2(11) . . . 3_775 ? Re1 P2 C21 C11 4.6(12) . . . 3_775 ? _refine_diff_density_max 2.017 _refine_diff_density_min -2.207 _refine_diff_density_rms 0.215 data_Complex4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H100 F6 N2 O4 P4 Re' _chemical_formula_weight 1265.64 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.5980 7.2320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0020 0.0020 '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' 'F' 'F' 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 '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, -z' _cell_length_a 9.5290(10) _cell_length_b 11.251(4) _cell_length_c 12.9660(10) _cell_angle_alpha 87.14(2) _cell_angle_beta 81.020(10) _cell_angle_gamma 74.65(2) _cell_volume 1324.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method ? _exptl_crystal_F_000 659 _exptl_absorpt_coefficient_mu 2.349 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5970 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.97 _reflns_number_total 5676 _reflns_number_observed 5362 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.4958P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5676 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_obs 0.0408 _refine_ls_wR_factor_all 0.1109 _refine_ls_wR_factor_obs 0.0918 _refine_ls_goodness_of_fit_all 1.138 _refine_ls_goodness_of_fit_obs 0.971 _refine_ls_restrained_S_all 1.138 _refine_ls_restrained_S_obs 0.971 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.5000 0.5000 0.5000 0.02297(10) Uani 1 d S . P1 P 0.65877(14) 0.46631(12) 0.63333(10) 0.0270(3) Uani 1 d . . P2 P 0.72258(14) 0.36688(13) 0.40551(10) 0.0274(3) Uani 1 d . . C121 C 0.6858(6) 0.5990(5) 0.6976(4) 0.0296(11) Uani 1 d . . C1 C 0.4030(6) 0.3637(5) 0.5639(4) 0.0315(11) Uani 1 d . . C21 C 0.8750(6) 0.4038(6) 0.4583(4) 0.0357(12) Uani 1 d . . H21A H 0.9685(6) 0.3502(6) 0.4282(4) 0.043 Uiso 1 calc R . H21B H 0.8765(6) 0.4886(6) 0.4418(4) 0.043 Uiso 1 calc R . C221 C 0.7664(6) 0.3880(5) 0.2641(4) 0.0334(12) Uani 1 d . . C11 C 0.8489(6) 0.3846(6) 0.5760(4) 0.0356(12) Uani 1 d . . H11A H 0.9186(6) 0.4147(6) 0.6075(4) 0.043 Uiso 1 calc R . H11B H 0.8655(6) 0.2972(6) 0.5915(4) 0.043 Uiso 1 calc R . C231 C 0.7728(6) 0.1980(5) 0.4163(4) 0.0335(12) Uani 1 d . . C131 C 0.6183(6) 0.3695(5) 0.7445(4) 0.0333(12) Uani 1 d . . N1 N 0.3447(6) 0.2903(5) 0.5999(5) 0.0512(14) Uani 1 d . . C122 C 0.7903(7) 0.5812(6) 0.7649(5) 0.0426(14) Uani 1 d . . H122 H 0.8486(7) 0.5025(6) 0.7758(5) 0.051 Uiso 1 calc R . C222 C 0.7478(6) 0.3017(6) 0.1966(4) 0.0400(13) Uani 1 d . . H222 H 0.7155(6) 0.2338(6) 0.2234(4) 0.048 Uiso 1 calc R . C226 C 0.8146(7) 0.4874(6) 0.2234(5) 0.0408(14) Uani 1 d . . H226 H 0.8277(7) 0.5450(6) 0.2676(5) 0.049 Uiso 1 calc R . C126 C 0.6013(7) 0.7153(6) 0.6811(5) 0.0425(14) Uani 1 d . . H126 H 0.5345(7) 0.7285(6) 0.6338(5) 0.051 Uiso 1 calc R . C123 C 0.8073(8) 0.6805(7) 0.8153(5) 0.052(2) Uani 1 d . . H123 H 0.8786(8) 0.6687(7) 0.8589(5) 0.063 Uiso 1 calc R . C223 C 0.7778(8) 0.3184(7) 0.0894(5) 0.051(2) Uani 1 d . . H223 H 0.7645(8) 0.2620(7) 0.0443(5) 0.061 Uiso 1 calc R . C225 C 0.8443(8) 0.5020(7) 0.1138(5) 0.052(2) Uani 1 d . . H225 H 0.8760(8) 0.5696(7) 0.0854(5) 0.062 Uiso 1 calc R . C124 C 0.7199(9) 0.7959(7) 0.8015(6) 0.056(2) Uani 1 d . . H124 H 0.7312(9) 0.8619(7) 0.8368(6) 0.068 Uiso 1 calc R . C125 C 0.6167(9) 0.8155(6) 0.7368(6) 0.054(2) Uani 1 d . . H125 H 0.5564(9) 0.8942(6) 0.7290(6) 0.065 Uiso 1 calc R . C224 C 0.8262(8) 0.4165(7) 0.0505(5) 0.056(2) Uani 1 d . . H224 H 0.8476(8) 0.4256(7) -0.0215(5) 0.068 Uiso 1 calc R . O1 O 0.2908(7) 0.1425(6) 0.7543(5) 0.076(2) Uani 1 d . . H#1 H 0.2946(118) 0.2433(102) 0.6943(85) 0.121(37) Uiso 1 d . . C132 C 0.5447(7) 0.4194(6) 0.8398(5) 0.0455(15) Uani 1 d . . H132 H 0.5193(7) 0.5044(6) 0.8483(5) 0.055 Uiso 1 calc R . C232 C 0.9101(7) 0.1318(6) 0.3672(5) 0.047(2) Uani 1 d . . H232 H 0.9746(7) 0.1741(6) 0.3312(5) 0.056 Uiso 1 calc R . C236 C 0.6830(7) 0.1319(6) 0.4725(5) 0.0417(14) Uani 1 d . . H236 H 0.5916(7) 0.1742(6) 0.5069(5) 0.050 Uiso 1 calc R . C233 C 0.9523(8) 0.0045(7) 0.3711(6) 0.058(2) Uani 1 d . . H233 H 1.0422(8) -0.0385(7) 0.3350(6) 0.070 Uiso 1 calc R . C235 C 0.7249(8) 0.0040(6) 0.4794(6) 0.052(2) Uani 1 d . . H235 H 0.6620(8) -0.0381(6) 0.5177(6) 0.063 Uiso 1 calc R . C136 C 0.6518(9) 0.2422(6) 0.7344(6) 0.053(2) Uani 1 d . . H136 H 0.6986(9) 0.2059(6) 0.6710(6) 0.064 Uiso 1 calc R . C234 C 0.8587(8) -0.0594(6) 0.4298(6) 0.058(2) Uani 1 d . . H234 H 0.8879(8) -0.1449(6) 0.4348(6) 0.070 Uiso 1 calc R . O2 O 0.0575(9) 0.2573(7) 0.7849(7) 0.101(2) Uani 1 d . . C133 C 0.5085(8) 0.3456(8) 0.9221(5) 0.057(2) Uani 1 d . . H133 H 0.4597(8) 0.3812(8) 0.9854(5) 0.069 Uiso 1 calc R . C134 C 0.5435(10) 0.2208(8) 0.9116(6) 0.066(2) Uani 1 d . . H134 H 0.5185(10) 0.1712(8) 0.9673(6) 0.080 Uiso 1 calc R . C#1 C 0.1608(12) 0.1741(9) 0.8035(7) 0.072(2) Uani 1 d . . F1 F 0.1320(13) 0.1375(8) 0.9817(5) 0.168(4) Uani 1 d . . C135 C 0.6157(11) 0.1692(7) 0.8184(8) 0.075(3) Uani 1 d . . H135 H 0.6409(11) 0.0840(7) 0.8113(8) 0.090 Uiso 1 calc R . F2 F 0.2219(16) -0.0121(9) 0.8905(8) 0.229(7) Uani 1 d . . C#2 C 0.1384(19) 0.0913(11) 0.8963(8) 0.112(5) Uani 1 d . . F3 F 0.0109(17) 0.0667(15) 0.8996(9) 0.255(8) Uani 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 Re 0.02018(15) 0.0244(2) 0.0237(2) 0.00044(10) -0.00238(10) -0.00534(11) P1 0.0253(6) 0.0280(7) 0.0268(7) -0.0004(5) -0.0046(5) -0.0048(5) P2 0.0240(6) 0.0291(7) 0.0269(7) -0.0010(5) -0.0012(5) -0.0045(5) C121 0.029(3) 0.028(3) 0.032(3) -0.001(2) -0.004(2) -0.008(2) C1 0.029(3) 0.036(3) 0.025(3) 0.002(2) 0.005(2) -0.006(2) C21 0.026(3) 0.038(3) 0.040(3) -0.011(2) -0.003(2) -0.003(2) C221 0.027(3) 0.039(3) 0.030(3) 0.001(2) -0.001(2) -0.003(2) C11 0.027(3) 0.041(3) 0.035(3) -0.003(2) -0.008(2) 0.001(2) C231 0.032(3) 0.030(3) 0.034(3) -0.004(2) -0.007(2) 0.001(2) C131 0.032(3) 0.036(3) 0.032(3) 0.005(2) -0.011(2) -0.007(2) N1 0.050(3) 0.043(3) 0.059(4) 0.006(3) 0.009(3) -0.020(3) C122 0.046(3) 0.044(3) 0.040(3) 0.003(3) -0.017(3) -0.009(3) C222 0.037(3) 0.048(4) 0.031(3) -0.005(3) -0.002(2) -0.005(3) C226 0.040(3) 0.043(3) 0.036(3) -0.003(3) 0.002(2) -0.009(3) C126 0.049(4) 0.034(3) 0.047(4) 0.001(3) -0.017(3) -0.009(3) C123 0.056(4) 0.063(5) 0.046(4) -0.008(3) -0.023(3) -0.019(4) C223 0.053(4) 0.066(5) 0.031(3) -0.006(3) -0.010(3) -0.008(3) C225 0.056(4) 0.057(4) 0.040(4) 0.011(3) 0.003(3) -0.019(3) C124 0.079(5) 0.044(4) 0.056(4) -0.010(3) -0.021(4) -0.024(4) C125 0.070(5) 0.036(4) 0.057(4) -0.005(3) -0.020(4) -0.007(3) C224 0.055(4) 0.075(5) 0.029(3) 0.007(3) 0.002(3) -0.004(4) O1 0.073(4) 0.077(4) 0.083(4) 0.021(3) -0.011(3) -0.035(3) C132 0.047(4) 0.044(4) 0.041(3) 0.006(3) -0.005(3) -0.006(3) C232 0.037(3) 0.043(4) 0.054(4) -0.003(3) -0.005(3) 0.001(3) C236 0.038(3) 0.036(3) 0.049(4) -0.001(3) -0.003(3) -0.008(3) C233 0.046(4) 0.052(4) 0.063(5) -0.016(4) -0.010(3) 0.014(3) C235 0.061(4) 0.039(4) 0.054(4) 0.007(3) -0.010(3) -0.009(3) C136 0.077(5) 0.033(3) 0.047(4) 0.001(3) -0.013(3) -0.009(3) C234 0.060(4) 0.029(3) 0.083(5) -0.006(3) -0.026(4) 0.005(3) O2 0.088(5) 0.073(5) 0.133(7) 0.002(4) 0.001(5) -0.014(4) C133 0.052(4) 0.076(5) 0.040(4) 0.014(3) -0.002(3) -0.018(4) C134 0.079(6) 0.076(6) 0.054(5) 0.029(4) -0.014(4) -0.040(5) C#1 0.098(7) 0.076(6) 0.056(5) -0.006(4) 0.001(5) -0.055(6) F1 0.300(12) 0.163(8) 0.057(4) 0.001(4) -0.016(6) -0.093(8) C135 0.103(7) 0.040(4) 0.090(7) 0.029(4) -0.030(5) -0.028(4) F2 0.310(15) 0.093(6) 0.178(9) 0.071(6) 0.102(10) 0.039(8) C#2 0.198(14) 0.078(7) 0.064(6) -0.014(5) 0.043(7) -0.077(9) F3 0.328(17) 0.361(19) 0.167(10) 0.118(11) -0.035(10) -0.272(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 Re C1 2.068(6) . ? Re C1 2.068(6) 2_666 ? Re P1 2.4225(13) . ? Re P1 2.4225(13) 2_666 ? Re P2 2.4357(14) 2_666 ? Re P2 2.4357(14) . ? P1 C131 1.817(6) . ? P1 C121 1.839(5) . ? P1 C11 1.856(5) . ? P2 C221 1.834(6) . ? P2 C231 1.836(6) . ? P2 C21 1.846(6) . ? C121 C126 1.369(8) . ? C121 C122 1.394(8) . ? C1 N1 1.154(7) . ? C21 C11 1.522(8) . ? C221 C226 1.370(8) . ? C221 C222 1.402(8) . ? C231 C236 1.381(8) . ? C231 C232 1.394(8) . ? C131 C132 1.388(8) . ? C131 C136 1.390(8) . ? C122 C123 1.379(9) . ? C222 C223 1.388(8) . ? C226 C225 1.415(9) . ? C126 C125 1.420(9) . ? C123 C124 1.365(10) . ? C223 C224 1.352(11) . ? C225 C224 1.356(10) . ? C124 C125 1.357(10) . ? O1 C#1 1.269(11) . ? C132 C133 1.377(9) . ? C232 C233 1.382(10) . ? C236 C235 1.390(9) . ? C233 C234 1.402(11) . ? C235 C234 1.363(10) . ? C136 C135 1.387(10) . ? O2 C#1 1.212(12) . ? C133 C134 1.364(11) . ? C134 C135 1.368(12) . ? C#1 C#2 1.508(13) . ? F1 C#2 1.231(12) . ? F1 F3 2.01(2) . ? F1 F2 2.020(13) . ? F2 C#2 1.222(15) . ? F2 F3 1.96(2) . ? C#2 F3 1.31(2) . ? 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 C1 Re C1 180.0 . 2_666 ? C1 Re P1 91.2(2) . . ? C1 Re P1 88.8(2) 2_666 . ? C1 Re P1 88.8(2) . 2_666 ? C1 Re P1 91.2(2) 2_666 2_666 ? P1 Re P1 180.0 . 2_666 ? C1 Re P2 82.14(15) . 2_666 ? C1 Re P2 97.86(15) 2_666 2_666 ? P1 Re P2 99.98(5) . 2_666 ? P1 Re P2 80.02(5) 2_666 2_666 ? C1 Re P2 97.86(15) . . ? C1 Re P2 82.14(15) 2_666 . ? P1 Re P2 80.02(5) . . ? P1 Re P2 99.98(5) 2_666 . ? P2 Re P2 180.0 2_666 . ? C131 P1 C121 101.8(3) . . ? C131 P1 C11 103.2(3) . . ? C121 P1 C11 102.9(3) . . ? C131 P1 Re 117.6(2) . . ? C121 P1 Re 119.8(2) . . ? C11 P1 Re 109.5(2) . . ? C221 P2 C231 101.0(3) . . ? C221 P2 C21 103.9(3) . . ? C231 P2 C21 101.2(3) . . ? C221 P2 Re 119.2(2) . . ? C231 P2 Re 123.9(2) . . ? C21 P2 Re 104.8(2) . . ? C126 C121 C122 119.7(5) . . ? C126 C121 P1 120.2(4) . . ? C122 C121 P1 120.1(4) . . ? N1 C1 Re 177.8(5) . . ? C11 C21 P2 107.1(4) . . ? C226 C221 C222 119.6(5) . . ? C226 C221 P2 121.2(4) . . ? C222 C221 P2 119.2(5) . . ? C21 C11 P1 111.4(4) . . ? C236 C231 C232 117.4(6) . . ? C236 C231 P2 123.6(4) . . ? C232 C231 P2 118.9(5) . . ? C132 C131 C136 117.5(6) . . ? C132 C131 P1 121.7(5) . . ? C136 C131 P1 120.6(5) . . ? C123 C122 C121 120.0(6) . . ? C223 C222 C221 119.6(6) . . ? C221 C226 C225 119.6(6) . . ? C121 C126 C125 119.4(6) . . ? C124 C123 C122 120.3(6) . . ? C224 C223 C222 120.2(7) . . ? C224 C225 C226 119.5(7) . . ? C125 C124 C123 120.8(6) . . ? C124 C125 C126 119.7(6) . . ? C223 C224 C225 121.6(6) . . ? C133 C132 C131 121.3(7) . . ? C233 C232 C231 121.3(7) . . ? C231 C236 C235 122.1(6) . . ? C232 C233 C234 119.6(6) . . ? C234 C235 C236 119.7(7) . . ? C135 C136 C131 120.4(7) . . ? C235 C234 C233 119.9(6) . . ? C134 C133 C132 120.6(7) . . ? C133 C134 C135 119.3(7) . . ? O2 C#1 O1 129.2(9) . . ? O2 C#1 C#2 118.5(11) . . ? O1 C#1 C#2 112.3(11) . . ? C#2 F1 F3 39.0(9) . . ? C#2 F1 F2 34.4(9) . . ? F3 F1 F2 58.1(7) . . ? C134 C135 C136 120.9(7) . . ? C#2 F2 F3 41.0(8) . . ? C#2 F2 F1 34.7(8) . . ? F3 F2 F1 60.8(6) . . ? F2 C#2 F1 110.8(16) . . ? F2 C#2 F3 101.3(12) . . ? F1 C#2 F3 104.8(12) . . ? F2 C#2 C#1 115.0(10) . . ? F1 C#2 C#1 114.8(9) . . ? F3 C#2 C#1 108.7(13) . . ? C#2 F3 F2 37.7(8) . . ? C#2 F3 F1 36.3(6) . . ? F2 F3 F1 61.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Re P1 C131 -11.2(3) . . . . ? C1 Re P1 C131 168.8(3) 2_666 . . . ? P1 Re P1 C131 -108.0(1000) 2_666 . . . ? P2 Re P1 C131 71.0(2) 2_666 . . . ? P2 Re P1 C131 -109.0(2) . . . . ? C1 Re P1 C121 -135.5(2) . . . . ? C1 Re P1 C121 44.5(2) 2_666 . . . ? P1 Re P1 C121 127.7(1000) 2_666 . . . ? P2 Re P1 C121 -53.3(2) 2_666 . . . ? P2 Re P1 C121 126.7(2) . . . . ? C1 Re P1 C11 106.1(3) . . . . ? C1 Re P1 C11 -73.9(3) 2_666 . . . ? P1 Re P1 C11 9.3(1000) 2_666 . . . ? P2 Re P1 C11 -171.7(2) 2_666 . . . ? P2 Re P1 C11 8.3(2) . . . . ? C1 Re P2 C221 122.8(3) . . . . ? C1 Re P2 C221 -57.2(3) 2_666 . . . ? P1 Re P2 C221 -147.3(2) . . . . ? P1 Re P2 C221 32.7(2) 2_666 . . . ? P2 Re P2 C221 67.0(1000) 2_666 . . . ? C1 Re P2 C231 -6.9(3) . . . . ? C1 Re P2 C231 173.1(3) 2_666 . . . ? P1 Re P2 C231 83.0(2) . . . . ? P1 Re P2 C231 -97.0(2) 2_666 . . . ? P2 Re P2 C231 -62.7(1000) 2_666 . . . ? C1 Re P2 C21 -121.6(3) . . . . ? C1 Re P2 C21 58.4(3) 2_666 . . . ? P1 Re P2 C21 -31.7(2) . . . . ? P1 Re P2 C21 148.3(2) 2_666 . . . ? P2 Re P2 C21 -177.4(1000) 2_666 . . . ? C131 P1 C121 C126 -122.5(5) . . . . ? C11 P1 C121 C126 130.8(5) . . . . ? Re P1 C121 C126 9.1(6) . . . . ? C131 P1 C121 C122 56.2(5) . . . . ? C11 P1 C121 C122 -50.4(5) . . . . ? Re P1 C121 C122 -172.2(4) . . . . ? C1 Re C1 N1 -139.9(1000) 2_666 . . . ? P1 Re C1 N1 120.6(138) . . . . ? P1 Re C1 N1 -59.4(138) 2_666 . . . ? P2 Re C1 N1 20.7(138) 2_666 . . . ? P2 Re C1 N1 -159.3(138) . . . . ? C221 P2 C21 C11 -178.3(4) . . . . ? C231 P2 C21 C11 -74.0(4) . . . . ? Re P2 C21 C11 55.8(4) . . . . ? C231 P2 C221 C226 -148.0(5) . . . . ? C21 P2 C221 C226 -43.5(5) . . . . ? Re P2 C221 C226 72.6(5) . . . . ? C231 P2 C221 C222 33.0(5) . . . . ? C21 P2 C221 C222 137.6(5) . . . . ? Re P2 C221 C222 -106.3(4) . . . . ? P2 C21 C11 P1 -50.7(5) . . . . ? C131 P1 C11 C21 148.9(4) . . . . ? C121 P1 C11 C21 -105.5(4) . . . . ? Re P1 C11 C21 23.0(5) . . . . ? C221 P2 C231 C236 -131.5(5) . . . . ? C21 P2 C231 C236 121.8(5) . . . . ? Re P2 C231 C236 5.3(6) . . . . ? C221 P2 C231 C232 49.9(5) . . . . ? C21 P2 C231 C232 -56.8(5) . . . . ? Re P2 C231 C232 -173.3(4) . . . . ? C121 P1 C131 C132 32.3(5) . . . . ? C11 P1 C131 C132 138.7(5) . . . . ? Re P1 C131 C132 -100.6(5) . . . . ? C121 P1 C131 C136 -152.0(5) . . . . ? C11 P1 C131 C136 -45.6(6) . . . . ? Re P1 C131 C136 75.0(5) . . . . ? C126 C121 C122 C123 0.7(9) . . . . ? P1 C121 C122 C123 -178.1(5) . . . . ? C226 C221 C222 C223 -0.3(9) . . . . ? P2 C221 C222 C223 178.7(5) . . . . ? C222 C221 C226 C225 0.3(9) . . . . ? P2 C221 C226 C225 -178.6(5) . . . . ? C122 C121 C126 C125 -3.0(9) . . . . ? P1 C121 C126 C125 175.7(5) . . . . ? C121 C122 C123 C124 1.4(11) . . . . ? C221 C222 C223 C224 0.7(10) . . . . ? C221 C226 C225 C224 -0.7(10) . . . . ? C122 C123 C124 C125 -1.1(12) . . . . ? C123 C124 C125 C126 -1.3(12) . . . . ? C121 C126 C125 C124 3.4(11) . . . . ? C222 C223 C224 C225 -1.2(11) . . . . ? C226 C225 C224 C223 1.2(11) . . . . ? C136 C131 C132 C133 1.2(10) . . . . ? P1 C131 C132 C133 177.0(5) . . . . ? C236 C231 C232 C233 2.6(9) . . . . ? P2 C231 C232 C233 -178.7(5) . . . . ? C232 C231 C236 C235 -1.1(9) . . . . ? P2 C231 C236 C235 -179.7(5) . . . . ? C231 C232 C233 C234 -3.3(11) . . . . ? C231 C236 C235 C234 0.2(10) . . . . ? C132 C131 C136 C135 -1.8(10) . . . . ? P1 C131 C136 C135 -177.6(6) . . . . ? C236 C235 C234 C233 -0.8(11) . . . . ? C232 C233 C234 C235 2.3(11) . . . . ? C131 C132 C133 C134 -0.5(11) . . . . ? C132 C133 C134 C135 0.3(12) . . . . ? C133 C134 C135 C136 -0.9(14) . . . . ? C131 C136 C135 C134 1.7(13) . . . . ? C#2 F1 F2 C#2 0.000(12) . . . . ? F3 F1 F2 C#2 44.7(13) . . . . ? C#2 F1 F2 F3 -44.7(13) . . . . ? F3 F1 F2 F3 0.000(3) . . . . ? F3 F2 C#2 F1 110.7(13) . . . . ? F1 F2 C#2 F1 0.000(8) . . . . ? F3 F2 C#2 F3 0.000(1) . . . . ? F1 F2 C#2 F3 -110.7(13) . . . . ? F3 F2 C#2 C#1 -117.0(17) . . . . ? F1 F2 C#2 C#1 132.3(21) . . . . ? F3 F1 C#2 F2 -108.5(14) . . . . ? F2 F1 C#2 F2 0.000(7) . . . . ? F3 F1 C#2 F3 0.000(2) . . . . ? F2 F1 C#2 F3 108.5(13) . . . . ? F3 F1 C#2 C#1 119.2(22) . . . . ? F2 F1 C#2 C#1 -132.4(23) . . . . ? O2 C#1 C#2 F2 154.5(15) . . . . ? O1 C#1 C#2 F2 -24.6(18) . . . . ? O2 C#1 C#2 F1 -75.2(18) . . . . ? O1 C#1 C#2 F1 105.8(15) . . . . ? O2 C#1 C#2 F3 41.8(15) . . . . ? O1 C#1 C#2 F3 -137.3(12) . . . . ? F2 C#2 F3 F2 0.000(1) . . . . ? F1 C#2 F3 F2 -115.3(16) . . . . ? C#1 C#2 F3 F2 121.5(12) . . . . ? F2 C#2 F3 F1 115.3(16) . . . . ? F1 C#2 F3 F1 0.000(2) . . . . ? C#1 C#2 F3 F1 -123.2(16) . . . . ? C#2 F2 F3 C#2 0.0 . . . . ? F1 F2 F3 C#2 37.6(10) . . . . ? C#2 F2 F3 F1 -37.6(10) . . . . ? F1 F2 F3 F1 0.000(3) . . . . ? C#2 F1 F3 C#2 0.000(3) . . . . ? F2 F1 F3 C#2 -39.2(12) . . . . ? C#2 F1 F3 F2 39.2(12) . . . . ? F2 F1 F3 F2 0.000(3) . . . . ? _refine_diff_density_max 0.981 _refine_diff_density_min -1.255 _refine_diff_density_rms 0.156 data_Complex5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H56 N2 O2 P4 Re' _chemical_formula_weight 1099.22 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 'P' 'P' 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.5980 7.2320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 '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+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 13.474(3) _cell_length_b 18.692(2) _cell_length_c 10.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.780(10) _cell_angle_gamma 90.00 _cell_volume 2435.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method ? _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 2.531 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4524 _diffrn_reflns_av_R_equivalents 0.1272 _diffrn_reflns_av_sigmaI/netI 0.1723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4266 _reflns_number_observed 2291 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+21.4897P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4263 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1796 _refine_ls_R_factor_obs 0.0803 _refine_ls_wR_factor_all 0.1690 _refine_ls_wR_factor_obs 0.1172 _refine_ls_goodness_of_fit_all 1.173 _refine_ls_goodness_of_fit_obs 1.144 _refine_ls_restrained_S_all 1.176 _refine_ls_restrained_S_obs 1.144 _refine_ls_shift/esd_max -0.030 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 1.0000 1.0000 0.5000 0.0261(2) Uani 1 d S . P1 P 0.8341(3) 0.9899(3) 0.5482(4) 0.0321(11) Uani 1 d . . P2 P 1.0592(3) 0.9322(2) 0.7124(5) 0.0313(10) Uani 1 d . . C22 C 1.1797(14) 0.9554(9) 0.8430(19) 0.040(5) Uani 1 d . . C11 C 0.8579(12) 0.9365(9) 0.7085(16) 0.038(4) Uani 1 d . . H11A H 0.8069(12) 0.9496(9) 0.7541(16) 0.046 Uiso 1 calc R . H11B H 0.8484(12) 0.8863(9) 0.6844(16) 0.046 Uiso 1 calc R . C21 C 0.9650(12) 0.9474(9) 0.8070(17) 0.040(4) Uani 1 d . . H21A H 0.9774(12) 0.9141(9) 0.8836(17) 0.048 Uiso 1 calc R . H21B H 0.9720(12) 0.9957(9) 0.8437(17) 0.048 Uiso 1 calc R . C224 C 1.3709(14) 0.9927(17) 1.0362(17) 0.067(7) Uani 1 d . . H224 H 1.4341(14) 1.0059(17) 1.0997(17) 0.081 Uiso 1 calc R . C222 C 1.1944(15) 1.0187(12) 0.9164(18) 0.064(8) Uani 1 d . . H222 H 1.1394(15) 1.0511(12) 0.8986(18) 0.076 Uiso 1 calc R . C12 C 0.7210(13) 0.9453(9) 0.4376(21) 0.048(5) Uani 1 d . . C122 C 0.7270(14) 0.8993(11) 0.3382(19) 0.057(6) Uani 1 d . . H122 H 0.7905(14) 0.8918(11) 0.3220(19) 0.068 Uiso 1 calc R . C225 C 1.3625(14) 0.9298(12) 0.9645(19) 0.066(6) Uani 1 d . . H225 H 1.4196(14) 0.8995(12) 0.9809(19) 0.079 Uiso 1 calc R . C126 C 0.6223(14) 0.9531(10) 0.4615(23) 0.062(6) Uani 1 d . . H126 H 0.6167(14) 0.9830(10) 0.5320(23) 0.075 Uiso 1 calc R . C125 C 0.5348(15) 0.9167(10) 0.3815(23) 0.063(6) Uani 1 d . . H125 H 0.4707(15) 0.9244(10) 0.3958(23) 0.075 Uiso 1 calc R . C226 C 1.2689(14) 0.9113(10) 0.8674(19) 0.052(5) Uani 1 d . . H226 H 1.2646(14) 0.8691(10) 0.8174(19) 0.062 Uiso 1 calc R . C223 C 1.2854(15) 1.0357(10) 1.0133(19) 0.055(5) Uani 1 d . . H223 H 1.2897(15) 1.0773(10) 1.0650(19) 0.066 Uiso 1 calc R . C123 C 0.6387(16) 0.8630(12) 0.2597(19) 0.065(6) Uani 1 d . . H123 H 0.6448(16) 0.8330(12) 0.1896(19) 0.078 Uiso 1 calc R . C124 C 0.5422(15) 0.8690(11) 0.2802(24) 0.066(6) Uani 1 d . . H124 H 0.4851(15) 0.8425(11) 0.2288(24) 0.079 Uiso 1 calc R . C23 C 1.0700(14) 0.8345(9) 0.7117(20) 0.037(5) Uani 1 d . . C13 C 0.7786(13) 1.0738(9) 0.5898(19) 0.041(4) Uani 1 d . . C232 C 1.0979(14) 0.7989(9) 0.6037(19) 0.047(5) Uani 1 d . . H232 H 1.1047(14) 0.8243(9) 0.5282(19) 0.056 Uiso 1 calc R . C132 C 0.7165(16) 1.1118(10) 0.4793(25) 0.063(6) Uani 1 d . . H132 H 0.7038(16) 1.0956(10) 0.3891(25) 0.076 Uiso 1 calc R . C236 C 1.0582(16) 0.7941(9) 0.8192(21) 0.060(6) Uani 1 d . . H236 H 1.0394(16) 0.8163(9) 0.8900(21) 0.072 Uiso 1 calc R . C234 C 1.0979(17) 0.6878(11) 0.7207(20) 0.063(6) Uani 1 d . . H234 H 1.1037(17) 0.6382(11) 0.7207(20) 0.075 Uiso 1 calc R . C233 C 1.1140(16) 0.7276(11) 0.6135(21) 0.059(5) Uani 1 d . . H233 H 1.1365(16) 0.7045(11) 0.5467(21) 0.071 Uiso 1 calc R . C235 C 1.0741(16) 0.7208(11) 0.8233(20) 0.062(6) Uani 1 d . . H235 H 1.0682(16) 0.6945(11) 0.8982(20) 0.075 Uiso 1 calc R . C133 C 0.6722(15) 1.1772(11) 0.5080(27) 0.068(7) Uani 1 d . . H133 H 0.6293(15) 1.2042(11) 0.4361(27) 0.082 Uiso 1 calc R . C134 C 0.6938(16) 1.2004(12) 0.6452(27) 0.074(7) Uani 1 d . . H134 H 0.6661(16) 1.2429(12) 0.6662(27) 0.088 Uiso 1 calc R . C136 C 0.7946(17) 1.0954(10) 0.7187(25) 0.069(7) Uani 1 d . . H136 H 0.8328(17) 1.0672(10) 0.7921(25) 0.083 Uiso 1 calc R . C135 C 0.7544(18) 1.1600(11) 0.7433(27) 0.074(7) Uani 1 d . . H135 H 0.7710(18) 1.1759(11) 0.8342(27) 0.089 Uiso 1 calc R . N1 N 1.0360(13) 1.1372(10) 0.7012(18) 0.055(5) Uani 1 d . . C1 C 1.0207(13) 1.0896(10) 0.6225(16) 0.040(5) Uani 1 d . . O2S O 1.0417(17) 1.2179(13) 0.9328(20) 0.141(9) Uani 1 d . . H2S H 1.0313(17) 1.1873(13) 0.8722(20) 0.038(58) Uiso 1 calc R . C2S C 1.1421(21) 1.2202(13) 1.0014(30) 0.102(10) Uani 1 d . . H2SA H 1.1818(21) 1.2105(13) 0.9394(30) 0.122 Uiso 1 calc R . H2SB H 1.1579(21) 1.1850(13) 1.0737(30) 0.122 Uiso 1 calc R . H2SC H 1.1596(21) 1.2669(13) 1.0411(30) 0.122 Uiso 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 Re 0.0256(4) 0.0243(4) 0.0309(4) 0.0010(7) 0.0125(3) -0.0001(7) P1 0.025(2) 0.041(3) 0.033(2) 0.001(2) 0.013(2) 0.003(2) P2 0.031(2) 0.032(2) 0.034(3) 0.004(2) 0.015(2) 0.004(2) C22 0.037(11) 0.031(10) 0.052(12) 0.015(9) 0.012(10) 0.002(8) C11 0.041(10) 0.047(11) 0.038(10) 0.013(9) 0.030(9) 0.011(9) C21 0.040(10) 0.040(10) 0.048(11) 0.012(9) 0.025(9) 0.020(9) C224 0.054(12) 0.099(18) 0.035(10) 0.022(16) -0.006(9) -0.035(17) C222 0.043(11) 0.099(25) 0.039(11) -0.022(13) -0.002(9) 0.008(12) C12 0.030(10) 0.035(11) 0.087(15) -0.017(10) 0.032(10) -0.009(8) C122 0.026(10) 0.085(16) 0.057(13) -0.010(12) 0.010(9) -0.020(11) C225 0.032(11) 0.081(16) 0.053(13) -0.023(12) -0.034(10) 0.007(11) C126 0.038(11) 0.053(13) 0.105(18) -0.003(12) 0.034(12) -0.003(10) C125 0.038(11) 0.043(12) 0.107(19) 0.004(13) 0.024(12) -0.014(10) C226 0.045(11) 0.053(12) 0.058(13) -0.003(10) 0.016(10) 0.013(10) C223 0.053(13) 0.052(12) 0.052(12) -0.013(10) 0.005(11) -0.006(11) C123 0.064(15) 0.087(17) 0.035(11) -0.023(11) 0.002(10) -0.001(13) C124 0.031(11) 0.049(13) 0.109(19) 0.017(13) 0.011(12) -0.007(10) C23 0.042(12) 0.027(9) 0.043(11) -0.007(9) 0.016(10) -0.016(9) C13 0.039(10) 0.042(11) 0.055(12) -0.010(10) 0.031(10) -0.006(9) C232 0.056(12) 0.025(10) 0.065(13) 0.025(9) 0.030(10) 0.012(9) C132 0.061(14) 0.042(13) 0.093(18) 0.021(12) 0.034(13) 0.007(11) C236 0.078(15) 0.037(11) 0.072(14) 0.035(11) 0.035(12) 0.030(11) C234 0.085(17) 0.047(13) 0.044(12) 0.007(11) 0.002(12) 0.006(12) C233 0.060(14) 0.054(14) 0.064(14) 0.003(11) 0.021(11) -0.001(11) C235 0.086(17) 0.056(13) 0.045(12) 0.039(11) 0.018(12) 0.014(12) C133 0.038(12) 0.053(14) 0.120(21) 0.027(14) 0.035(13) 0.004(11) C134 0.043(13) 0.059(16) 0.109(21) -0.033(15) 0.009(14) 0.004(12) C136 0.073(16) 0.047(13) 0.097(19) -0.016(13) 0.040(14) 0.016(12) C135 0.066(16) 0.055(14) 0.103(20) -0.021(14) 0.028(15) 0.002(13) N1 0.037(10) 0.076(14) 0.044(10) -0.022(11) -0.001(8) -0.008(9) C1 0.032(10) 0.060(13) 0.014(9) 0.021(9) -0.012(7) -0.006(9) O2S 0.137(19) 0.210(24) 0.092(15) -0.075(16) 0.056(14) -0.001(19) C2S 0.112(24) 0.066(17) 0.155(29) -0.007(18) 0.082(23) -0.016(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 Re C1 2.05(2) 3_776 ? Re C1 2.05(2) . ? Re P2 2.418(4) . ? Re P2 2.418(4) 3_776 ? Re P1 2.437(4) 3_776 ? Re P1 2.437(4) . ? P1 C12 1.80(2) . ? P1 C13 1.84(2) . ? P1 C11 1.85(2) . ? P2 C22 1.81(2) . ? P2 C23 1.83(2) . ? P2 C21 1.833(14) . ? C22 C222 1.38(3) . ? C22 C226 1.42(2) . ? C11 C21 1.50(2) . ? C224 C223 1.37(3) . ? C224 C225 1.37(3) . ? C222 C223 1.36(2) . ? C12 C122 1.35(2) . ? C12 C126 1.43(2) . ? C122 C123 1.39(2) . ? C225 C226 1.39(2) . ? C126 C125 1.39(3) . ? C125 C124 1.39(3) . ? C123 C124 1.38(3) . ? C23 C236 1.38(2) . ? C23 C232 1.43(2) . ? C13 C136 1.32(3) . ? C13 C132 1.38(3) . ? C232 C233 1.35(2) . ? C132 C133 1.43(3) . ? C236 C235 1.39(2) . ? C234 C235 1.33(3) . ? C234 C233 1.39(2) . ? C133 C134 1.40(3) . ? C134 C135 1.32(3) . ? C136 C135 1.38(2) . ? N1 C1 1.17(2) . ? O2S C2S 1.32(3) . ? 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 C1 Re C1 180.000(4) 3_776 . ? C1 Re P2 93.4(4) 3_776 . ? C1 Re P2 86.6(4) . . ? C1 Re P2 86.6(4) 3_776 3_776 ? C1 Re P2 93.4(4) . 3_776 ? P2 Re P2 180.0 . 3_776 ? C1 Re P1 84.5(5) 3_776 3_776 ? C1 Re P1 95.5(5) . 3_776 ? P2 Re P1 98.42(15) . 3_776 ? P2 Re P1 81.58(14) 3_776 3_776 ? C1 Re P1 95.5(5) 3_776 . ? C1 Re P1 84.5(5) . . ? P2 Re P1 81.58(14) . . ? P2 Re P1 98.42(15) 3_776 . ? P1 Re P1 180.0 3_776 . ? C12 P1 C13 102.3(8) . . ? C12 P1 C11 100.7(9) . . ? C13 P1 C11 103.3(8) . . ? C12 P1 Re 124.4(6) . . ? C13 P1 Re 116.2(6) . . ? C11 P1 Re 107.1(5) . . ? C22 P2 C23 100.8(8) . . ? C22 P2 C21 100.9(8) . . ? C23 P2 C21 103.0(8) . . ? C22 P2 Re 120.4(6) . . ? C23 P2 Re 121.6(7) . . ? C21 P2 Re 107.1(5) . . ? C222 C22 C226 115.6(18) . . ? C222 C22 P2 123.4(15) . . ? C226 C22 P2 120.8(14) . . ? C21 C11 P1 112.8(11) . . ? C11 C21 P2 108.0(11) . . ? C223 C224 C225 119.1(18) . . ? C223 C222 C22 122.8(20) . . ? C122 C12 C126 117.7(17) . . ? C122 C12 P1 122.1(13) . . ? C126 C12 P1 120.0(15) . . ? C12 C122 C123 120.3(18) . . ? C224 C225 C226 120.2(19) . . ? C125 C126 C12 121.2(20) . . ? C124 C125 C126 120.5(19) . . ? C225 C226 C22 121.1(18) . . ? C222 C223 C224 121.0(20) . . ? C124 C123 C122 123.6(20) . . ? C123 C124 C125 116.6(19) . . ? C236 C23 C232 118.3(16) . . ? C236 C23 P2 121.0(15) . . ? C232 C23 P2 120.5(13) . . ? C136 C13 C132 121.6(19) . . ? C136 C13 P1 122.2(16) . . ? C132 C13 P1 116.2(15) . . ? C233 C232 C23 118.6(17) . . ? C13 C132 C133 117.6(22) . . ? C23 C236 C235 120.8(19) . . ? C235 C234 C233 119.8(19) . . ? C232 C233 C234 121.9(20) . . ? C234 C235 C236 120.5(18) . . ? C134 C133 C132 119.6(21) . . ? C135 C134 C133 117.8(22) . . ? C13 C136 C135 119.6(23) . . ? C134 C135 C136 123.5(24) . . ? N1 C1 Re 174.7(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Re P1 C12 -25.3(9) 3_776 . . . ? C1 Re P1 C12 154.7(9) . . . . ? P2 Re P1 C12 -117.9(8) . . . . ? P2 Re P1 C12 62.1(8) 3_776 . . . ? P1 Re P1 C12 -127.7(1000) 3_776 . . . ? C1 Re P1 C13 -153.9(8) 3_776 . . . ? C1 Re P1 C13 26.1(8) . . . . ? P2 Re P1 C13 113.5(7) . . . . ? P2 Re P1 C13 -66.5(7) 3_776 . . . ? P1 Re P1 C13 103.7(1000) 3_776 . . . ? C1 Re P1 C11 91.2(7) 3_776 . . . ? C1 Re P1 C11 -88.8(7) . . . . ? P2 Re P1 C11 -1.4(6) . . . . ? P2 Re P1 C11 178.6(6) 3_776 . . . ? P1 Re P1 C11 -11.2(1000) 3_776 . . . ? C1 Re P2 C22 128.5(8) 3_776 . . . ? C1 Re P2 C22 -51.5(8) . . . . ? P2 Re P2 C22 0.0(1000) 3_776 . . . ? P1 Re P2 C22 43.5(7) 3_776 . . . ? P1 Re P2 C22 -136.5(7) . . . . ? C1 Re P2 C23 0.4(8) 3_776 . . . ? C1 Re P2 C23 -179.6(8) . . . . ? P2 Re P2 C23 0.0(1000) 3_776 . . . ? P1 Re P2 C23 -84.6(7) 3_776 . . . ? P1 Re P2 C23 95.4(7) . . . . ? C1 Re P2 C21 -117.4(8) 3_776 . . . ? C1 Re P2 C21 62.6(8) . . . . ? P2 Re P2 C21 0.0(1000) 3_776 . . . ? P1 Re P2 C21 157.7(6) 3_776 . . . ? P1 Re P2 C21 -22.3(6) . . . . ? C23 P2 C22 C222 -157.0(16) . . . . ? C21 P2 C22 C222 -51.3(17) . . . . ? Re P2 C22 C222 66.0(17) . . . . ? C23 P2 C22 C226 28.6(16) . . . . ? C21 P2 C22 C226 134.2(15) . . . . ? Re P2 C22 C226 -108.4(14) . . . . ? C12 P1 C11 C21 163.4(12) . . . . ? C13 P1 C11 C21 -91.1(12) . . . . ? Re P1 C11 C21 32.1(13) . . . . ? P1 C11 C21 P2 -52.4(14) . . . . ? C22 P2 C21 C11 175.1(12) . . . . ? C23 P2 C21 C11 -81.0(13) . . . . ? Re P2 C21 C11 48.4(12) . . . . ? C226 C22 C222 C223 -4.8(29) . . . . ? P2 C22 C222 C223 -179.5(16) . . . . ? C13 P1 C12 C122 151.0(17) . . . . ? C11 P1 C12 C122 -102.6(18) . . . . ? Re P1 C12 C122 16.9(21) . . . . ? C13 P1 C12 C126 -34.6(18) . . . . ? C11 P1 C12 C126 71.7(17) . . . . ? Re P1 C12 C126 -168.8(13) . . . . ? C126 C12 C122 C123 2.1(31) . . . . ? P1 C12 C122 C123 176.6(16) . . . . ? C223 C224 C225 C226 1.7(32) . . . . ? C122 C12 C126 C125 -2.6(31) . . . . ? P1 C12 C126 C125 -177.1(16) . . . . ? C12 C126 C125 C124 3.2(32) . . . . ? C224 C225 C226 C22 -1.8(32) . . . . ? C222 C22 C226 C225 3.2(27) . . . . ? P2 C22 C226 C225 178.0(15) . . . . ? C22 C222 C223 C224 5.0(32) . . . . ? C225 C224 C223 C222 -3.2(32) . . . . ? C12 C122 C123 C124 -2.4(35) . . . . ? C122 C123 C124 C125 2.9(33) . . . . ? C126 C125 C124 C123 -3.2(31) . . . . ? C22 P2 C23 C236 72.6(18) . . . . ? C21 P2 C23 C236 -31.4(18) . . . . ? Re P2 C23 C236 -151.1(14) . . . . ? C22 P2 C23 C232 -103.1(16) . . . . ? C21 P2 C23 C232 152.9(15) . . . . ? Re P2 C23 C232 33.2(18) . . . . ? C12 P1 C13 C136 127.0(17) . . . . ? C11 P1 C13 C136 22.7(18) . . . . ? Re P1 C13 C136 -94.3(16) . . . . ? C12 P1 C13 C132 -51.0(16) . . . . ? C11 P1 C13 C132 -155.3(14) . . . . ? Re P1 C13 C132 87.7(14) . . . . ? C236 C23 C232 C233 -1.7(29) . . . . ? P2 C23 C232 C233 174.2(15) . . . . ? C136 C13 C132 C133 2.0(28) . . . . ? P1 C13 C132 C133 180.0(13) . . . . ? C232 C23 C236 C235 0.7(31) . . . . ? P2 C23 C236 C235 -175.1(17) . . . . ? C23 C232 C233 C234 4.1(31) . . . . ? C235 C234 C233 C232 -5.6(34) . . . . ? C233 C234 C235 C236 4.5(34) . . . . ? C23 C236 C235 C234 -2.2(35) . . . . ? C13 C132 C133 C134 0.6(28) . . . . ? C132 C133 C134 C135 -0.4(31) . . . . ? C132 C13 C136 C135 -4.6(31) . . . . ? P1 C13 C136 C135 177.5(15) . . . . ? C133 C134 C135 C136 -2.3(35) . . . . ? C13 C136 C135 C134 4.9(35) . . . . ? C1 Re C1 N1 11.5(1000) 3_776 . . . ? P2 Re C1 N1 6.5(173) . . . . ? P2 Re C1 N1 -173.5(173) 3_776 . . . ? P1 Re C1 N1 -91.7(174) 3_776 . . . ? P1 Re C1 N1 88.3(174) . . . . ? _refine_diff_density_max 1.572 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.204