# Copyright The Royal Society of Chemistry, 1998 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C43 H38 N3 O P2 Re' _chemical_formula_weight 860.90 _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' 0.0033 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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pnma (No.62)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.816(4) _cell_length_b 21.028(7) _cell_length_c 15.085(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3748.1(20) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 9 _cell_measurement_theta_max 15 _exptl_crystal_description parallelepipeds _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 3.365 _exptl_absorpt_correction_type 'empirical (XEMP in SHELXTL/PC)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.76 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens-Nicolet R3m/V' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.5 _diffrn_reflns_number 3384 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3384 _reflns_number_observed 2590 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3 diffractometer software' _computing_cell_refinement 'P3 diffractometer software' _computing_data_reduction 'P3 diffractometer software' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 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^)+(0.1000P)^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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3367 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_obs 0.0484 _refine_ls_wR_factor_all 0.3022 _refine_ls_wR_factor_obs 0.1299 _refine_ls_goodness_of_fit_all 1.186 _refine_ls_goodness_of_fit_obs 1.259 _refine_ls_restrained_S_all 3.264 _refine_ls_restrained_S_obs 1.309 _refine_ls_shift/esd_max -2.225 _refine_ls_shift/esd_mean 0.009 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 0.18777(4) 0.2500 0.06292(3) 0.0332(2) Uani 1 d S . P1 P 0.0782(2) 0.34491(11) 0.02950(13) 0.0356(5) Uani 1 d . . O1 O 0.1816(7) 0.2500 -0.0713(5) 0.051(2) Uani 1 d S . N1 N 0.3110(5) 0.3157(4) 0.0516(4) 0.040(2) Uani 1 d . . H1A H 0.3758(5) 0.3067(4) 0.0743(4) 0.048 Uiso 1 calc R . N2 N 0.1578(8) 0.2500 0.1756(6) 0.042(2) Uani 1 d S . C1 C 0.1925(8) 0.3952(4) -0.0110(5) 0.044(2) Uani 1 d . . C2 C 0.2996(7) 0.3731(4) 0.0109(5) 0.038(2) Uani 1 d . . C3 C 0.3917(9) 0.4107(5) -0.0162(6) 0.057(3) Uani 1 d . . H3A H 0.4647(9) 0.3967(5) -0.0039(6) 0.068 Uiso 1 calc R . C4 C 0.3778(11) 0.4670(6) -0.0603(6) 0.065(3) Uani 1 d . . H4A H 0.4406(11) 0.4914(6) -0.0752(6) 0.077 Uiso 1 calc R . C5 C 0.2685(12) 0.4880(6) -0.0830(7) 0.071(3) Uani 1 d . . H5A H 0.2579(12) 0.5253(6) -0.1150(7) 0.086 Uiso 1 calc R . C6 C 0.1788(9) 0.4520(6) -0.0567(6) 0.057(3) Uani 1 d . . H6A H 0.1060(9) 0.4660(6) -0.0697(6) 0.068 Uiso 1 calc R . C7 C 0.1431(10) 0.2500 0.2678(7) 0.040(3) Uani 1 d S . C8 C 0.1381(7) 0.3067(6) 0.3133(6) 0.055(3) Uani 1 d . . H8A H 0.1367(7) 0.3452(6) 0.2830(6) 0.065 Uiso 1 calc R . C9 C 0.1350(9) 0.3052(7) 0.4062(7) 0.077(4) Uani 1 d . . H9A H 0.1328(9) 0.3434(7) 0.4373(7) 0.092 Uiso 1 calc R . C10 C 0.1353(15) 0.2500 0.4518(9) 0.086(7) Uani 1 d S . H10A H 0.1356(15) 0.2500 0.5134(9) 0.103 Uiso 1 calc SR . C11 C 0.2751(13) 0.2500 -0.1270(9) 0.066(4) Uani 1 d S . H11A H 0.2504(13) 0.2500 -0.1876(9) 0.099 Uiso 1 calc SR . H11B H 0.3199(13) 0.2127 -0.1159(9) 0.099 Uiso 0.50 calc PR . H11C H 0.3199(13) 0.2873 -0.1159(9) 0.099 Uiso 0.50 calc PR . C12 C -0.0289(9) 0.3524(5) -0.0544(6) 0.049(2) Uani 1 d . . C13 C -0.1305(9) 0.3824(7) -0.0413(7) 0.075(4) Uani 1 d . . H13A H -0.1465(9) 0.3981(7) 0.0150(7) 0.089 Uiso 1 calc R . C14 C -0.2103(11) 0.3905(8) -0.1071(10) 0.093(5) Uani 1 d . . H14A H -0.2818(11) 0.4066(8) -0.0944(10) 0.111 Uiso 1 calc R . C15 C -0.1802(13) 0.3739(7) -0.1927(11) 0.106(6) Uani 1 d . . H15A H -0.2320(13) 0.3798(7) -0.2384(11) 0.127 Uiso 1 calc R . C16 C -0.0731(14) 0.3484(8) -0.2122(9) 0.108(5) Uani 1 d . . H16A H -0.0521(14) 0.3390(8) -0.2701(9) 0.130 Uiso 1 calc R . C17 C -0.0011(12) 0.3380(7) -0.1432(8) 0.100(5) Uani 1 d . . H17A H 0.0696(12) 0.3206(7) -0.1552(8) 0.120 Uiso 1 calc R . C18 C 0.0181(7) 0.3856(4) 0.1257(5) 0.038(2) Uani 1 d . . C19 C 0.0546(8) 0.4432(4) 0.1543(5) 0.049(2) Uani 1 d . . H19A H 0.1117(8) 0.4643(4) 0.1237(5) 0.059 Uiso 1 calc R . C20 C 0.0064(11) 0.4711(5) 0.2299(6) 0.067(3) Uani 1 d . . H20A H 0.0307(11) 0.5109(5) 0.2486(6) 0.080 Uiso 1 calc R . C21 C -0.0730(10) 0.4410(6) 0.2745(6) 0.068(3) Uani 1 d . . H21A H -0.1040(10) 0.4598(6) 0.3247(6) 0.082 Uiso 1 calc R . C22 C -0.1107(9) 0.3821(5) 0.2479(6) 0.055(3) Uani 1 d . . H22A H -0.1671(9) 0.3614(5) 0.2798(6) 0.067 Uiso 1 calc R . C23 C -0.0640(7) 0.3534(5) 0.1731(5) 0.047(2) Uani 1 d . . H23A H -0.0878(7) 0.3132(5) 0.1553(5) 0.057 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 0.0371(3) 0.0438(3) 0.0187(3) 0.000 0.0007(2) 0.000 P1 0.0405(11) 0.0436(12) 0.0227(10) -0.0010(9) -0.0040(9) -0.0023(10) O1 0.056(6) 0.064(6) 0.031(5) 0.000 0.002(4) 0.000 N1 0.032(4) 0.051(4) 0.036(4) 0.004(3) -0.003(3) -0.003(3) N2 0.045(6) 0.062(7) 0.017(5) 0.000 -0.010(4) 0.000 C1 0.059(5) 0.048(5) 0.026(4) 0.009(4) 0.008(4) -0.008(4) C2 0.045(5) 0.042(5) 0.028(4) -0.001(4) 0.000(4) -0.008(4) C3 0.057(6) 0.069(7) 0.045(5) 0.000(5) 0.011(5) -0.018(5) C4 0.076(8) 0.068(7) 0.050(6) 0.010(5) 0.014(5) -0.024(6) C5 0.089(8) 0.071(8) 0.054(6) 0.025(6) 0.015(6) -0.013(7) C6 0.069(7) 0.060(6) 0.042(6) 0.009(5) 0.011(5) 0.001(5) C7 0.029(6) 0.074(9) 0.017(5) 0.000 0.003(5) 0.000 C8 0.044(5) 0.086(7) 0.034(5) -0.015(5) -0.006(4) 0.005(5) C9 0.060(7) 0.132(12) 0.038(6) -0.034(7) 0.000(5) 0.016(8) C10 0.057(10) 0.180(25) 0.019(7) 0.000 0.004(7) 0.000 C11 0.072(9) 0.100(13) 0.026(7) 0.000 0.012(7) 0.000 C12 0.060(6) 0.049(5) 0.039(5) -0.006(4) -0.018(4) -0.001(5) C13 0.043(6) 0.133(12) 0.047(6) 0.004(7) -0.002(5) 0.003(7) C14 0.070(8) 0.134(14) 0.073(9) 0.032(9) -0.018(7) 0.014(8) C15 0.117(12) 0.102(11) 0.098(12) -0.023(9) -0.071(10) 0.027(9) C16 0.145(14) 0.121(12) 0.058(7) -0.014(8) -0.063(9) 0.028(11) C17 0.114(10) 0.126(12) 0.059(7) -0.037(8) -0.041(7) 0.049(10) C18 0.042(4) 0.047(5) 0.025(4) 0.000(4) -0.005(3) 0.007(4) C19 0.065(6) 0.049(5) 0.033(4) -0.003(4) 0.004(4) -0.009(5) C20 0.112(9) 0.056(6) 0.033(5) -0.006(5) -0.010(6) -0.001(7) C21 0.084(8) 0.088(8) 0.033(5) -0.007(6) 0.010(6) 0.022(7) C22 0.049(5) 0.084(8) 0.033(5) 0.005(5) 0.006(4) -0.002(6) C23 0.042(5) 0.057(6) 0.043(5) 0.001(4) 0.004(4) -0.004(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 Re N2 1.736(9) . ? Re N1 2.014(7) . ? Re N1 2.014(7) 7_565 ? Re O1 2.026(8) . ? Re P1 2.432(2) 7_565 ? Re P1 2.432(2) . ? P1 C12 1.797(9) . ? P1 C1 1.821(9) . ? P1 C18 1.827(8) . ? O1 C11 1.39(2) . ? N1 C2 1.362(11) . ? N2 C7 1.401(14) . ? C1 C2 1.388(12) . ? C1 C6 1.389(14) . ? C2 C3 1.405(12) . ? C3 C4 1.37(2) . ? C4 C5 1.41(2) . ? C5 C6 1.36(2) . ? C7 C8 1.377(11) 7_565 ? C7 C8 1.377(11) . ? C8 C9 1.403(13) . ? C9 C10 1.349(15) . ? C10 C9 1.349(15) 7_565 ? C12 C13 1.369(15) . ? C12 C17 1.414(14) . ? C13 C14 1.38(2) . ? C14 C15 1.38(2) . ? C15 C16 1.41(2) . ? C16 C17 1.361(14) . ? C18 C19 1.356(12) . ? C18 C23 1.383(12) . ? C19 C20 1.403(13) . ? C20 C21 1.32(2) . ? C21 C22 1.377(15) . ? C22 C23 1.394(12) . ? 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 N2 Re N1 103.3(3) . . ? N2 Re N1 103.3(3) . 7_565 ? N1 Re N1 86.6(4) . 7_565 ? N2 Re O1 166.2(4) . . ? N1 Re O1 86.7(3) . . ? N1 Re O1 86.7(3) 7_565 . ? N2 Re P1 95.4(2) . 7_565 ? N1 Re P1 158.5(2) . 7_565 ? N1 Re P1 78.7(2) 7_565 7_565 ? O1 Re P1 76.91(14) . 7_565 ? N2 Re P1 95.4(2) . . ? N1 Re P1 78.7(2) . . ? N1 Re P1 158.5(2) 7_565 . ? O1 Re P1 76.91(14) . . ? P1 Re P1 110.32(11) 7_565 . ? C12 P1 C1 103.6(4) . . ? C12 P1 C18 104.1(4) . . ? C1 P1 C18 106.4(4) . . ? C12 P1 Re 126.4(3) . . ? C1 P1 Re 98.7(3) . . ? C18 P1 Re 115.2(3) . . ? C11 O1 Re 125.1(8) . . ? C2 N1 Re 125.1(5) . . ? C7 N2 Re 175.4(9) . . ? C2 C1 C6 120.8(9) . . ? C2 C1 P1 113.7(6) . . ? C6 C1 P1 125.4(8) . . ? N1 C2 C1 119.6(7) . . ? N1 C2 C3 123.6(9) . . ? C1 C2 C3 116.7(8) . . ? C4 C3 C2 122.4(11) . . ? C3 C4 C5 120.0(10) . . ? C6 C5 C4 118.0(10) . . ? C5 C6 C1 122.1(11) . . ? C8 C7 C8 119.9(11) 7_565 . ? C8 C7 N2 120.0(6) 7_565 . ? C8 C7 N2 120.0(6) . . ? C7 C8 C9 118.7(11) . . ? C10 C9 C8 121.9(13) . . ? C9 C10 C9 118.8(14) 7_565 . ? C13 C12 C17 116.1(10) . . ? C13 C12 P1 123.8(8) . . ? C17 C12 P1 119.0(8) . . ? C12 C13 C14 123.5(12) . . ? C13 C14 C15 117.6(13) . . ? C14 C15 C16 121.5(12) . . ? C17 C16 C15 117.7(14) . . ? C16 C17 C12 123.0(13) . . ? C19 C18 C23 119.7(8) . . ? C19 C18 P1 123.2(7) . . ? C23 C18 P1 117.0(7) . . ? C18 C19 C20 120.2(9) . . ? C21 C20 C19 120.3(10) . . ? C20 C21 C22 120.9(10) . . ? C21 C22 C23 119.9(10) . . ? C18 C23 C22 119.0(9) . . ? _refine_diff_density_max 1.550 _refine_diff_density_min -2.188 _refine_diff_density_rms 0.161 data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H35 Cl N3 P2 Re' _chemical_formula_weight 865.32 _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' 0.0033 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) (No.19)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.178(4) _cell_length_b 17.680(6) _cell_length_c 20.254(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3644.6(23) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description parallelepipeds _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 3.530 _exptl_absorpt_correction_type 'empirical (XEMP in SHELXTL/PC)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.90 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens-Nicolet R3m/V' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 1984 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 20.04 _reflns_number_total 1964 _reflns_number_observed 1555 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3 diffractometer software' _computing_cell_refinement 'P3 diffractometer software' _computing_data_reduction 'P3 diffractometer software' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 1964 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all 0.1120 _refine_ls_wR_factor_obs 0.1060 _refine_ls_goodness_of_fit_all 0.779 _refine_ls_goodness_of_fit_obs 0.841 _refine_ls_restrained_S_all 0.779 _refine_ls_restrained_S_obs 0.841 _refine_ls_shift/esd_max 0.005 _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 0.84554(8) 0.88965(5) 0.21950(4) 0.0344(3) Uani 1 d . . Cl Cl 0.6673(6) 0.9399(3) 0.2893(3) 0.0464(14) Uani 1 d . . P1 P 0.8456(7) 0.7639(3) 0.2693(3) 0.0419(15) Uani 1 d . . P2 P 0.9922(6) 0.8668(3) 0.1278(3) 0.037(2) Uani 1 d . . N1 N 0.7030(15) 0.8346(9) 0.1655(8) 0.034(5) Uiso 1 d . . N2 N 0.7915(15) 0.9782(9) 0.1611(8) 0.033(5) Uiso 1 d . . N3 N 0.9617(16) 0.9199(8) 0.2752(9) 0.038(5) Uiso 1 d . . C11 C 0.7196(19) 0.7162(11) 0.2227(12) 0.039(5) Uiso 1 d . . C12 C 0.6810(25) 0.6406(14) 0.2333(12) 0.065(8) Uiso 1 d . . C13 C 0.5745(24) 0.6113(16) 0.1960(11) 0.066(7) Uiso 1 d . . C14 C 0.5119(24) 0.6552(14) 0.1517(12) 0.060(7) Uiso 1 d . . C15 C 0.5554(24) 0.7307(13) 0.1405(11) 0.052(7) Uiso 1 d . . C16 C 0.6614(24) 0.7598(11) 0.1765(10) 0.040(5) Uiso 1 d . . C21 C 0.9241(21) 0.9309(12) 0.0685(10) 0.038(6) Uiso 1 d . . C22 C 0.9643(22) 0.9352(13) 0.0015(11) 0.043(6) Uiso 1 d . . C23 C 0.9139(27) 0.9939(15) -0.0370(13) 0.066(8) Uiso 1 d . . C24 C 0.8259(24) 1.0457(13) -0.0118(10) 0.046(6) Uiso 1 d . . C25 C 0.7862(24) 1.0428(14) 0.0533(12) 0.058(7) Uiso 1 d . . C26 C 0.8290(21) 0.9836(10) 0.0954(9) 0.029(5) Uiso 1 d . . C31 C 1.0396(20) 0.9348(11) 0.3280(10) 0.031(5) Uiso 1 d . . C32 C 1.1621(29) 0.9632(13) 0.3251(12) 0.061(7) Uiso 1 d . . C33 C 1.2364(30) 0.9768(16) 0.3838(14) 0.079(9) Uiso 1 d . . C34 C 1.1799(28) 0.9679(15) 0.4444(13) 0.069(8) Uiso 1 d . . C35 C 1.0526(26) 0.9409(14) 0.4478(13) 0.060(7) Uiso 1 d . . C36 C 0.9842(27) 0.9239(14) 0.3901(13) 0.066(8) Uiso 1 d . . C41 C 0.7893(20) 0.7467(11) 0.3539(8) 0.056(7) Uiso 1 d G . C42 C 0.8636(16) 0.7056(11) 0.3990(11) 0.095(10) Uiso 1 d G . C43 C 0.8155(24) 0.6926(12) 0.4622(10) 0.141(15) Uiso 1 d G . C44 C 0.6932(26) 0.7208(14) 0.4804(8) 0.115(13) Uiso 1 d G . C45 C 0.6190(18) 0.7619(13) 0.4353(12) 0.125(13) Uiso 1 d G . C46 C 0.6670(19) 0.7748(11) 0.3721(11) 0.111(11) Uiso 1 d G . C51 C 1.0000(13) 0.7146(9) 0.2656(8) 0.055(7) Uiso 1 d G . C52 C 1.0176(14) 0.6539(9) 0.2229(8) 0.064(7) Uiso 1 d G . C53 C 1.1392(18) 0.6185(8) 0.2188(8) 0.077(7) Uiso 1 d G . C54 C 1.2432(13) 0.6437(11) 0.2575(9) 0.093(11) Uiso 1 d G . C55 C 1.2256(15) 0.7043(11) 0.3002(8) 0.077(9) Uiso 1 d G . C56 C 1.1040(18) 0.7398(8) 0.3043(7) 0.065(8) Uiso 1 d G . C61 C 1.0108(17) 0.7775(7) 0.0835(7) 0.049(7) Uiso 1 d G . C62 C 0.8978(12) 0.7407(10) 0.0622(9) 0.063(8) Uiso 1 d G . C63 C 0.9075(15) 0.6716(9) 0.0298(9) 0.072(8) Uiso 1 d G . C64 C 1.0300(20) 0.6393(7) 0.0188(8) 0.079(9) Uiso 1 d G . C65 C 1.1430(14) 0.6761(10) 0.0401(9) 0.087(9) Uiso 1 d G . C66 C 1.1333(13) 0.7452(10) 0.0725(8) 0.066(8) Uiso 1 d G . C71 C 1.1586(12) 0.9003(8) 0.1433(7) 0.045(6) Uiso 1 d G . C72 C 1.1971(14) 0.9704(8) 0.1190(7) 0.059(8) Uiso 1 d G . C73 C 1.3220(16) 0.9980(7) 0.1327(8) 0.057(7) Uiso 1 d G . C74 C 1.4085(12) 0.9555(9) 0.1707(8) 0.059(7) Uiso 1 d G . C75 C 1.3700(14) 0.8854(9) 0.1950(7) 0.075(8) Uiso 1 d G . C76 C 1.2451(15) 0.8578(7) 0.1813(7) 0.050(7) Uiso 1 d G . 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 0.0335(5) 0.0303(5) 0.0394(5) -0.0016(5) 0.0009(5) 0.0015(5) Cl 0.043(3) 0.046(3) 0.050(4) -0.011(3) 0.002(4) 0.003(3) P1 0.045(3) 0.035(3) 0.046(4) 0.000(3) 0.002(4) 0.002(4) P2 0.030(3) 0.039(4) 0.043(4) 0.006(3) -0.002(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N3 1.72(2) . ? Re N2 2.04(2) . ? Re N1 2.06(2) . ? Re P2 2.416(6) . ? Re P1 2.441(6) . ? Re Cl 2.465(6) . ? P1 C51 1.799(13) . ? P1 C11 1.80(2) . ? P1 C41 1.83(2) . ? P2 C61 1.825(12) . ? P2 C21 1.79(2) . ? P2 C71 1.822(12) . ? N1 C16 1.41(2) . ? N2 C26 1.39(2) . ? N3 C31 1.36(3) . ? C11 C16 1.35(3) . ? C11 C12 1.41(3) . ? C12 C13 1.42(3) . ? C13 C14 1.35(3) . ? C14 C15 1.43(3) . ? C15 C16 1.40(3) . ? C21 C22 1.42(3) . ? C21 C26 1.45(3) . ? C22 C23 1.40(3) . ? C23 C24 1.38(3) . ? C24 C25 1.38(3) . ? C25 C26 1.42(3) . ? C31 C32 1.35(3) . ? C31 C36 1.39(3) . ? C32 C33 1.43(3) . ? C33 C34 1.36(4) . ? C34 C35 1.38(4) . ? C35 C36 1.39(3) . ? C41 C42 1.39 . ? C41 C46 1.39 . ? C42 C43 1.39 . ? C43 C44 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C51 C52 1.39 . ? C51 C56 1.39 . ? C52 C53 1.39 . ? C53 C54 1.39 . ? C54 C55 1.39 . ? C55 C56 1.39 . ? C61 C62 1.39 . ? C61 C66 1.39 . ? C62 C63 1.39 . ? C63 C64 1.39 . ? C64 C65 1.39 . ? C65 C66 1.39 . ? C71 C72 1.39 . ? C71 C76 1.39 . ? C72 C73 1.39 . ? C73 C74 1.39 . ? C74 C75 1.39 . ? C75 C76 1.39 . ? 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 N3 Re N2 109.1(7) . . ? N3 Re N1 168.3(7) . . ? N2 Re N1 82.2(7) . . ? N3 Re P2 97.5(6) . . ? N2 Re P2 81.3(5) . . ? N1 Re P2 87.0(5) . . ? N3 Re P1 90.7(5) . . ? N2 Re P1 159.9(5) . . ? N1 Re P1 77.9(5) . . ? P2 Re P1 99.5(2) . . ? N3 Re Cl 91.0(5) . . ? N2 Re Cl 81.8(5) . . ? N1 Re Cl 87.5(5) . . ? P2 Re Cl 162.8(2) . . ? P1 Re Cl 95.2(2) . . ? C51 P1 C11 111.9(9) . . ? C51 P1 C41 103.4(9) . . ? C11 P1 C41 100.9(10) . . ? C51 P1 Re 115.1(6) . . ? C11 P1 Re 102.1(7) . . ? C41 P1 Re 122.5(7) . . ? C61 P2 C21 104.9(9) . . ? C61 P2 C71 105.6(8) . . ? C21 P2 C71 105.6(9) . . ? C61 P2 Re 125.9(6) . . ? C21 P2 Re 99.8(7) . . ? C71 P2 Re 112.8(5) . . ? C16 N1 Re 124.8(14) . . ? C26 N2 Re 122.3(13) . . ? C31 N3 Re 168.2(15) . . ? C16 C11 C12 121.7(21) . . ? C16 C11 P1 114.1(16) . . ? C12 C11 P1 124.2(18) . . ? C13 C12 C11 118.5(24) . . ? C14 C13 C12 120.5(26) . . ? C13 C14 C15 119.9(24) . . ? C14 C15 C16 120.0(21) . . ? C11 C16 C15 119.3(20) . . ? C11 C16 N1 121.0(20) . . ? C15 C16 N1 119.6(19) . . ? C22 C21 C26 121.2(19) . . ? C22 C21 P2 124.3(17) . . ? C26 C21 P2 114.4(15) . . ? C23 C22 C21 117.8(21) . . ? C22 C23 C24 121.8(23) . . ? C23 C24 C25 121.3(23) . . ? C24 C25 C26 120.8(22) . . ? N2 C26 C25 122.9(19) . . ? N2 C26 C21 120.0(17) . . ? C25 C26 C21 117.0(18) . . ? C32 C31 N3 125.3(20) . . ? C32 C31 C36 117.9(21) . . ? N3 C31 C36 116.7(20) . . ? C31 C32 C33 121.1(24) . . ? C34 C33 C32 120.3(27) . . ? C33 C34 C35 118.7(27) . . ? C36 C35 C34 120.1(25) . . ? C35 C36 C31 121.7(24) . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 122.1(14) . . ? C46 C41 P1 117.9(14) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P1 120.8(11) . . ? C56 C51 P1 119.1(11) . . ? C51 C52 C53 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P2 118.2(11) . . ? C66 C61 P2 121.8(11) . . ? C61 C62 C63 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P2 119.4(9) . . ? C76 C71 P2 120.6(9) . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? _refine_diff_density_max 1.059 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.134 data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C47 H45 N3 O1.50 P2 Re' _chemical_formula_weight 924.00 _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' 0.0033 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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.307(4) _cell_length_b 13.333(6) _cell_length_c 27.743(11) _cell_angle_alpha 88.64(3) _cell_angle_beta 80.65(3) _cell_angle_gamma 79.48(3) _cell_volume 4057.4(28) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description parallelepipeds _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method ? _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 3.115 _exptl_absorpt_correction_type 'empirical (XEMP in SHELXTL/PC)' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.83 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens-Nicolet R3m/V' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 9106 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9099 _reflns_number_observed 7612 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3 diffractometer software' _computing_cell_refinement 'P3 diffractometer software' _computing_data_reduction 'P3 diffractometer software' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.1000P)^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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9098 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_obs 0.0505 _refine_ls_wR_factor_all 0.1642 _refine_ls_wR_factor_obs 0.1452 _refine_ls_goodness_of_fit_all 1.321 _refine_ls_goodness_of_fit_obs 1.304 _refine_ls_restrained_S_all 1.322 _refine_ls_restrained_S_obs 1.304 _refine_ls_shift/esd_max -6.111 _refine_ls_shift/esd_mean 0.010 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 0.92915(5) 0.24809(4) 0.39160(2) 0.0302(2) Uani 1 d . . P1A P 0.7304(3) 0.3435(3) 0.42555(13) 0.0324(8) Uani 1 d . . P2A P 0.9253(3) 0.2204(3) 0.30632(13) 0.0345(8) Uani 1 d . . O1A O 0.8302(8) 0.1379(6) 0.3920(3) 0.029(2) Uani 1 d . . N1A N 0.9287(10) 0.2192(8) 0.4650(4) 0.033(3) Uani 1 d . . N2A N 1.0792(11) 0.1311(8) 0.3731(5) 0.042(3) Uani 1 d . . N3A N 0.9879(9) 0.3594(7) 0.3824(4) 0.036(3) Uani 1 d . . C1A C 0.7138(13) 0.2899(10) 0.4859(5) 0.038(3) Uani 1 d . . C2A C 0.8210(13) 0.2341(10) 0.4986(5) 0.040(3) Uani 1 d . . C3A C 0.8128(14) 0.1974(10) 0.5483(5) 0.045(4) Uani 1 d . . H3AA H 0.8817(14) 0.1614(10) 0.5594(5) 0.054 Uiso 1 calc R . C4A C 0.7023(15) 0.2160(11) 0.5792(5) 0.047(4) Uani 1 d . . H4AA H 0.6983(15) 0.1905(11) 0.6108(5) 0.057 Uiso 1 calc R . C5A C 0.5984(14) 0.2702(11) 0.5655(5) 0.047(4) Uani 1 d . . H5AA H 0.5262(14) 0.2824(11) 0.5877(5) 0.056 Uiso 1 calc R . C6A C 0.6020(13) 0.3062(10) 0.5188(5) 0.038(3) Uani 1 d . . H6AA H 0.5314(13) 0.3413(10) 0.5087(5) 0.045 Uiso 1 calc R . C7A C 1.0368(12) 0.1718(11) 0.4854(5) 0.043(4) Uani 1 d . . H7AA H 1.0303(12) 0.1021(11) 0.4947(5) 0.051 Uiso 1 calc R . H7AB H 1.0413(12) 0.2088(11) 0.5145(5) 0.051 Uiso 1 calc R . C8A C 1.1532(13) 0.1718(11) 0.4483(6) 0.047(4) Uani 1 d . . H8AA H 1.1528(13) 0.2398(11) 0.4351(6) 0.056 Uiso 1 calc R . H8AB H 1.2235(13) 0.1540(11) 0.4648(6) 0.056 Uiso 1 calc R . C9A C 1.1644(13) 0.0988(11) 0.4077(6) 0.046(4) Uani 1 d . . H9AA H 1.2471(13) 0.0892(11) 0.3899(6) 0.055 Uiso 1 calc R . H9AB H 1.1507(13) 0.0334(11) 0.4213(6) 0.055 Uiso 1 calc R . C10A C 1.0129(14) 0.0936(10) 0.3000(5) 0.043(4) Uani 1 d . . C11A C 1.0853(12) 0.0684(10) 0.3362(5) 0.038(3) Uani 1 d . . C12A C 1.1672(15) -0.0306(12) 0.3299(6) 0.057(4) Uani 1 d . . H12A H 1.2185(15) -0.0515(12) 0.3527(6) 0.068 Uiso 1 calc R . C13A C 1.1696(18) -0.0919(13) 0.2919(7) 0.068(5) Uani 1 d . . H13A H 1.2218(18) -0.1548(13) 0.2893(7) 0.081 Uiso 1 calc R . C14A C 1.0975(16) -0.0645(12) 0.2568(7) 0.059(4) Uani 1 d . . H14A H 1.1008(16) -0.1082(12) 0.2308(7) 0.071 Uiso 1 calc R . C15A C 1.0197(16) 0.0289(12) 0.2605(6) 0.057(4) Uani 1 d . . H15A H 0.9717(16) 0.0487(12) 0.2365(6) 0.069 Uiso 1 calc R . C16A C 1.0138(13) 0.4579(10) 0.3763(6) 0.046(4) Uani 1 d . . C17A C 1.0510(13) 0.5006(12) 0.4147(6) 0.047(4) Uani 1 d . . H17A H 1.0603(13) 0.4632(12) 0.4430(6) 0.057 Uiso 1 calc R . C18A C 1.0745(15) 0.5985(13) 0.4113(7) 0.058(4) Uani 1 d . . H18A H 1.0948(15) 0.6290(13) 0.4379(7) 0.069 Uiso 1 calc R . C19A C 1.0675(16) 0.6508(13) 0.3678(8) 0.071(6) Uani 1 d . . H19A H 1.0866(16) 0.7159(13) 0.3647(8) 0.085 Uiso 1 calc R . C20A C 1.0337(16) 0.6087(12) 0.3304(8) 0.064(5) Uani 1 d . . H20A H 1.0268(16) 0.6454(12) 0.3018(8) 0.077 Uiso 1 calc R . C21A C 1.0096(14) 0.5135(11) 0.3338(6) 0.052(4) Uani 1 d . . H21A H 0.9895(14) 0.4843(11) 0.3068(6) 0.062 Uiso 1 calc R . C22A C 0.8471(15) 0.0464(11) 0.4203(6) 0.049(4) Uiso 1 d . . H22A H 0.7951(15) 0.0573(11) 0.4519(6) 0.059 Uiso 1 calc R . H22B H 0.9311(15) 0.0302(11) 0.4258(6) 0.059 Uiso 1 calc R . C23A C 0.8176(19) -0.0397(14) 0.3951(7) 0.077(6) Uiso 1 d . . H23A H 0.8294(19) -0.1000(14) 0.4147(7) 0.116 Uiso 1 calc R . H23B H 0.8700(19) -0.0513(14) 0.3641(7) 0.116 Uiso 1 calc R . H23C H 0.7342(19) -0.0240(14) 0.3901(7) 0.116 Uiso 1 calc R . C24A C 0.7271(13) 0.4791(10) 0.4342(5) 0.037(3) Uiso 1 d . . C25A C 0.7291(14) 0.5193(11) 0.4792(5) 0.045(4) Uiso 1 d . . H25A H 0.7269(14) 0.4774(11) 0.5065(5) 0.054 Uiso 1 calc R . C26A C 0.7345(15) 0.6197(12) 0.4844(6) 0.054(4) Uiso 1 d . . H26A H 0.7347(15) 0.6464(12) 0.5151(6) 0.065 Uiso 1 calc R . C27A C 0.7396(15) 0.6822(13) 0.4433(6) 0.058(4) Uiso 1 d . . H27A H 0.7429(15) 0.7508(13) 0.4466(6) 0.069 Uiso 1 calc R . C28A C 0.7398(14) 0.6440(11) 0.3999(6) 0.050(4) Uiso 1 d . . H28A H 0.7440(14) 0.6859(11) 0.3726(6) 0.060 Uiso 1 calc R . C29A C 0.7338(14) 0.5425(11) 0.3944(6) 0.045(4) Uiso 1 d . . H29A H 0.7344(14) 0.5168(11) 0.3635(6) 0.054 Uiso 1 calc R . C30A C 0.5877(13) 0.3387(10) 0.4041(5) 0.039(3) Uiso 1 d . . C31A C 0.4981(13) 0.4251(10) 0.4015(5) 0.041(3) Uiso 1 d . . H31A H 0.5128(13) 0.4890(10) 0.4088(5) 0.049 Uiso 1 calc R . C32A C 0.3847(16) 0.4162(12) 0.3878(6) 0.056(4) Uiso 1 d . . H32A H 0.3261(16) 0.4738(12) 0.3849(6) 0.068 Uiso 1 calc R . C33A C 0.3644(16) 0.3235(11) 0.3793(6) 0.053(4) Uiso 1 d . . H33A H 0.2862(16) 0.3190(11) 0.3743(6) 0.064 Uiso 1 calc R . C34A C 0.4451(20) 0.2363(16) 0.3772(8) 0.087(6) Uiso 1 d . . H34A H 0.4303(20) 0.1746(16) 0.3668(8) 0.104 Uiso 1 calc R . C35A C 0.5526(15) 0.2477(12) 0.3920(6) 0.051(4) Uiso 1 d . . H35A H 0.6087(15) 0.1880(12) 0.3943(6) 0.061 Uiso 1 calc R . C36A C 1.0139(13) 0.2883(10) 0.2604(5) 0.038(3) Uiso 1 d . . C37A C 0.9757(15) 0.3233(11) 0.2170(6) 0.051(4) Uiso 1 d . . H37A H 0.9001(15) 0.3137(11) 0.2109(6) 0.061 Uiso 1 calc R . C38A C 1.0487(17) 0.3725(13) 0.1826(7) 0.066(5) Uiso 1 d . . H38A H 1.0231(17) 0.3950(13) 0.1533(7) 0.079 Uiso 1 calc R . C39A C 1.1591(18) 0.3871(13) 0.1925(7) 0.069(5) Uiso 1 d . . H39A H 1.2069(18) 0.4220(13) 0.1701(7) 0.083 Uiso 1 calc R . C40A C 1.2027(19) 0.3506(14) 0.2358(7) 0.073(5) Uiso 1 d . . H40A H 1.2791(19) 0.3591(14) 0.2415(7) 0.088 Uiso 1 calc R . C41A C 1.1277(14) 0.3014(11) 0.2701(6) 0.049(4) Uiso 1 d . . H41A H 1.1535(14) 0.2775(11) 0.2991(6) 0.059 Uiso 1 calc R . C42A C 0.7806(13) 0.2277(10) 0.2859(5) 0.039(3) Uiso 1 d . . C43A C 0.7089(14) 0.3236(11) 0.2824(6) 0.048(4) Uiso 1 d . . H43A H 0.7380(14) 0.3816(11) 0.2894(6) 0.058 Uiso 1 calc R . C44A C 0.5984(16) 0.3333(13) 0.2692(6) 0.057(4) Uiso 1 d . . H44A H 0.5518(16) 0.3979(13) 0.2669(6) 0.069 Uiso 1 calc R . C45A C 0.5536(17) 0.2479(12) 0.2589(6) 0.060(4) Uiso 1 d . . H45A H 0.4793(17) 0.2554(12) 0.2477(6) 0.072 Uiso 1 calc R . C46A C 0.6180(16) 0.1520(13) 0.2652(6) 0.061(5) Uiso 1 d . . H46A H 0.5852(16) 0.0946(13) 0.2604(6) 0.073 Uiso 1 calc R . C47A C 0.7326(14) 0.1416(11) 0.2788(5) 0.048(4) Uiso 1 d . . H47A H 0.7770(14) 0.0770(11) 0.2831(5) 0.058 Uiso 1 calc R . Re2 Re 0.32476(4) 0.24969(4) 0.90335(2) 0.0279(2) Uani 1 d . . P1B P 0.3650(3) 0.0992(3) 0.85171(13) 0.0326(8) Uani 1 d . . P2B P 0.4434(3) 0.3696(3) 0.86084(12) 0.0315(8) Uani 1 d . . O1B O 0.2261(7) 0.2902(6) 0.8498(3) 0.032(2) Uani 1 d . . N1B N 0.1850(10) 0.1749(8) 0.9366(4) 0.038(3) Uani 1 d . . N2B N 0.2359(10) 0.3857(7) 0.9373(4) 0.033(3) Uani 1 d . . N3B N 0.4361(10) 0.2072(8) 0.9404(4) 0.032(3) Uani 1 d . . C1B C 0.2291(12) 0.0475(9) 0.8726(5) 0.034(3) Uani 1 d . . C2B C 0.1540(12) 0.0975(9) 0.9161(5) 0.031(3) Uani 1 d . . C3B C 0.0406(13) 0.0597(11) 0.9316(6) 0.046(4) Uani 1 d . . H3BA H -0.0147(13) 0.0906(11) 0.9579(6) 0.055 Uiso 1 calc R . C4B C 0.0147(15) -0.0204(12) 0.9080(7) 0.059(5) Uani 1 d . . H4BA H -0.0555(15) -0.0454(12) 0.9206(7) 0.071 Uiso 1 calc R . C5B C 0.0870(16) -0.0669(12) 0.8663(6) 0.052(4) Uani 1 d . . H5BA H 0.0641(16) -0.1186(12) 0.8500(6) 0.062 Uiso 1 calc R . C6B C 0.1966(14) -0.0318(11) 0.8500(5) 0.045(4) Uani 1 d . . H6BA H 0.2489(14) -0.0632(11) 0.8230(5) 0.053 Uiso 1 calc R . C7B C 0.1094(14) 0.2096(11) 0.9822(5) 0.045(4) Uani 1 d . . H7BA H 0.1048(14) 0.1515(11) 1.0038(5) 0.055 Uiso 1 calc R . H7BB H 0.0276(14) 0.2366(11) 0.9761(5) 0.055 Uiso 1 calc R . C8B C 0.1546(14) 0.2909(10) 1.0082(5) 0.047(4) Uani 1 d . . H8BA H 0.1069(14) 0.3026(10) 1.0405(5) 0.057 Uiso 1 calc R . H8BB H 0.2388(14) 0.2665(10) 1.0120(5) 0.057 Uiso 1 calc R . C9B C 0.1460(15) 0.3902(10) 0.9808(5) 0.047(4) Uani 1 d . . H9BA H 0.0654(15) 0.4083(10) 0.9719(5) 0.056 Uiso 1 calc R . H9BB H 0.1563(15) 0.4434(10) 1.0022(5) 0.056 Uiso 1 calc R . C10B C 0.3354(12) 0.4868(9) 0.8759(5) 0.033(3) Uani 1 d . . C11B C 0.2424(11) 0.4789(10) 0.9149(4) 0.030(3) Uani 1 d . . C12B C 0.1580(13) 0.5711(10) 0.9294(6) 0.044(4) Uani 1 d . . H12B H 0.0947(13) 0.5706(10) 0.9553(6) 0.053 Uiso 1 calc R . C13B C 0.1710(14) 0.6608(11) 0.9048(6) 0.048(4) Uani 1 d . . H13B H 0.1162(14) 0.7201(11) 0.9151(6) 0.057 Uiso 1 calc R . C14B C 0.2597(14) 0.6660(11) 0.8664(6) 0.049(4) Uani 1 d . . H14B H 0.2638(14) 0.7274(11) 0.8501(6) 0.059 Uiso 1 calc R . C15B C 0.3467(13) 0.5773(10) 0.8511(5) 0.043(4) Uani 1 d . . H15B H 0.4097(13) 0.5796(10) 0.8252(5) 0.052 Uiso 1 calc R . C16B C 0.5237(12) 0.1841(10) 0.9683(5) 0.034(3) Uani 1 d . . C17B C 0.5893(15) 0.0879(14) 0.9724(6) 0.061(5) Uani 1 d . . H17B H 0.5725(15) 0.0342(14) 0.9554(6) 0.074 Uiso 1 calc R . C18B C 0.6813(17) 0.0690(17) 1.0016(7) 0.080(6) Uani 1 d . . H18B H 0.7243(17) 0.0033(17) 1.0046(7) 0.096 Uiso 1 calc R . C19B C 0.7056(18) 0.1476(19) 1.0250(6) 0.078(6) Uani 1 d . . H19B H 0.7701(18) 0.1364(19) 1.0426(6) 0.094 Uiso 1 calc R . C20B C 0.6387(17) 0.2440(16) 1.0238(7) 0.074(6) Uani 1 d . . H20B H 0.6534(17) 0.2966(16) 1.0421(7) 0.089 Uiso 1 calc R . C21B C 0.5525(17) 0.2602(13) 0.9959(6) 0.060(5) Uani 1 d . . H21B H 0.5084(17) 0.3260(13) 0.9947(6) 0.072 Uiso 1 calc R . C22B C 0.1016(14) 0.3315(11) 0.8562(6) 0.048(4) Uiso 1 d . . H22C H 0.0869(14) 0.3936(11) 0.8754(6) 0.057 Uiso 1 calc R . H22D H 0.0568(14) 0.2837(11) 0.8745(6) 0.057 Uiso 1 calc R . C23B C 0.0548(22) 0.3544(17) 0.8106(8) 0.095(7) Uiso 1 d . . H23D H -0.0306(22) 0.3824(17) 0.8176(8) 0.143 Uiso 1 calc R . H23E H 0.0669(22) 0.2929(17) 0.7917(8) 0.143 Uiso 1 calc R . H23F H 0.0973(22) 0.4029(17) 0.7925(8) 0.143 Uiso 1 calc R . C24B C 0.3717(13) 0.1089(10) 0.7862(5) 0.039(3) Uiso 1 d . . C25B C 0.2705(13) 0.1328(10) 0.7657(5) 0.040(3) Uiso 1 d . . H25B H 0.1952(13) 0.1445(10) 0.7859(5) 0.048 Uiso 1 calc R . C26B C 0.2734(15) 0.1408(11) 0.7163(6) 0.050(4) Uiso 1 d . . H26B H 0.2009(15) 0.1572(11) 0.7037(6) 0.060 Uiso 1 calc R . C27B C 0.3828(15) 0.1248(12) 0.6850(6) 0.056(4) Uiso 1 d . . H27B H 0.3839(15) 0.1295(12) 0.6515(6) 0.068 Uiso 1 calc R . C28B C 0.4904(18) 0.1019(13) 0.7033(7) 0.067(5) Uiso 1 d . . H28B H 0.5649(18) 0.0923(13) 0.6825(7) 0.080 Uiso 1 calc R . C29B C 0.4852(15) 0.0934(11) 0.7544(6) 0.051(4) Uiso 1 d . . H29B H 0.5571(15) 0.0773(11) 0.7674(6) 0.061 Uiso 1 calc R . C30B C 0.4984(13) 0.0006(10) 0.8587(5) 0.037(3) Uiso 1 d . . C31B C 0.4919(18) -0.0986(13) 0.8691(6) 0.065(5) Uiso 1 d . . H31B H 0.4172(18) -0.1199(13) 0.8719(6) 0.078 Uiso 1 calc R . C32B C 0.5976(23) -0.1703(18) 0.8757(9) 0.100(7) Uiso 1 d . . H32B H 0.5922(23) -0.2364(18) 0.8861(9) 0.120 Uiso 1 calc R . C33B C 0.7053(21) -0.1391(16) 0.8665(8) 0.083(6) Uiso 1 d . . H33B H 0.7763(21) -0.1866(16) 0.8674(8) 0.100 Uiso 1 calc R . C34B C 0.7139(18) -0.0421(13) 0.8561(6) 0.065(5) Uiso 1 d . . H34B H 0.7900(18) -0.0230(13) 0.8520(6) 0.078 Uiso 1 calc R . C35B C 0.6124(15) 0.0305(13) 0.8515(6) 0.056(4) Uiso 1 d . . H35B H 0.6196(15) 0.0976(13) 0.8437(6) 0.067 Uiso 1 calc R . C36B C 0.5788(14) 0.3848(11) 0.8871(5) 0.045(4) Uiso 1 d . . C37B C 0.5783(16) 0.4727(12) 0.9126(6) 0.057(4) Uiso 1 d . . C38B C 0.6791(21) 0.4770(16) 0.9347(8) 0.084(6) Uiso 1 d . . C39B C 0.7862(19) 0.3957(15) 0.9289(7) 0.077(6) Uiso 1 d . . C40B C 0.7734(17) 0.3130(12) 0.9031(6) 0.059(4) Uiso 1 d . . C41B C 0.6737(13) 0.3051(10) 0.8811(5) 0.040(3) Uiso 1 d . . C42B C 0.4928(13) 0.3727(10) 0.7944(5) 0.040(3) Uiso 1 d . . C43B C 0.4079(17) 0.3617(13) 0.7649(7) 0.063(5) Uiso 1 d . . C44B C 0.4472(21) 0.3634(15) 0.7129(8) 0.084(6) Uiso 1 d . . C45B C 0.5636(19) 0.3788(14) 0.6951(7) 0.074(5) Uiso 1 d . . C46B C 0.6426(21) 0.3943(16) 0.7229(8) 0.087(6) Uiso 1 d . . C47B C 0.6089(18) 0.3920(13) 0.7751(7) 0.067(5) Uiso 1 d . . OW O 0.5382(12) 0.0155(9) 0.5460(5) 0.073(3) Uiso 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 Re1 0.0264(3) 0.0304(3) 0.0345(4) 0.0055(2) -0.0057(3) -0.0069(2) P1A 0.028(2) 0.035(2) 0.036(2) 0.0066(15) -0.006(2) -0.010(2) P2A 0.033(2) 0.038(2) 0.033(2) 0.0034(15) -0.009(2) -0.005(2) O1A 0.028(5) 0.027(4) 0.032(5) 0.006(4) -0.013(4) -0.001(4) N1A 0.024(6) 0.043(6) 0.031(6) 0.014(5) -0.003(5) -0.005(5) N2A 0.035(7) 0.035(6) 0.063(8) -0.001(6) -0.020(6) -0.009(5) N3A 0.016(6) 0.027(6) 0.059(8) -0.001(5) 0.007(5) -0.002(5) C1A 0.049(9) 0.032(7) 0.034(8) 0.012(6) -0.010(7) -0.009(7) C2A 0.037(8) 0.030(7) 0.055(9) 0.012(6) -0.006(7) -0.015(7) C3A 0.051(10) 0.037(8) 0.047(9) 0.012(7) -0.013(8) -0.010(7) C4A 0.058(11) 0.051(9) 0.031(8) 0.004(7) 0.003(8) -0.018(8) C5A 0.045(10) 0.064(10) 0.028(8) 0.007(7) 0.012(7) -0.020(8) C6A 0.031(8) 0.049(8) 0.032(8) -0.003(6) -0.002(6) -0.004(7) C7A 0.032(8) 0.052(9) 0.046(9) 0.000(7) -0.008(7) -0.013(7) C8A 0.037(9) 0.054(9) 0.058(10) 0.010(7) -0.035(8) -0.005(7) C9A 0.028(8) 0.049(9) 0.059(10) 0.005(7) -0.014(7) 0.001(7) C10A 0.041(9) 0.033(7) 0.050(9) 0.008(6) 0.004(8) -0.002(7) C11A 0.024(7) 0.036(7) 0.048(9) 0.005(7) 0.005(7) -0.005(6) C12A 0.044(10) 0.061(10) 0.058(11) 0.005(8) -0.009(8) 0.007(8) C13A 0.070(13) 0.051(10) 0.071(13) -0.001(9) -0.011(11) 0.018(9) C14A 0.057(11) 0.050(9) 0.067(12) -0.014(8) -0.007(9) 0.001(9) C15A 0.059(11) 0.053(9) 0.056(11) -0.003(8) -0.010(9) 0.001(9) C16A 0.029(8) 0.037(8) 0.076(12) 0.001(8) -0.008(8) -0.016(7) C17A 0.037(9) 0.065(10) 0.041(9) -0.002(7) 0.003(7) -0.019(8) C18A 0.044(10) 0.061(10) 0.074(12) -0.012(9) -0.020(9) -0.014(8) C19A 0.052(11) 0.042(9) 0.106(17) 0.005(10) 0.032(11) -0.017(9) C20A 0.059(12) 0.045(10) 0.082(14) 0.010(9) 0.008(10) -0.012(9) C21A 0.044(9) 0.053(9) 0.053(10) 0.004(8) 0.020(8) -0.019(8) Re2 0.0198(3) 0.0349(3) 0.0267(3) 0.0023(2) -0.0008(2) -0.0019(2) P1B 0.026(2) 0.036(2) 0.034(2) 0.0015(15) -0.002(2) -0.004(2) P2B 0.025(2) 0.039(2) 0.028(2) 0.0016(14) 0.0036(15) -0.006(2) O1B 0.017(4) 0.046(5) 0.033(5) 0.012(4) -0.014(4) 0.002(4) N1B 0.026(6) 0.036(6) 0.039(7) 0.012(5) 0.023(5) 0.005(5) N2B 0.034(6) 0.029(6) 0.031(6) 0.002(4) -0.005(5) 0.004(5) N3B 0.039(7) 0.037(6) 0.021(6) 0.006(4) -0.019(5) -0.001(5) C1B 0.029(7) 0.028(7) 0.038(8) 0.002(6) 0.011(6) -0.008(6) C2B 0.026(7) 0.030(7) 0.034(7) 0.006(6) -0.001(6) -0.004(6) C3B 0.034(8) 0.045(8) 0.057(10) 0.013(7) -0.001(7) -0.012(7) C4B 0.042(10) 0.063(11) 0.083(14) 0.041(10) -0.028(10) -0.025(9) C5B 0.068(12) 0.053(9) 0.043(9) 0.010(7) -0.017(9) -0.026(9) C6B 0.049(10) 0.051(9) 0.037(8) 0.010(7) -0.005(7) -0.022(8) C7B 0.040(9) 0.051(9) 0.041(9) 0.012(7) -0.002(7) -0.001(7) C8B 0.041(9) 0.048(9) 0.044(9) 0.005(7) 0.006(7) 0.003(7) C9B 0.056(10) 0.040(8) 0.042(9) -0.004(6) -0.001(8) -0.009(7) C10B 0.031(8) 0.037(7) 0.032(7) 0.001(6) -0.018(6) -0.002(6) C11B 0.012(6) 0.046(8) 0.022(7) 0.007(5) 0.011(5) 0.004(6) C12B 0.036(8) 0.045(8) 0.050(9) -0.008(7) 0.000(7) -0.010(7) C13B 0.042(9) 0.042(8) 0.060(11) -0.009(7) -0.020(8) 0.003(7) C14B 0.048(10) 0.044(8) 0.050(10) 0.005(7) 0.001(8) -0.004(8) C15B 0.038(9) 0.047(8) 0.040(8) 0.000(7) 0.016(7) -0.014(7) C16B 0.022(7) 0.044(8) 0.034(8) 0.006(6) -0.009(6) 0.002(6) C17B 0.047(10) 0.075(12) 0.059(11) 0.016(9) -0.012(9) -0.001(9) C18B 0.052(12) 0.110(16) 0.061(13) 0.029(12) -0.010(10) 0.023(12) C19B 0.061(13) 0.148(20) 0.037(10) 0.000(11) -0.038(9) -0.021(14) C20B 0.055(12) 0.091(14) 0.084(15) 0.005(11) -0.034(11) -0.014(11) C21B 0.065(12) 0.066(11) 0.048(10) -0.001(8) -0.013(9) -0.005(10) _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 N3A 1.731(10) . ? Re1 O1A 2.001(8) . ? Re1 N1A 2.061(10) . ? Re1 N2A 2.089(12) . ? Re1 P2A 2.412(4) . ? Re1 P1A 2.425(4) . ? P1A C1A 1.799(13) . ? P1A C30A 1.820(14) . ? P1A C24A 1.822(13) . ? P2A C10A 1.794(14) . ? P2A C42A 1.803(14) . ? P2A C36A 1.820(14) . ? O1A C22A 1.43(2) . ? N1A C2A 1.39(2) . ? N1A C7A 1.46(2) . ? N2A C11A 1.32(2) . ? N2A C9A 1.47(2) . ? N3A C16A 1.40(2) . ? C1A C2A 1.39(2) . ? C1A C6A 1.42(2) . ? C2A C3A 1.45(2) . ? C3A C4A 1.38(2) . ? C4A C5A 1.37(2) . ? C5A C6A 1.37(2) . ? C7A C8A 1.53(2) . ? C8A C9A 1.48(2) . ? C10A C15A 1.39(2) . ? C10A C11A 1.39(2) . ? C11A C12A 1.46(2) . ? C12A C13A 1.34(2) . ? C13A C14A 1.37(2) . ? C14A C15A 1.38(2) . ? C16A C21A 1.38(2) . ? C16A C17A 1.38(2) . ? C17A C18A 1.38(2) . ? C18A C19A 1.39(2) . ? C19A C20A 1.33(3) . ? C20A C21A 1.34(2) . ? C22A C23A 1.48(2) . ? C24A C25A 1.37(2) . ? C24A C29A 1.37(2) . ? C25A C26A 1.36(2) . ? C26A C27A 1.40(2) . ? C27A C28A 1.32(2) . ? C28A C29A 1.38(2) . ? C30A C31A 1.40(2) . ? C30A C35A 1.41(2) . ? C31A C32A 1.42(2) . ? C32A C33A 1.33(2) . ? C33A C34A 1.34(2) . ? C34A C35A 1.38(3) . ? C36A C37A 1.38(2) . ? C36A C41A 1.40(2) . ? C37A C38A 1.39(2) . ? C38A C39A 1.37(2) . ? C39A C40A 1.41(2) . ? C40A C41A 1.40(2) . ? C42A C47A 1.39(2) . ? C42A C43A 1.39(2) . ? C43A C44A 1.34(2) . ? C44A C45A 1.38(2) . ? C45A C46A 1.37(2) . ? C46A C47A 1.39(2) . ? Re2 N3B 1.758(10) . ? Re2 O1B 2.005(8) . ? Re2 N2B 2.072(10) . ? Re2 N1B 2.098(11) . ? Re2 P1B 2.424(4) . ? Re2 P2B 2.434(4) . ? P1B C1B 1.804(13) . ? P1B C24B 1.811(14) . ? P1B C30B 1.844(14) . ? P2B C10B 1.810(13) . ? P2B C42B 1.839(15) . ? P2B C36B 1.84(2) . ? O1B C22B 1.40(2) . ? N1B C2B 1.32(2) . ? N1B C7B 1.44(2) . ? N2B C11B 1.38(2) . ? N2B C9B 1.44(2) . ? N3B C16B 1.34(2) . ? C1B C6B 1.38(2) . ? C1B C2B 1.46(2) . ? C2B C3B 1.46(2) . ? C3B C4B 1.37(2) . ? C4B C5B 1.39(2) . ? C5B C6B 1.41(2) . ? C7B C8B 1.52(2) . ? C8B C9B 1.51(2) . ? C10B C15B 1.39(2) . ? C10B C11B 1.40(2) . ? C11B C12B 1.43(2) . ? C12B C13B 1.38(2) . ? C13B C14B 1.35(2) . ? C14B C15B 1.42(2) . ? C16B C17B 1.37(2) . ? C16B C21B 1.40(2) . ? C17B C18B 1.40(2) . ? C18B C19B 1.34(3) . ? C19B C20B 1.37(3) . ? C20B C21B 1.33(2) . ? C22B C23B 1.45(2) . ? C24B C25B 1.34(2) . ? C24B C29B 1.42(2) . ? C25B C26B 1.37(2) . ? C26B C27B 1.37(2) . ? C27B C28B 1.37(2) . ? C28B C29B 1.41(2) . ? C30B C31B 1.36(2) . ? C30B C35B 1.40(2) . ? C31B C32B 1.42(3) . ? C32B C33B 1.34(3) . ? C33B C34B 1.34(2) . ? C34B C35B 1.38(2) . ? C36B C41B 1.36(2) . ? C36B C37B 1.38(2) . ? C37B C38B 1.39(3) . ? C38B C39B 1.46(3) . ? C39B C40B 1.37(2) . ? C40B C41B 1.39(2) . ? C42B C43B 1.39(2) . ? C42B C47B 1.40(2) . ? C43B C44B 1.44(3) . ? C44B C45B 1.38(3) . ? C45B C46B 1.32(3) . ? C46B C47B 1.44(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 N3A Re1 O1A 165.3(4) . . ? N3A Re1 N1A 103.8(5) . . ? O1A Re1 N1A 86.7(4) . . ? N3A Re1 N2A 104.7(5) . . ? O1A Re1 N2A 85.0(4) . . ? N1A Re1 N2A 91.1(5) . . ? N3A Re1 P2A 95.0(4) . . ? O1A Re1 P2A 76.1(3) . . ? N1A Re1 P2A 160.2(3) . . ? N2A Re1 P2A 77.9(3) . . ? N3A Re1 P1A 91.1(3) . . ? O1A Re1 P1A 80.6(3) . . ? N1A Re1 P1A 79.6(3) . . ? N2A Re1 P1A 163.2(3) . . ? P2A Re1 P1A 106.71(12) . . ? C1A P1A C30A 105.0(7) . . ? C1A P1A C24A 105.8(6) . . ? C30A P1A C24A 104.2(6) . . ? C1A P1A Re1 99.7(5) . . ? C30A P1A Re1 125.9(5) . . ? C24A P1A Re1 114.2(5) . . ? C10A P2A C42A 111.5(7) . . ? C10A P2A C36A 101.4(6) . . ? C42A P2A C36A 105.0(6) . . ? C10A P2A Re1 98.8(5) . . ? C42A P2A Re1 119.2(5) . . ? C36A P2A Re1 119.3(5) . . ? C22A O1A Re1 124.2(8) . . ? C2A N1A C7A 114.3(11) . . ? C2A N1A Re1 121.8(9) . . ? C7A N1A Re1 123.7(9) . . ? C11A N2A C9A 116.4(12) . . ? C11A N2A Re1 121.1(9) . . ? C9A N2A Re1 120.5(9) . . ? C16A N3A Re1 169.8(9) . . ? C2A C1A C6A 122.4(12) . . ? C2A C1A P1A 114.6(11) . . ? C6A C1A P1A 123.0(10) . . ? N1A C2A C1A 120.5(12) . . ? N1A C2A C3A 123.6(13) . . ? C1A C2A C3A 115.9(13) . . ? C4A C3A C2A 119.6(14) . . ? C5A C4A C3A 123.1(14) . . ? C6A C5A C4A 119.2(14) . . ? C5A C6A C1A 119.7(13) . . ? N1A C7A C8A 111.0(11) . . ? C9A C8A C7A 112.1(12) . . ? N2A C9A C8A 114.1(11) . . ? C15A C10A C11A 121.9(13) . . ? C15A C10A P2A 124.5(12) . . ? C11A C10A P2A 113.2(11) . . ? N2A C11A C10A 121.3(12) . . ? N2A C11A C12A 123.5(14) . . ? C10A C11A C12A 115.2(13) . . ? C13A C12A C11A 121.3(15) . . ? C12A C13A C14A 121.9(16) . . ? C13A C14A C15A 119.3(16) . . ? C14A C15A C10A 120.4(16) . . ? C21A C16A C17A 117.8(14) . . ? C21A C16A N3A 124.4(14) . . ? C17A C16A N3A 117.7(14) . . ? C18A C17A C16A 120.3(15) . . ? C17A C18A C19A 119.1(16) . . ? C20A C19A C18A 120.5(16) . . ? C19A C20A C21A 120.5(18) . . ? C20A C21A C16A 121.7(17) . . ? O1A C22A C23A 110.9(13) . . ? C25A C24A C29A 118.0(13) . . ? C25A C24A P1A 121.8(11) . . ? C29A C24A P1A 119.9(11) . . ? C26A C25A C24A 121.0(14) . . ? C25A C26A C27A 119.4(15) . . ? C28A C27A C26A 120.1(16) . . ? C27A C28A C29A 120.7(15) . . ? C28A C29A C24A 120.7(14) . . ? C31A C30A C35A 113.3(14) . . ? C31A C30A P1A 122.8(11) . . ? C35A C30A P1A 123.7(11) . . ? C30A C31A C32A 120.5(14) . . ? C33A C32A C31A 118.5(15) . . ? C32A C33A C34A 126.6(18) . . ? C33A C34A C35A 112.8(19) . . ? C34A C35A C30A 127.8(17) . . ? C37A C36A C41A 120.2(14) . . ? C37A C36A P2A 123.5(12) . . ? C41A C36A P2A 116.3(11) . . ? C36A C37A C38A 121.1(16) . . ? C39A C38A C37A 118.7(17) . . ? C38A C39A C40A 122.1(19) . . ? C41A C40A C39A 118.3(18) . . ? C36A C41A C40A 119.6(15) . . ? C47A C42A C43A 118.9(14) . . ? C47A C42A P2A 122.3(11) . . ? C43A C42A P2A 118.3(11) . . ? C44A C43A C42A 120.9(15) . . ? C43A C44A C45A 120.3(16) . . ? C46A C45A C44A 120.4(17) . . ? C45A C46A C47A 119.3(17) . . ? C42A C47A C46A 119.9(15) . . ? N3B Re2 O1B 168.2(4) . . ? N3B Re2 N2B 101.9(4) . . ? O1B Re2 N2B 86.5(4) . . ? N3B Re2 N1B 100.2(5) . . ? O1B Re2 N1B 87.8(4) . . ? N2B Re2 N1B 90.9(4) . . ? N3B Re2 P1B 96.9(3) . . ? O1B Re2 P1B 75.8(3) . . ? N2B Re2 P1B 160.3(3) . . ? N1B Re2 P1B 80.0(3) . . ? N3B Re2 P2B 92.2(4) . . ? O1B Re2 P2B 81.2(3) . . ? N2B Re2 P2B 78.8(3) . . ? N1B Re2 P2B 165.4(3) . . ? P1B Re2 P2B 106.38(12) . . ? C1B P1B C24B 104.4(7) . . ? C1B P1B C30B 108.4(6) . . ? C24B P1B C30B 103.5(6) . . ? C1B P1B Re2 99.9(4) . . ? C24B P1B Re2 121.5(4) . . ? C30B P1B Re2 117.8(5) . . ? C10B P2B C42B 105.7(6) . . ? C10B P2B C36B 105.1(6) . . ? C42B P2B C36B 104.5(7) . . ? C10B P2B Re2 99.1(5) . . ? C42B P2B Re2 125.2(5) . . ? C36B P2B Re2 115.0(5) . . ? C22B O1B Re2 125.9(8) . . ? C2B N1B C7B 114.8(11) . . ? C2B N1B Re2 123.0(9) . . ? C7B N1B Re2 122.0(9) . . ? C11B N2B C9B 114.5(10) . . ? C11B N2B Re2 121.7(8) . . ? C9B N2B Re2 122.8(8) . . ? C16B N3B Re2 174.3(10) . . ? C6B C1B C2B 121.9(12) . . ? C6B C1B P1B 124.1(11) . . ? C2B C1B P1B 114.1(9) . . ? N1B C2B C3B 124.5(13) . . ? N1B C2B C1B 121.1(11) . . ? C3B C2B C1B 114.3(12) . . ? C4B C3B C2B 120.9(15) . . ? C3B C4B C5B 124.0(15) . . ? C4B C5B C6B 116.6(15) . . ? C1B C6B C5B 122.2(15) . . ? N1B C7B C8B 114.1(12) . . ? C9B C8B C7B 112.4(13) . . ? N2B C9B C8B 112.9(12) . . ? C15B C10B C11B 123.3(12) . . ? C15B C10B P2B 122.3(11) . . ? C11B C10B P2B 114.4(9) . . ? N2B C11B C10B 120.0(11) . . ? N2B C11B C12B 123.8(11) . . ? C10B C11B C12B 116.2(12) . . ? C13B C12B C11B 119.9(14) . . ? C14B C13B C12B 122.8(14) . . ? C13B C14B C15B 119.5(14) . . ? C10B C15B C14B 118.3(13) . . ? N3B C16B C17B 124.0(14) . . ? N3B C16B C21B 120.3(13) . . ? C17B C16B C21B 115.7(14) . . ? C16B C17B C18B 121.3(18) . . ? C19B C18B C17B 118.5(18) . . ? C18B C19B C20B 122.2(17) . . ? C21B C20B C19B 118.2(19) . . ? C20B C21B C16B 124.0(17) . . ? O1B C22B C23B 113.7(15) . . ? C25B C24B C29B 117.3(14) . . ? C25B C24B P1B 121.8(12) . . ? C29B C24B P1B 120.9(11) . . ? C24B C25B C26B 122.8(15) . . ? C25B C26B C27B 120.5(16) . . ? C28B C27B C26B 120.2(17) . . ? C27B C28B C29B 118.4(18) . . ? C28B C29B C24B 120.9(16) . . ? C31B C30B C35B 119.1(15) . . ? C31B C30B P1B 123.7(13) . . ? C35B C30B P1B 117.2(11) . . ? C30B C31B C32B 121.0(19) . . ? C33B C32B C31B 117.6(22) . . ? C34B C33B C32B 122.1(23) . . ? C33B C34B C35B 121.6(20) . . ? C34B C35B C30B 118.3(16) . . ? C41B C36B C37B 123.6(15) . . ? C41B C36B P2B 116.4(11) . . ? C37B C36B P2B 119.9(12) . . ? C36B C37B C38B 117.5(17) . . ? C37B C38B C39B 122.2(19) . . ? C40B C39B C38B 113.7(19) . . ? C39B C40B C41B 125.7(17) . . ? C36B C41B C40B 117.1(14) . . ? C43B C42B C47B 122.1(16) . . ? C43B C42B P2B 117.1(12) . . ? C47B C42B P2B 120.7(13) . . ? C42B C43B C44B 116.9(17) . . ? C45B C44B C43B 119.3(20) . . ? C46B C45B C44B 124.0(22) . . ? C45B C46B C47B 119.1(22) . . ? C42B C47B C46B 118.4(18) . . ? _refine_diff_density_max 1.292 _refine_diff_density_min -2.196 _refine_diff_density_rms 0.239