Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ICAC@MAHENDRA.IACS.RES.IN _publ_contact_author_name 'Prof Animesh Chakravorty' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Kolkata West Bengal 700 032 INDIA ; _publ_section_title ; Tertiary phosphine binding to pyridylazole chelated rhenium via substitution in phosphine oxide precursors : geometrical preference, twin isomerization and effects of diphosphine spacer length and metal oxidation state. ; loop_ _publ_author_name 'Animesh Chakravorty' 'Jaydip Gangopadhyay' 'Suman Sengupta' data_op1 _database_code_CSD 214947 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H19 Cl3 N2 O P Re S' _chemical_formula_weight 658.95 _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' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.597(2) _cell_length_b 8.445(2) _cell_length_c 12.674(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.20(3) _cell_angle_gamma 90.00 _cell_volume 1127.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description Parallopiped _exptl_crystal_colour Violet _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method ? _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 5.922 _exptl_absorpt_correction_type semi-emperical _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 0.210 _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 R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2211 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2095 _reflns_number_observed 2055 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 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^)+(0.0628P)^2^+0.0089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(11) _refine_ls_number_reflns 2090 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_obs 0.0281 _refine_ls_wR_factor_all 0.0707 _refine_ls_wR_factor_obs 0.0694 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.027 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.027 _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 0.31049(2) 0.25096(5) 0.23166(2) 0.02929(12) Uani 1 d . . Cl2 Cl 0.3712(2) 0.5133(3) 0.2773(2) 0.0491(5) Uani 1 d . . Cl3 Cl 0.2505(2) -0.0136(3) 0.1900(2) 0.0442(5) Uani 1 d . . Cl1 Cl 0.5145(2) 0.1628(3) 0.3108(2) 0.0418(5) Uani 1 d . . S S 0.0278(2) 0.4852(4) -0.0125(2) 0.0556(7) Uani 1 d . . P P 0.2709(2) 0.1645(3) 0.48702(15) 0.0323(4) Uani 1 d . . O O 0.2352(5) 0.2282(10) 0.3757(4) 0.037(2) Uani 1 d . . N1 N 0.3633(6) 0.2861(10) 0.0822(5) 0.039(2) Uani 1 d . . N2 N 0.1453(6) 0.3339(9) 0.1490(5) 0.0321(14) Uani 1 d . . C1 C 0.4730(8) 0.2391(16) 0.0475(7) 0.044(2) Uani 1 d . . H1A H 0.5318 0.1857 0.0944 0.053 Uiso 1 calc R . C2 C 0.5018(8) 0.2662(20) -0.0527(6) 0.051(2) Uani 1 d . . H2A H 0.5754 0.2243 -0.0754 0.061 Uiso 1 calc R . C3 C 0.4187(9) 0.3584(14) -0.1220(7) 0.050(2) Uani 1 d . . H3A H 0.4386 0.3828 -0.1898 0.060 Uiso 1 calc R . C4 C 0.3102(9) 0.4104(14) -0.0882(7) 0.052(2) Uani 1 d . . H4A H 0.2551 0.4729 -0.1326 0.063 Uiso 1 calc R . C5 C 0.2792(8) 0.3712(11) 0.0136(6) 0.036(2) Uani 1 d . . C6 C 0.1634(7) 0.3991(10) 0.0546(6) 0.036(2) Uani 1 d . . C12 C -0.0590(7) 0.4260(12) 0.0916(6) 0.040(2) Uani 1 d . . C11 C -0.1855(9) 0.4527(14) 0.0999(8) 0.054(3) Uani 1 d . . H8A H -0.2348 0.5111 0.0486 0.065 Uiso 1 calc R . C10 C -0.2377(9) 0.3907(16) 0.1863(8) 0.056(3) Uani 1 d . . H9A H -0.3234 0.4057 0.1928 0.068 Uiso 1 calc R . C9 C -0.1623(8) 0.3054(15) 0.2639(8) 0.055(3) Uani 1 d . . H10A H -0.1988 0.2616 0.3207 0.066 Uiso 1 calc R . C8 C -0.0347(8) 0.2859(13) 0.2568(6) 0.044(3) Uani 1 d . . H11A H 0.0156 0.2330 0.3103 0.052 Uiso 1 calc R . C7 C 0.0187(7) 0.3450(10) 0.1704(6) 0.033(2) Uani 1 d . . C13 C 0.3114(10) -0.0397(13) 0.4863(8) 0.054(3) Uani 1 d . . H13A H 0.2422 -0.0986 0.4502 0.081 Uiso 1 calc R . H13B H 0.3281 -0.0770 0.5580 0.081 Uiso 1 calc R . H13C H 0.3858 -0.0537 0.4502 0.081 Uiso 1 calc R . C14 C 0.4008(8) 0.2709(23) 0.5543(7) 0.058(3) Uani 1 d . . H14A H 0.3803 0.3816 0.5553 0.087 Uiso 1 calc R . H14B H 0.4749 0.2559 0.5180 0.087 Uiso 1 calc R . H14C H 0.4172 0.2326 0.6258 0.087 Uiso 1 calc R . C15 C 0.1364(8) 0.1823(11) 0.5607(6) 0.033(2) Uani 1 d . . C16 C 0.0281(8) 0.0961(14) 0.5303(8) 0.052(2) Uani 1 d . . H16A H 0.0244 0.0315 0.4706 0.063 Uiso 1 calc R . C17 C -0.0745(10) 0.1049(14) 0.5878(10) 0.062(3) Uani 1 d . . H17A H -0.1459 0.0435 0.5678 0.074 Uiso 1 calc R . C18 C -0.0734(10) 0.2012(14) 0.6728(9) 0.059(3) Uani 1 d . . H18A H -0.1429 0.2044 0.7117 0.071 Uiso 1 calc R . C19 C 0.0303(11) 0.2940(16) 0.7016(8) 0.069(4) Uani 1 d . . H19A H 0.0296 0.3631 0.7586 0.082 Uiso 1 calc R . C20 C 0.1373(9) 0.2863(15) 0.6464(7) 0.054(3) Uani 1 d . . H20A H 0.2078 0.3492 0.6664 0.065 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 0.0253(2) 0.0404(2) 0.0234(2) 0.00287(15) 0.00845(10) -0.0010(2) Cl2 0.0496(12) 0.0467(12) 0.0524(12) -0.0075(10) 0.0112(10) -0.0068(10) Cl3 0.0467(11) 0.0444(12) 0.0424(10) -0.0014(9) 0.0086(9) -0.0079(10) Cl1 0.0303(9) 0.0592(14) 0.0373(10) 0.0025(10) 0.0095(8) 0.0023(10) S 0.043(2) 0.078(2) 0.0462(13) 0.0252(14) 0.0061(11) 0.0080(14) P 0.0257(9) 0.0464(12) 0.0258(9) 0.0028(9) 0.0069(7) -0.0004(9) O 0.034(2) 0.050(6) 0.028(2) 0.005(3) 0.012(2) 0.006(3) N1 0.038(3) 0.048(7) 0.032(3) -0.003(3) 0.010(2) -0.007(3) N2 0.031(3) 0.034(3) 0.032(3) 0.003(3) 0.006(2) -0.001(3) C1 0.039(4) 0.054(6) 0.044(4) 0.007(5) 0.020(3) -0.004(5) C2 0.051(4) 0.063(6) 0.043(4) -0.003(7) 0.024(4) 0.001(7) C3 0.060(6) 0.066(6) 0.029(4) 0.006(4) 0.020(4) -0.015(5) C4 0.051(5) 0.071(7) 0.037(4) 0.012(5) 0.012(4) -0.018(5) C5 0.039(4) 0.045(5) 0.025(4) 0.010(3) 0.002(3) -0.009(4) C6 0.035(4) 0.044(5) 0.030(4) 0.010(4) 0.000(3) -0.002(4) C12 0.029(4) 0.050(5) 0.040(4) -0.003(4) 0.002(3) -0.001(4) C11 0.037(4) 0.066(7) 0.057(6) 0.002(5) -0.007(4) 0.005(5) C10 0.032(4) 0.088(9) 0.050(5) -0.013(5) 0.010(4) 0.004(5) C9 0.036(4) 0.092(10) 0.039(4) -0.005(5) 0.012(4) 0.001(5) C8 0.035(4) 0.060(8) 0.038(4) -0.002(4) 0.012(3) -0.002(4) C7 0.029(4) 0.040(4) 0.030(4) -0.001(3) 0.006(3) -0.001(3) C13 0.056(6) 0.054(6) 0.057(6) 0.010(5) 0.026(5) 0.021(5) C14 0.037(4) 0.083(9) 0.056(5) -0.021(7) 0.013(3) -0.015(7) C15 0.034(4) 0.045(4) 0.023(4) 0.006(3) 0.014(3) -0.001(4) C16 0.040(5) 0.060(6) 0.060(6) -0.009(5) 0.021(4) -0.008(5) C17 0.047(5) 0.051(6) 0.095(8) 0.005(6) 0.039(5) -0.009(5) C18 0.051(6) 0.072(8) 0.060(6) 0.013(5) 0.035(5) 0.008(5) C19 0.068(7) 0.086(11) 0.056(6) -0.024(6) 0.030(5) 0.002(6) C20 0.052(5) 0.067(9) 0.045(5) -0.017(5) 0.016(4) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N1 2.054(6) . y Re N2 2.063(6) . y Re O 2.078(5) . y Re Cl2 2.361(3) . y Re Cl3 2.367(2) . y Re Cl1 2.402(2) . y S C6 1.747(8) . ? S C12 1.760(9) . ? P O 1.520(6) . y P C13 1.777(11) . ? P C14 1.782(11) . ? P C15 1.793(8) . ? N1 C1 1.346(11) . ? N1 C5 1.378(11) . ? N2 C6 1.350(10) . ? N2 C7 1.400(10) . ? C1 C2 1.358(10) . ? C2 C3 1.41(2) . ? C3 C4 1.343(14) . ? C4 C5 1.405(11) . ? C5 C6 1.403(11) . ? C12 C11 1.375(13) . ? C12 C7 1.401(12) . ? C11 C10 1.38(2) . ? C10 C9 1.40(2) . ? C9 C8 1.375(12) . ? C8 C7 1.380(11) . ? C15 C16 1.379(13) . ? C15 C20 1.396(13) . ? C16 C17 1.375(14) . ? C17 C18 1.35(2) . ? C18 C19 1.37(2) . ? C19 C20 1.396(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re N2 77.5(3) . . y N1 Re O 172.7(3) . . y N2 Re O 95.3(2) . . y N1 Re Cl2 89.8(2) . . y N2 Re Cl2 90.0(2) . . y O Re Cl2 89.5(2) . . y N1 Re Cl3 91.4(2) . . y N2 Re Cl3 90.8(2) . . y O Re Cl3 89.4(2) . . y Cl2 Re Cl3 178.71(8) . . y N1 Re Cl1 96.2(2) . . y N2 Re Cl1 173.6(2) . . y O Re Cl1 91.0(2) . . y Cl2 Re Cl1 88.81(8) . . y Cl3 Re Cl1 90.49(8) . . y C6 S C12 89.2(4) . . ? O P C13 112.0(5) . . ? O P C14 111.6(6) . . ? C13 P C14 108.5(7) . . ? O P C15 108.7(4) . . ? C13 P C15 106.9(5) . . ? C14 P C15 109.0(4) . . ? P O Re 140.1(4) . . y C1 N1 C5 118.1(7) . . ? C1 N1 Re 126.1(6) . . ? C5 N1 Re 115.8(5) . . ? C6 N2 C7 112.0(7) . . ? C6 N2 Re 113.2(5) . . ? C7 N2 Re 134.7(5) . . ? N1 C1 C2 123.0(9) . . ? C1 C2 C3 119.2(9) . . ? C4 C3 C2 118.7(8) . . ? C3 C4 C5 120.6(10) . . ? N1 C5 C6 112.7(6) . . ? N1 C5 C4 120.2(8) . . ? C6 C5 C4 126.9(8) . . ? N2 C6 C5 118.3(7) . . ? N2 C6 S 114.4(6) . . ? C5 C6 S 126.6(6) . . ? C11 C12 C7 121.9(8) . . ? C11 C12 S 127.1(7) . . ? C7 C12 S 111.0(6) . . ? C12 C11 C10 118.3(9) . . ? C11 C10 C9 120.4(9) . . ? C8 C9 C10 120.5(10) . . ? C9 C8 C7 119.9(9) . . ? C8 C7 N2 127.8(7) . . ? C8 C7 C12 118.9(7) . . ? N2 C7 C12 113.3(7) . . ? C16 C15 C20 119.0(8) . . ? C16 C15 P 119.7(7) . . ? C20 C15 P 121.3(7) . . ? C17 C16 C15 120.3(10) . . ? C18 C17 C16 121.2(10) . . ? C17 C18 C19 119.7(9) . . ? C18 C19 C20 120.8(10) . . ? C15 C20 C19 118.8(10) . . ? _refine_diff_density_max 2.542 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.134 #end# data_test7 _database_code_CSD 214948 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30.50 H24 Cl4 N3 O4 P Re S' _chemical_formula_weight 887.56 _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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.989(3) _cell_length_b 14.769(3) _cell_length_c 16.881(3) _cell_angle_alpha 86.26(3) _cell_angle_beta 88.95(3) _cell_angle_gamma 75.15(3) _cell_volume 3364.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description Parallopiped _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method ? _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 4.079 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.215 _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 R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10539 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10539 _reflns_number_observed 8711 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 38 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^)+(0.1078P)^2^+7.1029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _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 10501 _refine_ls_number_parameters 808 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_obs 0.0595 _refine_ls_wR_factor_all 0.1710 _refine_ls_wR_factor_obs 0.1482 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max -0.343 _refine_ls_shift/esd_mean 0.011 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 -0.14337(3) 0.76549(3) 0.38482(2) 0.04301(14) Uani 1 d . . Re51 Re 0.48717(3) 0.76844(3) 0.65470(2) 0.04032(13) Uani 1 d . . Cl1 Cl -0.1738(3) 0.6594(2) 0.3012(2) 0.0749(9) Uani 1 d . . Cl2 Cl -0.3120(2) 0.8254(2) 0.4091(2) 0.0640(7) Uani 1 d . . Cl3 Cl 0.0261(2) 0.7143(2) 0.3739(2) 0.0562(6) Uani 1 d . . Cl52 Cl 0.6462(2) 0.7893(2) 0.6470(2) 0.0601(7) Uani 1 d . . Cl51 Cl 0.4309(2) 0.9004(2) 0.7238(2) 0.0705(8) Uani 1 d . . Cl53 Cl 0.3340(2) 0.7353(2) 0.6542(2) 0.0569(6) Uani 1 d . . O1 O -0.1475(5) 0.8610(4) 0.2917(4) 0.045(2) Uani 1 d . . O51 O 0.5223(5) 0.6860(5) 0.7543(4) 0.048(2) Uani 1 d . . O2 O 0.1162(8) 0.6534(9) 0.5646(7) 0.103(3) Uani 1 d . . O3 O 0.0976(8) 0.7013(8) 0.6811(6) 0.094(3) Uani 1 d . . O4 O 0.1823(11) 0.5626(8) 0.6633(8) 0.127(5) Uani 1 d . . O52 O 0.1646(12) 0.5766(18) 0.8191(11) 0.205(10) Uani 1 d . . S1 S -0.1174(3) 0.8762(3) 0.6258(2) 0.0717(9) Uani 1 d . . S51 S 0.5690(3) 0.6162(3) 0.4285(2) 0.0725(9) Uani 1 d . . P1 P -0.1327(2) 0.8658(2) 0.2015(2) 0.0490(6) Uani 1 d . . P51 P 0.5118(2) 0.6426(2) 0.8377(2) 0.0452(6) Uani 1 d . . C1 C -0.1340(8) 0.5824(8) 0.4875(8) 0.065(3) Uani 1 d . . H1A H -0.1410 0.5568 0.4398 0.078 Uiso 1 calc R . C2 C -0.1240(9) 0.5267(9) 0.5557(9) 0.074(4) Uani 1 d . . H2A H -0.1278 0.4649 0.5544 0.089 Uiso 1 calc R . C3 C -0.1084(10) 0.5610(11) 0.6262(10) 0.085(5) Uani 1 d . . H3A H -0.0988 0.5222 0.6725 0.102 Uiso 1 calc R . C4 C -0.1070(10) 0.6540(11) 0.6277(9) 0.081(4) Uani 1 d . . H4A H -0.0977 0.6797 0.6749 0.097 Uiso 1 calc R . C5 C -0.1201(7) 0.7077(8) 0.5563(6) 0.052(3) Uani 1 d . . C6 C -0.1185(8) 0.8071(8) 0.5493(6) 0.052(3) Uani 1 d . . C12 C -0.1245(7) 0.9703(8) 0.5584(7) 0.059(3) Uani 1 d . . C11 C -0.1269(9) 1.0655(10) 0.5726(9) 0.077(4) Uani 1 d . . H11A H -0.1254 1.0849 0.6238 0.092 Uiso 1 calc R . C10 C -0.1316(9) 1.1267(9) 0.5070(10) 0.073(4) Uani 1 d . . H10A H -0.1345 1.1892 0.5144 0.088 Uiso 1 calc R . C9 C -0.1323(8) 1.0994(8) 0.4309(9) 0.066(3) Uani 1 d . . H9A H -0.1332 1.1426 0.3881 0.079 Uiso 1 calc R . C8 C -0.1318(9) 1.0085(7) 0.4176(8) 0.062(3) Uani 1 d . . H8A H -0.1360 0.9915 0.3660 0.074 Uiso 1 calc R . C7 C -0.1250(7) 0.9420(7) 0.4802(6) 0.047(2) Uani 1 d . . C13 C -0.0331(9) 0.7714(8) 0.1710(6) 0.059(3) Uani 1 d . . C14 C 0.0623(9) 0.7722(9) 0.1888(8) 0.068(3) Uani 1 d . . H14A H 0.0736 0.8216 0.2155 0.081 Uiso 1 calc R . C15 C 0.1415(10) 0.7008(11) 0.1674(8) 0.080(4) Uani 1 d . . H15A H 0.2061 0.7024 0.1775 0.096 Uiso 1 calc R . C16 C 0.1212(12) 0.6254(11) 0.1298(9) 0.090(5) Uani 1 d . . H16A H 0.1732 0.5751 0.1171 0.108 Uiso 1 calc R . C17 C 0.0270(12) 0.6247(11) 0.1117(10) 0.094(5) Uani 1 d . . H17A H 0.0154 0.5747 0.0860 0.113 Uiso 1 calc R . C18 C -0.0503(11) 0.6968(8) 0.1312(8) 0.072(4) Uani 1 d . . H18A H -0.1145 0.6966 0.1181 0.087 Uiso 1 calc R . C19 C -0.2468(9) 0.8676(8) 0.1524(8) 0.063(3) Uani 1 d . . C20 C -0.2482(13) 0.8602(13) 0.0702(8) 0.099(5) Uani 1 d . . H20A H -0.1908 0.8504 0.0397 0.119 Uiso 1 calc R . C21 C -0.3399(19) 0.8682(16) 0.0370(11) 0.124(7) Uani 1 d . . H21A H -0.3435 0.8629 -0.0174 0.149 Uiso 1 calc R . C22 C -0.4243(17) 0.8833(14) 0.0797(16) 0.126(8) Uani 1 d . . H22A H -0.4840 0.8885 0.0542 0.151 Uiso 1 calc R . C23 C -0.4233(11) 0.8911(10) 0.1600(11) 0.086(4) Uani 1 d . . H23A H -0.4818 0.9027 0.1891 0.103 Uiso 1 calc R . C24 C -0.3328(9) 0.8814(9) 0.1974(9) 0.069(3) Uani 1 d . . H24A H -0.3301 0.8840 0.2522 0.083 Uiso 1 calc R . C25 C -0.1053(10) 0.9747(8) 0.1757(7) 0.062(3) Uani 1 d . . C26 C -0.0320(11) 0.9823(10) 0.1218(9) 0.084(4) Uani 1 d . . H26A H 0.0044 0.9294 0.0978 0.100 Uiso 1 calc R . C27 C -0.0126(14) 1.0684(12) 0.1033(12) 0.115(7) Uani 1 d . . H27A H 0.0342 1.0751 0.0650 0.138 Uiso 1 calc R . C28 C -0.0652(15) 1.1451(11) 0.1439(12) 0.112(6) Uani 1 d . . H28A H -0.0468 1.2013 0.1368 0.135 Uiso 1 calc R . C29 C -0.1408(12) 1.1413(9) 0.1926(9) 0.077(4) Uani 1 d . . H29A H -0.1786 1.1947 0.2152 0.093 Uiso 1 calc R . C30 C -0.1602(9) 1.0558(8) 0.2075(8) 0.064(3) Uani 1 d . . H30A H -0.2129 1.0519 0.2407 0.077 Uiso 1 calc R . C51 C 0.4040(8) 0.9372(8) 0.5348(8) 0.065(3) Uani 1 d . . H51A H 0.3882 0.9730 0.5787 0.078 Uiso 1 calc R . C52 C 0.3814(9) 0.9773(11) 0.4585(10) 0.079(4) Uani 1 d . . H52A H 0.3520 1.0414 0.4520 0.095 Uiso 1 calc R . C53 C 0.4003(10) 0.9276(12) 0.3944(9) 0.081(4) Uani 1 d . . H53A H 0.3831 0.9559 0.3441 0.097 Uiso 1 calc R . C54 C 0.4461(9) 0.8328(11) 0.4044(8) 0.074(4) Uani 1 d . . H54A H 0.4602 0.7965 0.3606 0.089 Uiso 1 calc R . C55 C 0.4707(7) 0.7926(8) 0.4798(6) 0.050(2) Uani 1 d . . C56 C 0.5219(7) 0.6951(8) 0.4968(6) 0.052(3) Uani 1 d . . C57 C 0.5913(7) 0.5681(7) 0.5774(7) 0.051(3) Uani 1 d . . C58 C 0.6218(8) 0.5144(8) 0.6470(8) 0.064(3) Uani 1 d . . H58A H 0.6093 0.5401 0.6962 0.077 Uiso 1 calc R . C59 C 0.6712(10) 0.4215(9) 0.6411(9) 0.077(4) Uani 1 d . . H59A H 0.6911 0.3833 0.6869 0.092 Uiso 1 calc R . C60 C 0.6911(10) 0.3854(10) 0.5694(11) 0.082(4) Uani 1 d . . H60A H 0.7254 0.3227 0.5674 0.098 Uiso 1 calc R . C61 C 0.6634(9) 0.4362(11) 0.5004(10) 0.080(5) Uani 1 d . . H61A H 0.6780 0.4093 0.4519 0.096 Uiso 1 calc R . C62 C 0.6114(8) 0.5319(9) 0.5041(7) 0.062(3) Uani 1 d . . C63 C 0.4909(8) 0.5297(8) 0.8295(6) 0.052(3) Uani 1 d . . C64 C 0.4080(9) 0.5242(9) 0.7864(7) 0.064(3) Uani 1 d . . H64A H 0.3634 0.5778 0.7649 0.077 Uiso 1 calc R . C65 C 0.3953(12) 0.4340(11) 0.7769(8) 0.082(4) Uani 1 d . . H65A H 0.3417 0.4280 0.7477 0.098 Uiso 1 calc R . C66 C 0.4577(14) 0.3572(10) 0.8085(10) 0.089(5) Uani 1 d . . H66A H 0.4455 0.2992 0.8016 0.107 Uiso 1 calc R . C67 C 0.5386(14) 0.3604(10) 0.8505(10) 0.090(5) Uani 1 d . . H67A H 0.5814 0.3056 0.8720 0.108 Uiso 1 calc R . C68 C 0.5560(10) 0.4483(9) 0.8606(8) 0.071(3) Uani 1 d . . H68A H 0.6115 0.4521 0.8884 0.085 Uiso 1 calc R . C69 C 0.6249(8) 0.6298(7) 0.8895(7) 0.053(3) Uani 1 d . . C70 C 0.7070(9) 0.6436(9) 0.8470(8) 0.065(3) Uani 1 d . . H70A H 0.7033 0.6595 0.7927 0.078 Uiso 1 calc R . C71 C 0.7934(10) 0.6331(11) 0.8878(10) 0.085(4) Uani 1 d . . H71A H 0.8481 0.6441 0.8605 0.102 Uiso 1 calc R . C72 C 0.8023(10) 0.6074(11) 0.9662(10) 0.086(5) Uani 1 d . . H72A H 0.8628 0.5987 0.9915 0.104 Uiso 1 calc R . C73 C 0.7235(13) 0.5946(12) 1.0072(9) 0.094(5) Uani 1 d . . H73A H 0.7295 0.5767 1.0612 0.113 Uiso 1 calc R . C74 C 0.6330(10) 0.6077(11) 0.9699(7) 0.076(4) Uani 1 d . . H74A H 0.5778 0.6016 0.9993 0.091 Uiso 1 calc R . C75 C 0.4142(8) 0.7101(8) 0.8956(6) 0.054(3) Uani 1 d . . C76 C 0.3365(9) 0.6784(11) 0.9267(7) 0.076(4) Uani 1 d . . H76A H 0.3313 0.6192 0.9150 0.091 Uiso 1 calc R . C77 C 0.2679(12) 0.7300(13) 0.9732(9) 0.094(5) Uani 1 d . . H77A H 0.2163 0.7064 0.9937 0.112 Uiso 1 calc R . C78 C 0.2741(13) 0.8161(16) 0.9903(9) 0.103(6) Uani 1 d . . H78A H 0.2273 0.8504 1.0240 0.123 Uiso 1 calc R . C79 C 0.3482(13) 0.8558(12) 0.9591(9) 0.092(5) Uani 1 d . . H79A H 0.3493 0.9167 0.9693 0.111 Uiso 1 calc R . C80 C 0.4200(10) 0.8014(9) 0.9126(7) 0.070(3) Uani 1 d . . H80A H 0.4720 0.8246 0.8925 0.084 Uiso 1 calc R . N1 N -0.1340(6) 0.6728(6) 0.4869(6) 0.053(2) Uani 1 d . . N2 N -0.1236(6) 0.8480(6) 0.4779(5) 0.046(2) Uani 1 d . . N51 N 0.4499(6) 0.8438(6) 0.5435(5) 0.051(2) Uani 1 d . . N52 N 0.5387(6) 0.6626(6) 0.5725(5) 0.047(2) Uani 1 d . . N3 N 0.1317(7) 0.6404(8) 0.6346(7) 0.066(3) Uani 1 d . . N53 N 0.0794(12) 0.5823(12) 0.8453(10) 0.105(5) Uani 1 d . . O54 O 0.0202(11) 0.5768(13) 0.7962(9) 0.149(6) Uani 1 d . . O53 O 0.0746(13) 0.5790(12) 0.9137(9) 0.153(6) Uani 1 d . . Cl4 Cl 0.2666(10) 0.9349(19) 0.1988(9) 0.444(17) Uani 1 d . . C31A C 0.3606(24) 0.8616(22) 0.2087(18) 0.028(7) Uiso 0.25 d P . C31B C 0.1904(28) 0.9159(27) 0.2378(21) 0.040(8) Uiso 0.25 d P . C31C C 0.2568(33) 1.0228(32) 0.1093(27) 0.053(10) Uiso 0.25 d P . Cl5B Cl 0.2337(28) 1.1165(29) 0.1625(22) 0.378(18) Uiso 0.50 d P . C31D C 0.2812(31) 1.0668(30) 0.2362(25) 0.051(10) Uiso 0.25 d P . Cl5A Cl 0.2853(18) 0.8103(17) 0.2704(14) 0.240(10) Uiso 0.50 d P . 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 0.0412(2) 0.0332(2) 0.0564(3) 0.0020(2) -0.0034(2) -0.0137(2) Re51 0.0368(2) 0.0353(2) 0.0478(2) -0.0002(2) 0.0002(2) -0.0080(2) Cl1 0.106(3) 0.053(2) 0.078(2) -0.0063(14) -0.012(2) -0.042(2) Cl2 0.0361(13) 0.070(2) 0.086(2) 0.0108(15) -0.0007(13) -0.0177(13) Cl3 0.0447(14) 0.0498(15) 0.069(2) 0.0040(12) 0.0000(12) -0.0041(11) Cl52 0.0467(14) 0.064(2) 0.074(2) 0.0099(14) -0.0037(12) -0.0257(13) Cl51 0.077(2) 0.0433(15) 0.085(2) -0.0158(14) -0.001(2) -0.0010(14) Cl53 0.0396(13) 0.058(2) 0.073(2) 0.0017(13) -0.0005(12) -0.0123(12) O1 0.044(4) 0.034(3) 0.058(4) 0.002(3) -0.008(3) -0.013(3) O51 0.049(4) 0.048(4) 0.046(4) 0.004(3) -0.004(3) -0.013(3) O2 0.078(7) 0.135(10) 0.088(7) 0.003(7) 0.000(6) -0.018(7) O3 0.112(8) 0.084(7) 0.099(7) -0.024(6) 0.016(6) -0.043(6) O4 0.168(13) 0.061(7) 0.142(10) 0.020(7) -0.021(9) -0.015(8) O52 0.094(11) 0.338(30) 0.175(16) 0.046(17) -0.002(10) -0.054(15) S1 0.072(2) 0.090(2) 0.058(2) -0.016(2) 0.0017(15) -0.026(2) S51 0.072(2) 0.095(3) 0.060(2) -0.025(2) 0.017(2) -0.036(2) P1 0.052(2) 0.0399(14) 0.055(2) -0.0044(12) -0.0031(12) -0.0114(12) P51 0.0450(14) 0.0446(14) 0.0459(14) 0.0014(11) -0.0012(11) -0.0119(11) C1 0.050(6) 0.038(6) 0.105(9) 0.023(6) 0.000(6) -0.012(5) C2 0.063(8) 0.059(8) 0.101(10) 0.033(7) -0.001(7) -0.026(6) C3 0.066(8) 0.077(10) 0.104(11) 0.052(9) 0.000(8) -0.017(7) C4 0.060(8) 0.095(11) 0.088(9) 0.035(8) -0.002(7) -0.030(7) C5 0.040(5) 0.057(7) 0.057(6) 0.010(5) 0.000(5) -0.014(5) C6 0.048(6) 0.057(6) 0.053(6) 0.005(5) -0.007(5) -0.016(5) C12 0.034(5) 0.062(7) 0.078(8) -0.014(6) -0.003(5) -0.002(5) C11 0.056(7) 0.080(10) 0.099(10) -0.054(9) 0.002(7) -0.012(7) C10 0.054(7) 0.040(6) 0.126(12) -0.024(7) -0.009(7) -0.007(5) C9 0.047(6) 0.034(6) 0.112(10) -0.015(6) -0.019(6) 0.001(5) C8 0.069(8) 0.033(5) 0.082(8) -0.004(5) -0.017(6) -0.008(5) C7 0.036(5) 0.032(5) 0.071(7) -0.010(5) -0.004(5) -0.002(4) C13 0.063(7) 0.056(7) 0.053(6) -0.010(5) 0.012(5) -0.006(6) C14 0.056(7) 0.065(8) 0.079(8) -0.010(6) 0.009(6) -0.010(6) C15 0.062(8) 0.092(11) 0.079(9) -0.013(8) 0.006(7) -0.006(7) C16 0.079(10) 0.076(10) 0.099(11) -0.011(8) 0.021(8) 0.009(8) C17 0.080(11) 0.077(10) 0.124(13) -0.039(9) 0.014(9) -0.014(8) C18 0.086(9) 0.051(7) 0.085(9) -0.024(6) 0.009(7) -0.020(7) C19 0.058(7) 0.047(6) 0.080(8) -0.004(6) -0.023(6) -0.002(5) C20 0.104(12) 0.121(14) 0.061(8) -0.008(8) -0.025(8) -0.007(10) C21 0.144(19) 0.148(19) 0.089(12) -0.030(12) -0.051(13) -0.046(16) C22 0.114(16) 0.097(14) 0.171(22) -0.008(14) -0.089(16) -0.031(12) C23 0.060(8) 0.065(9) 0.132(14) -0.003(9) -0.029(8) -0.014(7) C24 0.054(7) 0.053(7) 0.092(9) 0.007(6) -0.016(6) -0.001(6) C25 0.081(8) 0.049(7) 0.057(7) -0.002(5) 0.009(6) -0.018(6) C26 0.094(10) 0.059(8) 0.097(10) -0.004(7) 0.035(8) -0.022(7) C27 0.121(14) 0.074(11) 0.152(16) 0.019(11) 0.056(12) -0.037(10) C28 0.133(16) 0.056(9) 0.153(17) 0.003(10) 0.030(13) -0.040(10) C29 0.097(11) 0.045(7) 0.089(9) 0.001(6) -0.004(8) -0.017(7) C30 0.065(7) 0.045(6) 0.081(8) 0.008(6) -0.010(6) -0.013(6) C51 0.049(6) 0.051(7) 0.094(9) 0.017(6) -0.013(6) -0.015(5) C52 0.051(7) 0.081(10) 0.106(11) 0.044(9) -0.020(7) -0.027(7) C53 0.061(8) 0.099(12) 0.079(9) 0.038(9) -0.019(7) -0.022(8) C54 0.052(7) 0.114(12) 0.063(7) 0.006(7) -0.008(6) -0.035(8) C55 0.041(5) 0.063(7) 0.046(6) 0.002(5) 0.000(4) -0.017(5) C56 0.042(5) 0.078(8) 0.045(6) -0.002(5) 0.003(4) -0.032(5) C57 0.038(5) 0.044(6) 0.071(7) -0.012(5) 0.013(5) -0.008(4) C58 0.051(6) 0.051(7) 0.083(8) -0.009(6) 0.010(6) 0.000(5) C59 0.063(8) 0.058(8) 0.101(10) -0.014(7) 0.011(7) 0.002(6) C60 0.063(8) 0.049(7) 0.132(13) -0.024(8) 0.022(9) -0.007(6) C61 0.056(8) 0.088(10) 0.112(12) -0.060(10) 0.028(8) -0.035(7) C62 0.050(6) 0.063(7) 0.081(8) -0.024(6) 0.015(6) -0.025(6) C63 0.055(6) 0.054(6) 0.049(6) 0.003(5) 0.008(5) -0.020(5) C64 0.060(7) 0.067(8) 0.071(7) 0.001(6) -0.002(6) -0.027(6) C65 0.115(12) 0.086(10) 0.066(8) -0.006(7) 0.009(8) -0.067(10) C66 0.123(14) 0.048(8) 0.104(11) 0.000(7) 0.016(10) -0.038(9) C67 0.115(13) 0.054(8) 0.100(11) 0.011(7) -0.005(10) -0.023(8) C68 0.064(8) 0.054(7) 0.091(9) 0.008(6) 0.005(7) -0.011(6) C69 0.043(6) 0.046(6) 0.065(7) -0.002(5) -0.016(5) -0.004(5) C70 0.055(7) 0.064(8) 0.077(8) 0.006(6) -0.004(6) -0.019(6) C71 0.047(7) 0.101(12) 0.106(12) -0.002(9) -0.011(7) -0.021(7) C72 0.048(8) 0.097(11) 0.110(12) -0.031(9) -0.024(8) -0.005(7) C73 0.103(13) 0.110(13) 0.066(9) -0.012(8) -0.030(9) -0.016(10) C74 0.061(8) 0.101(11) 0.062(8) 0.002(7) -0.008(6) -0.018(7) C75 0.049(6) 0.071(7) 0.041(5) -0.004(5) 0.000(4) -0.013(5) C76 0.056(7) 0.092(10) 0.069(8) 0.016(7) 0.015(6) -0.007(7) C77 0.077(10) 0.101(13) 0.096(11) -0.001(10) 0.036(8) -0.015(9) C78 0.076(11) 0.137(17) 0.070(9) -0.010(10) 0.000(8) 0.020(11) C79 0.094(11) 0.089(11) 0.075(9) -0.035(8) -0.018(8) 0.020(9) C80 0.077(9) 0.070(8) 0.065(7) -0.021(6) 0.000(6) -0.020(7) N1 0.036(4) 0.047(5) 0.070(6) 0.013(4) 0.000(4) -0.006(4) N2 0.038(4) 0.044(5) 0.056(5) -0.009(4) -0.004(4) -0.008(4) N51 0.045(5) 0.055(5) 0.057(5) 0.014(4) -0.006(4) -0.023(4) N52 0.047(5) 0.052(5) 0.045(4) -0.005(4) 0.010(4) -0.018(4) N3 0.051(6) 0.063(7) 0.086(8) 0.008(6) -0.005(5) -0.025(5) N53 0.087(11) 0.129(13) 0.089(11) 0.034(9) 0.002(9) -0.019(9) O54 0.095(9) 0.231(19) 0.119(11) 0.049(11) -0.009(8) -0.051(11) O53 0.185(16) 0.167(15) 0.097(10) 0.021(10) 0.013(10) -0.037(12) Cl4 0.261(13) 0.915(46) 0.295(15) -0.405(24) 0.088(11) -0.320(21) _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 O1 2.034(6) . y Re1 N2 2.113(8) . y Re1 N1 2.115(8) . y Re1 Cl1 2.298(3) . y Re1 Cl3 2.304(3) . y Re1 Cl2 2.336(3) . y Re51 O51 2.002(6) . y Re51 N51 2.122(8) . y Re51 N52 2.134(8) . y Re51 Cl51 2.292(3) . y Re51 Cl53 2.317(3) . y Re51 Cl52 2.323(3) . y O1 P1 1.532(7) . y O51 P51 1.529(7) . y O2 N3 1.200(14) . ? O3 N3 1.228(14) . ? O4 N3 1.256(14) . ? O52 N53 1.25(2) . ? S1 C6 1.700(12) . ? S1 C12 1.722(13) . ? S51 C56 1.696(11) . ? S51 C62 1.725(14) . ? P1 C25 1.773(12) . ? P1 C13 1.795(11) . ? P1 C19 1.804(12) . ? P51 C63 1.780(11) . ? P51 C69 1.783(10) . ? P51 C75 1.787(11) . ? C1 N1 1.334(14) . ? C1 C2 1.36(2) . ? C2 C3 1.36(2) . ? C3 C4 1.38(2) . ? C4 C5 1.39(2) . ? C5 N1 1.346(14) . ? C5 C6 1.47(2) . ? C6 N2 1.307(13) . ? C12 C7 1.41(2) . ? C12 C11 1.43(2) . ? C11 C10 1.38(2) . ? C10 C9 1.37(2) . ? C9 C8 1.37(2) . ? C8 C7 1.38(2) . ? C7 N2 1.387(13) . ? C13 C14 1.38(2) . ? C13 C18 1.40(2) . ? C14 C15 1.38(2) . ? C15 C16 1.41(2) . ? C16 C17 1.36(2) . ? C17 C18 1.36(2) . ? C19 C24 1.39(2) . ? C19 C20 1.40(2) . ? C20 C21 1.38(2) . ? C21 C22 1.35(3) . ? C22 C23 1.37(3) . ? C23 C24 1.40(2) . ? C25 C26 1.38(2) . ? C25 C30 1.38(2) . ? C26 C27 1.38(2) . ? C27 C28 1.40(2) . ? C28 C29 1.34(2) . ? C29 C30 1.37(2) . ? C51 N51 1.363(14) . ? C51 C52 1.39(2) . ? C52 C53 1.33(2) . ? C53 C54 1.38(2) . ? C54 C55 1.38(2) . ? C55 N51 1.339(14) . ? C55 C56 1.45(2) . ? C56 N52 1.339(13) . ? C57 C62 1.38(2) . ? C57 C58 1.38(2) . ? C57 N52 1.399(13) . ? C58 C59 1.38(2) . ? C59 C60 1.35(2) . ? C60 C61 1.35(2) . ? C61 C62 1.42(2) . ? C63 C68 1.39(2) . ? C63 C64 1.40(2) . ? C64 C65 1.41(2) . ? C65 C66 1.33(2) . ? C66 C67 1.36(2) . ? C67 C68 1.40(2) . ? C69 C74 1.38(2) . ? C69 C70 1.40(2) . ? C70 C71 1.37(2) . ? C71 C72 1.35(2) . ? C72 C73 1.34(2) . ? C73 C74 1.39(2) . ? C75 C76 1.37(2) . ? C75 C80 1.42(2) . ? C76 C77 1.34(2) . ? C77 C78 1.35(2) . ? C78 C79 1.39(3) . ? C79 C80 1.38(2) . ? N53 O53 1.15(2) . ? N53 O54 1.20(2) . ? Cl4 C31B 1.32(4) . ? Cl4 C31A 1.48(4) . ? Cl4 C31C 1.91(5) . ? Cl4 Cl5A 2.10(3) . ? Cl4 C31D 2.15(5) . ? C31A Cl5A 1.74(4) . ? C31B Cl5A 1.83(4) . ? C31C Cl5B 1.66(6) . ? Cl5B C31D 1.48(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 O1 Re1 N2 99.0(3) . . y O1 Re1 N1 175.5(3) . . y N2 Re1 N1 76.7(4) . . y O1 Re1 Cl1 90.6(2) . . y N2 Re1 Cl1 169.8(3) . . y N1 Re1 Cl1 93.7(3) . . y O1 Re1 Cl3 90.6(2) . . y N2 Re1 Cl3 88.7(2) . . y N1 Re1 Cl3 87.9(2) . . y Cl1 Re1 Cl3 94.39(13) . . y O1 Re1 Cl2 91.3(2) . . y N2 Re1 Cl2 84.7(2) . . y N1 Re1 Cl2 89.6(2) . . y Cl1 Re1 Cl2 91.90(13) . . y Cl3 Re1 Cl2 173.38(11) . . y O51 Re51 N51 174.4(3) . . y O51 Re51 N52 97.4(3) . . y N51 Re51 N52 77.5(3) . . y O51 Re51 Cl51 92.5(2) . . y N51 Re51 Cl51 92.8(3) . . y N52 Re51 Cl51 169.8(2) . . y O51 Re51 Cl53 89.8(2) . . y N51 Re51 Cl53 88.0(2) . . y N52 Re51 Cl53 88.9(2) . . y Cl51 Re51 Cl53 93.59(12) . . y O51 Re51 Cl52 90.5(2) . . y N51 Re51 Cl52 91.2(2) . . y N52 Re51 Cl52 85.4(2) . . y Cl51 Re51 Cl52 92.10(12) . . y Cl53 Re51 Cl52 174.28(10) . . y P1 O1 Re1 140.4(4) . . y P51 O51 Re51 159.4(5) . . y C6 S1 C12 89.3(5) . . ? C56 S51 C62 89.6(5) . . ? O1 P1 C25 106.5(5) . . ? O1 P1 C13 111.8(5) . . ? C25 P1 C13 109.7(6) . . ? O1 P1 C19 109.9(5) . . ? C25 P1 C19 107.1(6) . . ? C13 P1 C19 111.5(6) . . ? O51 P51 C63 108.7(4) . . ? O51 P51 C69 108.1(5) . . ? C63 P51 C69 108.9(5) . . ? O51 P51 C75 114.6(5) . . ? C63 P51 C75 108.5(5) . . ? C69 P51 C75 107.8(5) . . ? N1 C1 C2 122.0(14) . . ? C1 C2 C3 120.3(13) . . ? C2 C3 C4 119.1(13) . . ? C3 C4 C5 117.6(15) . . ? N1 C5 C4 122.7(12) . . ? N1 C5 C6 114.1(9) . . ? C4 C5 C6 123.2(12) . . ? N2 C6 C5 117.3(10) . . ? N2 C6 S1 116.5(8) . . ? C5 C6 S1 126.1(8) . . ? C7 C12 C11 120.6(12) . . ? C7 C12 S1 110.3(9) . . ? C11 C12 S1 129.1(11) . . ? C10 C11 C12 116.8(12) . . ? C9 C10 C11 122.6(11) . . ? C10 C9 C8 120.3(13) . . ? C9 C8 C7 120.7(12) . . ? C8 C7 N2 128.5(10) . . ? C8 C7 C12 118.8(10) . . ? N2 C7 C12 112.6(10) . . ? C14 C13 C18 119.6(11) . . ? C14 C13 P1 118.7(9) . . ? C18 C13 P1 121.7(10) . . ? C13 C14 C15 120.9(13) . . ? C14 C15 C16 117.9(14) . . ? C17 C16 C15 121.3(13) . . ? C18 C17 C16 120.2(15) . . ? C17 C18 C13 120.0(14) . . ? C24 C19 C20 121.5(13) . . ? C24 C19 P1 118.4(10) . . ? C20 C19 P1 120.1(11) . . ? C21 C20 C19 116.0(17) . . ? C22 C21 C20 123.2(17) . . ? C21 C22 C23 120.9(16) . . ? C22 C23 C24 118.7(17) . . ? C19 C24 C23 119.6(14) . . ? C26 C25 C30 117.9(11) . . ? C26 C25 P1 121.9(9) . . ? C30 C25 P1 120.2(9) . . ? C25 C26 C27 120.2(14) . . ? C26 C27 C28 118.0(14) . . ? C29 C28 C27 122.9(14) . . ? C28 C29 C30 117.1(14) . . ? C29 C30 C25 123.3(13) . . ? N51 C51 C52 118.2(13) . . ? C53 C52 C51 122.5(14) . . ? C52 C53 C54 118.5(13) . . ? C53 C54 C55 119.5(14) . . ? N51 C55 C54 121.0(11) . . ? N51 C55 C56 115.0(9) . . ? C54 C55 C56 124.1(11) . . ? N52 C56 C55 119.0(10) . . ? N52 C56 S51 115.1(9) . . ? C55 C56 S51 125.8(8) . . ? C62 C57 C58 121.9(11) . . ? C62 C57 N52 112.7(10) . . ? C58 C57 N52 125.4(10) . . ? C59 C58 C57 117.8(12) . . ? C60 C59 C58 120.7(14) . . ? C61 C60 C59 123.0(13) . . ? C60 C61 C62 118.0(12) . . ? C57 C62 C61 118.6(13) . . ? C57 C62 S51 111.5(9) . . ? C61 C62 S51 129.9(11) . . ? C68 C63 C64 119.9(12) . . ? C68 C63 P51 122.2(10) . . ? C64 C63 P51 117.8(9) . . ? C63 C64 C65 117.1(13) . . ? C66 C65 C64 121.8(14) . . ? C65 C66 C67 122.4(14) . . ? C66 C67 C68 118.3(14) . . ? C63 C68 C67 120.4(14) . . ? C74 C69 C70 119.3(11) . . ? C74 C69 P51 121.9(9) . . ? C70 C69 P51 118.8(9) . . ? C71 C70 C69 117.9(13) . . ? C72 C71 C70 122.6(14) . . ? C73 C72 C71 119.6(13) . . ? C72 C73 C74 120.5(14) . . ? C69 C74 C73 119.9(13) . . ? C76 C75 C80 118.2(12) . . ? C76 C75 P51 124.5(10) . . ? C80 C75 P51 117.3(9) . . ? C77 C76 C75 122.2(16) . . ? C76 C77 C78 119.6(16) . . ? C77 C78 C79 122.4(15) . . ? C80 C79 C78 117.6(16) . . ? C79 C80 C75 119.8(14) . . ? C1 N1 C5 118.1(10) . . ? C1 N1 Re1 125.8(9) . . ? C5 N1 Re1 116.0(7) . . ? C6 N2 C7 111.2(9) . . ? C6 N2 Re1 115.8(7) . . ? C7 N2 Re1 132.6(7) . . ? C55 N51 C51 120.3(10) . . ? C55 N51 Re51 115.5(7) . . ? C51 N51 Re51 124.1(8) . . ? C56 N52 C57 111.0(9) . . ? C56 N52 Re51 112.9(7) . . ? C57 N52 Re51 136.0(7) . . ? O2 N3 O3 121.8(12) . . ? O2 N3 O4 120.7(14) . . ? O3 N3 O4 117.5(13) . . ? O53 N53 O54 130.7(19) . . ? O53 N53 O52 113.7(20) . . ? O54 N53 O52 114.6(18) . . ? C31B Cl4 C31A 115.0(29) . . ? C31B Cl4 C31C 124.9(25) . . ? C31A Cl4 C31C 116.9(19) . . ? C31B Cl4 Cl5A 59.8(20) . . ? C31A Cl4 Cl5A 55.2(18) . . ? C31C Cl4 Cl5A 162.9(17) . . ? C31B Cl4 C31D 107.1(21) . . ? C31A Cl4 C31D 111.1(18) . . ? C31C Cl4 C31D 70.0(20) . . ? Cl5A Cl4 C31D 126.1(14) . . ? Cl4 C31A Cl5A 80.7(19) . . ? Cl4 C31B Cl5A 81.5(23) . . ? Cl5B C31C Cl4 95.0(26) . . ? C31D Cl5B C31C 96.0(32) . . ? Cl5B C31D Cl4 91.3(26) . . ? C31A Cl5A C31B 82.8(19) . . ? C31A Cl5A Cl4 44.1(12) . . ? C31B Cl5A Cl4 38.7(13) . . ? _refine_diff_density_max 3.684 _refine_diff_density_min -3.227 _refine_diff_density_rms 0.194 #end# data_oxafac _database_code_CSD 214949 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H19 Cl3 N2 O P Re' _chemical_formula_weight 626.89 _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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.266(5) _cell_length_b 14.394(4) _cell_length_c 16.311(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.40(3) _cell_angle_gamma 90.00 _cell_volume 2132.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallopiped _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 6.163 _exptl_absorpt_correction_type semi-emperical _exptl_absorpt_correction_T_min 0.145 _exptl_absorpt_correction_T_max 0.220 _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 R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3358 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.49 _reflns_number_total 3149 _reflns_number_observed 2431 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 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^)+(0.0506P)^2^+11.3996P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _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 3140 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_obs 0.0405 _refine_ls_wR_factor_all 0.1189 _refine_ls_wR_factor_obs 0.0920 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.197 _refine_ls_restrained_S_obs 1.065 _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 0.55559(4) 0.96102(3) 0.25700(2) 0.0348(2) Uani 1 d . . Cl1 Cl 0.7573(3) 0.8924(2) 0.2054(2) 0.0527(7) Uani 1 d . . Cl2 Cl 0.4031(3) 0.8373(2) 0.2023(2) 0.0577(8) Uani 1 d . . Cl3 Cl 0.6329(3) 0.8933(2) 0.3894(2) 0.0551(7) Uani 1 d . . P P 0.3572(3) 1.0259(2) 0.3101(2) 0.0409(7) Uani 1 d . . N1 N 0.5023(8) 1.0396(6) 0.1475(5) 0.035(2) Uani 1 d . . N2 N 0.6931(9) 1.0744(5) 0.2808(5) 0.035(2) Uani 1 d . . C1 C 0.3904(11) 1.0226(8) 0.0824(6) 0.043(3) Uani 1 d . . H1A H 0.3288 0.9721 0.0849 0.051 Uiso 1 calc R . C2 C 0.3660(13) 1.0771(9) 0.0139(6) 0.051(3) Uani 1 d . . H2A H 0.2881 1.0634 -0.0298 0.061 Uiso 1 calc R . C3 C 0.4537(15) 1.1525(9) 0.0072(7) 0.063(3) Uani 1 d . . H3A H 0.4372 1.1891 -0.0408 0.075 Uiso 1 calc R . C4 C 0.5670(13) 1.1724(7) 0.0734(7) 0.048(3) Uani 1 d . . H4A H 0.6286 1.2232 0.0719 0.057 Uiso 1 calc R . C5 C 0.5853(12) 1.1145(7) 0.1416(6) 0.042(3) Uani 1 d . . C6 C 0.6929(11) 1.1271(7) 0.2156(6) 0.038(2) Uani 1 d . . C7 C 0.8100(11) 1.1089(8) 0.3409(6) 0.042(3) Uani 1 d . . C8 C 0.8630(12) 1.0828(8) 0.4233(7) 0.051(3) Uani 1 d . . H8A H 0.8209 1.0347 0.4486 0.061 Uiso 1 calc R . C9 C 0.9825(13) 1.1329(9) 0.4652(8) 0.059(3) Uani 1 d . . H9A H 1.0223 1.1178 0.5205 0.071 Uiso 1 calc R . C10 C 1.0443(13) 1.2043(9) 0.4280(9) 0.065(4) Uani 1 d . . H10A H 1.1247 1.2356 0.4591 0.078 Uiso 1 calc R . C11 C 0.9916(13) 1.2313(9) 0.3465(8) 0.059(3) Uani 1 d . . H11A H 1.0320 1.2798 0.3209 0.070 Uiso 1 calc R . C12 C 0.8732(11) 1.1794(7) 0.3065(7) 0.041(2) Uani 1 d . . C13 C 0.2618(14) 0.9480(9) 0.3679(8) 0.067(4) Uani 1 d . . H13A H 0.3313 0.9197 0.4123 0.101 Uiso 1 calc R . H13B H 0.2129 0.9007 0.3311 0.101 Uiso 1 calc R . H13C H 0.1904 0.9823 0.3911 0.101 Uiso 1 calc R . C14 C 0.4123(14) 1.1184(9) 0.3835(7) 0.064(3) Uani 1 d . . H14A H 0.4887 1.0968 0.4280 0.096 Uiso 1 calc R . H14B H 0.3293 1.1383 0.4061 0.096 Uiso 1 calc R . H14C H 0.4485 1.1696 0.3557 0.096 Uiso 1 calc R . C15 C 0.2170(11) 1.0728(7) 0.2311(6) 0.040(3) Uani 1 d . . C16 C 0.1052(15) 1.0204(9) 0.1882(9) 0.069(4) Uani 1 d . . H16A H 0.0962 0.9591 0.2046 0.083 Uiso 1 calc R . C17 C 0.0059(15) 1.0543(11) 0.1222(9) 0.079(4) Uani 1 d . . H17A H -0.0685 1.0159 0.0943 0.095 Uiso 1 calc R . C18 C 0.0141(16) 1.1429(11) 0.0969(9) 0.077(4) Uani 1 d . . H18A H -0.0549 1.1659 0.0523 0.092 Uiso 1 calc R . C19 C 0.1255(14) 1.1988(9) 0.1379(8) 0.062(3) Uani 1 d . . H19A H 0.1332 1.2599 0.1207 0.074 Uiso 1 calc R . C20 C 0.2260(14) 1.1639(8) 0.2046(7) 0.052(3) Uani 1 d . . H20A H 0.3011 1.2020 0.2323 0.062 Uiso 1 calc R . O O 0.7968(8) 1.1931(5) 0.2256(4) 0.045(2) 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 0.0479(3) 0.0247(2) 0.0358(2) 0.0018(2) 0.0183(2) -0.0009(2) Cl1 0.063(2) 0.043(2) 0.060(2) 0.0062(14) 0.0304(14) 0.0109(14) Cl2 0.077(2) 0.035(2) 0.066(2) -0.0083(14) 0.025(2) -0.0158(14) Cl3 0.075(2) 0.047(2) 0.046(2) 0.0147(14) 0.0185(14) 0.0044(15) P 0.055(2) 0.034(2) 0.0395(15) 0.0000(13) 0.0222(12) -0.0009(13) N1 0.046(5) 0.030(5) 0.032(4) -0.006(4) 0.015(4) 0.002(4) N2 0.047(5) 0.025(4) 0.036(5) 0.004(4) 0.016(4) 0.002(4) C1 0.046(6) 0.045(7) 0.042(6) -0.010(5) 0.020(5) -0.004(5) C2 0.067(7) 0.052(7) 0.031(6) 0.007(5) 0.005(5) 0.011(6) C3 0.101(10) 0.046(8) 0.043(7) 0.015(6) 0.019(7) 0.011(7) C4 0.070(8) 0.029(6) 0.048(7) 0.005(5) 0.024(6) 0.000(5) C5 0.063(7) 0.024(6) 0.044(6) 0.000(5) 0.022(5) 0.004(5) C6 0.051(6) 0.025(6) 0.044(6) -0.006(5) 0.024(5) -0.003(5) C7 0.051(6) 0.040(6) 0.040(6) -0.006(5) 0.015(5) -0.001(5) C8 0.056(7) 0.043(7) 0.049(7) 0.002(6) 0.002(5) -0.009(6) C9 0.065(8) 0.049(8) 0.058(7) -0.018(6) 0.001(6) 0.007(6) C10 0.056(7) 0.062(9) 0.075(10) -0.034(8) 0.008(7) -0.007(7) C11 0.060(8) 0.042(7) 0.081(9) -0.019(7) 0.033(7) -0.008(6) C12 0.041(6) 0.037(6) 0.048(6) -0.011(5) 0.018(5) 0.000(5) C13 0.079(9) 0.076(10) 0.058(8) 0.017(7) 0.042(7) -0.001(7) C14 0.075(8) 0.067(9) 0.053(7) -0.022(7) 0.023(6) 0.005(7) C15 0.042(6) 0.039(6) 0.044(6) 0.004(5) 0.019(5) 0.005(5) C16 0.074(9) 0.043(8) 0.094(10) 0.010(7) 0.021(8) -0.016(7) C17 0.058(8) 0.089(12) 0.083(10) 0.005(9) -0.006(7) -0.024(8) C18 0.070(9) 0.094(12) 0.070(9) 0.023(9) 0.023(7) 0.022(9) C19 0.073(9) 0.055(8) 0.059(8) 0.008(7) 0.016(7) -0.002(7) C20 0.072(8) 0.045(7) 0.042(6) -0.004(6) 0.017(6) 0.004(6) O 0.057(4) 0.028(4) 0.055(5) -0.006(3) 0.024(4) -0.008(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 2.060(8) . y Re N1 2.089(8) . y Re Cl2 2.338(3) . y Re Cl3 2.349(3) . y Re P 2.373(3) . y Re Cl1 2.408(3) . y P C15 1.772(11) . ? P C14 1.796(12) . ? P C13 1.805(11) . ? N1 C5 1.339(13) . ? N1 C1 1.352(13) . ? N2 C6 1.305(12) . ? N2 C7 1.401(13) . ? C1 C2 1.347(15) . ? C2 C3 1.37(2) . ? C3 C4 1.38(2) . ? C4 C5 1.374(14) . ? C5 C6 1.417(14) . ? C6 O 1.339(12) . ? C7 C12 1.349(14) . ? C7 C8 1.388(15) . ? C8 C9 1.38(2) . ? C9 C10 1.37(2) . ? C10 C11 1.38(2) . ? C11 C12 1.379(15) . ? C12 O 1.383(12) . ? C15 C16 1.36(2) . ? C15 C20 1.388(15) . ? C16 C17 1.36(2) . ? C17 C18 1.35(2) . ? C18 C19 1.37(2) . ? C19 C20 1.38(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 N2 Re N1 76.4(3) . . y N2 Re Cl2 168.6(2) . . y N1 Re Cl2 93.6(2) . . y N2 Re Cl3 95.2(2) . . y N1 Re Cl3 171.3(2) . . y Cl2 Re Cl3 94.97(11) . . y N2 Re P 96.5(2) . . y N1 Re P 91.7(2) . . y Cl2 Re P 89.17(11) . . y Cl3 Re P 86.86(10) . . y N2 Re Cl1 84.1(2) . . y N1 Re Cl1 89.5(2) . . y Cl2 Re Cl1 90.39(11) . . y Cl3 Re Cl1 91.99(10) . . y P Re Cl1 178.73(9) . . y C15 P C14 105.9(6) . . ? C15 P C13 104.6(6) . . ? C14 P C13 102.5(6) . . ? C15 P Re 113.2(3) . . ? C14 P Re 113.4(4) . . ? C13 P Re 116.2(4) . . ? C5 N1 C1 116.9(9) . . ? C5 N1 Re 117.1(7) . . ? C1 N1 Re 126.0(7) . . ? C6 N2 C7 103.9(8) . . ? C6 N2 Re 114.0(7) . . ? C7 N2 Re 140.9(7) . . ? C2 C1 N1 121.5(10) . . ? C1 C2 C3 121.4(11) . . ? C2 C3 C4 118.2(11) . . ? C5 C4 C3 117.5(11) . . ? N1 C5 C4 124.5(10) . . ? N1 C5 C6 111.1(9) . . ? C4 C5 C6 124.5(10) . . ? N2 C6 O 115.4(9) . . ? N2 C6 C5 120.4(9) . . ? O C6 C5 124.2(9) . . ? C12 C7 C8 120.5(10) . . ? C12 C7 N2 108.3(9) . . ? C8 C7 N2 131.2(10) . . ? C9 C8 C7 115.6(11) . . ? C10 C9 C8 122.3(12) . . ? C9 C10 C11 122.5(12) . . ? C10 C11 C12 113.6(12) . . ? C7 C12 C11 125.5(11) . . ? C7 C12 O 108.8(9) . . ? C11 C12 O 125.7(10) . . ? C16 C15 C20 116.8(11) . . ? C16 C15 P 122.5(9) . . ? C20 C15 P 120.3(9) . . ? C15 C16 C17 122.4(12) . . ? C18 C17 C16 120.7(14) . . ? C17 C18 C19 119.2(13) . . ? C18 C19 C20 119.7(13) . . ? C19 C20 C15 121.1(12) . . ? C6 O C12 103.6(8) . . ? _refine_diff_density_max 2.780 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.164 #end# data_sjs2 _database_code_CSD 214950 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H23 Cl3 N2 O2 P Re' _chemical_formula_weight 706.97 _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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.008(4) _cell_length_b 8.481(2) _cell_length_c 34.252(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.65(3) _cell_angle_gamma 90.00 _cell_volume 5213.7(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description Parallopiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method ? _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 5.056 _exptl_absorpt_correction_type semi-emperical _exptl_absorpt_correction_T_min 0.130 _exptl_absorpt_correction_T_max 0.210 _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 R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4580 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4580 _reflns_number_observed 4058 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _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^)+(0.0775P)^2^+15.4599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _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 4563 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_obs 0.0391 _refine_ls_wR_factor_all 0.1263 _refine_ls_wR_factor_obs 0.1053 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.117 _refine_ls_restrained_S_all 1.260 _refine_ls_restrained_S_obs 1.117 _refine_ls_shift/esd_max -0.002 _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 0.598977(11) 0.86641(2) 0.608024(6) 0.03027(12) Uani 1 d . . Cl3 Cl 0.61595(10) 0.6195(2) 0.63910(5) 0.0457(4) Uani 1 d . . Cl1 Cl 0.51996(9) 0.7525(2) 0.55410(4) 0.0432(3) Uani 1 d . . Cl2 Cl 0.49389(8) 0.9387(2) 0.64057(5) 0.0458(4) Uani 1 d . . N1 N 0.5985(3) 1.0770(6) 0.57516(14) 0.0335(10) Uani 1 d . . N2 N 0.6902(3) 0.8429(5) 0.57403(14) 0.0319(10) Uani 1 d . . P P 0.67559(8) 0.9962(2) 0.65947(4) 0.0357(3) Uani 1 d . . O1 O 0.7630(2) 0.9523(5) 0.53124(13) 0.0462(10) Uani 1 d . . C1 C 0.5476(3) 1.1955(7) 0.5764(2) 0.0393(13) Uani 1 d . . H1A H 0.5092 1.1845 0.5928 0.047 Uiso 1 calc R . C2 C 0.5507(4) 1.3302(8) 0.5545(2) 0.051(2) Uani 1 d . . H2A H 0.5152 1.4090 0.5563 0.061 Uiso 1 calc R . C3 C 0.6070(5) 1.3482(9) 0.5297(3) 0.068(2) Uani 1 d . . H3A H 0.6101 1.4394 0.5148 0.081 Uiso 1 calc R . C4 C 0.6577(4) 1.2308(9) 0.5273(3) 0.065(2) Uani 1 d . . H4A H 0.6954 1.2402 0.5105 0.077 Uiso 1 calc R . C5 C 0.6528(3) 1.0954(8) 0.5504(2) 0.0401(13) Uani 1 d . . C6 C 0.7017(3) 0.9634(7) 0.5515(2) 0.0366(12) Uani 1 d . . C7 C 0.7489(3) 0.7376(7) 0.5682(2) 0.0359(12) Uani 1 d . . C12 C 0.7928(3) 0.8078(8) 0.5419(2) 0.0397(13) Uani 1 d . . C11 C 0.8558(4) 0.7377(9) 0.5287(2) 0.052(2) Uani 1 d . . H9A H 0.8848 0.7872 0.5111 0.063 Uiso 1 calc R . C10 C 0.8726(4) 0.5882(10) 0.5438(2) 0.056(2) Uani 1 d . . H10A H 0.9141 0.5352 0.5359 0.067 Uiso 1 calc R . C9 C 0.8289(4) 0.5167(9) 0.5701(2) 0.053(2) Uani 1 d . . H11A H 0.8425 0.4173 0.5797 0.064 Uiso 1 calc R . C8 C 0.7656(4) 0.5876(8) 0.5827(2) 0.0476(15) Uani 1 d . . H12A H 0.7359 0.5375 0.5999 0.057 Uiso 1 calc R . C13 C 0.7737(3) 0.9816(7) 0.6507(2) 0.0393(13) Uani 1 d . . C14 C 0.8095(4) 1.0960(9) 0.6301(2) 0.058(2) Uani 1 d . . H14A H 0.7843 1.1873 0.6219 0.069 Uiso 1 calc R . C15 C 0.8822(5) 1.0742(12) 0.6219(3) 0.072(2) Uani 1 d . . H15A H 0.9056 1.1508 0.6078 0.086 Uiso 1 calc R . C16 C 0.9203(4) 0.9429(13) 0.6340(3) 0.078(3) Uani 1 d . . H16A H 0.9698 0.9316 0.6285 0.093 Uiso 1 calc R . C17 C 0.8868(5) 0.8261(12) 0.6542(3) 0.076(2) Uani 1 d . . H17A H 0.9130 0.7357 0.6623 0.091 Uiso 1 calc R . C18 C 0.8123(4) 0.8467(9) 0.6623(3) 0.059(2) Uani 1 d . . H18A H 0.7886 0.7684 0.6757 0.071 Uiso 1 calc R . C19 C 0.6737(3) 0.9449(7) 0.7113(2) 0.0400(13) Uani 1 d . . C20 C 0.7279(4) 1.0070(9) 0.7379(2) 0.052(2) Uani 1 d . . H20A H 0.7674 1.0628 0.7287 0.062 Uiso 1 calc R . C21 C 0.7245(5) 0.9878(10) 0.7776(2) 0.063(2) Uani 1 d . . H21A H 0.7622 1.0279 0.7950 0.075 Uiso 1 calc R . C22 C 0.6656(5) 0.9096(12) 0.7916(2) 0.069(2) Uani 1 d . . H22A H 0.6615 0.9018 0.8184 0.083 Uiso 1 calc R . C23 C 0.6115(5) 0.8416(11) 0.7651(2) 0.070(2) Uani 1 d . . H23A H 0.5723 0.7843 0.7742 0.084 Uiso 1 calc R . C24 C 0.6168(5) 0.8605(9) 0.7252(2) 0.058(2) Uani 1 d . . H24A H 0.5810 0.8149 0.7076 0.070 Uiso 1 calc R . C25 C 0.6553(4) 1.2061(8) 0.6611(2) 0.055(2) Uani 1 d . . H25A H 0.6039 1.2211 0.6656 0.083 Uiso 1 calc R . H25B H 0.6650 1.2536 0.6365 0.083 Uiso 1 calc R . H25C H 0.6864 1.2543 0.6818 0.083 Uiso 1 calc R . O2 O 0.5519(6) 0.4626(16) 0.7301(3) 0.085(4) Uani 0.50 d P . O3 O 0.5000 1.1999(14) 0.7500 0.184(9) Uani 1 d S . 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 0.0281(2) 0.0301(2) 0.0332(2) 0.00146(8) 0.00580(10) -0.00016(8) Cl3 0.0500(9) 0.0378(8) 0.0497(9) 0.0118(6) 0.0054(7) 0.0003(6) Cl1 0.0422(8) 0.0459(8) 0.0411(8) -0.0037(6) 0.0015(6) -0.0046(7) Cl2 0.0341(7) 0.0556(10) 0.0495(8) -0.0006(7) 0.0142(6) 0.0044(7) N1 0.032(2) 0.028(2) 0.041(3) 0.004(2) 0.004(2) 0.001(2) N2 0.027(2) 0.033(2) 0.036(2) -0.001(2) 0.004(2) 0.002(2) P 0.0348(8) 0.0357(8) 0.0367(7) -0.0013(6) 0.0040(6) -0.0012(6) O1 0.041(2) 0.048(3) 0.051(2) 0.005(2) 0.016(2) 0.006(2) C1 0.035(3) 0.035(3) 0.048(3) 0.001(3) 0.006(3) 0.004(3) C2 0.046(4) 0.036(3) 0.069(5) 0.005(3) 0.003(3) 0.011(3) C3 0.066(5) 0.044(4) 0.094(6) 0.027(4) 0.013(5) 0.002(3) C4 0.051(4) 0.057(5) 0.088(6) 0.032(4) 0.027(4) 0.007(3) C5 0.037(3) 0.039(3) 0.045(3) 0.003(3) 0.009(3) -0.003(3) C6 0.030(3) 0.038(3) 0.043(3) 0.005(3) 0.013(2) -0.003(2) C7 0.028(3) 0.041(3) 0.038(3) -0.001(2) 0.001(2) 0.006(2) C12 0.035(3) 0.044(3) 0.040(3) -0.002(3) 0.002(2) 0.006(3) C11 0.033(3) 0.066(5) 0.060(4) -0.004(4) 0.014(3) 0.001(3) C10 0.035(3) 0.069(5) 0.063(4) -0.017(4) 0.001(3) 0.018(3) C9 0.044(4) 0.051(4) 0.065(4) 0.006(3) -0.001(3) 0.014(3) C8 0.051(4) 0.046(3) 0.046(3) 0.000(3) 0.006(3) 0.010(3) C13 0.033(3) 0.046(3) 0.039(3) -0.006(3) 0.004(2) -0.011(3) C14 0.052(4) 0.051(4) 0.071(5) -0.002(4) 0.012(4) -0.013(3) C15 0.056(5) 0.081(6) 0.084(6) -0.012(5) 0.037(4) -0.026(5) C16 0.032(4) 0.104(7) 0.099(7) -0.045(6) 0.020(4) -0.014(4) C17 0.046(4) 0.085(6) 0.097(7) -0.021(5) 0.010(4) 0.014(5) C18 0.046(4) 0.057(4) 0.076(5) 0.003(4) 0.015(4) 0.004(3) C19 0.042(3) 0.043(3) 0.035(3) -0.002(3) 0.003(3) 0.004(3) C20 0.056(4) 0.061(4) 0.039(3) -0.007(3) 0.000(3) 0.003(3) C21 0.074(5) 0.069(5) 0.042(4) -0.007(3) -0.013(4) 0.018(4) C22 0.072(5) 0.100(6) 0.035(3) 0.002(4) 0.005(4) 0.027(5) C23 0.066(5) 0.101(7) 0.046(4) 0.017(4) 0.020(4) 0.009(5) C24 0.049(4) 0.083(6) 0.043(4) 0.003(3) 0.003(3) -0.001(4) C25 0.061(4) 0.039(4) 0.065(4) -0.010(3) -0.006(4) 0.006(3) O2 0.074(8) 0.102(9) 0.083(8) -0.025(7) 0.043(6) -0.076(7) O3 0.350(24) 0.063(7) 0.120(10) 0.000 -0.096(13) 0.000 _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 2.098(5) . y Re N1 2.110(5) . y Re Cl2 2.354(2) . y Re Cl3 2.3578(15) . y Re P 2.414(2) . y Re Cl1 2.438(2) . y N1 C5 1.354(8) . ? N1 C1 1.363(8) . ? N2 C6 1.308(7) . ? N2 C7 1.412(7) . ? P C25 1.818(7) . ? P C13 1.820(6) . ? P C19 1.830(6) . ? O1 C6 1.353(7) . ? O1 C12 1.375(8) . ? C1 C2 1.371(9) . ? C2 C3 1.383(12) . ? C3 C4 1.356(11) . ? C4 C5 1.401(9) . ? C5 C6 1.422(9) . ? C7 C12 1.380(9) . ? C7 C8 1.389(9) . ? C12 C11 1.388(9) . ? C11 C10 1.393(11) . ? C10 C9 1.383(11) . ? C9 C8 1.390(10) . ? C13 C18 1.381(10) . ? C13 C14 1.388(9) . ? C14 C15 1.374(11) . ? C15 C16 1.356(14) . ? C16 C17 1.376(15) . ? C17 C18 1.403(11) . ? C19 C24 1.366(10) . ? C19 C20 1.385(9) . ? C20 C21 1.377(10) . ? C21 C22 1.370(13) . ? C22 C23 1.400(13) . ? C23 C24 1.389(11) . ? 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 75.7(2) . . y N2 Re Cl2 169.40(13) . . y N1 Re Cl2 93.66(13) . . y N2 Re Cl3 95.02(13) . . y N1 Re Cl3 170.76(13) . . y Cl2 Re Cl3 95.58(6) . . y N2 Re P 91.23(14) . . y N1 Re P 88.89(13) . . y Cl2 Re P 88.25(6) . . y Cl3 Re P 91.73(6) . . y N2 Re Cl1 88.69(14) . . y N1 Re Cl1 87.38(13) . . y Cl2 Re Cl1 91.13(6) . . y Cl3 Re Cl1 92.09(6) . . y P Re Cl1 176.18(5) . . y C5 N1 C1 117.1(5) . . ? C5 N1 Re 117.4(4) . . ? C1 N1 Re 125.5(4) . . ? C6 N2 C7 104.7(5) . . ? C6 N2 Re 115.0(4) . . ? C7 N2 Re 140.2(4) . . ? C25 P C13 105.7(3) . . ? C25 P C19 100.6(3) . . ? C13 P C19 103.8(3) . . ? C25 P Re 111.4(2) . . ? C13 P Re 110.7(2) . . ? C19 P Re 123.0(2) . . ? C6 O1 C12 104.1(4) . . ? N1 C1 C2 122.7(6) . . ? C1 C2 C3 119.5(6) . . ? C4 C3 C2 119.1(7) . . ? C3 C4 C5 119.7(7) . . ? N1 C5 C4 121.9(6) . . ? N1 C5 C6 111.7(5) . . ? C4 C5 C6 126.3(6) . . ? N2 C6 O1 115.0(5) . . ? N2 C6 C5 120.1(5) . . ? O1 C6 C5 124.8(5) . . ? C12 C7 C8 120.7(6) . . ? C12 C7 N2 107.2(5) . . ? C8 C7 N2 132.1(6) . . ? O1 C12 C7 109.0(5) . . ? O1 C12 C11 127.4(6) . . ? C7 C12 C11 123.6(6) . . ? C12 C11 C10 115.4(7) . . ? C9 C10 C11 121.5(6) . . ? C10 C9 C8 122.5(7) . . ? C7 C8 C9 116.4(7) . . ? C18 C13 C14 118.8(6) . . ? C18 C13 P 118.8(5) . . ? C14 C13 P 122.2(5) . . ? C15 C14 C13 120.1(8) . . ? C16 C15 C14 121.0(8) . . ? C15 C16 C17 120.9(8) . . ? C16 C17 C18 118.4(9) . . ? C13 C18 C17 120.9(8) . . ? C24 C19 C20 118.6(6) . . ? C24 C19 P 122.4(5) . . ? C20 C19 P 118.7(5) . . ? C21 C20 C19 121.3(7) . . ? C22 C21 C20 120.1(7) . . ? C21 C22 C23 119.4(7) . . ? C24 C23 C22 119.3(8) . . ? C19 C24 C23 121.2(8) . . ? _refine_diff_density_max 2.023 _refine_diff_density_min -2.520 _refine_diff_density_rms 0.185 #end#