# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1746 data_716re _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H42 Cl4 N4 O P2 Re' _chemical_formula_weight 1044.77 _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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.957(4) _cell_length_b 12.383(3) _cell_length_c 17.046(6) _cell_angle_alpha 88.36(2) _cell_angle_beta 74.21(2) _cell_angle_gamma 84.10(2) _cell_volume 2415.8(12) _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 parallelopiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method ? _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 2.839 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.137 _exptl_absorpt_correction_T_max 0.207 _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 7237 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.50 _reflns_number_total 7109 _reflns_number_observed 5904 _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 15 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^)+(0.0883P)^2^+2.0168P] 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 7094 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_obs 0.0467 _refine_ls_wR_factor_all 0.1533 _refine_ls_wR_factor_obs 0.1273 _refine_ls_goodness_of_fit_all 1.125 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.218 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max -0.001 _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 -0.35933(3) 0.97147(3) 0.67477(2) 0.03748(14) Uani 1 d . . Cl1 Cl -0.4931(2) 0.8394(2) 0.6841(2) 0.0595(6) Uani 1 d . . Cl2 Cl -0.2363(2) 0.8804(2) 0.55735(13) 0.0569(6) Uani 1 d . . Cl3 Cl -0.4770(2) 1.0479(2) 0.79847(13) 0.0589(6) Uani 1 d . . Cl4 Cl 0.1610(3) 1.1545(4) 0.7498(2) 0.1103(13) Uani 1 d . . P1 P -0.1873(2) 0.7929(2) 0.76933(12) 0.0388(5) Uani 1 d . . P2 P -0.2912(2) 0.4779(2) 0.7084(2) 0.0537(6) Uani 1 d . . O1 O -0.2626(5) 0.8813(4) 0.7402(3) 0.0425(13) Uani 1 d . . N1 N -0.4409(6) 1.0708(5) 0.6088(4) 0.042(2) Uani 1 d . . N2 N -0.4397(7) 1.2180(6) 0.5328(4) 0.054(2) Uani 1 d . . N3 N -0.2842(7) 1.1742(6) 0.5949(4) 0.048(2) Uani 1 d . . N4 N -0.2627(6) 1.0970(5) 0.6471(4) 0.041(2) Uani 1 d . . C1 C -0.5411(8) 1.0798(8) 0.5812(5) 0.051(2) Uani 1 d . . H1A H -0.5984(8) 1.0319(8) 0.5922(5) 0.062 Uiso 1 calc R . C2 C -0.5397(9) 1.1696(8) 0.5362(6) 0.056(2) Uani 1 d . . H2A H -0.5971(9) 1.1956(8) 0.5111(6) 0.067 Uiso 1 calc R . C3 C -0.3819(7) 1.1565(7) 0.5771(5) 0.042(2) Uani 1 d . . C4 C -0.4100(10) 1.3212(8) 0.4947(7) 0.071(3) Uani 1 d . . H4A H -0.4667(10) 1.3477(8) 0.4666(7) 0.107 Uiso 1 calc R . H4B H -0.3340(10) 1.3116(8) 0.4566(7) 0.107 Uiso 1 calc R . H4C H -0.4095(10) 1.3725(8) 0.5357(7) 0.107 Uiso 1 calc R . C5 C -0.1591(7) 1.1095(7) 0.6710(5) 0.045(2) Uani 1 d . . C6 C -0.0587(8) 1.1333(8) 0.6152(5) 0.054(2) Uani 1 d . . H6A H -0.0563(8) 1.1407(8) 0.5604(5) 0.065 Uiso 1 calc R . C7 C 0.0395(9) 1.1464(10) 0.6407(7) 0.073(3) Uani 1 d . . H7A H 0.1082(9) 1.1609(10) 0.6024(7) 0.087 Uiso 1 calc R . C8 C 0.0371(9) 1.1383(9) 0.7208(6) 0.065(3) Uani 1 d . . C9 C -0.0646(10) 1.1163(9) 0.7765(6) 0.071(3) Uani 1 d . . H9A H -0.0670(10) 1.1120(9) 0.8315(6) 0.085 Uiso 1 calc R . C10 C -0.1628(8) 1.1004(8) 0.7532(5) 0.053(2) Uani 1 d . . H10A H -0.2306(8) 1.0838(8) 0.7916(5) 0.064 Uiso 1 calc R . C11 C -0.0369(7) 0.8202(7) 0.7392(5) 0.047(2) Uani 1 d . . C12 C 0.0118(8) 0.8472(9) 0.6590(6) 0.060(3) Uani 1 d . . H12A H -0.0342(8) 0.8544(9) 0.6227(6) 0.072 Uiso 1 calc R . C13 C 0.1281(10) 0.8634(11) 0.6324(8) 0.082(3) Uani 1 d . . H13A H 0.1600(10) 0.8819(11) 0.5783(8) 0.098 Uiso 1 calc R . C14 C 0.1972(10) 0.8528(11) 0.6845(10) 0.089(4) Uani 1 d . . H14A H 0.2762(10) 0.8627(11) 0.6659(10) 0.107 Uiso 1 calc R . C15 C 0.1492(11) 0.8272(13) 0.7645(11) 0.108(5) Uani 1 d . . H15A H 0.1960(11) 0.8204(13) 0.8003(11) 0.130 Uiso 1 calc R . C16 C 0.0323(10) 0.8116(10) 0.7930(7) 0.080(3) Uani 1 d . . H16A H 0.0003(10) 0.7954(10) 0.8476(7) 0.096 Uiso 1 calc R . C17 C -0.2406(7) 0.7825(7) 0.8771(5) 0.046(2) Uani 1 d . . C18 C -0.3139(10) 0.8685(9) 0.9190(6) 0.069(3) Uani 1 d . . H18A H -0.3327(10) 0.9300(9) 0.8907(6) 0.082 Uiso 1 calc R . C19 C -0.3588(13) 0.8634(11) 1.0021(6) 0.093(4) Uani 1 d . . H19A H -0.4096(13) 0.9204(11) 1.0299(6) 0.112 Uiso 1 calc R . C20 C -0.3287(12) 0.7746(13) 1.0438(7) 0.097(4) Uani 1 d . . H20A H -0.3574(12) 0.7727(13) 1.1002(7) 0.116 Uiso 1 calc R . C21 C -0.2585(13) 0.6896(11) 1.0049(7) 0.093(4) Uani 1 d . . H21A H -0.2405(13) 0.6286(11) 1.0339(7) 0.111 Uiso 1 calc R . C22 C -0.2127(10) 0.6943(9) 0.9201(6) 0.074(3) Uani 1 d . . H22A H -0.1627(10) 0.6365(9) 0.8928(6) 0.089 Uiso 1 calc R . C23 C -0.1866(8) 0.6628(7) 0.7263(6) 0.051(2) Uani 1 d . . H23A H -0.1536(8) 0.6669(7) 0.6678(6) 0.062 Uiso 1 calc R . H23B H -0.1357(8) 0.6108(7) 0.7475(6) 0.062 Uiso 1 calc R . C24 C -0.3072(8) 0.6201(7) 0.7432(6) 0.051(2) Uani 1 d . . H24A H -0.3553(8) 0.6649(7) 0.7149(6) 0.061 Uiso 1 calc R . H24B H -0.3456(8) 0.6240(7) 0.8012(6) 0.061 Uiso 1 calc R . C25 C -0.4422(8) 0.4553(7) 0.7146(5) 0.047(2) Uani 1 d . . C26 C -0.5283(10) 0.5335(9) 0.7001(7) 0.072(3) Uani 1 d . . H26A H -0.5103(10) 0.6045(9) 0.6886(7) 0.086 Uiso 1 calc R . C27 C -0.6363(10) 0.5085(10) 0.7024(8) 0.080(3) Uani 1 d . . H27A H -0.6917(10) 0.5614(10) 0.6922(8) 0.096 Uiso 1 calc R . C28 C -0.6638(11) 0.4028(10) 0.7202(7) 0.079(3) Uani 1 d . . H28A H -0.7388(11) 0.3855(10) 0.7232(7) 0.094 Uiso 1 calc R . C29 C -0.5826(10) 0.3241(8) 0.7332(6) 0.066(3) Uani 1 d . . H29A H -0.6010(10) 0.2530(8) 0.7436(6) 0.080 Uiso 1 calc R . C30 C -0.4734(9) 0.3507(7) 0.7311(5) 0.056(2) Uani 1 d . . H30A H -0.4186(9) 0.2969(7) 0.7409(5) 0.067 Uiso 1 calc R . C31 C -0.2298(8) 0.4934(7) 0.5976(6) 0.058(2) Uani 1 d . . C32 C -0.1475(9) 0.4122(9) 0.5577(8) 0.074(3) Uani 1 d . . H32A H -0.1247(9) 0.3541(9) 0.5875(8) 0.089 Uiso 1 calc R . C33 C -0.0986(12) 0.4158(12) 0.4744(9) 0.100(5) Uani 1 d . . H33A H -0.0426(12) 0.3611(12) 0.4486(9) 0.120 Uiso 1 calc R . C34 C -0.1335(13) 0.5008(14) 0.4300(8) 0.099(5) Uani 1 d . . H34A H -0.1027(13) 0.5021(14) 0.3737(8) 0.119 Uiso 1 calc R . C35 C -0.2121(13) 0.5825(12) 0.4674(7) 0.095(4) Uani 1 d . . H35A H -0.2308(13) 0.6416(12) 0.4368(7) 0.114 Uiso 1 calc R . C36 C -0.2653(11) 0.5796(9) 0.5506(6) 0.075(3) Uani 1 d . . H36A H -0.3233(11) 0.6334(9) 0.5751(6) 0.090 Uiso 1 calc R . C37 C -0.6380(23) 0.6081(24) 1.0234(18) 0.181(10) Uani 1 d . . H37A H -0.6428(23) 0.5434(24) 1.0528(18) 0.218 Uiso 1 calc R . C38 C -0.6563(22) 0.7073(30) 1.0628(13) 0.169(10) Uani 1 d . . H38A H -0.6773(22) 0.7115(30) 1.1194(13) 0.202 Uiso 1 calc R . C39 C -0.6434(26) 0.7917(20) 1.0193(18) 0.181(11) Uani 1 d . . H39A H -0.6536(26) 0.8581(20) 1.0458(18) 0.217 Uiso 1 calc R . C40 C -0.6167(19) 0.7925(18) 0.9397(14) 0.141(7) Uani 1 d . . H40A H -0.6102(19) 0.8582(18) 0.9117(14) 0.170 Uiso 1 calc R . C41 C -0.5991(13) 0.7017(20) 0.8990(10) 0.114(5) Uani 1 d . . H41A H -0.5773(13) 0.7028(20) 0.8423(10) 0.137 Uiso 1 calc R . C42 C -0.6122(20) 0.6077(21) 0.9383(16) 0.160(8) Uani 1 d . . H42A H -0.6044(20) 0.5431(21) 0.9098(16) 0.192 Uiso 1 calc R . C43 C 0.0627(44) 0.9029(25) 0.9876(18) 0.181(13) Uani 1 d . . H43A H 0.0963(44) 0.8287(25) 0.9824(18) 0.217 Uiso 1 d R . C44 C -0.0576(36) 0.9070(32) 1.0272(13) 0.159(12) Uani 1 d . . H44A H -0.0947(36) 0.8447(32) 1.0445(13) 0.191 Uiso 1 calc R . C45 C -0.1150(28) 1.0064(43) 1.0384(18) 0.186(13) Uani 1 d . . H45A H -0.1958(28) 1.0010(43) 1.0657(18) 0.223 Uiso 1 d 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 0.0346(2) 0.0410(2) 0.0368(2) 0.00168(13) -0.00871(13) -0.00710(13) Cl1 0.0490(13) 0.0526(13) 0.085(2) 0.0157(12) -0.0285(12) -0.0178(11) Cl2 0.0528(13) 0.073(2) 0.0437(12) -0.0171(11) -0.0100(10) -0.0039(11) Cl3 0.0568(14) 0.0612(14) 0.0454(12) 0.0013(10) 0.0033(10) 0.0091(11) Cl4 0.075(2) 0.155(3) 0.123(3) -0.003(2) -0.048(2) -0.050(2) P1 0.0348(11) 0.0429(12) 0.0390(11) -0.0059(9) -0.0099(9) -0.0036(9) P2 0.058(2) 0.0447(13) 0.065(2) 0.0002(11) -0.0270(13) -0.0060(11) O1 0.038(3) 0.050(3) 0.039(3) 0.001(2) -0.011(2) -0.002(3) N1 0.041(4) 0.044(4) 0.042(4) 0.001(3) -0.015(3) -0.005(3) N2 0.069(5) 0.053(5) 0.045(4) 0.008(3) -0.022(4) -0.013(4) N3 0.061(5) 0.043(4) 0.043(4) 0.010(3) -0.015(4) -0.015(3) N4 0.044(4) 0.037(4) 0.038(4) -0.001(3) -0.004(3) -0.005(3) C1 0.045(5) 0.058(6) 0.057(5) 0.001(4) -0.021(4) -0.007(4) C2 0.064(6) 0.053(6) 0.057(6) 0.001(4) -0.029(5) 0.002(5) C3 0.039(5) 0.044(5) 0.043(5) 0.005(4) -0.013(4) -0.003(4) C4 0.086(8) 0.059(6) 0.080(7) 0.025(5) -0.037(6) -0.025(6) C5 0.044(5) 0.049(5) 0.042(5) -0.009(4) -0.010(4) -0.013(4) C6 0.049(5) 0.072(6) 0.038(5) 0.004(4) -0.002(4) -0.022(5) C7 0.047(6) 0.100(9) 0.069(7) 0.001(6) -0.001(5) -0.035(6) C8 0.055(6) 0.082(7) 0.067(7) -0.013(5) -0.023(5) -0.024(5) C9 0.074(7) 0.093(8) 0.054(6) -0.007(5) -0.025(5) -0.033(6) C10 0.052(5) 0.067(6) 0.044(5) 0.005(4) -0.011(4) -0.025(5) C11 0.036(5) 0.052(5) 0.054(5) -0.010(4) -0.013(4) -0.003(4) C12 0.033(5) 0.086(7) 0.057(6) -0.009(5) -0.003(4) 0.000(5) C13 0.049(7) 0.102(9) 0.080(8) -0.005(7) 0.008(6) -0.011(6) C14 0.043(6) 0.101(10) 0.124(12) -0.010(8) -0.022(7) -0.007(6) C15 0.058(8) 0.146(14) 0.140(14) 0.005(11) -0.054(9) -0.022(8) C16 0.058(7) 0.111(10) 0.080(8) 0.012(7) -0.032(6) -0.024(6) C17 0.042(5) 0.049(5) 0.048(5) -0.004(4) -0.016(4) -0.004(4) C18 0.073(7) 0.078(7) 0.046(6) -0.001(5) -0.008(5) 0.015(6) C19 0.130(12) 0.089(9) 0.044(6) -0.004(6) -0.013(7) 0.036(8) C20 0.104(10) 0.136(12) 0.036(6) 0.001(7) -0.001(6) 0.001(9) C21 0.136(12) 0.085(9) 0.051(7) 0.027(6) -0.022(7) 0.004(8) C22 0.085(8) 0.070(7) 0.060(6) 0.006(5) -0.015(6) 0.014(6) C23 0.045(5) 0.055(6) 0.051(5) -0.017(4) -0.007(4) -0.003(4) C24 0.044(5) 0.055(6) 0.055(5) -0.008(4) -0.014(4) -0.008(4) C25 0.058(6) 0.040(5) 0.046(5) 0.002(4) -0.015(4) -0.013(4) C26 0.079(8) 0.062(7) 0.084(8) 0.022(6) -0.033(6) -0.028(6) C27 0.060(7) 0.073(8) 0.117(10) 0.014(7) -0.039(7) -0.017(6) C28 0.071(8) 0.092(9) 0.083(8) 0.022(7) -0.029(6) -0.042(7) C29 0.087(8) 0.047(6) 0.067(7) 0.008(5) -0.020(6) -0.023(6) C30 0.073(7) 0.045(5) 0.049(5) 0.002(4) -0.013(5) -0.015(5) C31 0.050(6) 0.044(5) 0.083(7) -0.017(5) -0.021(5) -0.012(4) C32 0.058(7) 0.059(7) 0.098(9) -0.010(6) -0.004(6) -0.013(5) C33 0.076(9) 0.094(10) 0.106(11) -0.050(9) 0.024(8) -0.011(8) C34 0.103(11) 0.122(12) 0.065(8) -0.028(8) 0.003(8) -0.034(10) C35 0.105(10) 0.112(11) 0.063(8) -0.004(7) -0.017(7) -0.003(9) C36 0.094(9) 0.074(7) 0.056(6) -0.006(5) -0.027(6) 0.011(6) C37 0.193(24) 0.184(25) 0.150(21) 0.089(19) -0.020(19) -0.039(20) C38 0.179(22) 0.239(31) 0.086(13) -0.018(18) -0.040(14) 0.008(23) C39 0.268(33) 0.144(20) 0.147(22) 0.038(17) -0.066(22) -0.079(20) C40 0.168(19) 0.121(16) 0.119(16) 0.031(13) -0.012(14) -0.027(14) C41 0.081(10) 0.154(17) 0.092(11) 0.016(12) -0.003(8) 0.003(11) C42 0.165(20) 0.146(20) 0.145(19) -0.013(16) 0.005(15) -0.026(15) C43 0.296(50) 0.158(24) 0.133(20) -0.017(17) -0.115(28) -0.066(27) C44 0.186(26) 0.233(39) 0.078(12) -0.018(15) -0.042(15) -0.096(27) C45 0.198(28) 0.205(30) 0.182(26) -0.066(28) -0.092(22) -0.021(32) _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 2.000(6) . y Re N4 2.002(7) . y Re O1 2.048(5) . y Re Cl3 2.355(2) . y Re Cl2 2.372(2) . y Re Cl1 2.375(2) . y Cl4 C8 1.716(10) . ? P1 O1 1.505(6) . y P1 C17 1.778(9) . ? P1 C23 1.788(9) . ? P1 C11 1.796(9) . ? P2 C25 1.829(9) . ? P2 C31 1.843(11) . ? P2 C24 1.849(9) . ? N1 C3 1.353(10) . ? N1 C1 1.395(11) . ? N2 C3 1.330(10) . ? N2 C2 1.379(12) . ? N2 C4 1.449(11) . ? N3 C3 1.324(11) . ? N3 N4 1.340(9) . y N4 C5 1.428(11) . ? C1 C2 1.332(12) . ? C5 C6 1.366(12) . ? C5 C10 1.392(12) . ? C6 C7 1.383(13) . ? C7 C8 1.359(14) . ? C8 C9 1.371(14) . ? C9 C10 1.372(13) . ? C11 C12 1.378(13) . ? C11 C16 1.388(13) . ? C12 C13 1.374(14) . ? C13 C14 1.36(2) . ? C14 C15 1.37(2) . ? C15 C16 1.38(2) . ? C17 C22 1.361(13) . ? C17 C18 1.387(13) . ? C18 C19 1.374(14) . ? C19 C20 1.36(2) . ? C20 C21 1.34(2) . ? C21 C22 1.402(15) . ? C23 C24 1.538(12) . ? C25 C30 1.386(12) . ? C25 C26 1.406(14) . ? C26 C27 1.349(15) . ? C27 C28 1.39(2) . ? C28 C29 1.36(2) . ? C29 C30 1.369(14) . ? C31 C32 1.382(14) . ? C31 C36 1.415(14) . ? C32 C33 1.38(2) . ? C33 C34 1.38(2) . ? C34 C35 1.35(2) . ? C35 C36 1.39(2) . ? C37 C38 1.39(3) . ? C37 C42 1.40(3) . ? C38 C39 1.26(3) . ? C39 C40 1.31(3) . ? C40 C41 1.31(2) . ? C41 C42 1.33(3) . ? C43 C45 1.35(4) 2_577 ? C43 C44 1.41(4) . ? C44 C45 1.34(4) . ? C45 C43 1.35(4) 2_577 ? 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 N4 75.4(3) . . y N1 Re O1 173.9(2) . . y N4 Re O1 98.5(2) . . y N1 Re Cl3 92.3(2) . . y N4 Re Cl3 94.1(2) . . y O1 Re Cl3 88.3(2) . . y N1 Re Cl2 92.7(2) . . y N4 Re Cl2 88.8(2) . . y O1 Re Cl2 86.8(2) . . y Cl3 Re Cl2 174.67(8) . . y N1 Re Cl1 92.0(2) . . y N4 Re Cl1 166.9(2) . . y O1 Re Cl1 94.1(2) . . y Cl3 Re Cl1 89.51(10) . . y Cl2 Re Cl1 88.64(9) . . y O1 P1 C17 108.4(4) . . ? O1 P1 C23 113.6(4) . . ? C17 P1 C23 108.1(4) . . ? O1 P1 C11 110.8(4) . . ? C17 P1 C11 111.6(4) . . ? C23 P1 C11 104.3(4) . . ? C25 P2 C31 101.5(4) . . ? C25 P2 C24 102.0(4) . . ? C31 P2 C24 101.4(4) . . ? P1 O1 Re 164.0(4) . . y C3 N1 C1 106.1(7) . . ? C3 N1 Re 113.6(5) . . ? C1 N1 Re 140.2(6) . . ? C3 N2 C2 106.6(7) . . ? C3 N2 C4 127.1(8) . . ? C2 N2 C4 126.0(8) . . ? C3 N3 N4 108.2(7) . . ? N3 N4 C5 112.7(7) . . ? N3 N4 Re 120.9(5) . . ? C5 N4 Re 126.0(5) . . ? C2 C1 N1 107.5(8) . . ? C1 C2 N2 109.1(8) . . ? N3 C3 N2 128.1(8) . . ? N3 C3 N1 121.2(7) . . ? N2 C3 N1 110.5(7) . . ? C6 C5 C10 119.9(8) . . ? C6 C5 N4 121.3(8) . . ? C10 C5 N4 118.7(7) . . ? C5 C6 C7 119.8(9) . . ? C8 C7 C6 121.0(9) . . ? C7 C8 C9 118.8(9) . . ? C7 C8 Cl4 119.6(8) . . ? C9 C8 Cl4 121.6(8) . . ? C8 C9 C10 121.7(9) . . ? C9 C10 C5 118.7(9) . . ? C12 C11 C16 119.3(9) . . ? C12 C11 P1 118.4(7) . . ? C16 C11 P1 122.3(8) . . ? C13 C12 C11 120.2(10) . . ? C14 C13 C12 120.9(12) . . ? C13 C14 C15 119.3(11) . . ? C14 C15 C16 121.0(12) . . ? C15 C16 C11 119.3(12) . . ? C22 C17 C18 118.7(9) . . ? C22 C17 P1 123.1(7) . . ? C18 C17 P1 118.2(7) . . ? C19 C18 C17 120.3(10) . . ? C20 C19 C18 119.8(11) . . ? C21 C20 C19 121.3(10) . . ? C20 C21 C22 119.1(11) . . ? C17 C22 C21 120.8(10) . . ? C24 C23 P1 114.8(6) . . ? C23 C24 P2 110.1(6) . . ? C30 C25 C26 116.7(9) . . ? C30 C25 P2 117.3(7) . . ? C26 C25 P2 125.9(7) . . ? C27 C26 C25 121.9(10) . . ? C26 C27 C28 119.2(11) . . ? C29 C28 C27 120.8(10) . . ? C28 C29 C30 119.4(10) . . ? C29 C30 C25 121.9(10) . . ? C32 C31 C36 118.3(11) . . ? C32 C31 P2 117.3(9) . . ? C36 C31 P2 124.3(8) . . ? C33 C32 C31 121.3(12) . . ? C34 C33 C32 119.5(12) . . ? C35 C34 C33 120.7(13) . . ? C34 C35 C36 121.1(14) . . ? C35 C36 C31 119.0(11) . . ? C38 C37 C42 118.2(22) . . ? C39 C38 C37 117.8(23) . . ? C38 C39 C40 124.7(27) . . ? C41 C40 C39 120.4(21) . . ? C40 C41 C42 120.3(19) . . ? C41 C42 C37 118.4(22) . . ? C45 C43 C44 121.6(30) 2_577 . ? C45 C44 C43 115.7(30) . . ? C44 C45 C43 122.7(33) . 2_577 ? _refine_diff_density_max 1.892 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.147 #end# data_710re _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H40 Cl4 N4 O P2 Re' _chemical_formula_weight 1030.74 _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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.110(6) _cell_length_b 10.668(5) _cell_length_c 20.760(7) _cell_angle_alpha 89.47(3) _cell_angle_beta 80.08(4) _cell_angle_gamma 81.41(4) _cell_volume 2180.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description Parallelopiped _exptl_crystal_colour dark _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method ? _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 3.143 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.530 _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 6515 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 23.51 _reflns_number_total 6424 _reflns_number_observed 5198 _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 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^)+(0.0744P)^2^+12.6943P] 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 6423 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_obs 0.0542 _refine_ls_wR_factor_all 0.1477 _refine_ls_wR_factor_obs 0.1279 _refine_ls_goodness_of_fit_all 1.070 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.085 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.87453(4) 0.95248(4) 0.69905(2) 0.0353(2) Uani 1 d . . P1 P 0.7416(2) 1.1455(2) 0.75634(12) 0.0343(6) Uani 1 d . . P2 P 0.7226(3) 1.3289(2) 0.87514(13) 0.0406(6) Uani 1 d . . N1 N 0.8963(8) 1.0482(7) 0.6127(4) 0.042(2) Uani 1 d . . N2 N 0.8165(10) 1.1040(9) 0.5229(4) 0.050(2) Uani 1 d . . N3 N 0.7001(8) 0.9675(8) 0.5976(4) 0.041(2) Uani 1 d . . N4 N 0.7179(8) 0.9154(7) 0.6543(3) 0.034(2) Uani 1 d . . Cl1 Cl 1.0684(3) 1.0318(3) 0.7225(2) 0.0577(8) Uani 1 d . . Cl2 Cl 0.8386(3) 0.8516(3) 0.80040(13) 0.0515(7) Uani 1 d . . Cl3 Cl 1.0164(3) 0.7647(2) 0.65060(14) 0.0519(7) Uani 1 d . . Cl4 Cl 0.3001(4) 0.6039(4) 0.7662(2) 0.0851(11) Uani 1 d . . O1 O 0.6400(8) 1.4165(7) 0.8363(3) 0.052(2) Uani 1 d . . C1 C 0.9809(11) 1.1240(10) 0.5782(6) 0.052(3) Uani 1 d . . H1A H 1.0586(11) 1.1465(10) 0.5903(6) 0.062 Uiso 1 calc R . C2 C 0.9305(12) 1.1601(10) 0.5231(6) 0.054(3) Uani 1 d . . H2A H 0.9666(12) 1.2133(10) 0.4912(6) 0.065 Uiso 1 calc R . C3 C 0.7982(10) 1.0375(9) 0.5778(5) 0.040(2) Uani 1 d . . C4 C 0.7279(13) 1.1203(13) 0.4737(6) 0.070(4) Uani 1 d . . H4A H 0.7645(13) 1.1724(13) 0.4393(6) 0.106 Uiso 1 calc R . H4B H 0.6389(13) 1.1602(13) 0.4937(6) 0.106 Uiso 1 calc R . H4C H 0.7219(13) 1.0389(13) 0.4560(6) 0.106 Uiso 1 calc R . C5 C 0.6176(10) 0.8372(9) 0.6800(5) 0.042(2) Uani 1 d . . C6 C 0.4844(11) 0.8718(10) 0.6711(5) 0.047(3) Uani 1 d . . H6A H 0.4610(11) 0.9437(10) 0.6474(5) 0.056 Uiso 1 calc R . C7 C 0.3861(11) 0.7994(10) 0.6972(6) 0.051(3) Uani 1 d . . H7A H 0.2961(11) 0.8226(10) 0.6922(6) 0.061 Uiso 1 calc R . C8 C 0.4245(11) 0.6926(11) 0.7308(5) 0.049(3) Uani 1 d . . C9 C 0.5578(11) 0.6534(10) 0.7383(5) 0.049(3) Uani 1 d . . H9A H 0.5811(11) 0.5800(10) 0.7609(5) 0.059 Uiso 1 calc R . C10 C 0.6551(10) 0.7254(9) 0.7116(5) 0.039(2) Uani 1 d . . H10A H 0.7458(10) 0.6994(9) 0.7147(5) 0.047 Uiso 1 calc R . C11 C 0.5597(10) 1.1440(10) 0.7789(5) 0.044(2) Uani 1 d . . C12 C 0.4642(11) 1.2520(12) 0.7773(6) 0.056(3) Uani 1 d . . H12A H 0.4917(11) 1.3274(12) 0.7613(6) 0.067 Uiso 1 calc R . C13 C 0.3259(12) 1.2465(14) 0.8002(6) 0.070(4) Uani 1 d . . H13A H 0.2619(12) 1.3187(14) 0.8001(6) 0.084 Uiso 1 calc R . C14 C 0.2859(14) 1.1353(15) 0.8226(7) 0.075(4) Uani 1 d . . H14A H 0.1942(14) 1.1318(15) 0.8371(7) 0.091 Uiso 1 calc R . C15 C 0.3791(12) 1.0284(13) 0.8240(6) 0.064(4) Uani 1 d . . H15A H 0.3509(12) 0.9531(13) 0.8398(6) 0.077 Uiso 1 calc R . C16 C 0.5165(11) 1.0330(11) 0.8017(5) 0.052(3) Uani 1 d . . H16A H 0.5796(11) 0.9602(11) 0.8022(5) 0.062 Uiso 1 calc R . C17 C 0.7699(10) 1.2810(9) 0.7057(5) 0.042(2) Uani 1 d . . C18 C 0.8755(12) 1.3479(11) 0.7104(6) 0.055(3) Uani 1 d . . H18A H 0.9261(12) 1.3263(11) 0.7433(6) 0.066 Uiso 1 calc R . C19 C 0.9104(16) 1.4459(12) 0.6687(8) 0.081(5) Uani 1 d . . H19A H 0.9823(16) 1.4886(12) 0.6728(8) 0.097 Uiso 1 calc R . C20 C 0.8338(20) 1.4744(13) 0.6223(9) 0.097(6) Uani 1 d . . H20A H 0.8521(20) 1.5403(13) 0.5941(9) 0.116 Uiso 1 calc R . C21 C 0.7274(18) 1.4086(13) 0.6148(7) 0.086(5) Uani 1 d . . H21A H 0.6781(18) 1.4301(13) 0.5813(7) 0.103 Uiso 1 calc R . C22 C 0.6951(13) 1.3120(10) 0.6566(5) 0.058(3) Uani 1 d . . H22A H 0.6241(13) 1.2686(10) 0.6517(5) 0.070 Uiso 1 calc R . C23 C 0.7936(11) 1.1756(9) 0.8344(5) 0.042(2) Uani 1 d . . H23A H 0.8918(11) 1.1686(9) 0.8270(5) 0.051 Uiso 1 calc R . H23B H 0.7689(11) 1.1090(9) 0.8641(5) 0.051 Uiso 1 calc R . C24 C 0.6265(11) 1.2925(10) 0.9528(5) 0.048(3) Uani 1 d . . C25 C 0.5382(16) 1.2050(15) 0.9596(7) 0.085(5) Uani 1 d . . H25A H 0.5343(16) 1.1553(15) 0.9236(7) 0.102 Uiso 1 calc R . C26 C 0.4561(17) 1.1889(18) 1.0176(9) 0.108(6) Uani 1 d . . H26A H 0.3961(17) 1.1301(18) 1.0205(9) 0.130 Uiso 1 calc R . C27 C 0.4620(14) 1.2594(15) 1.0719(7) 0.078(4) Uani 1 d . . H27A H 0.4078(14) 1.2480(15) 1.1119(7) 0.094 Uiso 1 calc R . C28 C 0.5478(15) 1.3450(15) 1.0658(7) 0.079(4) Uani 1 d . . H28A H 0.5516(15) 1.3936(15) 1.1022(7) 0.095 Uiso 1 calc R . C29 C 0.6292(13) 1.3633(12) 1.0085(6) 0.066(3) Uani 1 d . . H29A H 0.6873(13) 1.4237(12) 1.0063(6) 0.079 Uiso 1 calc R . C30 C 0.8682(11) 1.3929(10) 0.8919(5) 0.048(3) Uani 1 d . . C31 C 0.8876(13) 1.5117(11) 0.8670(6) 0.062(3) Uani 1 d . . H31A H 0.8242(13) 1.5567(11) 0.8445(6) 0.074 Uiso 1 calc R . C32 C 1.0013(14) 1.5624(14) 0.8757(7) 0.075(4) Uani 1 d . . H32A H 1.0151(14) 1.6415(14) 0.8590(7) 0.090 Uiso 1 calc R . C33 C 1.0928(15) 1.4962(15) 0.9090(7) 0.077(4) Uani 1 d . . H33A H 1.1691(15) 1.5311(15) 0.9146(7) 0.092 Uiso 1 calc R . C34 C 1.0756(13) 1.3774(14) 0.9349(6) 0.069(4) Uani 1 d . . H34A H 1.1388(13) 1.3341(14) 0.9580(6) 0.082 Uiso 1 calc R . C35 C 0.9630(12) 1.3253(12) 0.9256(6) 0.059(3) Uani 1 d . . H35A H 0.9505(12) 1.2454(12) 0.9417(6) 0.070 Uiso 1 calc R . C36 C 0.1364(16) 0.9857(17) 0.9800(8) 0.093(5) Uani 1 d . . H36A H 0.2294(16) 0.9698(17) 0.9585(8) 0.140 Uiso 1 d R . C37 C 0.0541(19) 0.9368(15) 0.9411(7) 0.087(5) Uani 1 d . . H37A H 0.0912(19) 0.8953(15) 0.9014(7) 0.104 Uiso 1 calc R . C38 C -0.0804(19) 0.9526(17) 0.9638(8) 0.093(5) Uani 1 d . . H38A H -0.1245(19) 0.9154(17) 0.9329(8) 0.140 Uiso 1 d R . C39 C 0.5903(86) 0.5483(64) 0.4702(37) 0.220(39) Uani 0.50 d P . H39B H 0.5271(86) 0.4887(64) 0.4768(37) 0.264 Uiso 0.50 d PR . C40 C 0.7030(60) 0.5457(38) 0.4063(23) 0.283(32) Uani 1 d . . H40A H 0.7426(60) 0.4696(38) 0.3817(23) 0.339 Uiso 1 d R . C41 C 0.6857(38) 0.6472(70) 0.3701(15) 0.262(31) Uani 1 d . . H41A H 0.6897(38) 0.6429(70) 0.3251(15) 0.314 Uiso 1 calc R . C42 C 0.6635(46) 0.7487(40) 0.4014(26) 0.223(20) Uani 1 d . . H42A H 0.6521(46) 0.8233(40) 0.3782(26) 0.267 Uiso 1 calc R . C43 C 0.6542(26) 0.7591(27) 0.4710(20) 0.149(11) Uani 1 d . . H43A H 0.6238(26) 0.8395(27) 0.4932(20) 0.179 Uiso 1 d R . C44A C 0.7339(47) 0.6856(49) 0.4921(19) 0.104(12) Uani 0.50 d P . H44A H 0.7707(47) 0.7061(49) 0.5297(19) 0.125 Uiso 0.50 d PR . C44 C 0.6002(60) 0.6553(56) 0.4998(23) 0.136(18) Uani 0.50 d P . H44B H 0.5677(60) 0.6562(56) 0.5461(23) 0.164 Uiso 0.50 d PR . C39A C 0.7811(45) 0.5751(66) 0.4541(34) 0.188(31) Uani 0.50 d P . H39A H 0.8593(45) 0.5210(66) 0.4643(34) 0.226 Uiso 0.50 d PR . 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 0.0333(2) 0.0344(2) 0.0375(2) -0.0040(2) -0.0061(2) -0.0024(2) P1 0.0348(14) 0.0362(14) 0.0318(13) -0.0035(11) -0.0061(11) -0.0040(11) P2 0.044(2) 0.0401(15) 0.0378(15) -0.0092(11) -0.0115(12) -0.0010(12) N1 0.042(5) 0.038(5) 0.043(5) -0.002(4) -0.001(4) -0.003(4) N2 0.060(6) 0.058(6) 0.031(5) 0.004(4) -0.002(4) -0.011(5) N3 0.042(5) 0.049(5) 0.035(5) 0.001(4) -0.010(4) -0.006(4) N4 0.039(5) 0.037(4) 0.021(4) -0.005(3) 0.000(3) 0.004(4) Cl1 0.0357(14) 0.054(2) 0.085(2) -0.0137(15) -0.0175(14) -0.0057(12) Cl2 0.065(2) 0.051(2) 0.0405(14) 0.0041(12) -0.0153(13) -0.0062(13) Cl3 0.048(2) 0.0402(14) 0.061(2) -0.0067(12) 0.0018(13) 0.0032(12) Cl4 0.066(2) 0.101(3) 0.095(3) 0.024(2) -0.008(2) -0.042(2) O1 0.059(5) 0.046(4) 0.048(4) -0.005(3) -0.015(4) 0.005(4) C1 0.047(6) 0.041(6) 0.060(8) -0.010(5) 0.013(6) -0.010(5) C2 0.059(7) 0.044(6) 0.053(7) 0.010(5) 0.008(6) -0.007(6) C3 0.048(6) 0.040(6) 0.030(5) -0.003(4) 0.000(5) -0.009(5) C4 0.066(8) 0.089(10) 0.057(8) 0.016(7) -0.016(7) -0.009(7) C5 0.031(5) 0.044(6) 0.046(6) -0.002(5) -0.003(5) 0.002(5) C6 0.057(7) 0.047(6) 0.037(6) 0.008(5) -0.015(5) -0.007(5) C7 0.038(6) 0.050(7) 0.070(8) 0.011(6) -0.021(5) -0.009(5) C8 0.039(6) 0.065(7) 0.044(6) -0.008(5) -0.001(5) -0.012(5) C9 0.052(7) 0.043(6) 0.054(7) 0.006(5) -0.016(5) -0.003(5) C10 0.040(6) 0.034(5) 0.042(6) -0.005(4) 0.001(5) -0.005(4) C11 0.031(5) 0.053(7) 0.045(6) -0.011(5) -0.003(5) -0.005(5) C12 0.047(7) 0.069(8) 0.053(7) 0.005(6) -0.014(5) -0.005(6) C13 0.042(7) 0.086(10) 0.074(9) 0.008(7) -0.001(6) 0.004(7) C14 0.047(8) 0.108(12) 0.072(9) -0.025(8) -0.007(7) -0.014(8) C15 0.049(7) 0.079(9) 0.064(8) -0.025(7) 0.008(6) -0.028(7) C16 0.048(7) 0.052(7) 0.053(7) -0.007(5) 0.000(5) -0.009(5) C17 0.048(6) 0.038(6) 0.035(6) -0.001(4) -0.007(5) 0.010(5) C18 0.052(7) 0.053(7) 0.057(7) -0.010(6) 0.004(6) -0.015(6) C19 0.078(10) 0.053(8) 0.086(10) 0.014(7) 0.035(9) 0.014(7) C20 0.129(16) 0.038(8) 0.099(13) 0.018(8) 0.036(12) 0.001(9) C21 0.123(14) 0.060(9) 0.058(9) 0.015(7) -0.013(9) 0.035(9) C22 0.067(8) 0.046(7) 0.049(7) -0.002(5) 0.009(6) 0.014(6) C23 0.051(6) 0.035(5) 0.040(6) -0.007(4) -0.014(5) 0.005(5) C24 0.046(6) 0.058(7) 0.039(6) -0.006(5) -0.008(5) -0.006(5) C25 0.097(11) 0.104(11) 0.063(9) -0.020(8) -0.002(8) -0.054(10) C26 0.095(12) 0.136(15) 0.094(13) 0.009(11) 0.025(10) -0.064(12) C27 0.066(9) 0.109(12) 0.047(8) -0.002(8) 0.015(7) 0.003(8) C28 0.076(10) 0.102(11) 0.057(9) -0.017(8) 0.005(7) -0.024(9) C29 0.069(8) 0.075(9) 0.051(7) -0.013(6) 0.004(6) -0.020(7) C30 0.048(6) 0.054(7) 0.042(6) -0.009(5) -0.005(5) -0.010(5) C31 0.069(8) 0.048(7) 0.071(8) 0.000(6) -0.021(7) -0.010(6) C32 0.066(9) 0.077(9) 0.089(10) -0.009(8) -0.010(8) -0.036(8) C33 0.066(9) 0.098(11) 0.075(9) -0.020(8) -0.004(7) -0.049(9) C34 0.054(8) 0.099(11) 0.058(8) -0.004(7) -0.020(6) -0.016(7) C35 0.056(7) 0.062(7) 0.059(7) -0.002(6) -0.014(6) -0.010(6) C36 0.073(10) 0.126(14) 0.077(11) 0.020(10) -0.003(9) -0.017(10) C37 0.119(14) 0.098(11) 0.042(8) -0.003(7) -0.006(9) -0.020(10) C38 0.104(13) 0.136(15) 0.056(9) 0.026(9) -0.030(9) -0.052(12) C39 0.386(126) 0.115(46) 0.176(64) 0.046(41) -0.153(77) 0.025(55) C40 0.472(82) 0.202(37) 0.173(36) -0.094(30) -0.194(51) 0.119(42) C41 0.172(28) 0.517(94) 0.092(20) -0.065(36) -0.091(19) 0.048(43) C42 0.291(51) 0.219(42) 0.214(44) 0.052(33) -0.140(42) -0.109(38) C43 0.106(17) 0.117(21) 0.225(35) -0.050(22) -0.040(21) 0.004(16) C44A 0.076(25) 0.145(39) 0.086(25) 0.016(26) -0.002(21) -0.016(27) C44 0.178(55) 0.107(36) 0.106(32) 0.015(30) -0.027(32) 0.037(35) C39A 0.080(31) 0.227(64) 0.202(60) 0.101(51) 0.051(34) 0.067(36) _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 2.050(8) . y Re N4 2.055(8) . y Re Cl2 2.351(3) . y Re Cl1 2.372(3) . y Re Cl3 2.401(3) . y Re P1 2.476(3) . y P1 C17 1.808(10) . ? P1 C11 1.820(10) . ? P1 C23 1.832(10) . ? P2 O1 1.486(8) . y P2 C30 1.799(11) . ? P2 C24 1.805(11) . ? P2 C23 1.837(9) . ? N1 C3 1.344(13) . ? N1 C1 1.372(13) . ? N2 C3 1.336(13) . ? N2 C2 1.376(14) . ? N2 C4 1.463(15) . ? N3 N4 1.325(11) . y N3 C3 1.337(12) . ? N4 C5 1.439(12) . ? Cl4 C8 1.745(11) . ? C1 C2 1.36(2) . ? C5 C6 1.386(14) . ? C5 C10 1.390(14) . ? C6 C7 1.383(14) . ? C7 C8 1.37(2) . ? C8 C9 1.385(15) . ? C9 C10 1.377(14) . ? C11 C16 1.375(15) . ? C11 C12 1.392(15) . ? C12 C13 1.41(2) . ? C13 C14 1.36(2) . ? C14 C15 1.37(2) . ? C15 C16 1.39(2) . ? C17 C22 1.38(2) . ? C17 C18 1.387(15) . ? C18 C19 1.40(2) . ? C19 C20 1.34(2) . ? C20 C21 1.40(2) . ? C21 C22 1.38(2) . ? C24 C25 1.38(2) . ? C24 C29 1.39(2) . ? C25 C26 1.37(2) . ? C26 C27 1.38(2) . ? C27 C28 1.34(2) . ? C28 C29 1.36(2) . ? C30 C35 1.39(2) . ? C30 C31 1.39(2) . ? C31 C32 1.38(2) . ? C32 C33 1.36(2) . ? C33 C34 1.40(2) . ? C34 C35 1.38(2) . ? C36 C38 1.34(2) 2_577 ? C36 C37 1.41(2) . ? C37 C38 1.35(2) . ? C38 C36 1.34(2) 2_577 ? C39 C44 1.33(7) . ? C39 C40 1.59(9) . ? C39 C39A 1.96(9) . ? C40 C41 1.32(6) . ? C40 C39A 1.43(8) . ? C41 C42 1.24(5) . ? C42 C43 1.44(4) . ? C43 C44A 1.18(5) . ? C43 C44 1.39(6) . ? C44A C39A 1.40(8) . ? C44A C44 1.42(7) . ? C44 C39A 1.98(6) . ? 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 N4 74.7(3) . . y N1 Re Cl2 176.7(2) . . y N4 Re Cl2 104.3(2) . . y N1 Re Cl1 88.2(3) . . y N4 Re Cl1 162.9(2) . . y Cl2 Re Cl1 92.77(11) . . y N1 Re Cl3 92.7(2) . . y N4 Re Cl3 91.1(2) . . y Cl2 Re Cl3 90.51(10) . . y Cl1 Re Cl3 90.13(11) . . y N1 Re P1 90.3(2) . . y N4 Re P1 93.7(2) . . y Cl2 Re P1 86.58(10) . . y Cl1 Re P1 85.84(10) . . y Cl3 Re P1 174.91(9) . . y C17 P1 C11 109.1(5) . . ? C17 P1 C23 106.8(5) . . ? C11 P1 C23 103.4(5) . . ? C17 P1 Re 108.7(3) . . ? C11 P1 Re 115.7(3) . . ? C23 P1 Re 112.6(3) . . ? O1 P2 C30 112.2(5) . . ? O1 P2 C24 112.4(5) . . ? C30 P2 C24 107.1(5) . . ? O1 P2 C23 114.1(4) . . ? C30 P2 C23 104.4(5) . . ? C24 P2 C23 106.0(5) . . ? C3 N1 C1 107.1(9) . . ? C3 N1 Re 113.2(6) . . ? C1 N1 Re 139.6(8) . . ? C3 N2 C2 107.1(9) . . ? C3 N2 C4 126.5(10) . . ? C2 N2 C4 126.3(9) . . ? N4 N3 C3 109.3(8) . . ? N3 N4 C5 113.7(8) . . ? N3 N4 Re 120.6(6) . . ? C5 N4 Re 125.6(6) . . ? C2 C1 N1 107.7(10) . . ? C1 C2 N2 107.8(9) . . ? N2 C3 N3 127.6(10) . . ? N2 C3 N1 110.2(9) . . ? N3 C3 N1 122.1(9) . . ? C6 C5 C10 120.3(10) . . ? C6 C5 N4 119.6(9) . . ? C10 C5 N4 120.1(9) . . ? C7 C6 C5 120.1(10) . . ? C8 C7 C6 118.4(10) . . ? C7 C8 C9 122.6(10) . . ? C7 C8 Cl4 118.6(8) . . ? C9 C8 Cl4 118.8(9) . . ? C10 C9 C8 118.6(10) . . ? C9 C10 C5 119.8(10) . . ? C16 C11 C12 119.2(10) . . ? C16 C11 P1 118.1(8) . . ? C12 C11 P1 122.6(8) . . ? C11 C12 C13 119.6(12) . . ? C14 C13 C12 120.0(13) . . ? C13 C14 C15 120.8(12) . . ? C14 C15 C16 119.7(13) . . ? C11 C16 C15 120.7(11) . . ? C22 C17 C18 118.2(10) . . ? C22 C17 P1 120.2(9) . . ? C18 C17 P1 121.3(8) . . ? C17 C18 C19 124.0(14) . . ? C20 C19 C18 115.9(16) . . ? C19 C20 C21 122.5(14) . . ? C22 C21 C20 120.5(15) . . ? C17 C22 C21 118.9(14) . . ? P1 C23 P2 116.8(5) . . ? C25 C24 C29 116.6(11) . . ? C25 C24 P2 123.1(9) . . ? C29 C24 P2 119.9(9) . . ? C26 C25 C24 121.9(13) . . ? C25 C26 C27 120.1(14) . . ? C28 C27 C26 118.4(13) . . ? C27 C28 C29 122.4(13) . . ? C28 C29 C24 120.6(12) . . ? C35 C30 C31 120.3(11) . . ? C35 C30 P2 122.2(9) . . ? C31 C30 P2 117.4(9) . . ? C32 C31 C30 119.7(13) . . ? C33 C32 C31 119.7(13) . . ? C32 C33 C34 121.9(12) . . ? C35 C34 C33 118.8(13) . . ? C34 C35 C30 119.7(12) . . ? C38 C36 C37 120.3(15) 2_577 . ? C38 C37 C36 117.2(14) . . ? C36 C38 C37 122.5(15) 2_577 . ? C44 C39 C40 102.5(60) . . ? C44 C39 C39A 71.1(51) . . ? C40 C39 C39A 46.1(35) . . ? C41 C40 C39A 106.9(45) . . ? C41 C40 C39 113.4(40) . . ? C39A C40 C39 80.8(32) . . ? C42 C41 C40 114.1(34) . . ? C41 C42 C43 124.6(44) . . ? C44A C43 C44 66.4(34) . . ? C44A C43 C42 113.6(34) . . ? C44 C43 C42 108.6(32) . . ? C43 C44A C39A 114.9(45) . . ? C43 C44A C44 64.1(31) . . ? C39A C44A C44 89.4(42) . . ? C39 C44 C43 126.9(51) . . ? C39 C44 C44A 114.5(58) . . ? C43 C44 C44A 49.4(34) . . ? C39 C44 C39A 69.6(49) . . ? C43 C44 C39A 78.1(36) . . ? C44A C44 C39A 44.9(32) . . ? C44A C39A C40 117.7(38) . . ? C44A C39A C39 85.0(35) . . ? C40 C39A C39 53.1(33) . . ? C44A C39A C44 45.7(27) . . ? C40 C39A C44 82.1(34) . . ? C39 C39A C44 39.3(24) . . ? _refine_diff_density_max 1.624 _refine_diff_density_min -2.802 _refine_diff_density_rms 0.159 #end# data_709re _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H31 Cl4 N4 O2 P2 Re' _chemical_formula_weight 929.58 _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 35.353(11) _cell_length_b 12.730(6) _cell_length_c 16.840(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.68(3) _cell_angle_gamma 90.00 _cell_volume 7331.5(51) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description rhombic _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method ? _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 3.732 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.194 _exptl_absorpt_correction_T_max 0.242 _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 5705 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 23.50 _reflns_number_total 5422 _reflns_number_observed 3386 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 10 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^)+(0.0374P)^2^+80.4023P] 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 5412 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_obs 0.0585 _refine_ls_wR_factor_all 0.1369 _refine_ls_wR_factor_obs 0.1060 _refine_ls_goodness_of_fit_all 1.115 _refine_ls_goodness_of_fit_obs 1.129 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.129 _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 0.087663(15) 0.29803(4) -0.02101(3) 0.0540(2) Uani 1 d . . Cl1 Cl 0.12880(13) 0.4147(3) 0.0727(3) 0.0959(14) Uani 1 d . . Cl2 Cl 0.05719(10) 0.2506(3) 0.0840(2) 0.0770(11) Uani 1 d . . Cl3 Cl 0.12343(10) 0.3366(3) -0.1179(2) 0.0789(11) Uani 1 d . . P1 P 0.14685(9) 0.1041(3) 0.0828(2) 0.0534(9) Uani 1 d . . P2 P 0.18710(9) 0.1355(3) 0.2718(2) 0.0509(8) Uani 1 d . . O1 O 0.1232(2) 0.1716(6) 0.0131(5) 0.060(2) Uani 1 d . . O2 O 0.1825(3) 0.0256(6) 0.2920(5) 0.067(2) Uani 1 d . . N1 N 0.0481(3) 0.4093(9) -0.0637(7) 0.065(3) Uani 1 d . . N2 N -0.0110(4) 0.4525(12) -0.1422(9) 0.089(4) Uani 1 d . . N3 N 0.0113(3) 0.2724(10) -0.1385(7) 0.072(3) Uani 1 d . . N4 N 0.0455(3) 0.2254(8) -0.1030(6) 0.056(3) Uani 1 d . . C1 C 0.0427(5) 0.5175(12) -0.0571(10) 0.088(5) Uani 1 d . . H1A H 0.0604(5) 0.5643(12) -0.0253(10) 0.106 Uiso 1 calc R . C2 C 0.0071(6) 0.5416(16) -0.1052(13) 0.107(6) Uani 1 d . . H2A H -0.0036(6) 0.6087(16) -0.1123(13) 0.128 Uiso 1 calc R . C3 C 0.0151(5) 0.3735(12) -0.1149(10) 0.071(4) Uani 1 d . . C4 C -0.0491(4) 0.4438(14) -0.1993(10) 0.114(7) Uani 1 d . . H4A H -0.0612(4) 0.5118(14) -0.2076(10) 0.171 Uiso 1 calc R . H4B H -0.0651(4) 0.3968(14) -0.1774(10) 0.171 Uiso 1 calc R . H4C H -0.0463(4) 0.4171(14) -0.2507(10) 0.171 Uiso 1 calc R . C5 C 0.0469(3) 0.1138(11) -0.1224(8) 0.062(4) Uani 1 d . . C6 C 0.0175(5) 0.0495(14) -0.1148(12) 0.114(7) Uani 1 d . . H6A H -0.0031(5) 0.0769(14) -0.0961(12) 0.137 Uiso 1 calc R . C7 C 0.0173(5) -0.0554(13) -0.1343(12) 0.110(6) Uani 1 d . . H7A H -0.0033(5) -0.0987(13) -0.1305(12) 0.132 Uiso 1 calc R . C8 C 0.0488(5) -0.0946(13) -0.1598(11) 0.096(5) Uani 1 d . . C9 C 0.0790(5) -0.0304(12) -0.1644(9) 0.076(4) Uani 1 d . . H9A H 0.1002(5) -0.0582(12) -0.1806(9) 0.091 Uiso 1 calc R . C10 C 0.0789(4) 0.0766(11) -0.1453(8) 0.066(4) Uani 1 d . . H10A H 0.0996(4) 0.1204(11) -0.1480(8) 0.080 Uiso 1 calc R . Cl4 Cl 0.0512(2) -0.2263(4) -0.1833(4) 0.145(2) Uani 1 d . . C11 C 0.1224(4) -0.0153(10) 0.0907(8) 0.054(3) Uani 1 d . . C12 C 0.1037(5) -0.0360(16) 0.1479(11) 0.122(7) Uani 1 d . . H12A H 0.1038(5) 0.0136(16) 0.1885(11) 0.147 Uiso 1 calc R . C13 C 0.0835(5) -0.1314(20) 0.1485(12) 0.145(9) Uani 1 d . . H13A H 0.0723(5) -0.1449(20) 0.1918(12) 0.175 Uiso 1 calc R . C14 C 0.0799(5) -0.2028(14) 0.0894(12) 0.100(5) Uani 1 d . . H14A H 0.0643(5) -0.2622(14) 0.0873(12) 0.120 Uiso 1 calc R . C15 C 0.1001(6) -0.1839(11) 0.0327(13) 0.108(6) Uani 1 d . . H15A H 0.0989(6) -0.2329(11) -0.0088(13) 0.129 Uiso 1 calc R . C16 C 0.1236(5) -0.0908(14) 0.0339(10) 0.103(6) Uani 1 d . . H16A H 0.1390(5) -0.0826(14) -0.0029(10) 0.123 Uiso 1 calc R . C17 C 0.1925(3) 0.0760(10) 0.0612(8) 0.055(3) Uani 1 d . . C18 C 0.2175(4) 0.0006(11) 0.1039(8) 0.065(4) Uani 1 d . . H18A H 0.2098(4) -0.0404(11) 0.1428(8) 0.078 Uiso 1 calc R . C19 C 0.2538(4) -0.0143(13) 0.0894(9) 0.077(4) Uani 1 d . . H19A H 0.2709(4) -0.0646(13) 0.1184(9) 0.093 Uiso 1 calc R . C20 C 0.2642(4) 0.0466(13) 0.0313(10) 0.083(5) Uani 1 d . . H20A H 0.2889(4) 0.0384(13) 0.0227(10) 0.100 Uiso 1 calc R . C21 C 0.2397(4) 0.1182(12) -0.0140(10) 0.084(5) Uani 1 d . . H21A H 0.2472(4) 0.1563(12) -0.0547(10) 0.100 Uiso 1 calc R . C22 C 0.2036(4) 0.1341(11) 0.0010(9) 0.074(4) Uani 1 d . . H22A H 0.1866(4) 0.1838(11) -0.0292(9) 0.089 Uiso 1 calc R . C23 C 0.1542(3) 0.1780(9) 0.1772(7) 0.055(3) Uani 1 d . . H23A H 0.1626(3) 0.2478(9) 0.1659(7) 0.065 Uiso 1 calc R . H23B H 0.1287(3) 0.1861(9) 0.1881(7) 0.065 Uiso 1 calc R . C24 C 0.2363(3) 0.1666(10) 0.2665(7) 0.048(3) Uani 1 d . . C25 C 0.2654(4) 0.0927(13) 0.2939(9) 0.084(5) Uani 1 d . . H25A H 0.2592(4) 0.0283(13) 0.3134(9) 0.101 Uiso 1 calc R . C26 C 0.3033(5) 0.1136(16) 0.2926(10) 0.096(5) Uani 1 d . . H26A H 0.3227(5) 0.0634(16) 0.3110(10) 0.115 Uiso 1 calc R . C27 C 0.3125(5) 0.2075(19) 0.2646(10) 0.100(6) Uani 1 d . . H27A H 0.3384(5) 0.2219(19) 0.2654(10) 0.120 Uiso 1 calc R . C28 C 0.2847(5) 0.2811(15) 0.2354(9) 0.088(5) Uani 1 d . . H28A H 0.2912(5) 0.3442(15) 0.2145(9) 0.106 Uiso 1 calc R . C29 C 0.2463(4) 0.2609(12) 0.2371(8) 0.072(4) Uani 1 d . . H29A H 0.2271(4) 0.3115(12) 0.2182(8) 0.087 Uiso 1 calc R . C30 C 0.1768(4) 0.2246(10) 0.3457(8) 0.055(3) Uani 1 d . . C31 C 0.1949(5) 0.2009(13) 0.4282(9) 0.093(5) Uani 1 d . . H31A H 0.2104(5) 0.1411(13) 0.4413(9) 0.111 Uiso 1 calc R . C32 C 0.1896(6) 0.2667(14) 0.4892(10) 0.102(6) Uani 1 d . . H32A H 0.2023(6) 0.2525(14) 0.5436(10) 0.123 Uiso 1 calc R . C33 C 0.1653(6) 0.3549(14) 0.4704(13) 0.104(7) Uani 1 d . . H33A H 0.1609(6) 0.3973(14) 0.5120(13) 0.124 Uiso 1 calc R . C34 C 0.1485(5) 0.3773(13) 0.3917(12) 0.087(5) Uani 1 d . . H34A H 0.1329(5) 0.4368(13) 0.3787(12) 0.105 Uiso 1 calc R . C35 C 0.1541(4) 0.3143(12) 0.3303(9) 0.074(4) Uani 1 d . . H35A H 0.1423(4) 0.3322(12) 0.2762(9) 0.089 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 0.0474(3) 0.0518(3) 0.0624(3) -0.0005(3) 0.0128(2) 0.0046(3) Cl1 0.106(3) 0.065(3) 0.105(3) -0.018(2) 0.004(3) -0.015(2) Cl2 0.079(2) 0.078(2) 0.085(3) 0.012(2) 0.041(2) 0.024(2) Cl3 0.072(2) 0.081(3) 0.093(3) 0.014(2) 0.039(2) 0.000(2) P1 0.047(2) 0.061(2) 0.048(2) -0.009(2) 0.004(2) 0.008(2) P2 0.055(2) 0.050(2) 0.046(2) -0.007(2) 0.009(2) 0.000(2) O1 0.057(5) 0.063(6) 0.052(5) -0.009(4) -0.001(4) 0.017(4) O2 0.087(7) 0.041(5) 0.071(6) -0.005(5) 0.017(5) -0.009(5) N1 0.078(8) 0.049(7) 0.075(8) -0.007(6) 0.032(7) 0.002(6) N2 0.079(10) 0.093(11) 0.103(11) 0.039(9) 0.040(8) 0.048(9) N3 0.038(6) 0.096(10) 0.079(8) 0.015(7) 0.005(5) 0.029(6) N4 0.046(6) 0.053(8) 0.068(7) 0.004(5) 0.011(5) 0.010(5) C1 0.110(14) 0.064(11) 0.104(13) 0.007(10) 0.053(11) 0.018(10) C2 0.095(14) 0.089(14) 0.146(19) 0.036(14) 0.046(13) 0.046(12) C3 0.071(11) 0.060(10) 0.087(12) 0.014(9) 0.032(9) 0.025(9) C4 0.070(11) 0.171(19) 0.104(13) 0.049(13) 0.025(10) 0.061(12) C5 0.031(7) 0.063(9) 0.085(10) -0.006(8) 0.000(7) 0.003(7) C6 0.076(12) 0.084(13) 0.182(20) -0.059(13) 0.033(12) -0.013(10) C7 0.067(11) 0.075(12) 0.179(20) -0.036(12) 0.015(12) -0.025(10) C8 0.079(12) 0.079(12) 0.122(15) -0.028(11) 0.010(11) 0.016(10) C9 0.086(11) 0.069(11) 0.078(11) -0.017(9) 0.030(9) 0.011(9) C10 0.057(9) 0.076(11) 0.066(9) -0.002(8) 0.014(7) 0.012(8) Cl4 0.146(5) 0.086(4) 0.186(6) -0.054(4) 0.010(4) 0.012(3) C11 0.059(8) 0.059(9) 0.043(8) -0.006(7) 0.011(7) -0.001(7) C12 0.114(14) 0.168(20) 0.101(14) -0.070(13) 0.056(12) -0.077(14) C13 0.119(16) 0.231(26) 0.096(15) -0.029(17) 0.045(12) -0.114(17) C14 0.112(13) 0.080(12) 0.117(15) -0.035(12) 0.046(12) -0.035(11) C15 0.150(17) 0.036(10) 0.147(17) 0.001(10) 0.057(14) -0.009(10) C16 0.135(16) 0.090(13) 0.102(14) -0.010(11) 0.063(12) -0.002(12) C17 0.049(8) 0.052(8) 0.061(9) -0.010(7) 0.010(7) 0.003(7) C18 0.058(9) 0.083(10) 0.056(9) 0.003(8) 0.018(7) 0.020(8) C19 0.068(10) 0.100(12) 0.060(10) 0.000(9) 0.011(8) 0.025(9) C20 0.046(8) 0.110(13) 0.101(13) 0.013(11) 0.032(9) 0.025(9) C21 0.073(11) 0.089(11) 0.100(13) 0.008(10) 0.044(10) 0.013(10) C22 0.066(10) 0.059(10) 0.096(12) 0.003(9) 0.017(9) 0.019(8) C23 0.049(7) 0.059(9) 0.050(8) -0.013(6) 0.003(6) 0.007(6) C24 0.051(7) 0.061(8) 0.029(7) -0.014(6) 0.005(6) 0.002(6) C25 0.066(10) 0.095(12) 0.079(11) -0.013(9) -0.003(8) 0.016(10) C26 0.062(11) 0.130(17) 0.088(13) -0.020(12) 0.004(9) 0.010(11) C27 0.066(11) 0.164(20) 0.077(12) -0.008(14) 0.032(9) -0.014(14) C28 0.065(10) 0.117(15) 0.086(11) -0.005(11) 0.026(9) -0.019(11) C29 0.060(9) 0.081(11) 0.071(10) 0.007(8) 0.007(7) 0.000(8) C30 0.063(8) 0.051(9) 0.053(9) -0.006(7) 0.020(7) -0.006(7) C31 0.141(14) 0.073(10) 0.074(11) -0.012(10) 0.045(10) 0.007(11) C32 0.168(18) 0.087(13) 0.062(11) -0.018(10) 0.048(12) -0.012(13) C33 0.141(17) 0.075(13) 0.126(17) -0.052(13) 0.091(15) -0.043(12) C34 0.088(12) 0.080(12) 0.102(13) -0.037(12) 0.041(11) 0.003(9) C35 0.071(9) 0.080(11) 0.065(9) -0.029(9) 0.005(7) -0.006(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N4 1.985(10) . y Re N1 1.993(11) . y Re O1 2.033(7) . y Re Cl3 2.356(4) . y Re Cl2 2.370(4) . y Re Cl1 2.377(4) . y P1 O1 1.523(8) . y P1 C11 1.770(13) . ? P1 C17 1.778(12) . ? P1 C23 1.808(11) . ? P2 O2 1.459(8) . y P2 C30 1.788(12) . ? P2 C23 1.801(11) . ? P2 C24 1.807(12) . ? N1 C3 1.34(2) . ? N1 C1 1.40(2) . ? N2 C3 1.36(2) . ? N2 C2 1.37(2) . ? N2 C4 1.45(2) . ? N3 N4 1.343(12) . y N3 C3 1.34(2) . ? N4 C5 1.46(2) . ? C1 C2 1.35(2) . ? C5 C6 1.36(2) . ? C5 C10 1.37(2) . ? C6 C7 1.38(2) . ? C7 C8 1.38(2) . ? C8 C9 1.36(2) . ? C8 Cl4 1.73(2) . ? C9 C10 1.40(2) . ? C11 C12 1.33(2) . ? C11 C16 1.36(2) . ? C12 C13 1.41(2) . ? C13 C14 1.33(2) . ? C14 C15 1.35(2) . ? C15 C16 1.44(2) . ? C17 C18 1.38(2) . ? C17 C22 1.39(2) . ? C18 C19 1.38(2) . ? C19 C20 1.37(2) . ? C20 C21 1.35(2) . ? C21 C22 1.38(2) . ? C24 C29 1.38(2) . ? C24 C25 1.39(2) . ? C25 C26 1.37(2) . ? C26 C27 1.35(2) . ? C27 C28 1.36(2) . ? C28 C29 1.39(2) . ? C30 C35 1.38(2) . ? C30 C31 1.41(2) . ? C31 C32 1.38(2) . ? C32 C33 1.40(2) . ? C33 C34 1.34(2) . ? C34 C35 1.36(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 N4 Re N1 75.2(4) . . y N4 Re O1 97.5(4) . . y N1 Re O1 172.7(4) . . y N4 Re Cl3 93.2(3) . . y N1 Re Cl3 93.0(3) . . y O1 Re Cl3 87.7(3) . . y N4 Re Cl2 89.8(3) . . y N1 Re Cl2 92.3(3) . . y O1 Re Cl2 87.3(3) . . y Cl3 Re Cl2 174.43(13) . . y N4 Re Cl1 168.0(3) . . y N1 Re Cl1 92.9(4) . . y O1 Re Cl1 94.4(2) . . y Cl3 Re Cl1 89.08(15) . . y Cl2 Re Cl1 88.9(2) . . y O1 P1 C11 111.1(5) . . ? O1 P1 C17 107.7(6) . . ? C11 P1 C17 109.1(6) . . ? O1 P1 C23 108.2(5) . . ? C11 P1 C23 110.2(6) . . ? C17 P1 C23 110.4(5) . . ? O2 P2 C30 113.1(6) . . ? O2 P2 C23 114.2(6) . . ? C30 P2 C23 103.0(6) . . ? O2 P2 C24 112.7(6) . . ? C30 P2 C24 105.3(5) . . ? C23 P2 C24 107.7(6) . . ? P1 O1 Re 147.5(5) . . y C3 N1 C1 105.7(13) . . ? C3 N1 Re 114.0(9) . . ? C1 N1 Re 140.3(12) . . ? C3 N2 C2 104.9(14) . . ? C3 N2 C4 127.2(17) . . ? C2 N2 C4 127.8(15) . . ? N4 N3 C3 106.5(11) . . ? N3 N4 C5 114.3(10) . . ? N3 N4 Re 122.3(8) . . ? C5 N4 Re 123.0(7) . . ? C2 C1 N1 107.6(17) . . ? C1 C2 N2 110.0(16) . . ? N1 C3 N3 121.4(12) . . ? N1 C3 N2 111.7(15) . . ? N3 C3 N2 126.7(16) . . ? C6 C5 C10 121.8(14) . . ? C6 C5 N4 119.7(12) . . ? C10 C5 N4 118.5(12) . . ? C5 C6 C7 121.4(16) . . ? C6 C7 C8 118.0(16) . . ? C9 C8 C7 120.3(15) . . ? C9 C8 Cl4 119.0(13) . . ? C7 C8 Cl4 120.7(15) . . ? C8 C9 C10 121.6(14) . . ? C5 C10 C9 116.9(14) . . ? C12 C11 C16 118.6(15) . . ? C12 C11 P1 124.6(12) . . ? C16 C11 P1 116.8(11) . . ? C11 C12 C13 121.6(16) . . ? C14 C13 C12 122.4(17) . . ? C13 C14 C15 116.1(17) . . ? C14 C15 C16 122.7(17) . . ? C11 C16 C15 118.0(15) . . ? C18 C17 C22 119.3(12) . . ? C18 C17 P1 121.9(11) . . ? C22 C17 P1 118.8(10) . . ? C17 C18 C19 120.4(13) . . ? C20 C19 C18 118.5(14) . . ? C21 C20 C19 122.5(13) . . ? C20 C21 C22 119.1(14) . . ? C21 C22 C17 120.1(13) . . ? P2 C23 P1 122.5(6) . . ? C29 C24 C25 118.3(13) . . ? C29 C24 P2 123.1(10) . . ? C25 C24 P2 118.6(11) . . ? C26 C25 C24 120.7(16) . . ? C27 C26 C25 119.8(17) . . ? C26 C27 C28 121.3(16) . . ? C27 C28 C29 119.2(16) . . ? C24 C29 C28 120.7(14) . . ? C35 C30 C31 117.4(12) . . ? C35 C30 P2 127.2(10) . . ? C31 C30 P2 115.4(10) . . ? C32 C31 C30 119.4(16) . . ? C31 C32 C33 120.8(17) . . ? C34 C33 C32 119.2(16) . . ? C33 C34 C35 120.8(17) . . ? C34 C35 C30 122.3(14) . . ? _refine_diff_density_max 1.119 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.129 #end#