# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2309 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H58 Cl N4 O15 Re' _chemical_formula_weight 1332.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.947(17) _cell_length_b 23.90(3) _cell_length_c 16.640(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.769(10) _cell_angle_gamma 90.00 _cell_volume 6298(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type DIFABS(Walker and Stuart, 1983) _exptl_absorpt_correction_T_min 0.303 _exptl_absorpt_correction_T_max 1.000 _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17787 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.04 _reflns_number_total 10509 _reflns_number_gt 4314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refinement two of the -CO2Et groups had high thermal motion and their dimensions were constrained. The relatively high shift/su_max value was due to methyl hydrogen atoms. The highest residual density was located close to the metal atom. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10509 _refine_ls_number_parameters 733 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.2151 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.3055 _refine_ls_wR_factor_gt 0.2500 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 3.288 _refine_ls_shift/su_mean 0.062 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.26370(4) 0.10708(2) 0.14822(4) 0.0870(3) Uani 1 d . . . Cl1 Cl 0.2891(3) 0.0523(2) 0.2723(3) 0.1270(16) Uani 1 d . . . C300 C 0.3700(13) 0.0835(8) 0.1115(12) 0.120(7) Uani 1 d . . . O300 O 0.4297(9) 0.0688(6) 0.0863(13) 0.188(9) Uani 1 d . . . C100 C 0.2355(8) 0.1464(6) 0.0433(10) 0.067(4) Uani 1 d . . . O100 O 0.2243(7) 0.1685(6) -0.0078(10) 0.128(5) Uani 1 d . . . C200 C 0.3210(12) 0.1726(8) 0.1923(12) 0.126(6) Uani 1 d . . . O200 O 0.3521(10) 0.2129(7) 0.2208(10) 0.172(6) Uani 1 d . . . N199 N 0.1392(8) 0.1199(5) 0.1868(7) 0.083(3) Uani 1 d . . . N175 N 0.1889(6) 0.0371(4) 0.1032(6) 0.066(3) Uani 1 d . . . C174 C 0.2153(8) -0.0059(6) 0.0599(9) 0.081(4) Uani 1 d . . . H174 H 0.2698 -0.0036 0.0456 0.097 Uiso 1 calc R . . C173 C 0.1694(8) -0.0523(5) 0.0351(9) 0.080(4) Uani 1 d . . . H173 H 0.1930 -0.0802 0.0060 0.096 Uiso 1 calc R . . C172 C 0.0882(6) -0.0572(5) 0.0534(7) 0.056(3) Uani 1 d . . . C171 C 0.0571(7) -0.0135(5) 0.0957(8) 0.070(3) Uani 1 d . . . H171 H 0.0019 -0.0144 0.1086 0.084 Uiso 1 calc R . . C170 C 0.1116(9) 0.0334(5) 0.1195(8) 0.069(3) Uani 1 d . . . C169 C 0.0804(8) 0.0798(5) 0.1663(9) 0.078(4) Uani 1 d . . . C168 C 0.0001(10) 0.0860(6) 0.1867(10) 0.093(4) Uani 1 d . . . H168 H -0.0391 0.0574 0.1756 0.112 Uiso 1 calc R . . C167 C -0.0231(10) 0.1354(7) 0.2245(9) 0.095(4) Uani 1 d . . . C166 C -0.1194(12) 0.1401(9) 0.2415(15) 0.164(9) Uani 1 d . . . H16A H -0.1516 0.1105 0.2137 0.197 Uiso 1 calc R . . H16B H -0.1419 0.1755 0.2223 0.197 Uiso 1 calc R . . H16C H -0.1226 0.1371 0.2986 0.197 Uiso 1 calc R . . C165 C 0.0383(11) 0.1730(6) 0.2458(10) 0.091(4) Uani 1 d . . . H165 H 0.0254 0.2050 0.2738 0.109 Uiso 1 calc R . . C164 C 0.1148(10) 0.1662(6) 0.2286(9) 0.083(4) Uani 1 d . . . H164 H 0.1549 0.1934 0.2450 0.100 Uiso 1 calc R . . C163 C 0.0328(8) -0.1066(5) 0.0316(7) 0.061(3) Uani 1 d . . . O162 O -0.0449(5) -0.1033(3) 0.0300(6) 0.076(2) Uani 1 d . . . N161 N 0.0767(6) -0.1537(4) 0.0208(6) 0.071(3) Uani 1 d . . . H161 H 0.1307 -0.1506 0.0246 0.085 Uiso 1 calc R . . C160 C 0.0423(7) -0.2080(5) 0.0038(7) 0.056(3) Uani 1 d . . . C159 C -0.0335(8) -0.2172(6) -0.0394(8) 0.078(4) Uani 1 d . . . H159 H -0.0650 -0.1866 -0.0602 0.093 Uiso 1 calc R . . C158 C -0.0663(8) -0.2705(6) -0.0542(9) 0.086(4) Uani 1 d . . . H158 H -0.1187 -0.2755 -0.0843 0.104 Uiso 1 calc R . . C157 C -0.0209(8) -0.3149(6) -0.0240(10) 0.091(4) Uani 1 d . . . H157 H -0.0419 -0.3509 -0.0328 0.110 Uiso 1 calc R . . C156 C 0.0588(8) -0.3062(6) 0.0211(8) 0.080(4) Uani 1 d . . . H156 H 0.0899 -0.3368 0.0426 0.097 Uiso 1 calc R . . C155 C 0.0907(7) -0.2534(5) 0.0336(8) 0.066(3) Uani 1 d . . . N154 N 0.1668(5) -0.2496(4) 0.0915(6) 0.064(3) Uani 1 d . . . H154 H 0.1683 -0.2675 0.1365 0.077 Uiso 1 calc R . . C152 C 0.2356(7) -0.2188(6) 0.0773(9) 0.070(3) Uani 1 d . . . C151 C 0.3105(7) -0.2224(6) 0.1391(9) 0.083(4) Uani 1 d . . . H15A H 0.3604 -0.2288 0.1123 0.100 Uiso 1 calc R . . H15B H 0.3176 -0.1870 0.1676 0.100 Uiso 1 calc R . . O153 O 0.2409(5) -0.1858(4) 0.0226(6) 0.083(3) Uani 1 d . . . O150 O 0.3029(4) -0.2673(3) 0.1979(5) 0.073(2) Uani 1 d . . . C16 C 0.3592(7) -0.2600(5) 0.2687(8) 0.065(3) Uani 1 d . . . C11 C 0.4449(7) -0.2782(5) 0.2658(8) 0.072(3) Uani 1 d . . . C12 C 0.5020(7) -0.2673(5) 0.3359(8) 0.070(3) Uani 1 d . . . H12 H 0.5578 -0.2788 0.3374 0.084 Uiso 1 calc R . . C13 C 0.4776(7) -0.2410(6) 0.3996(9) 0.086(4) Uani 1 d . . . H13 H 0.5176 -0.2308 0.4424 0.103 Uiso 1 calc R . . C14 C 0.3921(8) -0.2285(7) 0.4028(9) 0.099(5) Uani 1 d . . . H14 H 0.3763 -0.2131 0.4501 0.119 Uiso 1 calc R . . C15 C 0.3313(7) -0.2379(6) 0.3399(9) 0.083(4) Uani 1 d . . . C17 C 0.2393(7) -0.2285(6) 0.3459(10) 0.085(4) Uani 1 d . . . H17A H 0.2060 -0.2426 0.2977 0.102 Uiso 1 calc R . . H17B H 0.2283 -0.1887 0.3498 0.102 Uiso 1 calc R . . C21 C 0.2141(8) -0.2581(10) 0.4197(10) 0.090(5) Uani 1 d . . . C22 C 0.2013(9) -0.2278(11) 0.486(2) 0.158(9) Uani 1 d . . . H22 H 0.1985 -0.1890 0.4824 0.190 Uiso 1 calc R . . C23 C 0.1919(11) -0.2557(12) 0.5623(12) 0.121(7) Uani 1 d . . . H23 H 0.1806 -0.2348 0.6069 0.145 Uiso 1 calc R . . C24 C 0.1993(12) -0.3097(11) 0.5679(15) 0.126(7) Uani 1 d . . . H24 H 0.1953 -0.3275 0.6170 0.151 Uiso 1 calc R . . C25 C 0.2133(11) -0.3407(10) 0.5002(14) 0.113(6) Uani 1 d . . . C26 C 0.2164(8) -0.3118(10) 0.4296(13) 0.101(5) Uani 1 d . . . C27 C 0.2358(10) -0.3985(12) 0.5157(11) 0.151(11) Uani 1 d . . . H27A H 0.1994 -0.4223 0.4796 0.181 Uiso 1 calc R . . H27B H 0.2272 -0.4079 0.5708 0.181 Uiso 1 calc R . . C31 C 0.3282(11) -0.4094(8) 0.5035(12) 0.108(6) Uani 1 d . . . C32 C 0.3891(11) -0.3767(8) 0.5456(10) 0.112(6) Uani 1 d . . . H32 H 0.3745 -0.3514 0.5841 0.134 Uiso 1 calc R . . C33 C 0.4722(11) -0.3815(7) 0.5304(11) 0.101(5) Uani 1 d . . . H33 H 0.5140 -0.3611 0.5611 0.121 Uiso 1 calc R . . C34 C 0.4926(10) -0.4147(8) 0.4728(11) 0.101(5) Uani 1 d . . . H34 H 0.5488 -0.4148 0.4628 0.121 Uiso 1 calc R . . C35 C 0.4361(10) -0.4507(8) 0.4244(10) 0.103(5) Uani 1 d . . . C36 C 0.3551(11) -0.4485(8) 0.4432(11) 0.104(5) Uani 1 d . . . C37 C 0.4567(10) -0.4865(6) 0.3563(9) 0.096(4) Uani 1 d . . . H37A H 0.4054 -0.4993 0.3244 0.115 Uiso 1 calc R . . H37B H 0.4891 -0.5189 0.3766 0.115 Uiso 1 calc R . . C43 C 0.6437(9) -0.4169(7) 0.2633(9) 0.087(4) Uani 1 d . . . H43 H 0.7015 -0.4214 0.2630 0.104 Uiso 1 calc R . . C42 C 0.5946(9) -0.4571(7) 0.3029(9) 0.090(4) Uani 1 d . . . H42 H 0.6214 -0.4884 0.3274 0.107 Uiso 1 calc R . . C41 C 0.5082(9) -0.4501(6) 0.3052(9) 0.084(4) Uani 1 d . . . C44 C 0.6028(8) -0.3725(6) 0.2269(8) 0.079(4) Uani 1 d . . . H44 H 0.6341 -0.3458 0.2026 0.095 Uiso 1 calc R . . C45 C 0.5150(7) -0.3647(5) 0.2240(7) 0.063(3) Uani 1 d . . . C46 C 0.4683(8) -0.4051(6) 0.2626(8) 0.080(4) Uani 1 d . . . C47 C 0.4763(7) -0.3095(5) 0.1966(8) 0.076(4) Uani 1 d . . . H47A H 0.4297 -0.3159 0.1547 0.092 Uiso 1 calc R . . H47B H 0.5181 -0.2869 0.1736 0.092 Uiso 1 calc R . . O250 O 0.2256(5) -0.3445(5) 0.3600(6) 0.091(3) Uani 1 d . . . C251 C 0.1604(11) -0.3828(7) 0.3326(9) 0.108(5) Uani 1 d . . . H25A H 0.1861 -0.4182 0.3207 0.129 Uiso 1 calc R . . H25B H 0.1263 -0.3893 0.3762 0.129 Uiso 1 calc R . . C252 C 0.1067(8) -0.3656(6) 0.2633(10) 0.079(4) Uani 1 d . . . O253 O 0.0380(6) -0.3947(4) 0.2507(7) 0.098(3) Uani 1 d . . . O254 O 0.1186(5) -0.3258(5) 0.2167(7) 0.104(3) Uani 1 d . . . C256 C -0.0937(12) -0.4215(10) 0.1811(19) 0.222(15) Uani 1 d . . . H25C H -0.0817 -0.4461 0.2266 0.267 Uiso 1 calc R . . H25D H -0.1049 -0.4433 0.1325 0.267 Uiso 1 calc R . . H25E H -0.1421 -0.3990 0.1881 0.267 Uiso 1 calc R . . C255 C -0.0205(11) -0.3850(7) 0.1747(16) 0.152(10) Uani 1 d . . . H25F H -0.0378 -0.3461 0.1706 0.183 Uiso 1 calc R . . H25G H 0.0068 -0.3947 0.1275 0.183 Uiso 1 calc R . . O450 O 0.3832(5) -0.3995(3) 0.2642(6) 0.075(2) Uani 1 d . . . C451 C 0.3292(9) -0.4013(7) 0.1881(11) 0.100(5) Uani 1 d . . . H45A H 0.2847 -0.3735 0.1877 0.120 Uiso 1 calc R . . H45B H 0.3616 -0.3935 0.1437 0.120 Uiso 1 calc R . . C452 C 0.2933(10) -0.4566(8) 0.1800(10) 0.100(5) Uani 1 d . . . O453 O 0.3341(7) -0.5020(5) 0.1762(9) 0.135(5) Uani 1 d . . . O454 O 0.2097(6) -0.4591(5) 0.1597(11) 0.169(7) Uani 1 d D . . C455 C 0.1669(18) -0.5111(10) 0.135(2) 0.26(2) Uani 1 d D . . H45C H 0.2089 -0.5403 0.1342 0.318 Uiso 1 calc R . . H45D H 0.1387 -0.5068 0.0809 0.318 Uiso 1 calc R . . C456 C 0.104(2) -0.5293(15) 0.189(3) 0.63(8) Uani 1 d D . . H45E H 0.0622 -0.5004 0.1918 0.751 Uiso 1 calc R . . H45F H 0.1315 -0.5364 0.2426 0.751 Uiso 1 calc R . . H45G H 0.0763 -0.5629 0.1681 0.751 Uiso 1 calc R . . O350 O 0.2902(6) -0.4797(5) 0.3995(8) 0.117(4) Uani 1 d D . . C351 C 0.2839(11) -0.5347(10) 0.4292(16) 0.184(11) Uani 1 d D . . H35A H 0.3146 -0.5390 0.4827 0.221 Uiso 1 calc R . . H35B H 0.3035 -0.5622 0.3929 0.221 Uiso 1 calc R . . C352 C 0.1869(16) -0.5383(12) 0.431(2) 0.37(3) Uiso 1 d D . . O353 O 0.172(2) -0.577(2) 0.477(2) 0.62(2) Uiso 1 d D . . O354 O 0.163(2) -0.547(2) 0.348(2) 0.62(2) Uiso 1 d D . . C355 C 0.168(5) -0.607(3) 0.339(4) 0.62(2) Uiso 1 d D . . H35C H 0.2247 -0.6188 0.3585 0.746 Uiso 1 calc R . . H35D H 0.1577 -0.6158 0.2818 0.746 Uiso 1 calc R . . C356 C 0.105(5) -0.640(3) 0.384(4) 0.62(2) Uiso 1 d D . . H35E H 0.1175 -0.6790 0.3808 0.746 Uiso 1 calc R . . H35F H 0.0489 -0.6327 0.3589 0.746 Uiso 1 calc R . . H35G H 0.1107 -0.6282 0.4393 0.746 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0880(5) 0.0819(5) 0.0908(6) 0.0056(4) 0.0098(3) -0.0141(3) Cl1 0.146(4) 0.119(3) 0.112(4) 0.007(3) -0.003(3) -0.004(3) C300 0.124(15) 0.100(12) 0.128(16) 0.034(12) -0.015(12) -0.052(11) O300 0.098(9) 0.124(11) 0.35(3) 0.056(13) 0.069(12) 0.011(8) C100 0.049(7) 0.061(9) 0.093(13) 0.005(8) 0.011(7) -0.009(5) O100 0.083(7) 0.130(12) 0.171(15) 0.011(10) 0.017(8) -0.016(7) C200 0.145(15) 0.105(14) 0.134(17) -0.029(12) 0.043(12) -0.035(11) O200 0.193(14) 0.139(12) 0.179(15) -0.031(11) 0.007(11) -0.076(10) N199 0.106(9) 0.078(8) 0.067(8) -0.001(6) 0.014(6) -0.011(6) N175 0.061(6) 0.060(6) 0.083(8) 0.007(6) 0.030(5) 0.003(4) C174 0.065(7) 0.074(9) 0.105(12) 0.018(9) 0.020(7) -0.005(6) C173 0.095(10) 0.059(8) 0.092(11) -0.003(7) 0.035(8) 0.004(6) C172 0.055(6) 0.054(7) 0.060(8) 0.015(6) 0.007(5) 0.007(5) C171 0.066(7) 0.081(9) 0.063(9) 0.024(7) 0.012(6) 0.008(6) C170 0.099(10) 0.047(7) 0.059(9) 0.007(6) 0.008(7) 0.006(6) C169 0.080(9) 0.065(8) 0.089(11) 0.011(8) 0.006(7) -0.004(7) C168 0.102(11) 0.065(8) 0.112(14) 0.005(9) 0.011(9) 0.002(7) C167 0.122(12) 0.082(10) 0.081(12) -0.021(9) 0.019(9) 0.013(9) C166 0.128(15) 0.141(17) 0.23(3) -0.066(18) 0.058(15) 0.023(13) C165 0.115(12) 0.069(9) 0.089(12) -0.017(8) 0.011(9) -0.002(8) C164 0.104(11) 0.060(9) 0.085(11) -0.005(8) 0.006(8) -0.009(7) C163 0.078(8) 0.055(7) 0.050(8) 0.002(6) 0.010(6) 0.003(6) O162 0.059(5) 0.068(5) 0.101(7) -0.003(5) 0.016(4) 0.009(4) N161 0.061(6) 0.070(7) 0.083(8) 0.007(6) 0.013(5) 0.011(5) C160 0.066(7) 0.052(7) 0.050(8) -0.008(6) 0.009(6) -0.007(5) C159 0.077(8) 0.090(10) 0.067(10) 0.001(8) 0.012(7) 0.010(7) C158 0.078(8) 0.086(10) 0.090(11) -0.025(8) -0.012(8) 0.004(7) C157 0.078(9) 0.074(9) 0.121(14) -0.018(9) 0.009(8) -0.010(7) C156 0.087(9) 0.079(9) 0.069(10) -0.013(7) -0.018(7) 0.015(7) C155 0.063(7) 0.078(9) 0.057(8) -0.010(7) 0.006(6) 0.001(6) N154 0.059(6) 0.070(6) 0.061(7) 0.006(5) 0.000(5) 0.004(4) C152 0.070(8) 0.065(8) 0.076(11) 0.002(7) 0.018(7) 0.009(6) C151 0.063(8) 0.078(9) 0.109(12) 0.017(9) 0.009(7) 0.004(6) O153 0.061(5) 0.098(7) 0.089(7) 0.017(6) 0.009(4) 0.005(4) O150 0.052(4) 0.076(6) 0.088(7) -0.005(5) -0.001(4) -0.002(4) C16 0.055(7) 0.062(7) 0.078(10) 0.002(7) 0.005(7) -0.002(5) C11 0.059(7) 0.081(9) 0.077(10) 0.008(7) 0.020(7) -0.003(6) C12 0.062(7) 0.071(8) 0.078(10) -0.019(7) 0.011(7) 0.003(5) C13 0.058(8) 0.106(11) 0.092(12) -0.028(9) 0.001(7) -0.005(6) C14 0.075(9) 0.153(15) 0.070(10) -0.051(10) 0.005(8) -0.001(8) C15 0.047(7) 0.119(11) 0.081(10) -0.030(9) 0.002(7) 0.001(6) C17 0.050(7) 0.089(10) 0.115(14) -0.012(9) 0.005(7) 0.006(6) C21 0.058(8) 0.142(16) 0.070(12) -0.018(12) 0.010(7) 0.033(9) C22 0.051(10) 0.21(2) 0.22(3) -0.02(3) 0.006(13) 0.026(10) C23 0.114(14) 0.19(2) 0.063(13) -0.038(14) 0.020(10) 0.018(14) C24 0.113(13) 0.128(17) 0.14(2) 0.012(16) 0.012(12) -0.014(12) C25 0.105(13) 0.150(17) 0.089(15) -0.014(15) 0.033(10) 0.035(11) C26 0.052(8) 0.137(17) 0.114(18) 0.020(15) 0.017(8) 0.021(8) C27 0.079(11) 0.31(4) 0.068(12) 0.061(16) 0.045(9) 0.002(14) C31 0.096(12) 0.123(14) 0.104(15) 0.047(12) 0.011(11) 0.005(10) C32 0.096(12) 0.176(18) 0.063(11) 0.004(11) 0.007(9) 0.010(11) C33 0.098(12) 0.132(14) 0.070(12) -0.001(10) -0.003(9) 0.017(9) C34 0.090(11) 0.132(14) 0.079(13) 0.014(11) 0.003(10) 0.012(10) C35 0.075(10) 0.153(15) 0.079(12) 0.043(12) 0.003(9) 0.017(9) C36 0.104(13) 0.111(13) 0.095(14) 0.022(11) -0.002(11) 0.011(10) C37 0.124(12) 0.090(11) 0.076(11) 0.007(9) 0.025(9) 0.023(9) C43 0.070(8) 0.110(11) 0.078(11) -0.004(9) -0.001(8) 0.014(8) C42 0.089(10) 0.103(11) 0.074(11) -0.007(9) -0.003(8) 0.037(8) C41 0.097(10) 0.088(10) 0.068(10) 0.006(8) 0.019(8) 0.019(8) C44 0.076(9) 0.107(10) 0.056(9) -0.017(8) 0.016(7) -0.004(7) C45 0.054(7) 0.081(8) 0.054(8) -0.001(7) 0.007(6) 0.013(6) C46 0.070(9) 0.115(12) 0.053(9) -0.006(8) 0.005(7) 0.007(7) C47 0.067(7) 0.086(9) 0.078(10) -0.001(8) 0.017(7) -0.008(6) O250 0.080(6) 0.114(8) 0.078(7) -0.017(6) 0.007(5) -0.004(5) C251 0.121(12) 0.135(14) 0.059(10) 0.013(10) -0.019(9) -0.019(10) C252 0.076(9) 0.071(9) 0.092(12) 0.021(8) 0.015(8) 0.008(7) O253 0.078(6) 0.085(7) 0.131(10) 0.022(6) 0.015(6) -0.015(5) O254 0.076(6) 0.101(8) 0.133(10) 0.005(7) 0.001(6) -0.008(5) C256 0.106(15) 0.17(2) 0.37(4) -0.04(3) -0.05(2) -0.043(14) C255 0.097(12) 0.118(15) 0.22(3) 0.068(15) -0.054(15) -0.019(10) O450 0.067(5) 0.083(6) 0.079(7) 0.014(5) 0.018(5) 0.004(4) C451 0.072(9) 0.114(13) 0.112(14) 0.008(10) 0.002(9) 0.000(8) C452 0.086(11) 0.114(14) 0.098(13) 0.009(10) 0.008(9) 0.010(9) O453 0.117(9) 0.092(8) 0.197(15) -0.007(9) 0.020(8) 0.002(7) O454 0.052(6) 0.135(10) 0.32(2) -0.012(11) 0.010(8) -0.018(6) C455 0.18(2) 0.16(3) 0.46(6) -0.10(3) 0.06(3) -0.08(2) C456 0.54(10) 0.23(4) 0.97(17) 0.21(7) -0.48(10) -0.19(5) O350 0.096(7) 0.117(9) 0.139(11) 0.037(8) 0.013(7) 0.007(6) C351 0.142(17) 0.17(2) 0.23(3) 0.11(2) -0.009(17) -0.025(15) _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 C200 1.915(19) . ? Re1 C300 1.95(3) . ? Re1 C100 1.987(16) . ? Re1 N175 2.138(10) . ? Re1 N199 2.179(12) . ? Re1 Cl1 2.438(5) . ? C300 O300 1.14(2) . ? C100 O100 1.000(16) . ? C200 O200 1.160(19) . ? N199 C169 1.354(16) . ? N199 C164 1.388(17) . ? N175 C170 1.295(15) . ? N175 C174 1.350(16) . ? C174 C173 1.366(17) . ? C173 C172 1.369(16) . ? C172 C171 1.383(16) . ? C172 C163 1.495(15) . ? C171 C170 1.445(17) . ? C170 C169 1.476(18) . ? C169 C168 1.371(19) . ? C168 C167 1.41(2) . ? C167 C165 1.35(2) . ? C167 C166 1.60(2) . ? C165 C164 1.295(19) . ? C163 O162 1.239(14) . ? C163 N161 1.347(14) . ? N161 C160 1.426(14) . ? C160 C159 1.349(15) . ? C160 C155 1.388(16) . ? C159 C158 1.389(18) . ? C158 C157 1.347(18) . ? C157 C156 1.413(17) . ? C156 C155 1.369(17) . ? C155 N154 1.460(14) . ? N154 C152 1.365(15) . ? C152 O153 1.214(15) . ? C152 C151 1.484(17) . ? C151 O150 1.467(15) . ? O150 C16 1.405(14) . ? C16 C15 1.416(18) . ? C16 C11 1.441(16) . ? C11 C12 1.417(17) . ? C11 C47 1.507(17) . ? C12 C13 1.329(18) . ? C13 C14 1.404(17) . ? C14 C15 1.359(17) . ? C15 C17 1.499(16) . ? C17 C21 1.51(2) . ? C21 C26 1.29(2) . ? C21 C22 1.35(3) . ? C22 C23 1.46(3) . ? C23 C24 1.30(3) . ? C24 C25 1.39(3) . ? C25 C26 1.37(2) . ? C25 C27 1.44(3) . ? C26 O250 1.42(2) . ? C27 C31 1.53(2) . ? C31 C32 1.37(2) . ? C31 C36 1.47(2) . ? C32 C33 1.38(2) . ? C33 C34 1.31(2) . ? C34 C35 1.42(2) . ? C35 C36 1.37(2) . ? C35 C37 1.49(2) . ? C36 O350 1.407(19) . ? C37 C41 1.52(2) . ? C43 C44 1.350(19) . ? C43 C42 1.45(2) . ? C42 C41 1.393(18) . ? C41 C46 1.399(18) . ? C44 C45 1.407(16) . ? C45 C46 1.418(18) . ? C45 C47 1.506(17) . ? C46 O450 1.368(15) . ? O250 C251 1.419(17) . ? C251 C252 1.414(19) . ? C252 O254 1.256(16) . ? C252 O253 1.294(16) . ? O253 C255 1.50(2) . ? C256 C255 1.47(3) . ? O450 C451 1.444(17) . ? C451 C452 1.44(2) . ? C452 O453 1.269(18) . ? C452 O454 1.338(17) . ? O454 C455 1.450(13) . ? C455 C456 1.49(2) . ? O350 C351 1.41(2) . ? C351 C352 1.553(18) . ? C352 O353 1.228(19) . ? C352 O354 1.40(2) . ? O354 C355 1.44(2) . ? C355 C356 1.53(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 C200 Re1 C300 87.9(7) . . ? C200 Re1 C100 89.9(7) . . ? C300 Re1 C100 88.7(7) . . ? C200 Re1 N175 174.4(6) . . ? C300 Re1 N175 97.7(6) . . ? C100 Re1 N175 90.2(5) . . ? C200 Re1 N199 100.5(6) . . ? C300 Re1 N199 171.1(5) . . ? C100 Re1 N199 94.1(5) . . ? N175 Re1 N199 73.9(4) . . ? C200 Re1 Cl1 95.2(6) . . ? C300 Re1 Cl1 92.7(5) . . ? C100 Re1 Cl1 174.8(4) . . ? N175 Re1 Cl1 84.6(3) . . ? N199 Re1 Cl1 83.8(3) . . ? O300 C300 Re1 176(2) . . ? O100 C100 Re1 175.6(16) . . ? O200 C200 Re1 176.6(18) . . ? C169 N199 C164 117.6(13) . . ? C169 N199 Re1 117.0(10) . . ? C164 N199 Re1 125.4(10) . . ? C170 N175 C174 115.1(11) . . ? C170 N175 Re1 119.1(8) . . ? C174 N175 Re1 125.8(8) . . ? N175 C174 C173 126.1(13) . . ? C174 C173 C172 119.3(12) . . ? C173 C172 C171 117.0(11) . . ? C173 C172 C163 124.2(11) . . ? C171 C172 C163 118.8(10) . . ? C172 C171 C170 119.0(11) . . ? N175 C170 C171 123.5(11) . . ? N175 C170 C169 116.5(11) . . ? C171 C170 C169 120.0(12) . . ? N199 C169 C168 120.0(14) . . ? N199 C169 C170 113.5(13) . . ? C168 C169 C170 126.4(13) . . ? C169 C168 C167 120.2(14) . . ? C165 C167 C168 117.2(15) . . ? C165 C167 C166 126.2(15) . . ? C168 C167 C166 116.6(15) . . ? C164 C165 C167 122.1(15) . . ? C165 C164 N199 122.6(13) . . ? O162 C163 N161 125.9(11) . . ? O162 C163 C172 121.0(10) . . ? N161 C163 C172 113.0(10) . . ? C163 N161 C160 126.4(10) . . ? C159 C160 C155 119.3(11) . . ? C159 C160 N161 123.6(11) . . ? C155 C160 N161 117.1(10) . . ? C160 C159 C158 122.6(12) . . ? C157 C158 C159 118.8(12) . . ? C158 C157 C156 119.5(13) . . ? C155 C156 C157 120.7(12) . . ? C156 C155 C160 119.0(11) . . ? C156 C155 N154 115.0(11) . . ? C160 C155 N154 124.8(10) . . ? C152 N154 C155 122.8(11) . . ? O153 C152 N154 127.4(12) . . ? O153 C152 C151 115.9(12) . . ? N154 C152 C151 116.5(12) . . ? O150 C151 C152 112.5(10) . . ? C16 O150 C151 111.9(9) . . ? O150 C16 C15 121.0(10) . . ? O150 C16 C11 116.7(12) . . ? C15 C16 C11 122.2(11) . . ? C12 C11 C16 115.9(12) . . ? C12 C11 C47 118.8(11) . . ? C16 C11 C47 125.3(12) . . ? C13 C12 C11 121.6(12) . . ? C12 C13 C14 120.5(13) . . ? C15 C14 C13 122.9(13) . . ? C14 C15 C16 116.1(11) . . ? C14 C15 C17 122.6(13) . . ? C16 C15 C17 121.2(11) . . ? C15 C17 C21 109.8(12) . . ? C26 C21 C22 116(2) . . ? C26 C21 C17 124.2(17) . . ? C22 C21 C17 119(2) . . ? C21 C22 C23 120(2) . . ? C24 C23 C22 120(2) . . ? C23 C24 C25 120(2) . . ? C26 C25 C24 117(2) . . ? C26 C25 C27 127.1(19) . . ? C24 C25 C27 115(2) . . ? C21 C26 C25 127(2) . . ? C21 C26 O250 116.6(19) . . ? C25 C26 O250 116.1(19) . . ? C25 C27 C31 111.3(16) . . ? C32 C31 C36 117.6(17) . . ? C32 C31 C27 118(2) . . ? C36 C31 C27 124.1(19) . . ? C31 C32 C33 119.7(18) . . ? C34 C33 C32 120.6(17) . . ? C33 C34 C35 125.6(17) . . ? C36 C35 C34 113.6(18) . . ? C36 C35 C37 119.7(17) . . ? C34 C35 C37 126.7(16) . . ? C35 C36 O350 121.3(18) . . ? C35 C36 C31 122.7(18) . . ? O350 C36 C31 115.7(16) . . ? C35 C37 C41 106.1(13) . . ? C44 C43 C42 117.9(13) . . ? C41 C42 C43 121.5(13) . . ? C42 C41 C46 118.1(14) . . ? C42 C41 C37 123.1(13) . . ? C46 C41 C37 118.6(13) . . ? C43 C44 C45 123.0(14) . . ? C44 C45 C46 117.9(12) . . ? C44 C45 C47 119.8(12) . . ? C46 C45 C47 121.1(11) . . ? O450 C46 C41 117.3(13) . . ? O450 C46 C45 121.1(12) . . ? C41 C46 C45 121.4(12) . . ? C45 C47 C11 111.3(11) . . ? C26 O250 C251 118.4(12) . . ? C252 C251 O250 115.2(14) . . ? O254 C252 O253 119.6(13) . . ? O254 C252 C251 127.1(14) . . ? O253 C252 C251 113.3(14) . . ? C252 O253 C255 119.0(12) . . ? C256 C255 O253 105.5(18) . . ? C46 O450 C451 118.1(11) . . ? C452 C451 O450 107.4(13) . . ? O453 C452 O454 116.7(16) . . ? O453 C452 C451 126.1(15) . . ? O454 C452 C451 115.9(14) . . ? C452 O454 C455 122.1(18) . . ? O454 C455 C456 114.4(18) . . ? C36 O350 C351 113.0(14) . . ? O350 C351 C352 99.9(15) . . ? O353 C352 O354 116(2) . . ? O353 C352 C351 108(2) . . ? O354 C352 C351 98.5(17) . . ? C352 O354 C355 104.1(19) . . ? O354 C355 C356 114(5) . . ? _refine_diff_density_max 2.584 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.147 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ;