# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2222 data_tmcg28 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H62 N2 O10 Rh2' _chemical_formula_weight 984.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 18.088 _cell_length_b 26.151 _cell_length_c 19.245 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9103.1 _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4079 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55544 _diffrn_reflns_av_R_equivalents 0.1350 _diffrn_reflns_av_sigmaI/netI 0.1411 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.12 _reflns_number_total 7178 _reflns_number_gt 3637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^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 SHELXL _refine_ls_extinction_coef 0.00069(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7178 _refine_ls_number_parameters 509 _refine_ls_number_restraints 396 _refine_ls_R_factor_all 0.1593 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2177 _refine_ls_wR_factor_gt 0.1951 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.80145(5) 0.23654(4) 0.17148(5) 0.0393(3) Uani 1 d . . . Rh2 Rh 0.75461(6) 0.28542(4) 0.07525(5) 0.0430(3) Uani 1 d . . . O1 O 0.8416(4) 0.3033(3) 0.2104(4) 0.043(2) Uani 1 d . . . O2 O 0.8009(5) 0.3478(3) 0.1187(4) 0.046(2) Uani 1 d . . . O3 O 0.7063(5) 0.2529(4) 0.2216(5) 0.065(3) Uani 1 d . . . O4 O 0.6627(5) 0.2986(3) 0.1317(6) 0.056(2) Uani 1 d . . . O5 O 0.8944(5) 0.2271(3) 0.1164(5) 0.057(2) Uani 1 d D . . O6 O 0.8514(6) 0.2713(3) 0.0250(4) 0.062(3) Uani 1 d D . . O7 O 0.7558(5) 0.1753(3) 0.1267(5) 0.074(3) Uani 1 d DU . . O8 O 0.7109(6) 0.2212(3) 0.0377(6) 0.079(3) Uani 1 d DU . . O9 O 0.8102(6) 0.4385(3) 0.1909(5) 0.071(3) Uani 1 d . . . O10 O 0.5696(6) 0.3545(4) 0.2177(8) 0.108(5) Uani 1 d . . . C1 C 0.8319(6) 0.3438(4) 0.1782(7) 0.041(3) Uani 1 d . . . C2 C 0.8545(8) 0.3950(6) 0.2114(8) 0.062(4) Uani 1 d . . . C3 C 0.8590(11) 0.3921(6) 0.2896(9) 0.095(6) Uani 1 d . . . H3A H 0.8736 0.4251 0.3080 0.114 Uiso 1 calc R . . H3B H 0.8952 0.3665 0.3029 0.114 Uiso 1 calc R . . H3C H 0.8110 0.3827 0.3083 0.114 Uiso 1 calc R . . C4 C 0.9302(9) 0.4097(6) 0.1816(11) 0.100(6) Uani 1 d . . . H4A H 0.9463 0.4417 0.2020 0.121 Uiso 1 calc R . . H4B H 0.9263 0.4135 0.1316 0.121 Uiso 1 calc R . . H4C H 0.9658 0.3831 0.1923 0.121 Uiso 1 calc R . . C5 C 0.7330(8) 0.4361(5) 0.1926(9) 0.067(4) Uani 1 d . . . C6 C 0.6980(9) 0.4792(5) 0.1666(9) 0.073(4) Uani 1 d . . . H6 H 0.7261 0.5076 0.1523 0.088 Uiso 1 calc R . . C7 C 0.6218(9) 0.4804(6) 0.1620(10) 0.085(5) Uani 1 d . . . H7 H 0.5977 0.5103 0.1475 0.102 Uiso 1 calc R . . C8 C 0.5812(9) 0.4375(6) 0.1787(10) 0.087(6) Uani 1 d . . . H8 H 0.5298 0.4370 0.1713 0.104 Uiso 1 calc R . . C9 C 0.6166(9) 0.3950(6) 0.2065(9) 0.072(4) Uani 1 d . . . C10 C 0.6922(8) 0.3948(6) 0.2146(8) 0.067(4) Uani 1 d . . . H10 H 0.7159 0.3665 0.2350 0.081 Uiso 1 calc R . . C11 C 0.5941(10) 0.3051(6) 0.2401(12) 0.098(6) Uani 1 d . . . C12 C 0.5307(9) 0.2702(7) 0.2276(14) 0.139(10) Uani 1 d . . . H12A H 0.4888 0.2811 0.2553 0.167 Uiso 1 calc R . . H12B H 0.5444 0.2356 0.2406 0.167 Uiso 1 calc R . . H12C H 0.5175 0.2710 0.1788 0.167 Uiso 1 calc R . . C13 C 0.6137(12) 0.3080(8) 0.3143(11) 0.132(10) Uani 1 d . . . H13A H 0.5721 0.3214 0.3404 0.158 Uiso 1 calc R . . H13B H 0.6560 0.3304 0.3202 0.158 Uiso 1 calc R . . H13C H 0.6259 0.2741 0.3313 0.158 Uiso 1 calc R . . C14 C 0.6614(8) 0.2840(6) 0.1916(10) 0.075(5) Uani 1 d . . . C15 C 0.8989(13) 0.2473(8) 0.0542(16) 0.047(8) Uiso 0.589(15) d PDU A 1 C16 C 0.9710(13) 0.2395(10) 0.0157(13) 0.070(7) Uiso 0.589(15) d PDU A 1 H16A H 0.9922 0.2729 0.0045 0.084 Uiso 0.589(15) calc PR A 1 H16B H 1.0058 0.2217 0.0464 0.084 Uiso 0.589(15) calc PR A 1 C17 C 0.963(2) 0.2094(10) -0.0497(14) 0.118(11) Uiso 0.589(15) d PDU A 1 H17A H 0.9146 0.2140 -0.0723 0.142 Uiso 0.589(15) calc PR A 1 H17B H 1.0031 0.2148 -0.0828 0.142 Uiso 0.589(15) calc PR A 1 C18 C 0.969(2) 0.1609(10) -0.0099(18) 0.135(12) Uiso 0.589(15) d PDU A 1 H18A H 1.0119 0.1623 0.0210 0.161 Uiso 0.589(15) calc PR A 1 H18B H 0.9246 0.1557 0.0184 0.161 Uiso 0.589(15) calc PR A 1 C19 C 0.977(2) 0.1181(10) -0.0601(19) 0.160(15) Uiso 0.589(15) d PDU A 1 H19A H 1.0276 0.1189 -0.0791 0.192 Uiso 0.589(15) calc PR A 1 H19B H 0.9429 0.1235 -0.0988 0.192 Uiso 0.589(15) calc PR A 1 C20 C 0.9634(15) 0.0665(10) -0.0297(19) 0.114(11) Uiso 0.589(15) d PDU A 1 H20A H 1.0007 0.0609 0.0065 0.137 Uiso 0.589(15) calc PR A 1 H20B H 0.9726 0.0412 -0.0662 0.137 Uiso 0.589(15) calc PR A 1 C21 C 0.8897(16) 0.0550(13) 0.001(2) 0.150(14) Uiso 0.589(15) d PDU A 1 H21A H 0.8972 0.0491 0.0511 0.180 Uiso 0.589(15) calc PR A 1 H21B H 0.8727 0.0225 -0.0187 0.180 Uiso 0.589(15) calc PR A 1 C22 C 0.8277(16) 0.0925(15) -0.006(3) 0.169(14) Uiso 0.589(15) d PDU A 1 H22A H 0.8441 0.1249 0.0145 0.203 Uiso 0.589(15) calc PR A 1 H22B H 0.8198 0.0985 -0.0555 0.203 Uiso 0.589(15) calc PR A 1 C23 C 0.7551(15) 0.0794(12) 0.0256(18) 0.104(9) Uiso 0.589(15) d PDU A 1 H23A H 0.7554 0.0870 0.0754 0.125 Uiso 0.589(15) calc PR A 1 H23B H 0.7446 0.0429 0.0195 0.125 Uiso 0.589(15) calc PR A 1 C24 C 0.6970(18) 0.1112(14) -0.0110(17) 0.177(14) Uiso 0.589(15) d PDU A 1 H24A H 0.6607 0.0904 -0.0362 0.212 Uiso 0.589(15) calc PR A 1 H24B H 0.7182 0.1372 -0.0417 0.212 Uiso 0.589(15) calc PR A 1 C25 C 0.6669(16) 0.1332(11) 0.0561(18) 0.107(10) Uiso 0.589(15) d PDU A 1 H25A H 0.6694 0.1076 0.0933 0.129 Uiso 0.589(15) calc PR A 1 H25B H 0.6151 0.1434 0.0501 0.129 Uiso 0.589(15) calc PR A 1 C26 C 0.7143(15) 0.1798(14) 0.075(2) 0.081(9) Uiso 0.589(15) d PDU A 1 C15' C 0.911(2) 0.2504(12) 0.062(2) 0.059(12) Uiso 0.411(15) d PDU A 2 C16' C 0.9876(16) 0.2580(11) 0.0319(17) 0.056(8) Uiso 0.411(15) d PDU A 2 H16C H 0.9924 0.2932 0.0151 0.067 Uiso 0.411(15) calc PR A 2 H16D H 1.0243 0.2529 0.0687 0.067 Uiso 0.411(15) calc PR A 2 C17' C 1.004(3) 0.2220(12) -0.0267(18) 0.106(13) Uiso 0.411(15) d PDU A 2 H17C H 1.0494 0.2293 -0.0519 0.127 Uiso 0.411(15) calc PR A 2 H17D H 0.9620 0.2168 -0.0586 0.127 Uiso 0.411(15) calc PR A 2 C18' C 1.011(3) 0.1815(12) 0.028(2) 0.120(14) Uiso 0.411(15) d PDU A 2 H18C H 0.9781 0.1883 0.0674 0.143 Uiso 0.411(15) calc PR A 2 H18D H 1.0619 0.1791 0.0448 0.143 Uiso 0.411(15) calc PR A 2 C19' C 0.988(3) 0.1333(15) -0.009(3) 0.164(17) Uiso 0.411(15) d PDU A 2 H19C H 0.9958 0.1382 -0.0593 0.197 Uiso 0.411(15) calc PR A 2 H19D H 1.0210 0.1054 0.0056 0.197 Uiso 0.411(15) calc PR A 2 C20' C 0.910(3) 0.1180(17) 0.003(4) 0.171(16) Uiso 0.411(15) d PDU A 2 H20C H 0.8775 0.1452 -0.0143 0.205 Uiso 0.411(15) calc PR A 2 H20D H 0.9019 0.1156 0.0536 0.205 Uiso 0.411(15) calc PR A 2 C21' C 0.886(2) 0.0680(17) -0.030(3) 0.114(14) Uiso 0.411(15) d PDU A 2 H21C H 0.8769 0.0740 -0.0790 0.137 Uiso 0.411(15) calc PR A 2 H21D H 0.9278 0.0439 -0.0263 0.137 Uiso 0.411(15) calc PR A 2 C22' C 0.819(2) 0.0434(14) 0.002(3) 0.138(15) Uiso 0.411(15) d PDU A 2 H22C H 0.8151 0.0083 -0.0155 0.165 Uiso 0.411(15) calc PR A 2 H22D H 0.8263 0.0412 0.0526 0.165 Uiso 0.411(15) calc PR A 2 C23' C 0.748(2) 0.070(2) -0.011(2) 0.162(16) Uiso 0.411(15) d PDU A 2 H23C H 0.7165 0.0481 -0.0399 0.194 Uiso 0.411(15) calc PR A 2 H23D H 0.7578 0.1015 -0.0371 0.194 Uiso 0.411(15) calc PR A 2 C24' C 0.708(2) 0.0829(11) 0.0553(18) 0.079(10) Uiso 0.411(15) d PDU A 2 H24C H 0.6632 0.0628 0.0633 0.095 Uiso 0.411(15) calc PR A 2 H24D H 0.7399 0.0832 0.0966 0.095 Uiso 0.411(15) calc PR A 2 C25' C 0.695(2) 0.1345(10) 0.0243(18) 0.075(10) Uiso 0.411(15) d PDU A 2 H25C H 0.6413 0.1386 0.0175 0.091 Uiso 0.411(15) calc PR A 2 H25D H 0.7179 0.1355 -0.0216 0.091 Uiso 0.411(15) calc PR A 2 C26' C 0.7222(15) 0.1794(15) 0.066(3) 0.053(9) Uiso 0.411(15) d PDU A 2 N1 N 0.8479(5) 0.1855(4) 0.2551(5) 0.044(2) Uani 1 d . . . C27 C 0.8603(8) 0.1372(6) 0.2388(6) 0.061(4) Uani 1 d . . . H27 H 0.8542 0.1274 0.1921 0.074 Uiso 1 calc R . . C28 C 0.8816(9) 0.1005(5) 0.2855(8) 0.070(4) Uani 1 d . . . H28 H 0.8896 0.0669 0.2697 0.084 Uiso 1 calc R . . C29 C 0.8915(7) 0.1114(5) 0.3551(7) 0.050(3) Uani 1 d . . . C30 C 0.9109(7) 0.0699(5) 0.4083(7) 0.066(4) Uani 1 d D . . C31 C 0.8493(15) 0.0303(11) 0.4109(17) 0.106(12) Uiso 0.57(2) d PDU B 1 H31A H 0.8617 0.0041 0.4448 0.159 Uiso 0.57(2) calc PR B 1 H31B H 0.8436 0.0147 0.3655 0.159 Uiso 0.57(2) calc PR B 1 H31C H 0.8034 0.0468 0.4242 0.159 Uiso 0.57(2) calc PR B 1 C32 C 0.9817(11) 0.0435(9) 0.3881(13) 0.060(8) Uiso 0.57(2) d PDU B 1 H32A H 0.9940 0.0179 0.4228 0.090 Uiso 0.57(2) calc PR B 1 H32B H 1.0213 0.0684 0.3852 0.090 Uiso 0.57(2) calc PR B 1 H32C H 0.9754 0.0270 0.3433 0.090 Uiso 0.57(2) calc PR B 1 C33 C 0.9196(17) 0.0911(11) 0.4807(12) 0.092(10) Uiso 0.57(2) d PDU B 1 H33A H 0.9330 0.0638 0.5123 0.138 Uiso 0.57(2) calc PR B 1 H33B H 0.8733 0.1063 0.4956 0.138 Uiso 0.57(2) calc PR B 1 H33C H 0.9580 0.1170 0.4808 0.138 Uiso 0.57(2) calc PR B 1 C31' C 0.8562(17) 0.0677(12) 0.4657(15) 0.065(11) Uiso 0.43(2) d PDU B 2 H31D H 0.8710 0.0418 0.4990 0.098 Uiso 0.43(2) calc PR B 2 H31E H 0.8079 0.0592 0.4470 0.098 Uiso 0.43(2) calc PR B 2 H31F H 0.8538 0.1007 0.4885 0.098 Uiso 0.43(2) calc PR B 2 C32' C 0.935(3) 0.0189(12) 0.381(2) 0.121(18) Uiso 0.43(2) d PDU B 2 H32D H 0.9469 -0.0034 0.4200 0.182 Uiso 0.43(2) calc PR B 2 H32E H 0.9783 0.0231 0.3521 0.182 Uiso 0.43(2) calc PR B 2 H32F H 0.8953 0.0038 0.3542 0.182 Uiso 0.43(2) calc PR B 2 C33' C 0.979(4) 0.090(2) 0.445(3) 0.16(2) Uiso 0.43(2) d PU B 2 H33D H 0.9949 0.0654 0.4802 0.247 Uiso 0.43(2) calc PR B 2 H33E H 0.9677 0.1222 0.4676 0.247 Uiso 0.43(2) calc PR B 2 H33F H 1.0187 0.0950 0.4119 0.247 Uiso 0.43(2) calc PR B 2 C34 C 0.8795(9) 0.1614(6) 0.3716(7) 0.065(4) Uani 1 d . . . H34 H 0.8845 0.1718 0.4182 0.078 Uiso 1 calc R . . C35 C 0.8600(8) 0.1975(5) 0.3221(8) 0.067(4) Uani 1 d . . . H35 H 0.8550 0.2318 0.3359 0.081 Uiso 1 calc R . . N2 N 0.7114(6) 0.3294(4) -0.0123(5) 0.050(3) Uani 1 d . . . C36 C 0.7041(9) 0.3080(5) -0.0751(8) 0.078(5) Uani 1 d . . . H36 H 0.7181 0.2735 -0.0801 0.094 Uiso 1 calc R . . C37 C 0.6769(8) 0.3335(5) -0.1338(7) 0.060(4) Uani 1 d . . . H37 H 0.6767 0.3171 -0.1773 0.072 Uiso 1 calc R . . C38 C 0.6504(6) 0.3829(4) -0.1273(6) 0.036(3) Uani 1 d . . . C39 C 0.6186(7) 0.4116(4) -0.1895(6) 0.055(4) Uani 1 d D . . C40 C 0.6793(14) 0.4307(14) -0.2361(17) 0.087(12) Uiso 0.52(4) d PDU C 1 H40A H 0.6579 0.4489 -0.2751 0.131 Uiso 0.52(4) calc PR C 1 H40B H 0.7080 0.4020 -0.2531 0.131 Uiso 0.52(4) calc PR C 1 H40C H 0.7112 0.4536 -0.2101 0.131 Uiso 0.52(4) calc PR C 1 C41 C 0.5653(15) 0.4541(10) -0.1697(16) 0.061(9) Uiso 0.52(4) d PDU C 1 H41A H 0.5475 0.4709 -0.2114 0.091 Uiso 0.52(4) calc PR C 1 H41B H 0.5906 0.4788 -0.1406 0.091 Uiso 0.52(4) calc PR C 1 H41C H 0.5238 0.4397 -0.1444 0.091 Uiso 0.52(4) calc PR C 1 C42 C 0.5715(15) 0.3725(8) -0.2316(15) 0.057(9) Uiso 0.52(4) d PDU C 1 H42A H 0.5503 0.3894 -0.2718 0.085 Uiso 0.52(4) calc PR C 1 H42B H 0.5322 0.3593 -0.2024 0.085 Uiso 0.52(4) calc PR C 1 H42C H 0.6028 0.3445 -0.2469 0.085 Uiso 0.52(4) calc PR C 1 C40' C 0.6742(16) 0.4549(12) -0.204(2) 0.087(13) Uiso 0.48(4) d PDU C 2 H40D H 0.6571 0.4752 -0.2430 0.130 Uiso 0.48(4) calc PR C 2 H40E H 0.7221 0.4403 -0.2149 0.130 Uiso 0.48(4) calc PR C 2 H40F H 0.6784 0.4765 -0.1632 0.130 Uiso 0.48(4) calc PR C 2 C41' C 0.5447(14) 0.4364(14) -0.1722(19) 0.076(11) Uiso 0.48(4) d PDU C 2 H41D H 0.5263 0.4545 -0.2126 0.114 Uiso 0.48(4) calc PR C 2 H41E H 0.5511 0.4603 -0.1341 0.114 Uiso 0.48(4) calc PR C 2 H41F H 0.5095 0.4102 -0.1588 0.114 Uiso 0.48(4) calc PR C 2 C42' C 0.612(2) 0.3803(12) -0.2558(15) 0.089(13) Uiso 0.48(4) d PDU C 2 H42D H 0.5911 0.4014 -0.2924 0.134 Uiso 0.48(4) calc PR C 2 H42E H 0.5797 0.3512 -0.2476 0.134 Uiso 0.48(4) calc PR C 2 H42F H 0.6603 0.3682 -0.2698 0.134 Uiso 0.48(4) calc PR C 2 C43 C 0.6547(7) 0.4041(4) -0.0616(6) 0.041(3) Uani 1 d . . . H43 H 0.6374 0.4375 -0.0540 0.049 Uiso 1 calc R . . C44 C 0.6844(6) 0.3763(4) -0.0068(6) 0.043(3) Uani 1 d . . . H44 H 0.6853 0.3918 0.0373 0.052 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 Rh1 0.0367(5) 0.0458(5) 0.0355(5) 0.0029(5) -0.0035(5) 0.0031(4) Rh2 0.0507(6) 0.0404(5) 0.0378(5) -0.0044(5) -0.0121(5) 0.0073(5) O1 0.039(5) 0.060(6) 0.030(4) 0.000(4) -0.008(4) 0.008(4) O2 0.049(5) 0.049(5) 0.041(5) -0.007(4) -0.003(5) 0.010(4) O3 0.042(5) 0.083(7) 0.070(7) 0.034(5) 0.007(5) -0.001(5) O4 0.043(5) 0.057(6) 0.069(7) 0.006(5) -0.023(5) -0.001(4) O5 0.070(6) 0.046(6) 0.053(6) 0.009(4) 0.011(5) 0.017(4) O6 0.097(7) 0.056(6) 0.032(5) -0.002(4) -0.002(5) 0.031(5) O7 0.077(7) 0.060(5) 0.086(7) 0.027(5) -0.047(6) -0.012(5) O8 0.093(7) 0.054(6) 0.091(8) 0.012(5) -0.050(6) 0.007(5) O9 0.075(7) 0.042(5) 0.095(8) -0.014(5) -0.024(6) 0.009(5) O10 0.074(8) 0.076(8) 0.174(13) 0.044(8) 0.054(8) 0.041(6) C1 0.023(6) 0.041(7) 0.059(9) -0.014(7) -0.017(6) -0.004(5) C2 0.060(9) 0.070(10) 0.055(9) -0.005(8) -0.019(7) 0.006(8) C3 0.139(17) 0.065(11) 0.081(13) -0.018(9) -0.050(12) 0.020(10) C4 0.063(11) 0.075(11) 0.16(2) 0.012(12) -0.021(12) -0.015(8) C5 0.056(10) 0.049(9) 0.096(13) -0.006(8) -0.011(8) 0.006(7) C6 0.061(10) 0.054(8) 0.105(13) 0.000(8) -0.021(10) -0.002(7) C7 0.070(12) 0.063(10) 0.122(16) 0.008(10) 0.007(11) 0.014(8) C8 0.061(10) 0.065(10) 0.135(16) 0.020(11) -0.004(11) 0.033(9) C9 0.069(11) 0.060(10) 0.087(12) 0.011(8) 0.016(9) 0.010(8) C10 0.059(10) 0.063(10) 0.079(11) -0.001(8) -0.014(9) 0.014(8) C11 0.088(13) 0.064(10) 0.140(19) 0.050(12) 0.026(13) 0.022(10) C12 0.051(10) 0.100(15) 0.27(3) 0.083(17) 0.033(15) -0.006(10) C13 0.140(19) 0.128(17) 0.127(19) 0.050(15) 0.090(17) 0.081(15) C14 0.048(9) 0.078(11) 0.100(14) -0.005(10) -0.008(9) 0.025(8) N1 0.040(6) 0.048(6) 0.045(7) 0.000(5) 0.007(5) -0.002(5) C27 0.071(10) 0.093(11) 0.020(7) 0.007(7) -0.007(6) 0.035(8) C28 0.105(13) 0.046(8) 0.058(11) 0.009(8) -0.010(9) 0.022(8) C29 0.045(8) 0.063(9) 0.043(8) 0.009(7) 0.005(6) 0.016(7) C30 0.071(10) 0.070(10) 0.057(10) 0.018(8) 0.008(8) 0.025(8) C34 0.098(12) 0.079(11) 0.019(7) 0.004(7) -0.016(7) 0.012(9) C35 0.086(11) 0.059(9) 0.057(10) -0.006(8) -0.011(9) -0.007(7) N2 0.058(7) 0.041(6) 0.050(7) -0.019(5) -0.008(5) 0.018(5) C36 0.117(13) 0.043(7) 0.074(11) -0.014(8) -0.053(11) 0.031(8) C37 0.075(10) 0.073(10) 0.032(7) -0.010(7) -0.008(7) 0.032(8) C38 0.040(7) 0.036(7) 0.033(7) 0.010(5) -0.001(5) 0.006(5) C39 0.063(9) 0.051(8) 0.050(9) 0.005(7) -0.013(7) 0.007(6) C43 0.058(8) 0.027(6) 0.037(8) 0.004(5) -0.007(6) 0.010(5) C44 0.049(8) 0.044(7) 0.036(7) -0.014(6) -0.008(6) 0.003(6) _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 Rh1 O7 1.997(9) . ? Rh1 O5 2.003(9) . ? Rh1 O3 2.018(9) . ? Rh1 O1 2.034(8) . ? Rh1 Rh2 2.4045(13) . ? Rh2 O8 1.993(9) . ? Rh2 O4 2.015(10) . ? Rh2 O2 2.015(8) . ? Rh2 O6 2.035(10) . ? O1 C1 1.237(13) . ? O2 C1 1.280(14) . ? O3 C14 1.286(17) . ? O4 C14 1.216(19) . ? O5 C15' 1.26(5) . ? O5 C15 1.31(4) . ? O6 C15 1.20(4) . ? O6 C15' 1.40(6) . ? O7 C26 1.26(5) . ? O7 C26' 1.33(6) . ? O8 C26' 1.23(5) . ? O8 C26 1.30(5) . ? O9 C5 1.398(16) . ? O9 C2 1.447(16) . ? O10 C9 1.374(18) . ? O10 C11 1.434(17) . ? C1 C2 1.538(17) . ? C2 C3 1.51(2) . ? C2 C4 1.53(2) . ? C5 C10 1.375(19) . ? C5 C6 1.387(19) . ? C6 C7 1.38(2) . ? C7 C8 1.38(2) . ? C8 C9 1.390(19) . ? C9 C10 1.38(2) . ? C11 C13 1.47(3) . ? C11 C12 1.48(3) . ? C11 C14 1.63(2) . ? C15 C16 1.513(15) . ? C16 C17 1.491(16) . ? C17 C18 1.487(16) . ? C18 C19 1.486(17) . ? C19 C20 1.493(16) . ? C20 C21 1.493(16) . ? C21 C22 1.495(16) . ? C22 C23 1.486(16) . ? C23 C24 1.514(16) . ? C24 C25 1.515(16) . ? C25 C26 1.531(16) . ? C15' C16' 1.508(16) . ? C16' C17' 1.497(17) . ? C17' C18' 1.499(17) . ? C18' C19' 1.504(17) . ? C19' C20' 1.498(17) . ? C20' C21' 1.513(17) . ? C21' C22' 1.510(17) . ? C22' C23' 1.481(17) . ? C23' C24' 1.508(17) . ? C24' C25' 1.496(16) . ? C25' C26' 1.503(16) . ? N1 C27 1.321(16) . ? N1 C35 1.345(17) . ? C27 C28 1.371(17) . ? C28 C29 1.381(19) . ? C29 C34 1.364(18) . ? C29 C30 1.534(18) . ? C30 C31' 1.485(18) . ? C30 C32' 1.496(19) . ? C30 C33' 1.52(6) . ? C30 C32 1.505(17) . ? C30 C33 1.509(18) . ? C30 C31 1.522(18) . ? C34 C35 1.386(18) . ? N2 C44 1.325(14) . ? N2 C36 1.337(16) . ? C36 C37 1.402(18) . ? C37 C38 1.384(16) . ? C38 C43 1.382(16) . ? C38 C39 1.525(16) . ? C39 C40 1.503(16) . ? C39 C42' 1.521(17) . ? C39 C41 1.521(16) . ? C39 C41' 1.524(16) . ? C39 C40' 1.540(16) . ? C39 C42 1.558(16) . ? C43 C44 1.390(15) . ? 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 O7 Rh1 O5 91.1(4) . . ? O7 Rh1 O3 91.4(4) . . ? O5 Rh1 O3 174.1(3) . . ? O7 Rh1 O1 174.2(3) . . ? O5 Rh1 O1 90.1(3) . . ? O3 Rh1 O1 86.9(4) . . ? O7 Rh1 Rh2 87.1(2) . . ? O5 Rh1 Rh2 87.3(2) . . ? O3 Rh1 Rh2 87.4(3) . . ? O1 Rh1 Rh2 87.3(2) . . ? O8 Rh2 O4 90.7(4) . . ? O8 Rh2 O2 176.3(4) . . ? O4 Rh2 O2 88.9(3) . . ? O8 Rh2 O6 90.9(4) . . ? O4 Rh2 O6 175.8(4) . . ? O2 Rh2 O6 89.2(3) . . ? O8 Rh2 Rh1 88.3(3) . . ? O4 Rh2 Rh1 88.1(3) . . ? O2 Rh2 Rh1 88.0(2) . . ? O6 Rh2 Rh1 88.1(2) . . ? C1 O1 Rh1 120.0(7) . . ? C1 O2 Rh2 119.1(7) . . ? C14 O3 Rh1 117.3(10) . . ? C14 O4 Rh2 118.2(9) . . ? C15' O5 C15 12(2) . . ? C15' O5 Rh1 126.0(19) . . ? C15 O5 Rh1 119.0(13) . . ? C15 O6 C15' 8.5(8) . . ? C15 O6 Rh2 119.1(13) . . ? C15' O6 Rh2 119.8(15) . . ? C26 O7 C26' 9.5(8) . . ? C26 O7 Rh1 121.0(17) . . ? C26' O7 Rh1 120.3(16) . . ? C26' O8 C26 9.8(9) . . ? C26' O8 Rh2 121(2) . . ? C26 O8 Rh2 119.1(17) . . ? C5 O9 C2 120.7(11) . . ? C9 O10 C11 123.4(13) . . ? O1 C1 O2 125.4(10) . . ? O1 C1 C2 120.0(11) . . ? O2 C1 C2 114.5(11) . . ? O9 C2 C3 109.9(12) . . ? O9 C2 C4 101.3(12) . . ? C3 C2 C4 109.7(14) . . ? O9 C2 C1 115.2(11) . . ? C3 C2 C1 112.6(13) . . ? C4 C2 C1 107.5(12) . . ? C10 C5 C6 120.4(13) . . ? C10 C5 O9 125.4(12) . . ? C6 C5 O9 114.2(13) . . ? C7 C6 C5 119.7(14) . . ? C8 C7 C6 119.9(14) . . ? C7 C8 C9 119.6(15) . . ? O10 C9 C10 126.5(14) . . ? O10 C9 C8 113.0(15) . . ? C10 C9 C8 120.3(15) . . ? C5 C10 C9 119.7(14) . . ? O10 C11 C13 108.6(18) . . ? O10 C11 C12 105.5(16) . . ? C13 C11 C12 112.0(18) . . ? O10 C11 C14 111.3(14) . . ? C13 C11 C14 113.1(15) . . ? C12 C11 C14 106.0(17) . . ? O4 C14 O3 127.7(15) . . ? O4 C14 C11 116.8(14) . . ? O3 C14 C11 115.4(16) . . ? O6 C15 O5 126.4(18) . . ? O6 C15 C16 117(3) . . ? O5 C15 C16 116(3) . . ? C17 C16 C15 113.4(19) . . ? C18 C17 C16 90.4(19) . . ? C19 C18 C17 108(2) . . ? C18 C19 C20 114(2) . . ? C19 C20 C21 119.4(19) . . ? C20 C21 C22 120.0(19) . . ? C23 C22 C21 118(3) . . ? C22 C23 C24 107(2) . . ? C23 C24 C25 94(2) . . ? C24 C25 C26 107(2) . . ? O7 C26 O8 123(2) . . ? O7 C26 C25 116(4) . . ? O8 C26 C25 121(4) . . ? O5 C15' O6 115(2) . . ? O5 C15' C16' 127(4) . . ? O6 C15' C16' 118(4) . . ? C17' C16' C15' 112(2) . . ? C16' C17' C18' 86(2) . . ? C17' C18' C19' 103(3) . . ? C20' C19' C18' 114(3) . . ? C19' C20' C21' 115(3) . . ? C22' C21' C20' 115(3) . . ? C23' C22' C21' 115(3) . . ? C22' C23' C24' 112(3) . . ? C25' C24' C23' 87(2) . . ? C24' C25' C26' 116(3) . . ? O8 C26' O7 122(2) . . ? O8 C26' C25' 114(4) . . ? O7 C26' C25' 124(4) . . ? C27 N1 C35 115.0(11) . . ? N1 C27 C28 124.2(13) . . ? C27 C28 C29 121.8(14) . . ? C34 C29 C28 113.9(12) . . ? C34 C29 C30 124.0(12) . . ? C28 C29 C30 122.0(13) . . ? C31' C30 C32' 115(2) . . ? C31' C30 C33' 102(3) . . ? C32' C30 C33' 104(3) . . ? C31' C30 C32 137.9(19) . . ? C32' C30 C32 42(2) . . ? C33' C30 C32 66(3) . . ? C31' C30 C33 52.8(16) . . ? C32' C30 C33 128(2) . . ? C33' C30 C33 50(3) . . ? C32 C30 C33 108.6(14) . . ? C31' C30 C31 57.3(16) . . ? C32' C30 C31 68(2) . . ? C33' C30 C31 144(3) . . ? C32 C30 C31 108.6(15) . . ? C33 C30 C31 107.2(15) . . ? C31' C30 C29 111.8(16) . . ? C32' C30 C29 118(2) . . ? C33' C30 C29 105(3) . . ? C32 C30 C29 110.3(13) . . ? C33 C30 C29 112.3(16) . . ? C31 C30 C29 109.7(17) . . ? C29 C34 C35 122.1(13) . . ? N1 C35 C34 122.9(13) . . ? C44 N2 C36 115.1(10) . . ? N2 C36 C37 124.3(12) . . ? C38 C37 C36 119.5(12) . . ? C43 C38 C37 116.0(10) . . ? C43 C38 C39 122.8(10) . . ? C37 C38 C39 121.2(10) . . ? C40 C39 C42' 74.8(16) . . ? C40 C39 C41 111.6(15) . . ? C42' C39 C41 124(2) . . ? C40 C39 C41' 129(2) . . ? C42' C39 C41' 110.0(16) . . ? C41 C39 C41' 22.6(14) . . ? C40 C39 C38 110.9(15) . . ? C42' C39 C38 115.1(16) . . ? C41 C39 C38 113.7(15) . . ? C41' C39 C38 111.6(17) . . ? C40 C39 C40' 33.9(14) . . ? C42' C39 C40' 107.3(16) . . ? C41 C39 C40' 85.5(16) . . ? C41' C39 C40' 107.4(15) . . ? C38 C39 C40' 104.9(16) . . ? C40 C39 C42 107.9(14) . . ? C42' C39 C42 33.5(14) . . ? C41 C39 C42 105.2(13) . . ? C41' C39 C42 85.0(15) . . ? C38 C39 C42 107.0(13) . . ? C40' C39 C42 138.2(18) . . ? C38 C43 C44 120.4(10) . . ? N2 C44 C43 124.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Rh1 Rh2 O8 0.8(5) . . . . ? O5 Rh1 Rh2 O8 92.1(4) . . . . ? O3 Rh1 Rh2 O8 -90.7(4) . . . . ? O1 Rh1 Rh2 O8 -177.7(4) . . . . ? O7 Rh1 Rh2 O4 91.6(4) . . . . ? O5 Rh1 Rh2 O4 -177.2(3) . . . . ? O3 Rh1 Rh2 O4 0.1(4) . . . . ? O1 Rh1 Rh2 O4 -87.0(3) . . . . ? O7 Rh1 Rh2 O2 -179.5(4) . . . . ? O5 Rh1 Rh2 O2 -88.2(3) . . . . ? O3 Rh1 Rh2 O2 89.0(4) . . . . ? O1 Rh1 Rh2 O2 2.0(3) . . . . ? O7 Rh1 Rh2 O6 -90.2(4) . . . . ? O5 Rh1 Rh2 O6 1.1(4) . . . . ? O3 Rh1 Rh2 O6 178.3(4) . . . . ? O1 Rh1 Rh2 O6 91.3(3) . . . . ? O7 Rh1 O1 C1 -15(4) . . . . ? O5 Rh1 O1 C1 87.2(9) . . . . ? O3 Rh1 O1 C1 -87.7(9) . . . . ? Rh2 Rh1 O1 C1 -0.1(8) . . . . ? O8 Rh2 O2 C1 0(7) . . . . ? O4 Rh2 O2 C1 83.6(8) . . . . ? O6 Rh2 O2 C1 -92.6(8) . . . . ? Rh1 Rh2 O2 C1 -4.5(8) . . . . ? O7 Rh1 O3 C14 -92.7(11) . . . . ? O5 Rh1 O3 C14 22(4) . . . . ? O1 Rh1 O3 C14 81.7(11) . . . . ? Rh2 Rh1 O3 C14 -5.7(11) . . . . ? O8 Rh2 O4 C14 94.3(12) . . . . ? O2 Rh2 O4 C14 -82.0(12) . . . . ? O6 Rh2 O4 C14 -18(5) . . . . ? Rh1 Rh2 O4 C14 6.0(11) . . . . ? O7 Rh1 O5 C15' 98.2(13) . . . . ? O3 Rh1 O5 C15' -17(4) . . . . ? O1 Rh1 O5 C15' -76.1(13) . . . . ? Rh2 Rh1 O5 C15' 11.2(12) . . . . ? O7 Rh1 O5 C15 86.4(6) . . . . ? O3 Rh1 O5 C15 -29(4) . . . . ? O1 Rh1 O5 C15 -87.9(6) . . . . ? Rh2 Rh1 O5 C15 -0.6(6) . . . . ? O8 Rh2 O6 C15 -90.3(7) . . . . ? O4 Rh2 O6 C15 22(5) . . . . ? O2 Rh2 O6 C15 86.0(6) . . . . ? Rh1 Rh2 O6 C15 -2.0(6) . . . . ? O8 Rh2 O6 C15' -100.1(10) . . . . ? O4 Rh2 O6 C15' 13(5) . . . . ? O2 Rh2 O6 C15' 76.2(9) . . . . ? Rh1 Rh2 O6 C15' -11.8(9) . . . . ? O5 Rh1 O7 C26 -95.4(9) . . . . ? O3 Rh1 O7 C26 79.2(9) . . . . ? O1 Rh1 O7 C26 7(4) . . . . ? Rh2 Rh1 O7 C26 -8.1(9) . . . . ? O5 Rh1 O7 C26' -84.4(9) . . . . ? O3 Rh1 O7 C26' 90.2(9) . . . . ? O1 Rh1 O7 C26' 18(4) . . . . ? Rh2 Rh1 O7 C26' 2.9(9) . . . . ? O4 Rh2 O8 C26' -93.2(11) . . . . ? O2 Rh2 O8 C26' -9(7) . . . . ? O6 Rh2 O8 C26' 82.9(11) . . . . ? Rh1 Rh2 O8 C26' -5.1(10) . . . . ? O4 Rh2 O8 C26 -82.2(9) . . . . ? O2 Rh2 O8 C26 2(7) . . . . ? O6 Rh2 O8 C26 93.9(9) . . . . ? Rh1 Rh2 O8 C26 5.9(9) . . . . ? Rh1 O1 C1 O2 -3.6(16) . . . . ? Rh1 O1 C1 C2 173.2(9) . . . . ? Rh2 O2 C1 O1 6.0(16) . . . . ? Rh2 O2 C1 C2 -170.9(8) . . . . ? C5 O9 C2 C3 -79.6(16) . . . . ? C5 O9 C2 C4 164.4(13) . . . . ? C5 O9 C2 C1 48.8(18) . . . . ? O1 C1 C2 O9 -149.2(12) . . . . ? O2 C1 C2 O9 27.9(17) . . . . ? O1 C1 C2 C3 -22.1(18) . . . . ? O2 C1 C2 C3 155.0(13) . . . . ? O1 C1 C2 C4 98.7(15) . . . . ? O2 C1 C2 C4 -84.1(14) . . . . ? C2 O9 C5 C10 2(2) . . . . ? C2 O9 C5 C6 -175.3(13) . . . . ? C10 C5 C6 C7 -1(3) . . . . ? O9 C5 C6 C7 176.5(15) . . . . ? C5 C6 C7 C8 -4(3) . . . . ? C6 C7 C8 C9 6(3) . . . . ? C11 O10 C9 C10 0(3) . . . . ? C11 O10 C9 C8 174.2(18) . . . . ? C7 C8 C9 O10 -177.3(17) . . . . ? C7 C8 C9 C10 -3(3) . . . . ? C6 C5 C10 C9 4(2) . . . . ? O9 C5 C10 C9 -172.8(15) . . . . ? O10 C9 C10 C5 171.3(16) . . . . ? C8 C9 C10 C5 -2(3) . . . . ? C9 O10 C11 C13 74(2) . . . . ? C9 O10 C11 C12 -165.4(18) . . . . ? C9 O10 C11 C14 -51(2) . . . . ? Rh2 O4 C14 O3 -13(2) . . . . ? Rh2 O4 C14 C11 168.0(11) . . . . ? Rh1 O3 C14 O4 13(2) . . . . ? Rh1 O3 C14 C11 -168.0(11) . . . . ? O10 C11 C14 O4 -29(2) . . . . ? C13 C11 C14 O4 -151.6(16) . . . . ? C12 C11 C14 O4 85.3(19) . . . . ? O10 C11 C14 O3 152.3(16) . . . . ? C13 C11 C14 O3 30(2) . . . . ? C12 C11 C14 O3 -93.5(19) . . . . ? C15' O6 C15 O5 99(15) . . . . ? Rh2 O6 C15 O5 2.2(9) . . . . ? C15' O6 C15 C16 -81(15) . . . . ? Rh2 O6 C15 C16 -177.8(9) . . . . ? C15' O5 C15 O6 -129(9) . . . . ? Rh1 O5 C15 O6 -0.9(9) . . . . ? C15' O5 C15 C16 51(9) . . . . ? Rh1 O5 C15 C16 179.1(9) . . . . ? O6 C15 C16 C17 -62.7(19) . . . . ? O5 C15 C16 C17 117.3(19) . . . . ? C15 C16 C17 C18 -85(3) . . . . ? C16 C17 C18 C19 -169(3) . . . . ? C17 C18 C19 C20 -164(3) . . . . ? C18 C19 C20 C21 60(5) . . . . ? C19 C20 C21 C22 7(7) . . . . ? C20 C21 C22 C23 180(4) . . . . ? C21 C22 C23 C24 -158(4) . . . . ? C22 C23 C24 C25 -126(3) . . . . ? C23 C24 C25 C26 85(3) . . . . ? C26' O7 C26 O8 -73(17) . . . . ? Rh1 O7 C26 O8 15.4(11) . . . . ? C26' O7 C26 C25 107(17) . . . . ? Rh1 O7 C26 C25 -164.6(11) . . . . ? C26' O8 C26 O7 93(19) . . . . ? Rh2 O8 C26 O7 -14.1(11) . . . . ? C26' O8 C26 C25 -87(19) . . . . ? Rh2 O8 C26 C25 165.9(11) . . . . ? C24 C25 C26 O7 -110(2) . . . . ? C24 C25 C26 O8 70(2) . . . . ? C15 O5 C15' O6 36(9) . . . . ? Rh1 O5 C15' O6 -21.8(12) . . . . ? C15 O5 C15' C16' -144(9) . . . . ? Rh1 O5 C15' C16' 158.2(12) . . . . ? C15 O6 C15' O5 -67(15) . . . . ? Rh2 O6 C15' O5 21.7(10) . . . . ? C15 O6 C15' C16' 113(15) . . . . ? Rh2 O6 C15' C16' -158.3(10) . . . . ? O5 C15' C16' C17' 101(2) . . . . ? O6 C15' C16' C17' -79(2) . . . . ? C15' C16' C17' C18' -74(4) . . . . ? C16' C17' C18' C19' 151(3) . . . . ? C17' C18' C19' C20' -98(6) . . . . ? C18' C19' C20' C21' -176(4) . . . . ? C19' C20' C21' C22' 159(5) . . . . ? C20' C21' C22' C23' 70(6) . . . . ? C21' C22' C23' C24' -125(4) . . . . ? C22' C23' C24' C25' 135(4) . . . . ? C23' C24' C25' C26' -123(3) . . . . ? C26 O8 C26' O7 -70(19) . . . . ? Rh2 O8 C26' O7 8.8(16) . . . . ? C26 O8 C26' C25' 110(19) . . . . ? Rh2 O8 C26' C25' -171.2(16) . . . . ? C26 O7 C26' O8 89(17) . . . . ? Rh1 O7 C26' O8 -7.7(15) . . . . ? C26 O7 C26' C25' -91(17) . . . . ? Rh1 O7 C26' C25' 172.3(15) . . . . ? C24' C25' C26' O8 179(3) . . . . ? C24' C25' C26' O7 -1(3) . . . . ? C35 N1 C27 C28 2(2) . . . . ? N1 C27 C28 C29 0(2) . . . . ? C27 C28 C29 C34 -1(2) . . . . ? C27 C28 C29 C30 176.4(13) . . . . ? C34 C29 C30 C31' 54(2) . . . . ? C28 C29 C30 C31' -123(2) . . . . ? C34 C29 C30 C32' -170(3) . . . . ? C28 C29 C30 C32' 13(3) . . . . ? C34 C29 C30 C33' -56(3) . . . . ? C28 C29 C30 C33' 127(3) . . . . ? C34 C29 C30 C32 -124.7(16) . . . . ? C28 C29 C30 C32 58.2(19) . . . . ? C34 C29 C30 C33 -3(2) . . . . ? C28 C29 C30 C33 179.6(16) . . . . ? C34 C29 C30 C31 115.7(18) . . . . ? C28 C29 C30 C31 -61.4(19) . . . . ? C28 C29 C34 C35 -1(2) . . . . ? C30 C29 C34 C35 -178.1(13) . . . . ? C27 N1 C35 C34 -4(2) . . . . ? C29 C34 C35 N1 3(2) . . . . ? C44 N2 C36 C37 6(2) . . . . ? N2 C36 C37 C38 -5(3) . . . . ? C36 C37 C38 C43 2(2) . . . . ? C36 C37 C38 C39 -178.5(13) . . . . ? C43 C38 C39 C40 103(2) . . . . ? C37 C38 C39 C40 -77(2) . . . . ? C43 C38 C39 C42' -174(2) . . . . ? C37 C38 C39 C42' 6(2) . . . . ? C43 C38 C39 C41 -24(2) . . . . ? C37 C38 C39 C41 156.3(17) . . . . ? C43 C38 C39 C41' -48(2) . . . . ? C37 C38 C39 C41' 132(2) . . . . ? C43 C38 C39 C40' 68(2) . . . . ? C37 C38 C39 C40' -112(2) . . . . ? C43 C38 C39 C42 -139.5(16) . . . . ? C37 C38 C39 C42 40.6(18) . . . . ? C37 C38 C43 C44 0.2(18) . . . . ? C39 C38 C43 C44 -179.8(11) . . . . ? C36 N2 C44 C43 -4.3(19) . . . . ? C38 C43 C44 N2 1.3(19) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 24.12 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.074 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.134 data_tmcg20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H58 N2 O12 Rh2' _chemical_formula_weight 1036.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 '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 13.854(2) _cell_length_b 14.0285(19) _cell_length_c 14.7149(19) _cell_angle_alpha 69.171(15) _cell_angle_beta 79.073(16) _cell_angle_gamma 63.860(15) _cell_volume 2397.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max .35 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11056 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.1591 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 24.26 _reflns_number_total 6978 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0131P)^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 6978 _refine_ls_number_parameters 557 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 0.708 _refine_ls_restrained_S_all 0.708 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.49758(4) 0.45066(4) 0.44866(4) 0.02865(15) Uani 1 d . . . Rh2 Rh 0.03932(4) 0.45537(4) 0.07839(4) 0.02827(15) Uani 1 d . . . O1 O 0.6591(3) 0.4034(3) 0.4264(3) 0.0375(10) Uani 1 d . . . O2 O 0.5343(3) 0.3100(3) 0.5662(3) 0.0381(11) Uani 1 d . . . O3 O 0.3364(3) 0.4997(3) 0.4816(3) 0.0376(10) Uani 1 d . . . O4 O 0.1211(3) 0.6324(4) 0.4590(4) 0.0626(14) Uani 1 d . . . O5 O 0.3426(4) 0.7895(3) 0.2084(3) 0.0530(13) Uani 1 d . . . O6 O 0.4657(3) 0.5961(3) 0.3359(3) 0.0368(10) Uani 1 d . . . O7 O 0.1108(3) 0.3095(3) 0.0450(3) 0.0379(11) Uani 1 d . . . O8 O -0.0947(3) 0.4250(3) 0.1316(3) 0.0346(10) Uani 1 d . . . O9 O -0.0346(3) 0.6091(3) 0.1011(3) 0.0380(11) Uani 1 d . . . O10 O 0.1686(3) 0.4922(3) 0.0150(3) 0.0351(10) Uani 1 d . . . O11 O 0.0625(4) 0.1500(3) -0.0368(4) 0.0570(13) Uani 1 d . . . O12 O -0.2181(3) 0.3050(3) 0.1861(3) 0.0521(12) Uani 1 d . . . C1 C 0.2936(5) 0.5665(5) 0.5320(4) 0.0371(16) Uani 1 d . . . C2 C 0.1692(5) 0.6193(6) 0.5421(5) 0.0513(19) Uani 1 d . . . C3 C 0.1340(6) 0.5375(6) 0.6246(6) 0.075(2) Uani 1 d . . . H3 H 0.1634 0.5245 0.6848 0.090 Uiso 1 calc R . . H3 H 0.1600 0.4675 0.6106 0.090 Uiso 1 calc R . . H3 H 0.0560 0.5683 0.6312 0.090 Uiso 1 calc R . . C4 C 0.1278(5) 0.7322(6) 0.5612(6) 0.077(3) Uani 1 d . . . H4 H 0.1605 0.7221 0.6186 0.093 Uiso 1 calc R . . H4 H 0.0502 0.7609 0.5716 0.093 Uiso 1 calc R . . H4 H 0.1466 0.7847 0.5055 0.093 Uiso 1 calc R . . C5 C 0.1515(6) 0.6767(5) 0.3650(6) 0.051(2) Uani 1 d . . . C6 C 0.1040(6) 0.6711(5) 0.2944(6) 0.060(2) Uani 1 d . . . H6 H 0.0496 0.6443 0.3116 0.072 Uiso 1 calc R . . C7 C 0.1361(6) 0.7049(5) 0.1989(6) 0.067(2) Uani 1 d . . . H7 H 0.1033 0.7003 0.1511 0.081 Uiso 1 calc R . . C8 C 0.2154(6) 0.7453(5) 0.1708(5) 0.056(2) Uani 1 d . . . H8 H 0.2370 0.7672 0.1049 0.067 Uiso 1 calc R . . C9 C 0.2624(6) 0.7530(5) 0.2419(6) 0.0477(19) Uani 1 d . . . C10 C 0.2274(5) 0.7232(5) 0.3382(5) 0.0479(18) Uani 1 d . . . H10 H 0.2547 0.7343 0.3857 0.057 Uiso 1 calc R . . C11 C 0.4061(6) 0.7939(5) 0.2718(5) 0.0463(19) Uani 1 d . . . C12 C 0.3426(6) 0.8948(5) 0.3096(5) 0.071(2) Uani 1 d . . . H12 H 0.3870 0.8965 0.3523 0.085 Uiso 1 calc R . . H12 H 0.2781 0.8887 0.3454 0.085 Uiso 1 calc R . . H12 H 0.3228 0.9630 0.2551 0.085 Uiso 1 calc R . . C13 C 0.5018(6) 0.8063(5) 0.2088(5) 0.067(2) Uani 1 d . . . H13 H 0.5495 0.8096 0.2469 0.080 Uiso 1 calc R . . H13 H 0.4775 0.8744 0.1544 0.080 Uiso 1 calc R . . H13 H 0.5399 0.7428 0.1844 0.080 Uiso 1 calc R . . C14 C 0.4484(5) 0.6841(5) 0.3553(5) 0.0405(17) Uani 1 d . . . C15 C -0.0920(5) 0.6905(5) 0.0367(5) 0.0360(16) Uani 1 d . . . C16 C -0.1443(5) 0.8065(5) 0.0535(5) 0.0455(19) Uani 1 d . . . C17 C -0.1783(5) 0.7944(5) 0.1592(5) 0.064(2) Uani 1 d . . . H17 H -0.2109 0.8674 0.1686 0.077 Uiso 1 calc R . . H17 H -0.1159 0.7471 0.1989 0.077 Uiso 1 calc R . . H17 H -0.2302 0.7610 0.1779 0.077 Uiso 1 calc R . . C18 C -0.2378(5) 0.8876(5) -0.0129(5) 0.073(2) Uani 1 d . . . H18 H -0.2691 0.9589 -0.0003 0.088 Uiso 1 calc R . . H18 H -0.2919 0.8578 -0.0004 0.088 Uiso 1 calc R . . H18 H -0.2120 0.8979 -0.0802 0.088 Uiso 1 calc R . . C19 C 0.1649(5) 0.5479(4) -0.0739(5) 0.0283(15) Uani 1 d . . . C20 C 0.0094(6) 0.1371(5) 0.0546(6) 0.064(2) Uani 1 d . . . C21 C 0.0394(8) 0.0356(6) 0.1246(8) 0.109(4) Uani 1 d . . . H21 H 0.0975 -0.0272 0.1130 0.131 Uiso 1 calc R . . C22 C -0.0166(8) 0.0268(6) 0.2121(9) 0.131(5) Uani 1 d . . . H22 H 0.0040 -0.0430 0.2606 0.158 Uiso 1 calc R . . C23 C -0.1024(7) 0.1171(6) 0.2315(7) 0.095(3) Uani 1 d . . . H23 H -0.1394 0.1096 0.2924 0.114 Uiso 1 calc R . . C24 C -0.1326(6) 0.2184(5) 0.1594(6) 0.055(2) Uani 1 d . . . C25 C -0.0798(5) 0.2277(5) 0.0707(5) 0.0481(18) Uani 1 d . . . H25 H -0.1041 0.2958 0.0203 0.058 Uiso 1 calc R . . C26 C -0.2577(5) 0.4150(5) 0.1159(5) 0.0383(16) Uani 1 d . . . C27 C -0.3197(5) 0.4184(5) 0.0402(5) 0.0546(19) Uani 1 d . . . H27 H -0.3460 0.4927 -0.0063 0.066 Uiso 1 calc R . . H27 H -0.3802 0.3999 0.0715 0.066 Uiso 1 calc R . . H27 H -0.2730 0.3648 0.0068 0.066 Uiso 1 calc R . . C28 C -0.3329(5) 0.4913(5) 0.1753(5) 0.0531(19) Uani 1 d . . . H28 H -0.3635 0.5675 0.1326 0.064 Uiso 1 calc R . . H28 H -0.2926 0.4875 0.2246 0.064 Uiso 1 calc R . . H28 H -0.3902 0.4673 0.2063 0.064 Uiso 1 calc R . . N1 N 0.1125(4) 0.3642(4) 0.2228(3) 0.0319(13) Uani 1 d . . . C29 C 0.1283(5) 0.2573(5) 0.2684(5) 0.0465(18) Uani 1 d . . . H29 H 0.1078 0.2214 0.2373 0.056 Uiso 1 calc R . . C30 C 0.1723(5) 0.1979(5) 0.3568(5) 0.051(2) Uani 1 d . . . H30 H 0.1828 0.1226 0.3839 0.061 Uiso 1 calc R . . C31 C 0.2022(5) 0.2464(5) 0.4082(5) 0.0430(18) Uani 1 d . . . C32 C 0.1849(5) 0.3566(5) 0.3619(5) 0.0483(18) Uani 1 d . . . H32 H 0.2032 0.3951 0.3919 0.058 Uiso 1 calc R . . C33 C 0.1406(5) 0.4103(5) 0.2716(5) 0.0435(17) Uani 1 d . . . H33 H 0.1297 0.4856 0.2425 0.052 Uiso 1 calc R . . C34 C 0.2516(5) 0.1803(6) 0.5065(5) 0.0549(19) Uani 1 d . . . C35 C 0.3552(8) 0.0897(10) 0.4975(7) 0.206(8) Uani 1 d . . . H35 H 0.3859 0.0478 0.5611 0.248 Uiso 1 calc R . . H35 H 0.4037 0.1206 0.4543 0.248 Uiso 1 calc R . . H35 H 0.3450 0.0406 0.4712 0.248 Uiso 1 calc R . . C36 C 0.2658(16) 0.2485(9) 0.5532(9) 0.253(11) Uani 1 d . . . H36 H 0.2973 0.2021 0.6159 0.304 Uiso 1 calc R . . H36 H 0.1965 0.3064 0.5624 0.304 Uiso 1 calc R . . H36 H 0.3131 0.2826 0.5126 0.304 Uiso 1 calc R . . C37 C 0.1818(9) 0.1319(10) 0.5751(8) 0.179(6) Uani 1 d . . . H37 H 0.2154 0.0900 0.6374 0.215 Uiso 1 calc R . . H37 H 0.1705 0.0824 0.5501 0.215 Uiso 1 calc R . . H37 H 0.1131 0.1911 0.5832 0.215 Uiso 1 calc R . . N2 N 0.4946(4) 0.3621(4) 0.3499(4) 0.0359(13) Uani 1 d . . . C38 C 0.5753(5) 0.2632(5) 0.3517(5) 0.0464(18) Uani 1 d . . . H38 H 0.6297 0.2307 0.3966 0.056 Uiso 1 calc R . . C39 C 0.5798(5) 0.2073(5) 0.2877(5) 0.0478(19) Uani 1 d . . . H39 H 0.6378 0.1382 0.2906 0.057 Uiso 1 calc R . . C40 C 0.5043(5) 0.2488(4) 0.2227(4) 0.0331(15) Uani 1 d . . . C41 C 0.4216(5) 0.3528(5) 0.2203(5) 0.0433(18) Uani 1 d . . . H41 H 0.3670 0.3873 0.1754 0.052 Uiso 1 calc R . . C42 C 0.4213(5) 0.4049(5) 0.2856(5) 0.0408(17) Uani 1 d . . . H42 H 0.3650 0.4749 0.2831 0.049 Uiso 1 calc R . . C43 C 0.5065(5) 0.1870(4) 0.1525(5) 0.0452(17) Uani 1 d D . . C44 C 0.5672(11) 0.2174(11) 0.0608(10) 0.084(5) Uiso 0.568(10) d PDU A 1 H44 H 0.5678 0.1777 0.0184 0.101 Uiso 0.568(10) calc PR A 1 H44 H 0.6406 0.1972 0.0750 0.101 Uiso 0.568(10) calc PR A 1 H44 H 0.5332 0.2972 0.0288 0.101 Uiso 0.568(10) calc PR A 1 C45 C 0.3933(9) 0.2160(10) 0.1283(11) 0.076(5) Uiso 0.568(10) d PDU A 1 H45 H 0.3965 0.1773 0.0840 0.091 Uiso 0.568(10) calc PR A 1 H45 H 0.3575 0.2959 0.0978 0.091 Uiso 0.568(10) calc PR A 1 H45 H 0.3535 0.1934 0.1876 0.091 Uiso 0.568(10) calc PR A 1 C46 C 0.5561(11) 0.0621(8) 0.2010(10) 0.074(5) Uiso 0.568(10) d PDU A 1 H46 H 0.5576 0.0243 0.1565 0.089 Uiso 0.568(10) calc PR A 1 H46 H 0.5136 0.0424 0.2593 0.089 Uiso 0.568(10) calc PR A 1 H46 H 0.6289 0.0393 0.2184 0.089 Uiso 0.568(10) calc PR A 1 C44' C 0.4534(13) 0.2629(12) 0.0605(12) 0.070(6) Uiso 0.432(10) d PDU A 2 H44' H 0.4592 0.2197 0.0193 0.084 Uiso 0.432(10) calc PR A 2 H44' H 0.4880 0.3138 0.0275 0.084 Uiso 0.432(10) calc PR A 2 H44' H 0.3781 0.3052 0.0742 0.084 Uiso 0.432(10) calc PR A 2 C45' C 0.6227(12) 0.1271(14) 0.1244(14) 0.082(6) Uiso 0.432(10) d PDU A 2 H45' H 0.6269 0.0885 0.0797 0.098 Uiso 0.432(10) calc PR A 2 H45' H 0.6615 0.0734 0.1823 0.098 Uiso 0.432(10) calc PR A 2 H45' H 0.6544 0.1808 0.0933 0.098 Uiso 0.432(10) calc PR A 2 C46' C 0.4596(16) 0.1074(14) 0.2039(15) 0.103(8) Uiso 0.432(10) d PDU A 2 H46' H 0.4611 0.0674 0.1615 0.124 Uiso 0.432(10) calc PR A 2 H46' H 0.3857 0.1466 0.2239 0.124 Uiso 0.432(10) calc PR A 2 H46' H 0.5005 0.0549 0.2610 0.124 Uiso 0.432(10) calc PR A 2 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 Rh1 0.0321(3) 0.0343(3) 0.0258(4) -0.0158(3) 0.0038(3) -0.0158(2) Rh2 0.0313(3) 0.0295(3) 0.0213(3) -0.0083(2) 0.0004(3) -0.0101(2) O1 0.032(2) 0.055(2) 0.036(3) -0.026(2) 0.001(2) -0.018(2) O2 0.057(3) 0.038(2) 0.026(3) -0.011(2) -0.008(2) -0.021(2) O3 0.038(2) 0.050(2) 0.038(3) -0.028(2) 0.008(2) -0.023(2) O4 0.046(3) 0.105(4) 0.053(4) -0.042(3) 0.005(3) -0.035(3) O5 0.074(3) 0.049(3) 0.036(3) -0.006(2) -0.015(3) -0.025(3) O6 0.053(3) 0.035(2) 0.025(3) -0.0110(19) 0.003(2) -0.022(2) O7 0.044(2) 0.030(2) 0.033(3) -0.015(2) -0.003(2) -0.0047(19) O8 0.032(2) 0.045(2) 0.024(3) -0.010(2) 0.004(2) -0.0159(19) O9 0.045(3) 0.032(2) 0.031(3) -0.013(2) -0.006(2) -0.006(2) O10 0.034(2) 0.041(2) 0.031(3) -0.008(2) 0.001(2) -0.0183(19) O11 0.065(3) 0.043(2) 0.063(4) -0.026(3) -0.006(3) -0.013(2) O12 0.058(3) 0.045(2) 0.046(3) -0.001(2) 0.005(2) -0.028(2) C1 0.041(4) 0.043(3) 0.022(4) -0.007(3) 0.000(3) -0.015(3) C2 0.031(4) 0.086(5) 0.052(5) -0.044(4) 0.010(3) -0.024(4) C3 0.066(5) 0.132(6) 0.050(6) -0.043(5) 0.017(4) -0.057(5) C4 0.034(4) 0.109(6) 0.094(7) -0.073(5) 0.006(4) -0.004(4) C5 0.043(4) 0.062(4) 0.050(6) -0.030(4) -0.003(4) -0.011(4) C6 0.056(5) 0.074(5) 0.058(6) -0.035(5) -0.016(4) -0.018(4) C7 0.080(6) 0.060(4) 0.060(6) -0.031(4) -0.029(5) -0.007(4) C8 0.076(5) 0.053(4) 0.047(5) -0.017(4) -0.016(4) -0.026(4) C9 0.052(5) 0.032(3) 0.052(6) -0.014(4) -0.019(4) -0.004(3) C10 0.044(4) 0.051(4) 0.046(5) -0.024(4) -0.012(4) -0.006(3) C11 0.056(4) 0.038(4) 0.042(5) -0.012(3) 0.002(4) -0.017(3) C12 0.098(6) 0.040(4) 0.071(6) -0.025(4) -0.013(5) -0.015(4) C13 0.096(6) 0.063(4) 0.051(6) -0.010(4) -0.008(5) -0.046(4) C14 0.028(4) 0.049(4) 0.050(5) -0.024(4) -0.001(3) -0.015(3) C15 0.039(4) 0.041(4) 0.037(5) -0.013(3) 0.000(3) -0.023(3) C16 0.049(4) 0.041(4) 0.046(5) -0.028(3) -0.005(4) -0.005(3) C17 0.071(5) 0.059(4) 0.051(5) -0.033(4) 0.001(4) -0.007(4) C18 0.066(5) 0.053(4) 0.079(6) -0.035(4) -0.023(4) 0.013(4) C19 0.034(4) 0.028(3) 0.020(4) -0.007(3) 0.003(3) -0.012(3) C20 0.073(5) 0.044(4) 0.066(6) -0.015(4) 0.002(5) -0.021(4) C21 0.118(8) 0.032(4) 0.117(9) 0.008(5) 0.025(7) -0.013(5) C22 0.127(8) 0.036(5) 0.137(11) 0.033(5) 0.029(8) -0.010(5) C23 0.098(6) 0.050(5) 0.083(7) 0.020(5) 0.012(6) -0.021(5) C24 0.062(5) 0.036(4) 0.059(6) 0.000(4) -0.003(4) -0.024(4) C25 0.051(4) 0.031(3) 0.059(6) -0.010(3) -0.007(4) -0.015(3) C26 0.040(4) 0.048(4) 0.032(4) -0.014(3) 0.009(3) -0.025(3) C27 0.057(4) 0.067(4) 0.052(5) -0.013(4) 0.004(4) -0.043(4) C28 0.045(4) 0.070(4) 0.041(5) -0.016(4) 0.015(3) -0.028(3) N1 0.031(3) 0.036(3) 0.025(3) -0.009(3) -0.008(2) -0.008(2) C29 0.064(5) 0.041(4) 0.038(5) -0.014(4) 0.003(4) -0.025(3) C30 0.061(5) 0.037(4) 0.034(5) 0.000(3) -0.001(4) -0.012(3) C31 0.040(4) 0.054(4) 0.024(4) -0.008(4) 0.000(3) -0.013(3) C32 0.058(4) 0.058(4) 0.035(5) -0.010(4) -0.005(4) -0.030(4) C33 0.045(4) 0.042(3) 0.041(5) -0.009(3) -0.004(4) -0.018(3) C34 0.053(4) 0.072(4) 0.032(5) -0.005(4) -0.004(4) -0.026(4) C35 0.107(8) 0.259(13) 0.069(8) -0.019(9) -0.045(7) 0.077(10) C36 0.53(3) 0.183(12) 0.108(11) 0.031(9) -0.187(16) -0.189(15) C37 0.129(9) 0.291(15) 0.058(8) 0.053(9) -0.034(7) -0.105(10) N2 0.034(3) 0.035(3) 0.042(4) -0.018(3) 0.008(3) -0.017(2) C38 0.049(4) 0.044(4) 0.039(5) -0.006(3) -0.016(3) -0.011(3) C39 0.049(4) 0.041(3) 0.057(5) -0.030(4) -0.007(4) -0.009(3) C40 0.037(4) 0.040(3) 0.033(4) -0.017(3) 0.005(3) -0.022(3) C41 0.043(4) 0.050(4) 0.041(5) -0.021(3) -0.008(3) -0.015(3) C42 0.033(4) 0.047(4) 0.044(5) -0.021(3) -0.006(3) -0.010(3) C43 0.051(4) 0.044(3) 0.047(5) -0.023(3) -0.001(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.030(4) . ? Rh1 O2 2.042(4) . ? Rh1 O6 2.046(4) . ? Rh1 O3 2.042(4) . ? Rh1 Rh1 2.4107(9) 2_666 ? Rh2 O7 2.038(3) . ? Rh2 O8 2.037(4) . ? Rh2 O10 2.046(4) . ? Rh2 O9 2.061(3) . ? Rh2 Rh2 2.4029(11) 2_565 ? O1 C1 1.251(7) 2_666 ? O2 C14 1.260(7) 2_666 ? O3 C1 1.271(6) . ? O4 C5 1.370(8) . ? O4 C2 1.419(7) . ? O5 C9 1.361(8) . ? O5 C11 1.431(8) . ? O6 C14 1.277(6) . ? O7 C15 1.278(7) 2_565 ? O8 C19 1.252(6) 2_565 ? O9 C15 1.245(7) . ? O10 C19 1.260(6) . ? O11 C20 1.397(8) . ? O11 C16 1.454(8) 2_565 ? O12 C24 1.388(7) . ? O12 C26 1.444(7) . ? C1 O1 1.251(7) 2_666 ? C1 C2 1.548(8) . ? C2 C3 1.519(10) . ? C2 C4 1.540(8) . ? C5 C6 1.371(9) . ? C5 C10 1.397(9) . ? C6 C7 1.369(10) . ? C7 C8 1.382(10) . ? C8 C9 1.389(9) . ? C9 C10 1.385(9) . ? C11 C13 1.507(9) . ? C11 C12 1.538(7) . ? C11 C14 1.535(9) . ? C14 O2 1.260(7) 2_666 ? C15 O7 1.278(7) 2_565 ? C15 C16 1.554(7) . ? C16 O11 1.454(8) 2_565 ? C16 C17 1.507(9) . ? C16 C18 1.523(8) . ? C19 O8 1.252(6) 2_565 ? C19 C26 1.538(8) 2_565 ? C20 C21 1.365(10) . ? C20 C25 1.385(8) . ? C21 C22 1.366(12) . ? C22 C23 1.379(10) . ? C23 C24 1.376(9) . ? C24 C25 1.362(9) . ? C26 C27 1.507(8) . ? C26 C28 1.526(7) . ? C26 C19 1.538(8) 2_565 ? N1 C33 1.320(7) . ? N1 C29 1.341(7) . ? C29 C30 1.356(8) . ? C30 C31 1.392(9) . ? C31 C32 1.377(8) . ? C31 C34 1.512(8) . ? C32 C33 1.378(8) . ? C34 C36 1.453(11) . ? C34 C35 1.461(9) . ? C34 C37 1.462(12) . ? N2 C42 1.309(7) . ? N2 C38 1.340(6) . ? C38 C39 1.402(8) . ? C39 C40 1.340(8) . ? C40 C41 1.396(7) . ? C40 C43 1.556(7) . ? C41 C42 1.396(7) . ? C43 C46' 1.447(15) . ? C43 C44' 1.473(14) . ? C43 C44 1.479(12) . ? C43 C46 1.513(11) . ? C43 C45 1.516(12) . ? C43 C45' 1.507(14) . ? 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 Rh1 O2 85.71(16) . . ? O1 Rh1 O6 92.47(16) . . ? O2 Rh1 O6 175.76(17) . . ? O1 Rh1 O3 175.28(16) . . ? O2 Rh1 O3 92.26(16) . . ? O6 Rh1 O3 89.27(15) . . ? O1 Rh1 Rh1 87.65(11) . 2_666 ? O2 Rh1 Rh1 88.52(10) . 2_666 ? O6 Rh1 Rh1 87.58(10) . 2_666 ? O3 Rh1 Rh1 88.04(10) . 2_666 ? O7 Rh2 O8 90.52(14) . . ? O7 Rh2 O10 89.56(14) . . ? O8 Rh2 O10 175.66(16) . . ? O7 Rh2 O9 175.67(17) . . ? O8 Rh2 O9 90.65(15) . . ? O10 Rh2 O9 88.96(14) . . ? O7 Rh2 Rh2 88.26(12) . 2_565 ? O8 Rh2 Rh2 87.51(11) . 2_565 ? O10 Rh2 Rh2 88.16(12) . 2_565 ? O9 Rh2 Rh2 87.63(12) . 2_565 ? C1 O1 Rh1 119.1(3) 2_666 . ? C14 O2 Rh1 117.7(4) 2_666 . ? C1 O3 Rh1 117.6(4) . . ? C5 O4 C2 124.2(6) . . ? C9 O5 C11 122.6(6) . . ? C14 O6 Rh1 118.0(4) . . ? C15 O7 Rh2 118.5(3) 2_565 . ? C19 O8 Rh2 119.1(4) 2_565 . ? C15 O9 Rh2 118.7(4) . . ? C19 O10 Rh2 117.8(4) . . ? C20 O11 C16 117.3(5) . 2_565 ? C24 O12 C26 119.3(5) . . ? O1 C1 O3 127.1(5) 2_666 . ? O1 C1 C2 115.4(5) 2_666 . ? O3 C1 C2 117.5(6) . . ? O4 C2 C3 104.4(6) . . ? O4 C2 C4 110.2(5) . . ? C3 C2 C4 110.9(5) . . ? O4 C2 C1 111.7(5) . . ? C3 C2 C1 108.2(6) . . ? C4 C2 C1 111.2(6) . . ? O4 C5 C6 115.7(8) . . ? O4 C5 C10 124.6(7) . . ? C6 C5 C10 119.7(8) . . ? C7 C6 C5 119.7(8) . . ? C6 C7 C8 121.8(7) . . ? C7 C8 C9 118.7(8) . . ? O5 C9 C8 114.8(7) . . ? O5 C9 C10 125.3(6) . . ? C8 C9 C10 119.8(7) . . ? C9 C10 C5 120.0(7) . . ? O5 C11 C13 104.3(6) . . ? O5 C11 C12 110.7(5) . . ? C13 C11 C12 110.5(6) . . ? O5 C11 C14 111.7(5) . . ? C13 C11 C14 107.5(5) . . ? C12 C11 C14 111.9(6) . . ? O2 C14 O6 127.2(6) 2_666 . ? O2 C14 C11 117.0(5) 2_666 . ? O6 C14 C11 115.7(6) . . ? O9 C15 O7 126.9(5) . 2_565 ? O9 C15 C16 118.1(6) . . ? O7 C15 C16 115.0(5) 2_565 . ? O11 C16 C17 103.9(5) 2_565 . ? O11 C16 C18 110.5(6) 2_565 . ? C17 C16 C18 111.6(5) . . ? O11 C16 C15 108.8(5) 2_565 . ? C17 C16 C15 110.4(5) . . ? C18 C16 C15 111.4(5) . . ? O8 C19 O10 127.1(6) 2_565 . ? O8 C19 C26 116.8(6) 2_565 2_565 ? O10 C19 C26 116.1(6) . 2_565 ? C21 C20 C25 120.1(8) . . ? C21 C20 O11 121.0(7) . . ? C25 C20 O11 118.7(6) . . ? C20 C21 C22 118.7(8) . . ? C21 C22 C23 122.1(7) . . ? C22 C23 C24 118.3(8) . . ? C25 C24 C23 120.3(7) . . ? C25 C24 O12 125.4(6) . . ? C23 C24 O12 114.3(7) . . ? C24 C25 C20 120.2(6) . . ? O12 C26 C27 110.3(5) . . ? O12 C26 C28 104.6(5) . . ? C27 C26 C28 110.0(5) . . ? O12 C26 C19 110.2(5) . 2_565 ? C27 C26 C19 114.2(5) . 2_565 ? C28 C26 C19 107.2(5) . 2_565 ? C33 N1 C29 114.9(5) . . ? N1 C29 C30 123.8(6) . . ? C29 C30 C31 121.3(6) . . ? C32 C31 C30 115.0(6) . . ? C32 C31 C34 123.6(6) . . ? C30 C31 C34 121.4(6) . . ? C31 C32 C33 119.9(6) . . ? N1 C33 C32 125.1(6) . . ? C36 C34 C35 109.4(11) . . ? C36 C34 C37 104.3(10) . . ? C35 C34 C37 108.3(8) . . ? C36 C34 C31 113.0(7) . . ? C35 C34 C31 110.3(6) . . ? C37 C34 C31 111.3(7) . . ? C42 N2 C38 117.4(5) . . ? N2 C38 C39 121.1(6) . . ? C40 C39 C38 122.3(5) . . ? C39 C40 C41 116.2(5) . . ? C39 C40 C43 123.1(5) . . ? C41 C40 C43 120.7(5) . . ? C42 C41 C40 119.1(6) . . ? N2 C42 C41 123.9(5) . . ? C46' C43 C44' 111.9(11) . . ? C46' C43 C44 140.1(10) . . ? C44' C43 C44 57.4(8) . . ? C46' C43 C46 47.8(8) . . ? C44' C43 C46 136.3(9) . . ? C44 C43 C46 110.0(7) . . ? C46' C43 C45 62.3(9) . . ? C44' C43 C45 53.7(8) . . ? C44 C43 C45 108.6(8) . . ? C46 C43 C45 106.3(8) . . ? C46' C43 C45' 110.2(10) . . ? C44' C43 C45' 105.7(10) . . ? C44 C43 C45' 50.8(7) . . ? C46 C43 C45' 64.1(8) . . ? C45 C43 C45' 141.5(9) . . ? C46' C43 C40 108.4(10) . . ? C44' C43 C40 113.4(7) . . ? C44 C43 C40 110.9(7) . . ? C46 C43 C40 110.2(7) . . ? C45 C43 C40 110.8(6) . . ? C45' C43 C40 107.3(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Rh1 O1 C1 -87.5(4) . . . 2_666 ? O6 Rh1 O1 C1 88.7(4) . . . 2_666 ? O3 Rh1 O1 C1 -23(2) . . . 2_666 ? Rh1 Rh1 O1 C1 1.2(4) 2_666 . . 2_666 ? O1 Rh1 O2 C14 84.5(4) . . . 2_666 ? O6 Rh1 O2 C14 20(2) . . . 2_666 ? O3 Rh1 O2 C14 -91.3(4) . . . 2_666 ? Rh1 Rh1 O2 C14 -3.3(4) 2_666 . . 2_666 ? O1 Rh1 O3 C1 30(2) . . . . ? O2 Rh1 O3 C1 94.0(4) . . . . ? O6 Rh1 O3 C1 -82.0(4) . . . . ? Rh1 Rh1 O3 C1 5.6(4) 2_666 . . . ? O1 Rh1 O6 C14 -94.6(4) . . . . ? O2 Rh1 O6 C14 -30(2) . . . . ? O3 Rh1 O6 C14 81.0(4) . . . . ? Rh1 Rh1 O6 C14 -7.1(4) 2_666 . . . ? O8 Rh2 O7 C15 85.8(5) . . . 2_565 ? O10 Rh2 O7 C15 -89.8(5) . . . 2_565 ? O9 Rh2 O7 C15 -20(2) . . . 2_565 ? Rh2 Rh2 O7 C15 -1.7(4) 2_565 . . 2_565 ? O7 Rh2 O8 C19 -84.5(3) . . . 2_565 ? O10 Rh2 O8 C19 6.5(19) . . . 2_565 ? O9 Rh2 O8 C19 91.3(3) . . . 2_565 ? Rh2 Rh2 O8 C19 3.7(3) 2_565 . . 2_565 ? O7 Rh2 O9 C15 20(2) . . . . ? O8 Rh2 O9 C15 -86.0(5) . . . . ? O10 Rh2 O9 C15 89.7(5) . . . . ? Rh2 Rh2 O9 C15 1.5(4) 2_565 . . . ? O7 Rh2 O10 C19 91.4(3) . . . . ? O8 Rh2 O10 C19 0.4(19) . . . . ? O9 Rh2 O10 C19 -84.5(3) . . . . ? Rh2 Rh2 O10 C19 3.2(3) 2_565 . . . ? Rh1 O3 C1 O1 -8.8(8) . . . 2_666 ? Rh1 O3 C1 C2 169.9(5) . . . . ? C5 O4 C2 C3 -163.5(5) . . . . ? C5 O4 C2 C4 77.4(7) . . . . ? C5 O4 C2 C1 -46.8(8) . . . . ? O1 C1 C2 O4 148.6(6) 2_666 . . . ? O3 C1 C2 O4 -30.2(9) . . . . ? O1 C1 C2 C3 -97.1(6) 2_666 . . . ? O3 C1 C2 C3 84.1(7) . . . . ? O1 C1 C2 C4 24.9(8) 2_666 . . . ? O3 C1 C2 C4 -153.8(6) . . . . ? C2 O4 C5 C6 173.0(5) . . . . ? C2 O4 C5 C10 -5.5(9) . . . . ? O4 C5 C6 C7 -174.5(5) . . . . ? C10 C5 C6 C7 4.0(9) . . . . ? C5 C6 C7 C8 -0.3(9) . . . . ? C6 C7 C8 C9 -0.8(9) . . . . ? C11 O5 C9 C8 -174.7(5) . . . . ? C11 O5 C9 C10 4.5(8) . . . . ? C7 C8 C9 O5 177.5(5) . . . . ? C7 C8 C9 C10 -1.8(8) . . . . ? O5 C9 C10 C5 -173.8(5) . . . . ? C8 C9 C10 C5 5.4(8) . . . . ? O4 C5 C10 C9 171.8(5) . . . . ? C6 C5 C10 C9 -6.5(8) . . . . ? C9 O5 C11 C13 164.3(5) . . . . ? C9 O5 C11 C12 -76.8(7) . . . . ? C9 O5 C11 C14 48.5(7) . . . . ? Rh1 O6 C14 O2 12.7(8) . . . 2_666 ? Rh1 O6 C14 C11 -169.9(4) . . . . ? O5 C11 C14 O2 -151.9(5) . . . 2_666 ? C13 C11 C14 O2 94.3(6) . . . 2_666 ? C12 C11 C14 O2 -27.2(8) . . . 2_666 ? O5 C11 C14 O6 30.4(7) . . . . ? C13 C11 C14 O6 -83.3(7) . . . . ? C12 C11 C14 O6 155.2(5) . . . . ? Rh2 O9 C15 O7 -0.6(9) . . . 2_565 ? Rh2 O9 C15 C16 -178.1(4) . . . . ? O9 C15 C16 O11 76.2(7) . . . 2_565 ? O7 C15 C16 O11 -101.6(6) 2_565 . . 2_565 ? O9 C15 C16 C17 -37.2(8) . . . . ? O7 C15 C16 C17 145.0(6) 2_565 . . . ? O9 C15 C16 C18 -161.8(6) . . . . ? O7 C15 C16 C18 20.4(8) 2_565 . . . ? Rh2 O10 C19 O8 -7.6(6) . . . 2_565 ? Rh2 O10 C19 C26 173.4(3) . . . 2_565 ? C16 O11 C20 C21 -98.9(8) 2_565 . . . ? C16 O11 C20 C25 86.0(7) 2_565 . . . ? C25 C20 C21 C22 -3.4(14) . . . . ? O11 C20 C21 C22 -178.5(9) . . . . ? C20 C21 C22 C23 0.2(17) . . . . ? C21 C22 C23 C24 0.8(15) . . . . ? C22 C23 C24 C25 1.4(12) . . . . ? C22 C23 C24 O12 -178.6(7) . . . . ? C26 O12 C24 C25 0.8(9) . . . . ? C26 O12 C24 C23 -179.2(6) . . . . ? C23 C24 C25 C20 -4.6(11) . . . . ? O12 C24 C25 C20 175.4(6) . . . . ? C21 C20 C25 C24 5.7(11) . . . . ? O11 C20 C25 C24 -179.2(6) . . . . ? C24 O12 C26 C27 73.4(6) . . . . ? C24 O12 C26 C28 -168.5(5) . . . . ? C24 O12 C26 C19 -53.6(7) . . . 2_565 ? C33 N1 C29 C30 -1.6(9) . . . . ? N1 C29 C30 C31 1.6(11) . . . . ? C29 C30 C31 C32 -0.8(9) . . . . ? C29 C30 C31 C34 -179.8(6) . . . . ? C30 C31 C32 C33 0.2(9) . . . . ? C34 C31 C32 C33 179.2(6) . . . . ? C29 N1 C33 C32 1.0(9) . . . . ? C31 C32 C33 N1 -0.3(10) . . . . ? C32 C31 C34 C36 7.7(13) . . . . ? C30 C31 C34 C36 -173.3(10) . . . . ? C32 C31 C34 C35 -115.1(9) . . . . ? C30 C31 C34 C35 63.9(10) . . . . ? C32 C31 C34 C37 124.7(9) . . . . ? C30 C31 C34 C37 -56.4(9) . . . . ? C42 N2 C38 C39 -0.8(9) . . . . ? N2 C38 C39 C40 -0.5(11) . . . . ? C38 C39 C40 C41 1.5(10) . . . . ? C38 C39 C40 C43 -178.7(6) . . . . ? C39 C40 C41 C42 -1.3(9) . . . . ? C43 C40 C41 C42 178.9(6) . . . . ? C38 N2 C42 C41 1.0(9) . . . . ? C40 C41 C42 N2 0.1(10) . . . . ? C39 C40 C43 C46' 83.4(11) . . . . ? C41 C40 C43 C46' -96.8(10) . . . . ? C39 C40 C43 C44' -151.8(10) . . . . ? C41 C40 C43 C44' 28.0(11) . . . . ? C39 C40 C43 C44 -89.4(9) . . . . ? C41 C40 C43 C44 90.4(8) . . . . ? C39 C40 C43 C46 32.6(10) . . . . ? C41 C40 C43 C46 -147.6(8) . . . . ? C39 C40 C43 C45 150.0(8) . . . . ? C41 C40 C43 C45 -30.3(9) . . . . ? C39 C40 C43 C45' -35.5(11) . . . . ? C41 C40 C43 C45' 144.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 24.26 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.568 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.073 data_tmcg8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Br2 N2 O10 Rh2' _chemical_formula_weight 920.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.3740 2.4560 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 '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/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 11.869(3) _cell_length_b 13.9267(17) _cell_length_c 20.613(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.78(2) _cell_angle_gamma 90.00 _cell_volume 3309.2(10) _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 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max .2 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 3.314 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23228 _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.18 _reflns_number_total 5214 _reflns_number_gt 3214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^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 5214 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.814 _refine_ls_restrained_S_all 0.814 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.70504(4) 0.37122(3) 0.37617(2) 0.03496(13) Uani 1 d . . . Rh2 Rh 0.61775(4) 0.31121(3) 0.26609(2) 0.03561(13) Uani 1 d . . . Br1 Br 1.23222(6) 0.21101(6) 0.50006(4) 0.0765(3) Uani 1 d . . . Br2 Br 0.86984(7) 0.05910(6) 0.60367(3) 0.0656(2) Uani 1 d . . . O1 O 0.6799(3) 0.2387(3) 0.41110(18) 0.0407(10) Uani 1 d . . . O2 O 0.6039(3) 0.1803(3) 0.30816(18) 0.0436(10) Uani 1 d . . . O3 O 0.8617(3) 0.3272(3) 0.36188(19) 0.0386(9) Uani 1 d . . . O4 O 0.7785(3) 0.2672(3) 0.26008(18) 0.0415(10) Uani 1 d . . . O5 O 0.7412(4) 0.0631(3) 0.46105(19) 0.0476(11) Uani 1 d . . . O6 O 1.0488(3) 0.2081(3) 0.3723(2) 0.0496(11) Uani 1 d . . . O7 O 0.5435(3) 0.4081(3) 0.3839(2) 0.0453(11) Uani 1 d . . . O8 O 0.4616(3) 0.3522(3) 0.2801(2) 0.0474(11) Uani 1 d . . . O9 O 0.7247(3) 0.4994(3) 0.3344(2) 0.0442(10) Uani 1 d . . . O10 O 0.6436(3) 0.4430(3) 0.23110(19) 0.0450(10) Uani 1 d . . . C1 C 0.6452(5) 0.1709(4) 0.3702(3) 0.0378(14) Uani 1 d . . . C2 C 0.6507(5) 0.0685(4) 0.3992(3) 0.0431(15) Uani 1 d . . . C3 C 0.5398(6) 0.0497(5) 0.4218(3) 0.0604(19) Uani 1 d . . . H3A H 0.4746 0.0530 0.3840 0.073 Uiso 1 calc R . . H3B H 0.5315 0.0972 0.4541 0.073 Uiso 1 calc R . . H3C H 0.5433 -0.0130 0.4415 0.073 Uiso 1 calc R . . C4 C 0.6712(6) -0.0074(4) 0.3506(3) 0.0544(18) Uani 1 d . . . H4A H 0.6122 -0.0027 0.3098 0.065 Uiso 1 calc R . . H4B H 0.6684 -0.0699 0.3698 0.065 Uiso 1 calc R . . H4C H 0.7459 0.0023 0.3414 0.065 Uiso 1 calc R . . C5 C 0.8518(6) 0.0955(4) 0.4651(3) 0.0430(16) Uani 1 d . . . C6 C 0.8947(5) 0.1275(4) 0.4127(3) 0.0425(15) Uani 1 d . . . H6 H 0.8484 0.1224 0.3695 0.051 Uiso 1 calc R . . C7 C 1.0032(5) 0.1668(4) 0.4217(3) 0.0447(16) Uani 1 d . . . C8 C 1.0784(5) 0.1652(4) 0.4856(4) 0.0505(17) Uani 1 d . . . C9 C 1.0370(6) 0.1294(5) 0.5384(3) 0.0554(19) Uani 1 d . . . H9 H 1.0863 0.1269 0.5808 0.067 Uiso 1 calc R . . C10 C 0.9257(6) 0.0980(4) 0.5294(3) 0.0468(16) Uani 1 d . . . C11 C 0.9759(5) 0.2273(4) 0.3061(3) 0.0430(15) Uani 1 d . . . C12 C 0.9553(6) 0.1348(5) 0.2658(3) 0.0583(18) Uani 1 d . . . H12A H 0.9075 0.1478 0.2221 0.070 Uiso 1 calc R . . H12B H 0.9172 0.0890 0.2881 0.070 Uiso 1 calc R . . H12C H 1.0284 0.1090 0.2617 0.070 Uiso 1 calc R . . C13 C 1.0463(5) 0.2986(5) 0.2768(4) 0.062(2) Uani 1 d . . . H13A H 1.0041 0.3161 0.2326 0.074 Uiso 1 calc R . . H13B H 1.1189 0.2700 0.2747 0.074 Uiso 1 calc R . . H13C H 1.0604 0.3548 0.3045 0.074 Uiso 1 calc R . . C14 C 0.8629(5) 0.2770(4) 0.3108(3) 0.0382(14) Uani 1 d . . . C15 C 0.4559(6) 0.3921(5) 0.3355(4) 0.0512(17) Uani 1 d . . . C16 C 0.3394(6) 0.4206(6) 0.3444(4) 0.081(2) Uani 1 d . . . H16A H 0.2812 0.4038 0.3051 0.097 Uiso 1 calc R . . H16B H 0.3379 0.4887 0.3515 0.097 Uiso 1 calc R . . H16C H 0.3241 0.3877 0.3823 0.097 Uiso 1 calc R . . C17 C 0.6907(5) 0.5090(4) 0.2709(3) 0.0394(15) Uani 1 d . . . C18 C 0.7097(6) 0.6048(4) 0.2421(3) 0.0585(19) Uani 1 d . . . H18A H 0.6806 0.6033 0.1945 0.070 Uiso 1 calc R . . H18B H 0.7912 0.6191 0.2527 0.070 Uiso 1 calc R . . H18C H 0.6695 0.6535 0.2608 0.070 Uiso 1 calc R . . N1 N 0.8033(4) 0.4200(4) 0.4786(2) 0.0415(12) Uani 1 d . . . C19 C 0.8228(6) 0.5128(4) 0.4957(3) 0.0490(16) Uani 1 d . . . H19 H 0.7807 0.5598 0.4681 0.059 Uiso 1 calc R . . C20 C 0.9024(6) 0.5410(5) 0.5525(3) 0.0579(19) Uani 1 d . . . H20 H 0.9143 0.6059 0.5626 0.069 Uiso 1 calc R . . C21 C 0.9641(6) 0.4723(5) 0.5940(3) 0.063(2) Uani 1 d . . . H21 H 1.0177 0.4897 0.6330 0.075 Uiso 1 calc R . . C22 C 0.9448(6) 0.3775(5) 0.5769(3) 0.067(2) Uani 1 d . . . H22 H 0.9858 0.3294 0.6038 0.080 Uiso 1 calc R . . C23 C 0.8643(6) 0.3552(5) 0.5195(3) 0.0568(19) Uani 1 d . . . H23 H 0.8516 0.2907 0.5086 0.068 Uiso 1 calc R . . N2 N 0.5564(4) 0.2554(3) 0.1624(2) 0.0395(12) Uani 1 d . . . C24 C 0.4923(6) 0.1761(5) 0.1444(3) 0.0586(19) Uani 1 d . . . H24 H 0.4551 0.1492 0.1750 0.070 Uiso 1 calc R . . C25 C 0.4786(7) 0.1329(6) 0.0836(4) 0.076(2) Uani 1 d . . . H25 H 0.4328 0.0783 0.0730 0.091 Uiso 1 calc R . . C26 C 0.5337(7) 0.1717(6) 0.0387(4) 0.074(2) Uani 1 d . . . H26 H 0.5265 0.1431 -0.0028 0.089 Uiso 1 calc R . . C27 C 0.5982(7) 0.2513(6) 0.0547(4) 0.079(2) Uani 1 d . . . H27 H 0.6356 0.2791 0.0245 0.095 Uiso 1 calc R . . C28 C 0.6075(6) 0.2905(5) 0.1170(3) 0.0569(18) Uani 1 d . . . H28 H 0.6528 0.3453 0.1280 0.068 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 Rh1 0.0389(3) 0.0350(3) 0.0271(3) -0.0018(2) 0.0003(2) 0.0023(2) Rh2 0.0373(3) 0.0399(3) 0.0255(2) 0.0012(2) -0.0006(2) -0.0023(2) Br1 0.0557(5) 0.0641(5) 0.0889(6) 0.0106(5) -0.0239(4) -0.0038(4) Br2 0.0869(6) 0.0683(5) 0.0356(4) 0.0027(4) 0.0027(4) 0.0213(4) O1 0.050(3) 0.039(2) 0.029(2) -0.001(2) 0.0003(19) -0.001(2) O2 0.059(3) 0.042(2) 0.024(2) 0.0006(19) -0.0018(19) -0.006(2) O3 0.037(2) 0.039(2) 0.036(2) -0.006(2) -0.0001(18) -0.0004(18) O4 0.046(2) 0.047(2) 0.028(2) -0.008(2) 0.002(2) 0.004(2) O5 0.057(3) 0.045(3) 0.033(2) 0.009(2) -0.005(2) -0.001(2) O6 0.040(3) 0.052(3) 0.052(3) -0.003(2) 0.000(2) 0.008(2) O7 0.043(3) 0.054(3) 0.038(2) -0.001(2) 0.007(2) 0.008(2) O8 0.043(2) 0.058(3) 0.038(3) 0.003(2) 0.004(2) -0.003(2) O9 0.049(3) 0.035(2) 0.044(3) 0.001(2) 0.002(2) -0.0010(19) O10 0.052(3) 0.043(3) 0.035(2) 0.003(2) 0.001(2) -0.008(2) C1 0.038(3) 0.038(4) 0.036(4) -0.001(3) 0.006(3) -0.003(3) C2 0.053(4) 0.039(4) 0.032(3) 0.000(3) -0.002(3) -0.001(3) C3 0.067(5) 0.065(5) 0.048(4) 0.013(4) 0.010(4) -0.023(4) C4 0.073(5) 0.035(4) 0.053(4) -0.006(3) 0.011(4) 0.000(3) C5 0.055(4) 0.030(3) 0.037(4) -0.004(3) -0.003(3) 0.004(3) C6 0.045(4) 0.040(4) 0.036(4) -0.002(3) -0.003(3) 0.004(3) C7 0.048(4) 0.036(4) 0.045(4) -0.003(3) 0.002(3) 0.005(3) C8 0.043(4) 0.041(4) 0.060(5) -0.007(3) -0.002(3) 0.007(3) C9 0.070(5) 0.045(4) 0.037(4) -0.005(3) -0.015(3) 0.023(4) C10 0.067(5) 0.031(4) 0.036(4) -0.007(3) 0.000(3) 0.013(3) C11 0.041(4) 0.043(4) 0.043(4) -0.009(3) 0.007(3) 0.002(3) C12 0.054(4) 0.064(5) 0.056(4) -0.014(4) 0.011(3) 0.008(4) C13 0.040(4) 0.079(5) 0.071(5) 0.001(4) 0.022(4) 0.000(4) C14 0.036(3) 0.039(4) 0.038(4) 0.006(3) 0.006(3) -0.001(3) C15 0.039(4) 0.054(4) 0.061(5) 0.011(4) 0.014(4) 0.008(3) C16 0.052(5) 0.119(7) 0.072(6) -0.016(5) 0.012(4) 0.009(5) C17 0.033(3) 0.041(4) 0.044(4) 0.010(3) 0.007(3) 0.002(3) C18 0.065(5) 0.051(4) 0.060(5) 0.003(4) 0.014(4) -0.013(3) N1 0.048(3) 0.041(3) 0.033(3) -0.005(3) 0.006(2) 0.003(3) C19 0.062(4) 0.040(4) 0.038(4) -0.005(3) -0.002(3) 0.010(3) C20 0.081(5) 0.039(4) 0.048(4) -0.014(3) 0.003(4) -0.002(4) C21 0.074(5) 0.064(5) 0.038(4) -0.007(4) -0.011(4) -0.010(4) C22 0.089(5) 0.053(5) 0.043(4) -0.001(4) -0.016(4) 0.012(4) C23 0.085(5) 0.041(4) 0.033(4) 0.002(3) -0.009(4) 0.002(4) N2 0.040(3) 0.044(3) 0.034(3) 0.004(2) 0.009(2) -0.011(2) C24 0.061(5) 0.063(5) 0.048(4) 0.000(4) 0.004(3) -0.021(4) C25 0.090(6) 0.068(5) 0.061(5) -0.016(5) -0.003(4) -0.023(5) C26 0.100(6) 0.078(6) 0.036(4) -0.017(4) 0.000(4) 0.012(5) C27 0.106(7) 0.093(7) 0.040(5) -0.003(4) 0.022(4) -0.013(5) C28 0.076(5) 0.055(4) 0.039(4) 0.006(4) 0.012(4) -0.018(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 Rh1 O9 2.019(4) . ? Rh1 O7 2.027(4) . ? Rh1 O1 2.028(4) . ? Rh1 O3 2.044(4) . ? Rh1 Rh2 2.4085(8) . ? Rh2 O10 2.022(4) . ? Rh2 O8 2.024(4) . ? Rh2 O4 2.035(4) . ? Rh2 O2 2.042(4) . ? Br1 C8 1.889(6) . ? Br2 C10 1.886(7) . ? O1 C1 1.268(6) . ? O2 C1 1.262(7) . ? O3 C14 1.268(7) . ? O4 C14 1.271(7) . ? O5 C5 1.372(7) . ? O5 C2 1.460(7) . ? O6 C7 1.387(7) . ? O6 C11 1.456(7) . ? O7 C15 1.277(8) . ? O8 C15 1.286(8) . ? O9 C17 1.282(7) . ? O10 C17 1.269(7) . ? C1 C2 1.543(8) . ? C2 C4 1.516(8) . ? C2 C3 1.519(8) . ? C5 C6 1.375(8) . ? C5 C10 1.405(8) . ? C6 C7 1.370(8) . ? C7 C8 1.405(9) . ? C8 C9 1.391(9) . ? C9 C10 1.362(9) . ? C11 C13 1.511(8) . ? C11 C12 1.522(8) . ? C11 C14 1.532(8) . ? C15 C16 1.492(8) . ? C17 C18 1.500(8) . ? N1 C23 1.327(7) . ? N1 C19 1.346(7) . ? C19 C20 1.374(8) . ? C20 C21 1.374(9) . ? C21 C22 1.372(9) . ? C22 C23 1.368(9) . ? N2 C28 1.323(7) . ? N2 C24 1.342(8) . ? C24 C25 1.364(9) . ? C25 C26 1.365(10) . ? C26 C27 1.343(10) . ? C27 C28 1.376(9) . ? 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 O9 Rh1 O7 90.95(16) . . ? O9 Rh1 O1 175.69(16) . . ? O7 Rh1 O1 88.92(16) . . ? O9 Rh1 O3 90.12(15) . . ? O7 Rh1 O3 175.32(16) . . ? O1 Rh1 O3 89.67(15) . . ? O9 Rh1 Rh2 88.43(12) . . ? O7 Rh1 Rh2 87.65(12) . . ? O1 Rh1 Rh2 87.26(11) . . ? O3 Rh1 Rh2 87.82(11) . . ? O10 Rh2 O8 90.94(16) . . ? O10 Rh2 O4 91.58(16) . . ? O8 Rh2 O4 175.32(16) . . ? O10 Rh2 O2 175.00(16) . . ? O8 Rh2 O2 91.28(16) . . ? O4 Rh2 O2 85.90(16) . . ? O10 Rh2 Rh1 87.32(12) . . ? O8 Rh2 Rh1 88.32(12) . . ? O4 Rh2 Rh1 87.87(11) . . ? O2 Rh2 Rh1 88.26(11) . . ? C1 O1 Rh1 119.6(4) . . ? C1 O2 Rh2 118.2(4) . . ? C14 O3 Rh1 118.5(4) . . ? C14 O4 Rh2 119.0(4) . . ? C5 O5 C2 122.0(4) . . ? C7 O6 C11 121.1(5) . . ? C15 O7 Rh1 120.3(4) . . ? C15 O8 Rh2 119.5(4) . . ? C17 O9 Rh1 119.2(4) . . ? C17 O10 Rh2 120.5(4) . . ? O2 C1 O1 125.7(5) . . ? O2 C1 C2 117.4(5) . . ? O1 C1 C2 117.0(5) . . ? O5 C2 C4 109.9(5) . . ? O5 C2 C3 103.6(5) . . ? C4 C2 C3 111.7(5) . . ? O5 C2 C1 110.0(5) . . ? C4 C2 C1 112.8(5) . . ? C3 C2 C1 108.5(5) . . ? O5 C5 C6 126.0(5) . . ? O5 C5 C10 116.1(6) . . ? C6 C5 C10 117.9(6) . . ? C7 C6 C5 122.4(6) . . ? C6 C7 O6 125.8(6) . . ? C6 C7 C8 119.2(6) . . ? O6 C7 C8 115.0(6) . . ? C9 C8 C7 118.4(6) . . ? C9 C8 Br1 120.4(5) . . ? C7 C8 Br1 121.2(5) . . ? C10 C9 C8 121.5(6) . . ? C9 C10 C5 120.2(6) . . ? C9 C10 Br2 120.0(5) . . ? C5 C10 Br2 119.8(5) . . ? O6 C11 C13 103.5(5) . . ? O6 C11 C12 109.8(5) . . ? C13 C11 C12 111.7(5) . . ? O6 C11 C14 110.9(5) . . ? C13 C11 C14 107.7(5) . . ? C12 C11 C14 112.8(5) . . ? O3 C14 O4 125.4(5) . . ? O3 C14 C11 119.1(5) . . ? O4 C14 C11 115.5(5) . . ? O7 C15 O8 124.3(6) . . ? O7 C15 C16 117.6(6) . . ? O8 C15 C16 118.1(6) . . ? O10 C17 O9 124.6(5) . . ? O10 C17 C18 118.3(5) . . ? O9 C17 C18 117.2(6) . . ? C23 N1 C19 116.9(5) . . ? N1 C19 C20 122.6(6) . . ? C19 C20 C21 119.2(6) . . ? C22 C21 C20 118.6(6) . . ? C23 C22 C21 118.7(7) . . ? N1 C23 C22 124.0(6) . . ? C28 N2 C24 115.7(5) . . ? N2 C24 C25 123.5(7) . . ? C24 C25 C26 118.5(7) . . ? C27 C26 C25 119.8(7) . . ? C26 C27 C28 118.1(7) . . ? N2 C28 C27 124.4(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Rh1 Rh2 O10 0.27(16) . . . . ? O7 Rh1 Rh2 O10 91.28(16) . . . . ? O1 Rh1 Rh2 O10 -179.69(16) . . . . ? O3 Rh1 Rh2 O10 -89.92(15) . . . . ? O9 Rh1 Rh2 O8 -90.75(16) . . . . ? O7 Rh1 Rh2 O8 0.26(17) . . . . ? O1 Rh1 Rh2 O8 89.29(16) . . . . ? O3 Rh1 Rh2 O8 179.07(16) . . . . ? O9 Rh1 Rh2 O4 91.95(16) . . . . ? O7 Rh1 Rh2 O4 -177.03(16) . . . . ? O1 Rh1 Rh2 O4 -88.01(16) . . . . ? O3 Rh1 Rh2 O4 1.77(16) . . . . ? O9 Rh1 Rh2 O2 177.91(16) . . . . ? O7 Rh1 Rh2 O2 -91.07(16) . . . . ? O1 Rh1 Rh2 O2 -2.04(16) . . . . ? O3 Rh1 Rh2 O2 87.73(15) . . . . ? O9 Rh1 O1 C1 7(2) . . . . ? O7 Rh1 O1 C1 95.7(4) . . . . ? O3 Rh1 O1 C1 -79.8(4) . . . . ? Rh2 Rh1 O1 C1 8.0(4) . . . . ? O10 Rh2 O2 C1 25(2) . . . . ? O8 Rh2 O2 C1 -91.4(4) . . . . ? O4 Rh2 O2 C1 84.9(4) . . . . ? Rh1 Rh2 O2 C1 -3.1(4) . . . . ? O9 Rh1 O3 C14 -97.0(4) . . . . ? O7 Rh1 O3 C14 6(2) . . . . ? O1 Rh1 O3 C14 78.7(4) . . . . ? Rh2 Rh1 O3 C14 -8.6(4) . . . . ? O10 Rh2 O4 C14 91.7(4) . . . . ? O8 Rh2 O4 C14 -31(2) . . . . ? O2 Rh2 O4 C14 -84.0(4) . . . . ? Rh1 Rh2 O4 C14 4.4(4) . . . . ? O9 Rh1 O7 C15 87.9(5) . . . . ? O1 Rh1 O7 C15 -87.8(5) . . . . ? O3 Rh1 O7 C15 -15(2) . . . . ? Rh2 Rh1 O7 C15 -0.5(4) . . . . ? O10 Rh2 O8 C15 -87.4(5) . . . . ? O4 Rh2 O8 C15 35(2) . . . . ? O2 Rh2 O8 C15 88.1(5) . . . . ? Rh1 Rh2 O8 C15 -0.1(4) . . . . ? O7 Rh1 O9 C17 -88.1(4) . . . . ? O1 Rh1 O9 C17 0(2) . . . . ? O3 Rh1 O9 C17 87.3(4) . . . . ? Rh2 Rh1 O9 C17 -0.5(4) . . . . ? O8 Rh2 O10 C17 88.2(4) . . . . ? O4 Rh2 O10 C17 -87.9(4) . . . . ? O2 Rh2 O10 C17 -28(2) . . . . ? Rh1 Rh2 O10 C17 -0.1(4) . . . . ? Rh2 O2 C1 O1 10.9(8) . . . . ? Rh2 O2 C1 C2 -171.0(4) . . . . ? Rh1 O1 C1 O2 -13.5(8) . . . . ? Rh1 O1 C1 C2 168.3(4) . . . . ? C5 O5 C2 C4 74.5(6) . . . . ? C5 O5 C2 C3 -166.0(5) . . . . ? C5 O5 C2 C1 -50.2(7) . . . . ? O2 C1 C2 O5 155.5(5) . . . . ? O1 C1 C2 O5 -26.1(7) . . . . ? O2 C1 C2 C4 32.5(7) . . . . ? O1 C1 C2 C4 -149.2(5) . . . . ? O2 C1 C2 C3 -91.8(6) . . . . ? O1 C1 C2 C3 86.5(6) . . . . ? C2 O5 C5 C6 -6.6(9) . . . . ? C2 O5 C5 C10 171.7(5) . . . . ? O5 C5 C6 C7 174.1(5) . . . . ? C10 C5 C6 C7 -4.2(9) . . . . ? C5 C6 C7 O6 -174.1(5) . . . . ? C5 C6 C7 C8 7.0(9) . . . . ? C11 O6 C7 C6 10.0(9) . . . . ? C11 O6 C7 C8 -171.0(5) . . . . ? C6 C7 C8 C9 -4.2(9) . . . . ? O6 C7 C8 C9 176.7(5) . . . . ? C6 C7 C8 Br1 176.1(4) . . . . ? O6 C7 C8 Br1 -3.0(7) . . . . ? C7 C8 C9 C10 -1.2(9) . . . . ? Br1 C8 C9 C10 178.6(5) . . . . ? C8 C9 C10 C5 3.9(9) . . . . ? C8 C9 C10 Br2 -175.2(5) . . . . ? O5 C5 C10 C9 -179.8(5) . . . . ? C6 C5 C10 C9 -1.3(9) . . . . ? O5 C5 C10 Br2 -0.6(7) . . . . ? C6 C5 C10 Br2 177.8(4) . . . . ? C7 O6 C11 C13 162.4(5) . . . . ? C7 O6 C11 C12 -78.1(6) . . . . ? C7 O6 C11 C14 47.2(7) . . . . ? Rh1 O3 C14 O4 15.4(7) . . . . ? Rh1 O3 C14 C11 -168.3(4) . . . . ? Rh2 O4 C14 O3 -13.3(8) . . . . ? Rh2 O4 C14 C11 170.3(4) . . . . ? O6 C11 C14 O3 26.8(7) . . . . ? C13 C11 C14 O3 -85.8(7) . . . . ? C12 C11 C14 O3 150.4(5) . . . . ? O6 C11 C14 O4 -156.5(5) . . . . ? C13 C11 C14 O4 90.9(6) . . . . ? C12 C11 C14 O4 -32.9(7) . . . . ? Rh1 O7 C15 O8 0.5(9) . . . . ? Rh1 O7 C15 C16 179.8(5) . . . . ? Rh2 O8 C15 O7 -0.2(8) . . . . ? Rh2 O8 C15 C16 -179.4(5) . . . . ? Rh2 O10 C17 O9 -0.3(8) . . . . ? Rh2 O10 C17 C18 178.9(4) . . . . ? Rh1 O9 C17 O10 0.6(7) . . . . ? Rh1 O9 C17 C18 -178.6(4) . . . . ? C23 N1 C19 C20 0.5(9) . . . . ? N1 C19 C20 C21 -0.7(10) . . . . ? C19 C20 C21 C22 0.7(11) . . . . ? C20 C21 C22 C23 -0.6(11) . . . . ? C19 N1 C23 C22 -0.4(10) . . . . ? C21 C22 C23 N1 0.4(11) . . . . ? C28 N2 C24 C25 -0.2(10) . . . . ? N2 C24 C25 C26 0.5(12) . . . . ? C24 C25 C26 C27 -0.8(13) . . . . ? C25 C26 C27 C28 0.8(13) . . . . ? C24 N2 C28 C27 0.2(10) . . . . ? C26 C27 C28 N2 -0.5(13) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 24.18 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.452 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.100 data_tmcg12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 Br4 N2 O12 Rh2' _chemical_formula_weight 1352.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.3740 2.4560 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1607(18) _cell_length_b 9.3522(9) _cell_length_c 19.047(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.727(14) _cell_angle_gamma 90.00 _cell_volume 2669.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 3.537 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13920 _diffrn_reflns_av_R_equivalents 0.1378 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3477 _reflns_number_gt 2540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^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 3477 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.44914(4) 0.56137(7) 0.03245(3) 0.0304(3) Uani 1 d . . . Br2 Br 0.06071(9) 0.69019(18) -0.17280(10) 0.1139(7) Uani 1 d . . . Br3 Br 0.06450(9) 0.2258(2) 0.01387(11) 0.1269(8) Uani 1 d . . . O1 O 0.5291(3) 0.5011(7) 0.1234(3) 0.0392(13) Uani 1 d . . . O2 O 0.3775(3) 0.6187(6) -0.0630(3) 0.0363(13) Uani 1 d . . . O3 O 0.5288(4) 0.7373(6) 0.0342(3) 0.0419(14) Uani 1 d . . . O4 O 0.3789(3) 0.3752(6) 0.0294(3) 0.0378(13) Uani 1 d . . . O5 O 0.2461(4) 0.1873(7) -0.0200(4) 0.0576(17) Uani 1 d . . . O6 O 0.2452(4) 0.5975(7) -0.1787(3) 0.0488(16) Uani 1 d . . . C1 C 0.5995(6) 0.4340(9) 0.1183(4) 0.038(2) Uani 1 d . . . C2 C 0.6617(5) 0.4059(9) 0.1890(4) 0.041(2) Uani 1 d . . . C3 C 0.6437(6) 0.2596(11) 0.2139(5) 0.056(3) Uani 1 d . . . H3 H 0.6823 0.2406 0.2584 0.067 Uiso 1 calc R . . H3 H 0.6554 0.1902 0.1786 0.067 Uiso 1 calc R . . H3 H 0.5819 0.2527 0.2210 0.067 Uiso 1 calc R . . C4 C 0.6491(6) 0.5181(12) 0.2444(5) 0.057(3) Uani 1 d . . . H4 H 0.6889 0.4976 0.2882 0.068 Uiso 1 calc R . . H4 H 0.5878 0.5163 0.2534 0.068 Uiso 1 calc R . . H4 H 0.6627 0.6119 0.2272 0.068 Uiso 1 calc R . . C5 C 0.4001(5) 0.2732(9) -0.0069(4) 0.037(2) Uani 1 d . . . C6 C 0.3382(6) 0.1430(10) -0.0174(5) 0.046(2) Uani 1 d . . . C7 C 0.3472(7) 0.0585(12) -0.0837(7) 0.074(3) Uani 1 d . . . H7 H 0.4086 0.0283 -0.0821 0.088 Uiso 1 calc R . . H7 H 0.3298 0.1179 -0.1252 0.088 Uiso 1 calc R . . H7 H 0.3088 -0.0250 -0.0862 0.088 Uiso 1 calc R . . C8 C 0.3559(7) 0.0522(11) 0.0486(6) 0.069(3) Uani 1 d . . . H8 H 0.4168 0.0172 0.0545 0.083 Uiso 1 calc R . . H8 H 0.3150 -0.0282 0.0441 0.083 Uiso 1 calc R . . H8 H 0.3473 0.1091 0.0896 0.083 Uiso 1 calc R . . C9 C 0.2095(6) 0.2996(10) -0.0581(5) 0.049(2) Uani 1 d . . . C29 C 0.2494(6) 0.3829(10) -0.1063(5) 0.045(2) Uani 1 d . . . H29 H 0.3056 0.3563 -0.1172 0.054 Uiso 1 calc R . . C11 C 0.2078(6) 0.5026(11) -0.1377(4) 0.046(2) Uani 1 d . . . C12 C 0.1208(6) 0.5344(12) -0.1276(6) 0.064(3) Uani 1 d . . . C28 C 0.0797(7) 0.4471(14) -0.0841(7) 0.080(4) Uani 1 d . . . H28 H 0.0202 0.4664 -0.0787 0.096 Uiso 1 calc R . . C14 C 0.1218(6) 0.3339(12) -0.0486(6) 0.068(3) Uani 1 d . . . N1 N 0.3537(4) 0.6690(7) 0.0918(4) 0.0381(16) Uani 1 d . . . C27 C 0.2642(6) 0.6645(11) 0.0695(5) 0.053(2) Uani 1 d . . . H27 H 0.2432 0.6231 0.0252 0.063 Uiso 1 calc R . . C26 C 0.2038(7) 0.7175(12) 0.1089(6) 0.065(3) Uani 1 d . . . H26 H 0.1427 0.7118 0.0907 0.078 Uiso 1 calc R . . C17 C 0.2290(7) 0.7784(11) 0.1738(6) 0.060(3) Uani 1 d . . . C18 C 0.1627(9) 0.8333(16) 0.2194(9) 0.098(5) Uani 1 d . . . C19 C 0.1171(14) 0.961(2) 0.1836(11) 0.171(10) Uani 1 d . . . H19 H 0.0744 0.9982 0.2121 0.205 Uiso 1 calc R . . H19 H 0.0862 0.9340 0.1372 0.205 Uiso 1 calc R . . H19 H 0.1610 1.0341 0.1783 0.205 Uiso 1 calc R . . C20 C 0.1031(12) 0.708(2) 0.2324(12) 0.162(9) Uani 1 d . . . H20 H 0.0595 0.7387 0.2616 0.194 Uiso 1 calc R . . H20 H 0.1394 0.6318 0.2566 0.194 Uiso 1 calc R . . H20 H 0.0725 0.6724 0.1873 0.194 Uiso 1 calc R . . C21 C 0.2061(12) 0.8752(19) 0.2931(9) 0.126(6) Uani 1 d . . . H21A H 0.1609 0.9098 0.3199 0.151 Uiso 1 calc R . . H21B H 0.2496 0.9501 0.2899 0.151 Uiso 1 calc R . . H21C H 0.2357 0.7926 0.3169 0.151 Uiso 1 calc R . . C24 C 0.3217(7) 0.7882(11) 0.1967(6) 0.059(3) Uani 1 d . . . H24 H 0.3440 0.8315 0.2404 0.071 Uiso 1 calc R . . C25 C 0.3797(6) 0.7327(10) 0.1535(5) 0.047(2) Uani 1 d . . . H25 H 0.4413 0.7410 0.1691 0.057 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0199(4) 0.0388(4) 0.0332(4) -0.0016(3) 0.0062(2) 0.0029(3) Br2 0.0546(8) 0.1359(13) 0.1592(14) 0.0892(11) 0.0425(8) 0.0404(8) Br3 0.0581(9) 0.1466(15) 0.1881(18) 0.1018(14) 0.0577(9) 0.0217(8) O1 0.019(3) 0.059(4) 0.040(3) -0.003(3) 0.004(2) 0.012(3) O2 0.019(3) 0.053(3) 0.038(3) -0.001(3) 0.006(2) 0.006(2) O3 0.025(3) 0.048(4) 0.053(4) -0.008(3) 0.008(3) -0.002(3) O4 0.029(3) 0.043(3) 0.045(3) -0.002(3) 0.016(2) 0.002(3) O5 0.029(3) 0.056(4) 0.087(5) 0.016(4) 0.008(3) -0.007(3) O6 0.023(3) 0.068(4) 0.054(4) 0.017(3) 0.003(3) 0.004(3) C1 0.031(5) 0.042(5) 0.042(5) 0.003(4) 0.006(4) -0.008(4) C2 0.022(4) 0.057(6) 0.044(5) 0.001(4) 0.006(3) 0.007(4) C3 0.037(5) 0.076(7) 0.054(6) 0.020(5) 0.004(4) 0.006(5) C4 0.040(5) 0.086(7) 0.040(5) -0.013(5) -0.006(4) -0.001(5) C5 0.023(5) 0.045(5) 0.044(5) 0.001(4) 0.003(4) 0.000(4) C6 0.026(5) 0.045(5) 0.068(6) 0.003(5) 0.007(4) -0.003(4) C7 0.047(6) 0.066(7) 0.106(9) -0.035(7) 0.004(6) -0.012(5) C8 0.055(7) 0.058(6) 0.093(8) 0.023(6) 0.006(6) -0.004(5) C9 0.033(5) 0.050(6) 0.063(6) 0.009(5) 0.005(4) -0.003(4) C29 0.026(5) 0.053(5) 0.054(5) 0.002(5) 0.000(4) 0.003(4) C11 0.036(5) 0.064(6) 0.035(5) 0.002(5) -0.002(4) -0.007(5) C12 0.029(5) 0.084(8) 0.080(7) 0.022(6) 0.013(5) 0.008(5) C28 0.020(5) 0.105(9) 0.115(10) 0.029(8) 0.014(5) 0.002(6) C14 0.035(6) 0.073(8) 0.100(8) 0.036(7) 0.019(5) 0.005(5) N1 0.035(4) 0.038(4) 0.042(4) 0.002(3) 0.009(3) -0.001(3) C27 0.043(6) 0.061(6) 0.054(6) -0.006(5) 0.005(4) 0.000(5) C26 0.026(5) 0.084(8) 0.089(8) -0.008(6) 0.022(5) 0.010(5) C17 0.055(7) 0.058(7) 0.074(7) -0.008(6) 0.038(5) 0.005(5) C18 0.074(9) 0.101(11) 0.134(12) -0.042(9) 0.064(9) -0.001(8) C19 0.17(2) 0.21(2) 0.154(17) -0.008(15) 0.061(15) 0.126(18) C20 0.105(13) 0.20(2) 0.21(2) -0.073(16) 0.125(14) -0.047(13) C21 0.139(15) 0.139(14) 0.120(12) -0.044(11) 0.086(11) 0.027(12) C24 0.054(7) 0.067(7) 0.061(6) -0.015(5) 0.026(5) -0.002(5) C25 0.035(5) 0.054(6) 0.055(6) -0.011(5) 0.014(4) -0.001(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 Rh1 O1 2.036(5) . ? Rh1 O4 2.037(6) . ? Rh1 O3 2.038(6) . ? Rh1 O2 2.043(5) . ? Rh1 Rh1 2.4087(12) 3_665 ? Br2 C12 1.859(10) . ? Br3 C14 1.872(10) . ? O1 C1 1.255(10) . ? O2 C1 1.259(10) 3_665 ? O3 C5 1.270(10) 3_665 ? O4 C5 1.248(10) . ? O5 C9 1.347(11) . ? O5 C6 1.450(11) . ? O6 C11 1.361(11) . ? O6 C2 1.454(10) 3_665 ? C1 O2 1.259(10) 3_665 ? C1 C2 1.545(12) . ? C2 O6 1.454(10) 3_665 ? C2 C3 1.487(13) . ? C2 C4 1.521(13) . ? C5 O3 1.270(10) 3_665 ? C5 C6 1.532(12) . ? C6 C8 1.507(14) . ? C6 C7 1.513(14) . ? C9 C14 1.406(14) . ? C9 C29 1.410(13) . ? C29 C11 1.376(13) . ? C11 C12 1.393(14) . ? C12 C28 1.379(15) . ? C28 C14 1.361(15) . ? N1 C25 1.323(11) . ? N1 C27 1.359(11) . ? C27 C26 1.363(14) . ? C26 C17 1.362(15) . ? C17 C24 1.410(14) . ? C17 C18 1.514(15) . ? C18 C19 1.49(2) . ? C18 C21 1.51(2) . ? C18 C20 1.53(2) . ? C24 C25 1.393(14) . ? 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 Rh1 O4 91.7(2) . . ? O1 Rh1 O3 86.3(2) . . ? O4 Rh1 O3 175.0(2) . . ? O1 Rh1 O2 175.4(2) . . ? O4 Rh1 O2 89.6(2) . . ? O3 Rh1 O2 92.1(2) . . ? O1 Rh1 Rh1 87.70(15) . 3_665 ? O4 Rh1 Rh1 87.17(15) . 3_665 ? O3 Rh1 Rh1 88.24(16) . 3_665 ? O2 Rh1 Rh1 87.93(15) . 3_665 ? C1 O1 Rh1 118.4(5) . . ? C1 O2 Rh1 117.6(5) 3_665 . ? C5 O3 Rh1 117.9(5) 3_665 . ? C5 O4 Rh1 119.4(5) . . ? C9 O5 C6 123.8(7) . . ? C11 O6 C2 124.1(7) . 3_665 ? O1 C1 O2 127.4(7) . 3_665 ? O1 C1 C2 115.6(7) . . ? O2 C1 C2 116.9(7) 3_665 . ? O6 C2 C3 104.5(7) 3_665 . ? O6 C2 C4 109.5(7) 3_665 . ? C3 C2 C4 111.4(8) . . ? O6 C2 C1 111.3(7) 3_665 . ? C3 C2 C1 108.5(7) . . ? C4 C2 C1 111.4(7) . . ? O4 C5 O3 126.3(7) . 3_665 ? O4 C5 C6 118.4(7) . . ? O3 C5 C6 115.2(7) 3_665 . ? O5 C6 C8 103.8(8) . . ? O5 C6 C7 109.2(8) . . ? C8 C6 C7 111.9(9) . . ? O5 C6 C5 110.2(7) . . ? C8 C6 C5 108.1(8) . . ? C7 C6 C5 113.2(8) . . ? O5 C9 C14 115.4(8) . . ? O5 C9 C29 126.8(8) . . ? C14 C9 C29 117.8(8) . . ? C11 C29 C9 121.3(8) . . ? O6 C11 C29 125.2(8) . . ? O6 C11 C12 115.2(8) . . ? C29 C11 C12 119.6(9) . . ? C28 C12 C11 118.8(9) . . ? C28 C12 Br2 120.5(8) . . ? C11 C12 Br2 120.7(8) . . ? C14 C28 C12 122.6(10) . . ? C28 C14 C9 119.7(9) . . ? C28 C14 Br3 120.5(8) . . ? C9 C14 Br3 119.8(7) . . ? C25 N1 C27 116.0(7) . . ? N1 C27 C26 122.7(9) . . ? C17 C26 C27 122.1(10) . . ? C26 C17 C24 115.9(9) . . ? C26 C17 C18 122.9(11) . . ? C24 C17 C18 121.1(11) . . ? C19 C18 C21 108.9(14) . . ? C19 C18 C17 108.1(13) . . ? C21 C18 C17 112.9(12) . . ? C19 C18 C20 116.5(17) . . ? C21 C18 C20 103.6(15) . . ? C17 C18 C20 107.0(11) . . ? C25 C24 C17 118.8(9) . . ? N1 C25 C24 124.3(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Rh1 O1 C1 90.3(6) . . . . ? O3 Rh1 O1 C1 -85.2(6) . . . . ? O2 Rh1 O1 C1 -16(3) . . . . ? Rh1 Rh1 O1 C1 3.2(6) 3_665 . . . ? O1 Rh1 O2 C1 25(3) . . . 3_665 ? O4 Rh1 O2 C1 -80.6(6) . . . 3_665 ? O3 Rh1 O2 C1 94.8(6) . . . 3_665 ? Rh1 Rh1 O2 C1 6.6(6) 3_665 . . 3_665 ? O1 Rh1 O3 C5 85.1(6) . . . 3_665 ? O4 Rh1 O3 C5 20(3) . . . 3_665 ? O2 Rh1 O3 C5 -90.6(6) . . . 3_665 ? Rh1 Rh1 O3 C5 -2.7(6) 3_665 . . 3_665 ? O1 Rh1 O4 C5 -94.9(6) . . . . ? O3 Rh1 O4 C5 -30(3) . . . . ? O2 Rh1 O4 C5 80.6(6) . . . . ? Rh1 Rh1 O4 C5 -7.3(5) 3_665 . . . ? Rh1 O1 C1 O2 -10.2(12) . . . 3_665 ? Rh1 O1 C1 C2 173.7(5) . . . . ? O1 C1 C2 O6 -148.8(7) . . . 3_665 ? O2 C1 C2 O6 34.7(10) 3_665 . . 3_665 ? O1 C1 C2 C3 96.7(9) . . . . ? O2 C1 C2 C3 -79.8(9) 3_665 . . . ? O1 C1 C2 C4 -26.3(11) . . . . ? O2 C1 C2 C4 157.2(8) 3_665 . . . ? Rh1 O4 C5 O3 12.4(11) . . . 3_665 ? Rh1 O4 C5 C6 -171.0(5) . . . . ? C9 O5 C6 C8 161.0(8) . . . . ? C9 O5 C6 C7 -79.5(11) . . . . ? C9 O5 C6 C5 45.4(11) . . . . ? O4 C5 C6 O5 33.2(10) . . . . ? O3 C5 C6 O5 -149.8(7) 3_665 . . . ? O4 C5 C6 C8 -79.6(10) . . . . ? O3 C5 C6 C8 97.3(9) 3_665 . . . ? O4 C5 C6 C7 155.8(8) . . . . ? O3 C5 C6 C7 -27.3(11) 3_665 . . . ? C6 O5 C9 C14 -174.2(9) . . . . ? C6 O5 C9 C29 6.7(14) . . . . ? O5 C9 C29 C11 -174.6(9) . . . . ? C14 C9 C29 C11 6.3(14) . . . . ? C2 O6 C11 C29 -6.9(13) 3_665 . . . ? C2 O6 C11 C12 172.3(8) 3_665 . . . ? C9 C29 C11 O6 172.6(8) . . . . ? C9 C29 C11 C12 -6.6(14) . . . . ? O6 C11 C12 C28 -177.1(10) . . . . ? C29 C11 C12 C28 2.2(16) . . . . ? O6 C11 C12 Br2 3.7(13) . . . . ? C29 C11 C12 Br2 -177.0(7) . . . . ? C11 C12 C28 C14 2(2) . . . . ? Br2 C12 C28 C14 -178.4(10) . . . . ? C12 C28 C14 C9 -3(2) . . . . ? C12 C28 C14 Br3 176.4(10) . . . . ? O5 C9 C14 C28 179.1(10) . . . . ? C29 C9 C14 C28 -1.7(17) . . . . ? O5 C9 C14 Br3 0.1(14) . . . . ? C29 C9 C14 Br3 179.3(7) . . . . ? C25 N1 C27 C26 -2.2(14) . . . . ? N1 C27 C26 C17 -0.3(17) . . . . ? C27 C26 C17 C24 2.3(17) . . . . ? C27 C26 C17 C18 -177.9(12) . . . . ? C26 C17 C18 C19 -68.3(18) . . . . ? C24 C17 C18 C19 111.6(16) . . . . ? C26 C17 C18 C21 171.3(12) . . . . ? C24 C17 C18 C21 -8.9(18) . . . . ? C26 C17 C18 C20 58.0(19) . . . . ? C24 C17 C18 C20 -122.2(15) . . . . ? C26 C17 C24 C25 -1.8(15) . . . . ? C18 C17 C24 C25 178.4(11) . . . . ? C27 N1 C25 C24 2.7(13) . . . . ? C17 C24 C25 N1 -0.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.420 _refine_diff_density_min -2.012 _refine_diff_density_rms 0.185 data_tmcg18 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H64 N2 O10 Rh2' _chemical_formula_weight 986.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2589(7) _cell_length_b 18.9042(16) _cell_length_c 27.476(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.132(10) _cell_angle_gamma 90.00 _cell_volume 4772.0(7) _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 'prims' _exptl_crystal_colour 'red' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30124 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.13 _reflns_number_total 7490 _reflns_number_gt 5518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^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 SHELXL _refine_ls_extinction_coef 0.00110(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7490 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7401(7) 0.6103(3) 0.43378(19) 0.0581(14) Uani 1 d . . . C2 C 0.6011(8) 0.5726(4) 0.4442(3) 0.094(2) Uani 1 d . . . H2A H 0.6144 0.5223 0.4422 0.113 Uiso 1 calc R . . H2B H 0.5216 0.5869 0.4205 0.113 Uiso 1 calc R . . H2C H 0.5801 0.5848 0.4765 0.113 Uiso 1 calc R . . C3 C 1.0952(6) 0.6743(3) 0.50223(16) 0.0536(12) Uani 1 d . . . C4 C 1.1820(8) 0.6774(4) 0.5519(2) 0.087(2) Uani 1 d . . . H4A H 1.2411 0.6357 0.5570 0.104 Uiso 1 calc R . . H4B H 1.1172 0.6799 0.5765 0.104 Uiso 1 calc R . . H4C H 1.2434 0.7185 0.5540 0.104 Uiso 1 calc R . . C5 C 1.1976(5) 0.7376(2) 0.38533(15) 0.0417(10) Uani 1 d . . . C6 C 1.3239(5) 0.7748(2) 0.36479(17) 0.0474(11) Uani 1 d . . . C7 C 1.3944(7) 0.7314(3) 0.3276(2) 0.0714(16) Uani 1 d . . . H7A H 1.4225 0.6861 0.3414 0.086 Uiso 1 calc R . . H7B H 1.4789 0.7557 0.3192 0.086 Uiso 1 calc R . . H7C H 1.3262 0.7250 0.2986 0.086 Uiso 1 calc R . . C8 C 1.4368(6) 0.7938(3) 0.4087(2) 0.0714(16) Uani 1 d . . . H8A H 1.4730 0.7512 0.4249 0.086 Uiso 1 calc R . . H8B H 1.3920 0.8228 0.4313 0.086 Uiso 1 calc R . . H8C H 1.5160 0.8191 0.3974 0.086 Uiso 1 calc R . . C9 C 1.1571(5) 0.8543(2) 0.31244(15) 0.0404(10) Uani 1 d . . . C10 C 1.1223(5) 0.9254(2) 0.30073(16) 0.0432(10) Uani 1 d . . . C11 C 1.2158(6) 0.9881(2) 0.3224(2) 0.0558(13) Uani 1 d . . . C12 C 1.2211(7) 0.9899(3) 0.3781(2) 0.0781(18) Uani 1 d . . . H12A H 1.2804 1.0288 0.3910 0.094 Uiso 1 calc R . . H12B H 1.2618 0.9464 0.3916 0.094 Uiso 1 calc R . . H12C H 1.1243 0.9955 0.3866 0.094 Uiso 1 calc R . . C13 C 1.1557(8) 1.0587(3) 0.3022(3) 0.093(2) Uani 1 d . . . H13A H 1.2170 1.0964 0.3162 0.112 Uiso 1 calc R . . H13B H 1.0589 1.0652 0.3106 0.112 Uiso 1 calc R . . H13C H 1.1533 1.0591 0.2672 0.112 Uiso 1 calc R . . C14 C 1.3712(7) 0.9812(3) 0.3086(2) 0.0803(18) Uani 1 d . . . H14A H 1.4290 1.0203 0.3221 0.096 Uiso 1 calc R . . H14B H 1.3679 0.9813 0.2736 0.096 Uiso 1 calc R . . H14C H 1.4136 0.9377 0.3215 0.096 Uiso 1 calc R . . C15 C 0.9936(6) 0.9355(2) 0.27026(16) 0.0484(12) Uani 1 d . . . H15 H 0.9700 0.9819 0.2613 0.058 Uiso 1 calc R . . C16 C 0.8950(6) 0.8833(2) 0.25156(16) 0.0464(11) Uani 1 d . . . C17 C 0.7500(7) 0.9013(3) 0.2219(2) 0.0741(18) Uani 1 d . . . C18 C 0.7217(12) 0.9771(4) 0.2179(5) 0.210(8) Uani 1 d . . . H18A H 0.6292 0.9850 0.1987 0.252 Uiso 1 calc R . . H18B H 0.7969 0.9995 0.2024 0.252 Uiso 1 calc R . . H18C H 0.7203 0.9967 0.2501 0.252 Uiso 1 calc R . . C19 C 0.6231(9) 0.8743(5) 0.2511(3) 0.117(3) Uani 1 d . . . H19A H 0.5306 0.8853 0.2328 0.141 Uiso 1 calc R . . H19B H 0.6305 0.8973 0.2825 0.141 Uiso 1 calc R . . H19C H 0.6313 0.8241 0.2557 0.141 Uiso 1 calc R . . C20 C 0.7218(9) 0.8642(4) 0.1741(2) 0.096(2) Uani 1 d . . . H20A H 0.6288 0.8784 0.1577 0.116 Uiso 1 calc R . . H20B H 0.7219 0.8140 0.1796 0.116 Uiso 1 calc R . . H20C H 0.7965 0.8761 0.1542 0.116 Uiso 1 calc R . . C21 C 0.9374(5) 0.8141(2) 0.26454(14) 0.0394(10) Uani 1 d . . . C22 C 1.0677(5) 0.8005(2) 0.29274(15) 0.0405(10) Uani 1 d . . . H22 H 1.0963 0.7538 0.2987 0.049 Uiso 1 calc R . . C23 C 0.8479(5) 0.6895(2) 0.26288(15) 0.0422(10) Uani 1 d . . . C24 C 0.6929(6) 0.6630(3) 0.24746(19) 0.0593(14) Uani 1 d . . . H24A H 0.6866 0.6139 0.2557 0.071 Uiso 1 calc R . . H24B H 0.6686 0.6690 0.2127 0.071 Uiso 1 calc R . . H24C H 0.6261 0.6897 0.2643 0.071 Uiso 1 calc R . . C25 C 0.9578(6) 0.6509(3) 0.23590(18) 0.0555(12) Uani 1 d . . . H25A H 0.9644 0.6024 0.2464 0.067 Uiso 1 calc R . . H25B H 1.0513 0.6730 0.2430 0.067 Uiso 1 calc R . . H25C H 0.9272 0.6527 0.2012 0.067 Uiso 1 calc R . . C26 C 0.8789(5) 0.6818(2) 0.31866(15) 0.0387(10) Uani 1 d . . . C27 C 1.1838(6) 0.4914(3) 0.35682(19) 0.0596(13) Uani 1 d . . . H27 H 1.1913 0.5248 0.3324 0.072 Uiso 1 calc R . . C28 C 1.2335(6) 0.4250(3) 0.34992(19) 0.0604(14) Uani 1 d . . . H28 H 1.2716 0.4140 0.3211 0.073 Uiso 1 calc R . . C29 C 1.2279(6) 0.3730(3) 0.38569(19) 0.0530(12) Uani 1 d . . . C30 C 1.1691(6) 0.3946(3) 0.42694(19) 0.0613(14) Uani 1 d . . . H30 H 1.1619 0.3626 0.4523 0.074 Uiso 1 calc R . . C31 C 1.1207(7) 0.4630(3) 0.43100(19) 0.0630(15) Uani 1 d . . . H31 H 1.0829 0.4761 0.4595 0.076 Uiso 1 calc R . . C32 C 1.2772(7) 0.2973(3) 0.3791(2) 0.0765(17) Uiso 1 d . . . C33 C 1.321(2) 0.2801(10) 0.3317(7) 0.141(7) Uiso 0.555(11) d P A 1 H33A H 1.3505 0.2315 0.3315 0.212 Uiso 0.555(11) calc PR A 1 H33B H 1.4001 0.3099 0.3254 0.212 Uiso 0.555(11) calc PR A 1 H33C H 1.2399 0.2874 0.3067 0.212 Uiso 0.555(11) calc PR A 1 C34 C 1.1559(14) 0.2451(6) 0.3896(4) 0.081(4) Uiso 0.555(11) d P A 1 H34A H 1.1291 0.2542 0.4216 0.122 Uiso 0.555(11) calc PR A 1 H34B H 1.1910 0.1975 0.3881 0.122 Uiso 0.555(11) calc PR A 1 H34C H 1.0725 0.2514 0.3655 0.122 Uiso 0.555(11) calc PR A 1 C35 C 1.398(2) 0.2799(10) 0.4235(6) 0.136(7) Uiso 0.555(11) d P A 1 H35A H 1.3633 0.2936 0.4536 0.204 Uiso 0.555(11) calc PR A 1 H35B H 1.4850 0.3055 0.4196 0.204 Uiso 0.555(11) calc PR A 1 H35C H 1.4175 0.2301 0.4241 0.204 Uiso 0.555(11) calc PR A 1 C33' C 1.4356(18) 0.2979(8) 0.3643(6) 0.086(5) Uiso 0.445(11) d P A 2 H33D H 1.4406 0.3307 0.3379 0.129 Uiso 0.445(11) calc PR A 2 H33E H 1.4602 0.2514 0.3540 0.129 Uiso 0.445(11) calc PR A 2 H33F H 1.5030 0.3119 0.3920 0.129 Uiso 0.445(11) calc PR A 2 C34' C 1.194(3) 0.2682(11) 0.3268(7) 0.120(7) Uiso 0.445(11) d P A 2 H34D H 1.2048 0.3022 0.3015 0.180 Uiso 0.445(11) calc PR A 2 H34E H 1.0930 0.2614 0.3295 0.180 Uiso 0.445(11) calc PR A 2 H34F H 1.2370 0.2241 0.3188 0.180 Uiso 0.445(11) calc PR A 2 C35' C 1.269(2) 0.2501(10) 0.4183(7) 0.109(6) Uiso 0.445(11) d P A 2 H35D H 1.3032 0.2044 0.4098 0.163 Uiso 0.445(11) calc PR A 2 H35E H 1.1694 0.2463 0.4247 0.163 Uiso 0.445(11) calc PR A 2 H35F H 1.3276 0.2674 0.4470 0.163 Uiso 0.445(11) calc PR A 2 C36 C 0.7888(6) 0.8663(3) 0.46780(17) 0.0519(12) Uani 1 d . . . H36 H 0.7803 0.8354 0.4936 0.062 Uiso 1 calc R . . C37 C 0.7593(6) 0.9359(3) 0.47441(18) 0.0598(14) Uani 1 d . . . H37 H 0.7320 0.9508 0.5042 0.072 Uiso 1 calc R . . C38 C 0.7694(5) 0.9853(2) 0.43725(16) 0.0481(12) Uani 1 d . . . C39 C 0.8066(6) 0.9564(3) 0.39452(18) 0.0574(13) Uani 1 d . . . H39 H 0.8120 0.9857 0.3676 0.069 Uiso 1 calc R . . C40 C 0.8359(6) 0.8861(2) 0.39051(17) 0.0535(13) Uani 1 d . . . H40 H 0.8621 0.8694 0.3610 0.064 Uiso 1 calc R . . C41 C 0.7439(6) 1.0636(3) 0.44422(19) 0.0609(13) Uiso 1 d . . . C42 C 0.7257(16) 1.1046(7) 0.3977(5) 0.099(4) Uiso 0.605(12) d P B 1 H42A H 0.6480 1.0845 0.3756 0.149 Uiso 0.605(12) calc PR B 1 H42B H 0.8144 1.1029 0.3830 0.149 Uiso 0.605(12) calc PR B 1 H42C H 0.7030 1.1529 0.4045 0.149 Uiso 0.605(12) calc PR B 1 C43 C 0.5953(14) 1.0736(7) 0.4656(5) 0.098(4) Uiso 0.605(12) d P B 1 H43A H 0.5171 1.0564 0.4424 0.146 Uiso 0.605(12) calc PR B 1 H43B H 0.5805 1.1229 0.4718 0.146 Uiso 0.605(12) calc PR B 1 H43C H 0.5976 1.0476 0.4957 0.146 Uiso 0.605(12) calc PR B 1 C44 C 0.8636(16) 1.0911(7) 0.4806(5) 0.090(4) Uiso 0.605(12) d P B 1 H44A H 0.8493 1.1408 0.4855 0.135 Uiso 0.605(12) calc PR B 1 H44B H 0.9553 1.0838 0.4684 0.135 Uiso 0.605(12) calc PR B 1 H44C H 0.8632 1.0665 0.5111 0.135 Uiso 0.605(12) calc PR B 1 C42' C 0.613(3) 1.0894(12) 0.4180(9) 0.120(8) Uiso 0.395(12) d P B 2 H42D H 0.6042 1.1391 0.4242 0.179 Uiso 0.395(12) calc PR B 2 H42E H 0.5317 1.0648 0.4285 0.179 Uiso 0.395(12) calc PR B 2 H42F H 0.6146 1.0818 0.3835 0.179 Uiso 0.395(12) calc PR B 2 C43' C 0.793(2) 1.0875(8) 0.4967(6) 0.071(5) Uiso 0.395(12) d P B 2 H43D H 0.8837 1.0652 0.5085 0.106 Uiso 0.395(12) calc PR B 2 H43E H 0.7207 1.0745 0.5173 0.106 Uiso 0.395(12) calc PR B 2 H43F H 0.8053 1.1379 0.4973 0.106 Uiso 0.395(12) calc PR B 2 C44' C 0.869(3) 1.1076(12) 0.4191(8) 0.115(8) Uiso 0.395(12) d P B 2 H44D H 0.9640 1.0944 0.4347 0.173 Uiso 0.395(12) calc PR B 2 H44E H 0.8550 1.1574 0.4231 0.173 Uiso 0.395(12) calc PR B 2 H44F H 0.8619 1.0964 0.3847 0.173 Uiso 0.395(12) calc PR B 2 O1 O 0.8427(4) 0.57142(18) 0.42357(13) 0.0597(9) Uani 1 d . . . O2 O 0.7377(4) 0.67680(17) 0.43532(12) 0.0526(8) Uani 1 d . . . O3 O 1.1142(4) 0.61993(17) 0.47655(12) 0.0575(9) Uani 1 d . . . O4 O 1.0106(4) 0.72527(16) 0.48939(10) 0.0498(8) Uani 1 d . . . O5 O 1.2019(3) 0.67087(15) 0.38562(12) 0.0480(8) Uani 1 d . . . O6 O 1.1031(3) 0.77650(14) 0.40092(10) 0.0403(7) Uani 1 d . . . O7 O 0.9451(4) 0.62541(14) 0.33335(11) 0.0482(8) Uani 1 d . . . O8 O 0.8375(3) 0.72988(14) 0.34528(10) 0.0399(7) Uani 1 d . . . O9 O 1.2814(3) 0.84396(16) 0.34453(12) 0.0488(8) Uani 1 d . . . O10 O 0.8368(4) 0.76268(15) 0.24782(11) 0.0483(8) Uani 1 d . . . Rh1 Rh 1.02676(4) 0.617534(17) 0.405589(12) 0.04172(14) Uani 1 d . . . Rh2 Rh 0.91710(4) 0.730315(17) 0.418439(11) 0.03660(13) Uani 1 d . . . N1 N 1.1256(5) 0.51114(18) 0.39601(14) 0.0491(10) Uani 1 d . . . N2 N 0.8287(4) 0.84013(19) 0.42709(13) 0.0404(8) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(4) 0.048(3) 0.054(3) 0.007(2) 0.008(3) -0.010(3) C2 0.081(5) 0.080(4) 0.127(6) 0.010(4) 0.033(4) -0.027(4) C3 0.065(3) 0.057(3) 0.039(2) 0.006(2) 0.006(2) 0.000(3) C4 0.102(5) 0.094(5) 0.056(3) -0.001(3) -0.019(3) 0.018(4) C5 0.043(3) 0.040(3) 0.039(2) 0.0020(19) -0.0052(19) 0.004(2) C6 0.040(3) 0.042(3) 0.059(3) 0.008(2) 0.004(2) 0.007(2) C7 0.064(4) 0.065(4) 0.092(4) 0.009(3) 0.037(3) 0.013(3) C8 0.042(3) 0.076(4) 0.090(4) 0.018(3) -0.015(3) -0.003(3) C9 0.041(3) 0.038(2) 0.044(2) 0.0031(19) 0.0106(19) 0.0031(19) C10 0.047(3) 0.037(2) 0.046(2) 0.0013(19) 0.010(2) -0.001(2) C11 0.058(3) 0.037(3) 0.073(3) -0.004(2) 0.009(3) -0.006(2) C12 0.081(4) 0.073(4) 0.079(4) -0.031(3) 0.007(3) -0.019(3) C13 0.107(5) 0.034(3) 0.130(6) -0.010(3) -0.020(4) -0.009(3) C14 0.074(4) 0.065(4) 0.107(5) 0.002(3) 0.028(4) -0.027(3) C15 0.067(3) 0.030(2) 0.045(2) 0.0031(19) -0.003(2) 0.004(2) C16 0.062(3) 0.032(2) 0.043(2) -0.0040(18) -0.001(2) 0.005(2) C17 0.076(4) 0.053(3) 0.083(4) -0.020(3) -0.031(3) 0.018(3) C18 0.188(11) 0.061(5) 0.326(16) -0.019(7) -0.187(12) 0.032(6) C19 0.077(6) 0.163(8) 0.110(6) -0.018(6) 0.009(4) 0.042(5) C20 0.126(6) 0.098(5) 0.054(3) -0.007(3) -0.031(4) 0.021(4) C21 0.054(3) 0.033(2) 0.031(2) -0.0082(17) 0.0037(19) -0.002(2) C22 0.048(3) 0.030(2) 0.044(2) 0.0044(18) 0.008(2) 0.0048(19) C23 0.055(3) 0.029(2) 0.041(2) -0.0043(17) -0.002(2) -0.002(2) C24 0.067(4) 0.047(3) 0.060(3) -0.006(2) -0.011(3) -0.009(2) C25 0.070(4) 0.046(3) 0.052(3) -0.005(2) 0.015(2) -0.002(2) C26 0.043(3) 0.027(2) 0.046(2) -0.0039(18) 0.0025(19) -0.0026(19) C27 0.076(4) 0.045(3) 0.059(3) 0.009(2) 0.016(3) 0.005(3) C28 0.072(4) 0.053(3) 0.061(3) 0.002(2) 0.026(3) 0.010(3) C29 0.051(3) 0.045(3) 0.065(3) 0.004(2) 0.015(2) 0.010(2) C30 0.083(4) 0.040(3) 0.063(3) 0.015(2) 0.020(3) 0.014(3) C31 0.093(4) 0.041(3) 0.058(3) 0.010(2) 0.024(3) 0.015(3) C36 0.060(3) 0.052(3) 0.045(3) 0.001(2) 0.014(2) 0.010(2) C37 0.078(4) 0.057(3) 0.046(3) -0.007(2) 0.015(2) 0.014(3) C38 0.053(3) 0.045(3) 0.043(2) -0.010(2) -0.006(2) 0.012(2) C39 0.083(4) 0.043(3) 0.048(3) 0.007(2) 0.014(3) 0.010(3) C40 0.079(4) 0.043(3) 0.041(3) -0.002(2) 0.017(2) 0.006(2) O1 0.063(2) 0.0427(19) 0.075(2) 0.0104(17) 0.0141(18) -0.0027(18) O2 0.050(2) 0.047(2) 0.064(2) 0.0035(15) 0.0168(16) -0.0021(15) O3 0.077(3) 0.0482(19) 0.0448(18) 0.0095(15) -0.0033(16) 0.0098(17) O4 0.066(2) 0.0477(19) 0.0351(16) 0.0019(13) 0.0022(14) 0.0072(17) O5 0.050(2) 0.0330(17) 0.062(2) 0.0049(14) 0.0114(15) 0.0078(14) O6 0.0412(18) 0.0330(15) 0.0467(17) 0.0007(12) 0.0054(13) 0.0018(13) O7 0.067(2) 0.0299(16) 0.0461(17) -0.0045(13) -0.0004(15) 0.0056(14) O8 0.0471(19) 0.0321(15) 0.0399(15) -0.0019(12) 0.0022(13) 0.0037(13) O9 0.0407(19) 0.0414(17) 0.063(2) 0.0075(14) -0.0007(15) -0.0042(14) O10 0.061(2) 0.0347(16) 0.0449(17) 0.0010(13) -0.0106(15) -0.0037(15) Rh1 0.0532(3) 0.0285(2) 0.0433(2) 0.00436(14) 0.00524(16) 0.00463(15) Rh2 0.0420(2) 0.0310(2) 0.0369(2) -0.00009(13) 0.00500(14) 0.00190(14) N1 0.066(3) 0.0314(19) 0.050(2) 0.0056(17) 0.0072(19) 0.0063(18) N2 0.038(2) 0.041(2) 0.042(2) -0.0043(16) 0.0042(15) 0.0014(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.259(6) . ? C1 O1 1.259(7) . ? C1 C2 1.529(8) . ? C3 O4 1.264(6) . ? C3 O3 1.272(6) . ? C3 C4 1.496(7) . ? C5 O6 1.258(5) . ? C5 O5 1.263(5) . ? C5 C6 1.532(7) . ? C6 O9 1.455(5) . ? C6 C7 1.520(7) . ? C6 C8 1.538(7) . ? C9 O9 1.374(5) . ? C9 C22 1.380(6) . ? C9 C10 1.409(6) . ? C10 C15 1.383(6) . ? C10 C11 1.543(6) . ? C11 C12 1.523(7) . ? C11 C13 1.525(7) . ? C11 C14 1.538(8) . ? C15 C16 1.398(6) . ? C16 C21 1.399(6) . ? C16 C17 1.521(7) . ? C17 C18 1.457(9) . ? C17 C20 1.483(8) . ? C17 C19 1.587(11) . ? C21 C22 1.375(6) . ? C21 O10 1.385(5) . ? C23 O10 1.445(5) . ? C23 C25 1.518(7) . ? C23 C24 1.529(7) . ? C23 C26 1.531(6) . ? C26 O8 1.256(5) . ? C26 O7 1.270(5) . ? C27 N1 1.316(6) . ? C27 C28 1.359(7) . ? C28 C29 1.394(7) . ? C29 C30 1.379(7) . ? C29 C32 1.520(8) . ? C30 C31 1.378(7) . ? C31 N1 1.328(6) . ? C32 C35' 1.409(19) . ? C32 C33 1.447(18) . ? C32 C34 1.549(13) . ? C32 C33' 1.569(17) . ? C32 C35 1.581(18) . ? C32 C34' 1.64(2) . ? C36 N2 1.317(6) . ? C36 C37 1.360(7) . ? C37 C38 1.395(7) . ? C38 C39 1.377(7) . ? C38 C41 1.515(7) . ? C39 C40 1.364(7) . ? C40 N2 1.337(6) . ? C41 C42' 1.42(2) . ? C41 C42 1.486(13) . ? C41 C44 1.490(13) . ? C41 C43' 1.525(16) . ? C41 C43 1.574(14) . ? C41 C44' 1.65(2) . ? O1 Rh1 2.029(4) . ? O2 Rh2 2.046(3) . ? O3 Rh1 2.017(3) . ? O4 Rh2 2.035(3) . ? O5 Rh1 2.041(3) . ? O6 Rh2 2.041(3) . ? O7 Rh1 2.040(3) . ? O8 Rh2 2.053(3) . ? Rh1 Rh2 2.4063(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 O2 C1 O1 127.3(5) . . ? O2 C1 C2 116.2(6) . . ? O1 C1 C2 116.5(5) . . ? O4 C3 O3 125.8(4) . . ? O4 C3 C4 118.0(5) . . ? O3 C3 C4 116.2(5) . . ? O6 C5 O5 127.2(4) . . ? O6 C5 C6 116.9(4) . . ? O5 C5 C6 115.9(4) . . ? O9 C6 C7 110.2(4) . . ? O9 C6 C5 111.7(4) . . ? C7 C6 C5 114.3(4) . . ? O9 C6 C8 102.5(4) . . ? C7 C6 C8 110.3(5) . . ? C5 C6 C8 107.1(4) . . ? O9 C9 C22 124.1(4) . . ? O9 C9 C10 115.6(4) . . ? C22 C9 C10 120.3(4) . . ? C15 C10 C9 115.2(4) . . ? C15 C10 C11 121.9(4) . . ? C9 C10 C11 122.9(4) . . ? C12 C11 C13 108.1(5) . . ? C12 C11 C14 109.6(5) . . ? C13 C11 C14 107.1(5) . . ? C12 C11 C10 110.5(4) . . ? C13 C11 C10 111.7(4) . . ? C14 C11 C10 109.7(4) . . ? C10 C15 C16 126.8(4) . . ? C15 C16 C21 114.7(4) . . ? C15 C16 C17 122.0(4) . . ? C21 C16 C17 123.2(4) . . ? C18 C17 C20 112.9(6) . . ? C18 C17 C16 113.5(5) . . ? C20 C17 C16 114.5(5) . . ? C18 C17 C19 102.5(8) . . ? C20 C17 C19 103.6(6) . . ? C16 C17 C19 108.5(5) . . ? C22 C21 O10 124.3(4) . . ? C22 C21 C16 121.1(4) . . ? O10 C21 C16 114.6(4) . . ? C21 C22 C9 121.7(4) . . ? O10 C23 C25 110.4(4) . . ? O10 C23 C24 101.7(4) . . ? C25 C23 C24 111.8(4) . . ? O10 C23 C26 112.0(3) . . ? C25 C23 C26 112.9(4) . . ? C24 C23 C26 107.4(4) . . ? O8 C26 O7 126.3(4) . . ? O8 C26 C23 118.8(4) . . ? O7 C26 C23 114.9(4) . . ? N1 C27 C28 123.8(5) . . ? C27 C28 C29 120.6(5) . . ? C30 C29 C28 115.1(4) . . ? C30 C29 C32 122.1(5) . . ? C28 C29 C32 122.7(5) . . ? C31 C30 C29 120.6(5) . . ? N1 C31 C30 122.9(5) . . ? C35' C32 C33 126.4(12) . . ? C35' C32 C29 117.3(9) . . ? C33 C32 C29 116.2(9) . . ? C35' C32 C34 48.9(9) . . ? C33 C32 C34 108.2(10) . . ? C29 C32 C34 110.0(7) . . ? C35' C32 C33' 110.2(11) . . ? C33 C32 C33' 52.9(9) . . ? C29 C32 C33' 109.2(7) . . ? C34 C32 C33' 140.8(9) . . ? C35' C32 C35 51.7(10) . . ? C33 C32 C35 113.5(12) . . ? C29 C32 C35 107.3(8) . . ? C34 C32 C35 100.5(9) . . ? C33' C32 C35 67.0(9) . . ? C35' C32 C34' 113.1(12) . . ? C33 C32 C34' 44.5(10) . . ? C29 C32 C34' 107.9(9) . . ? C34 C32 C34' 71.2(9) . . ? C33' C32 C34' 97.3(10) . . ? C35 C32 C34' 144.6(11) . . ? N2 C36 C37 124.0(5) . . ? C36 C37 C38 121.1(4) . . ? C39 C38 C37 113.9(4) . . ? C39 C38 C41 123.7(4) . . ? C37 C38 C41 122.4(4) . . ? C40 C39 C38 121.9(4) . . ? N2 C40 C39 123.0(4) . . ? C42' C41 C42 52.0(10) . . ? C42' C41 C44 137.5(11) . . ? C42 C41 C44 112.9(8) . . ? C42' C41 C38 114.1(10) . . ? C42 C41 C38 113.8(6) . . ? C44 C41 C38 108.2(6) . . ? C42' C41 C43' 120.9(13) . . ? C42 C41 C43' 130.3(9) . . ? C44 C41 C43' 32.2(7) . . ? C38 C41 C43' 112.1(7) . . ? C42' C41 C43 54.3(10) . . ? C42 C41 C43 104.3(8) . . ? C44 C41 C43 108.6(8) . . ? C38 C41 C43 108.7(6) . . ? C43' C41 C43 77.4(9) . . ? C42' C41 C44' 102.4(13) . . ? C42 C41 C44' 52.2(9) . . ? C44 C41 C44' 66.5(9) . . ? C38 C41 C44' 108.1(9) . . ? C43' C41 C44' 96.0(11) . . ? C43 C41 C44' 142.2(10) . . ? C1 O1 Rh1 118.9(3) . . ? C1 O2 Rh2 117.9(4) . . ? C3 O3 Rh1 119.2(3) . . ? C3 O4 Rh2 118.6(3) . . ? C5 O5 Rh1 118.0(3) . . ? C5 O6 Rh2 118.3(3) . . ? C26 O7 Rh1 118.5(3) . . ? C26 O8 Rh2 118.3(3) . . ? C9 O9 C6 122.6(3) . . ? C21 O10 C23 123.8(3) . . ? O3 Rh1 O1 91.31(15) . . ? O3 Rh1 O7 174.23(13) . . ? O1 Rh1 O7 92.70(14) . . ? O3 Rh1 O5 90.68(14) . . ? O1 Rh1 O5 175.35(13) . . ? O7 Rh1 O5 85.03(13) . . ? O3 Rh1 Rh2 87.95(10) . . ? O1 Rh1 Rh2 87.85(10) . . ? O7 Rh1 Rh2 88.04(8) . . ? O5 Rh1 Rh2 88.02(8) . . ? O4 Rh2 O6 88.57(13) . . ? O4 Rh2 O2 91.16(14) . . ? O6 Rh2 O2 175.70(12) . . ? O4 Rh2 O8 174.95(12) . . ? O6 Rh2 O8 88.95(12) . . ? O2 Rh2 O8 90.98(13) . . ? O4 Rh2 Rh1 87.82(9) . . ? O6 Rh2 Rh1 87.75(8) . . ? O2 Rh2 Rh1 87.95(9) . . ? O8 Rh2 Rh1 87.68(8) . . ? C27 N1 C31 116.9(4) . . ? C36 N2 C40 116.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C5 C6 O9 -28.4(5) . . . . ? O5 C5 C6 O9 153.1(4) . . . . ? O6 C5 C6 C7 -154.4(4) . . . . ? O5 C5 C6 C7 27.0(6) . . . . ? O6 C5 C6 C8 83.1(5) . . . . ? O5 C5 C6 C8 -95.5(5) . . . . ? O9 C9 C10 C15 -177.1(4) . . . . ? C22 C9 C10 C15 1.9(6) . . . . ? O9 C9 C10 C11 -0.4(6) . . . . ? C22 C9 C10 C11 178.6(4) . . . . ? C15 C10 C11 C12 115.0(5) . . . . ? C9 C10 C11 C12 -61.4(6) . . . . ? C15 C10 C11 C13 -5.4(7) . . . . ? C9 C10 C11 C13 178.2(5) . . . . ? C15 C10 C11 C14 -124.0(5) . . . . ? C9 C10 C11 C14 59.5(6) . . . . ? C9 C10 C15 C16 1.9(7) . . . . ? C11 C10 C15 C16 -174.8(5) . . . . ? C10 C15 C16 C21 -2.3(8) . . . . ? C10 C15 C16 C17 174.5(5) . . . . ? C15 C16 C17 C18 -3.7(11) . . . . ? C21 C16 C17 C18 172.8(8) . . . . ? C15 C16 C17 C20 128.0(6) . . . . ? C21 C16 C17 C20 -55.5(8) . . . . ? C15 C16 C17 C19 -116.9(6) . . . . ? C21 C16 C17 C19 59.6(7) . . . . ? C15 C16 C21 C22 -1.2(7) . . . . ? C17 C16 C21 C22 -177.9(5) . . . . ? C15 C16 C21 O10 177.3(4) . . . . ? C17 C16 C21 O10 0.5(7) . . . . ? O10 C21 C22 C9 -173.4(4) . . . . ? C16 C21 C22 C9 4.9(7) . . . . ? O9 C9 C22 C21 173.6(4) . . . . ? C10 C9 C22 C21 -5.2(7) . . . . ? O10 C23 C26 O8 27.0(6) . . . . ? C25 C23 C26 O8 152.5(4) . . . . ? C24 C23 C26 O8 -83.8(5) . . . . ? O10 C23 C26 O7 -153.4(4) . . . . ? C25 C23 C26 O7 -27.9(5) . . . . ? C24 C23 C26 O7 95.8(5) . . . . ? N1 C27 C28 C29 -1.4(9) . . . . ? C27 C28 C29 C30 0.2(8) . . . . ? C27 C28 C29 C32 177.9(6) . . . . ? C28 C29 C30 C31 0.0(9) . . . . ? C32 C29 C30 C31 -177.7(6) . . . . ? C29 C30 C31 N1 1.0(10) . . . . ? C30 C29 C32 C35' -3.6(13) . . . . ? C28 C29 C32 C35' 178.9(11) . . . . ? C30 C29 C32 C33 172.9(11) . . . . ? C28 C29 C32 C33 -4.6(13) . . . . ? C30 C29 C32 C34 49.6(9) . . . . ? C28 C29 C32 C34 -127.9(7) . . . . ? C30 C29 C32 C33' -129.9(8) . . . . ? C28 C29 C32 C33' 52.7(9) . . . . ? C30 C29 C32 C35 -58.9(10) . . . . ? C28 C29 C32 C35 123.7(9) . . . . ? C30 C29 C32 C34' 125.5(10) . . . . ? C28 C29 C32 C34' -52.0(11) . . . . ? N2 C36 C37 C38 0.2(9) . . . . ? C36 C37 C38 C39 1.8(8) . . . . ? C36 C37 C38 C41 -177.1(5) . . . . ? C37 C38 C39 C40 -2.3(8) . . . . ? C41 C38 C39 C40 176.6(5) . . . . ? C38 C39 C40 N2 1.0(9) . . . . ? C39 C38 C41 C42' 72.0(13) . . . . ? C37 C38 C41 C42' -109.2(13) . . . . ? C39 C38 C41 C42 14.7(10) . . . . ? C37 C38 C41 C42 -166.5(8) . . . . ? C39 C38 C41 C44 -111.7(8) . . . . ? C37 C38 C41 C44 67.1(9) . . . . ? C39 C38 C41 C43' -145.8(9) . . . . ? C37 C38 C41 C43' 33.0(11) . . . . ? C39 C38 C41 C43 130.5(7) . . . . ? C37 C38 C41 C43 -50.7(8) . . . . ? C39 C38 C41 C44' -41.2(11) . . . . ? C37 C38 C41 C44' 137.6(10) . . . . ? O2 C1 O1 Rh1 -1.6(7) . . . . ? C2 C1 O1 Rh1 176.7(4) . . . . ? O1 C1 O2 Rh2 1.2(7) . . . . ? C2 C1 O2 Rh2 -177.1(4) . . . . ? O4 C3 O3 Rh1 9.1(7) . . . . ? C4 C3 O3 Rh1 -170.7(4) . . . . ? O3 C3 O4 Rh2 -9.7(7) . . . . ? C4 C3 O4 Rh2 170.1(4) . . . . ? O6 C5 O5 Rh1 8.0(6) . . . . ? C6 C5 O5 Rh1 -173.6(3) . . . . ? O5 C5 O6 Rh2 -11.2(6) . . . . ? C6 C5 O6 Rh2 170.4(3) . . . . ? O8 C26 O7 Rh1 -12.0(6) . . . . ? C23 C26 O7 Rh1 168.4(3) . . . . ? O7 C26 O8 Rh2 13.6(6) . . . . ? C23 C26 O8 Rh2 -166.8(3) . . . . ? C22 C9 O9 C6 -6.1(7) . . . . ? C10 C9 O9 C6 172.8(4) . . . . ? C7 C6 O9 C9 79.4(5) . . . . ? C5 C6 O9 C9 -48.9(5) . . . . ? C8 C6 O9 C9 -163.2(4) . . . . ? C22 C21 O10 C23 7.9(7) . . . . ? C16 C21 O10 C23 -170.5(4) . . . . ? C25 C23 O10 C21 -78.2(5) . . . . ? C24 C23 O10 C21 163.0(4) . . . . ? C26 C23 O10 C21 48.6(5) . . . . ? C3 O3 Rh1 O1 -91.5(4) . . . . ? C3 O3 Rh1 O7 42.5(16) . . . . ? C3 O3 Rh1 O5 84.3(4) . . . . ? C3 O3 Rh1 Rh2 -3.7(4) . . . . ? C1 O1 Rh1 O3 88.9(4) . . . . ? C1 O1 Rh1 O7 -86.9(4) . . . . ? C1 O1 Rh1 O5 -26.3(19) . . . . ? C1 O1 Rh1 Rh2 1.0(4) . . . . ? C26 O7 Rh1 O3 -42.0(16) . . . . ? C26 O7 Rh1 O1 91.9(3) . . . . ? C26 O7 Rh1 O5 -84.1(3) . . . . ? C26 O7 Rh1 Rh2 4.1(3) . . . . ? C5 O5 Rh1 O3 -89.1(3) . . . . ? C5 O5 Rh1 O1 26.1(18) . . . . ? C5 O5 Rh1 O7 87.0(3) . . . . ? C5 O5 Rh1 Rh2 -1.2(3) . . . . ? C3 O4 Rh2 O6 -82.9(4) . . . . ? C3 O4 Rh2 O2 92.8(4) . . . . ? C3 O4 Rh2 O8 -22.3(16) . . . . ? C3 O4 Rh2 Rh1 4.9(4) . . . . ? C5 O6 Rh2 O4 95.2(3) . . . . ? C5 O6 Rh2 O2 8.8(18) . . . . ? C5 O6 Rh2 O8 -80.4(3) . . . . ? C5 O6 Rh2 Rh1 7.3(3) . . . . ? C1 O2 Rh2 O4 -88.0(4) . . . . ? C1 O2 Rh2 O6 -1.7(18) . . . . ? C1 O2 Rh2 O8 87.4(4) . . . . ? C1 O2 Rh2 Rh1 -0.2(3) . . . . ? C26 O8 Rh2 O4 19.8(15) . . . . ? C26 O8 Rh2 O6 80.4(3) . . . . ? C26 O8 Rh2 O2 -95.3(3) . . . . ? C26 O8 Rh2 Rh1 -7.4(3) . . . . ? O3 Rh1 Rh2 O4 -0.50(14) . . . . ? O1 Rh1 Rh2 O4 90.88(14) . . . . ? O7 Rh1 Rh2 O4 -176.34(13) . . . . ? O5 Rh1 Rh2 O4 -91.25(13) . . . . ? O3 Rh1 Rh2 O6 88.15(13) . . . . ? O1 Rh1 Rh2 O6 179.54(13) . . . . ? O7 Rh1 Rh2 O6 -87.69(13) . . . . ? O5 Rh1 Rh2 O6 -2.60(12) . . . . ? O3 Rh1 Rh2 O2 -91.74(14) . . . . ? O1 Rh1 Rh2 O2 -0.36(14) . . . . ? O7 Rh1 Rh2 O2 92.42(14) . . . . ? O5 Rh1 Rh2 O2 177.51(13) . . . . ? O3 Rh1 Rh2 O8 177.19(13) . . . . ? O1 Rh1 Rh2 O8 -91.42(13) . . . . ? O7 Rh1 Rh2 O8 1.35(12) . . . . ? O5 Rh1 Rh2 O8 86.44(12) . . . . ? C28 C27 N1 C31 2.2(8) . . . . ? C30 C31 N1 C27 -2.0(9) . . . . ? C37 C36 N2 C40 -1.7(8) . . . . ? C39 C40 N2 C36 1.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 24.13 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.814 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.098 data_tmcg16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H77 Cl6 N O12 Rh2' _chemical_formula_weight 1350.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1320 0.1590 '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/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 17.918(3) _cell_length_b 9.4795(7) _cell_length_c 36.978(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.107(16) _cell_angle_gamma 90.00 _cell_volume 6280.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max .25 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39346 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 24.13 _reflns_number_total 9884 _reflns_number_gt 4712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9884 _refine_ls_number_parameters 652 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 0.748 _refine_ls_restrained_S_all 0.748 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.25001(4) 0.49446(6) 0.302552(14) 0.04256(17) Uani 1 d . . . Rh2 Rh 0.24998(4) 0.25672(6) 0.325274(14) 0.04252(18) Uani 1 d . . . O1 O 0.3262(3) 0.5426(5) 0.34048(13) 0.0543(14) Uani 1 d . . . O2 O 0.3296(3) 0.3198(5) 0.36089(12) 0.0443(12) Uani 1 d . . . O3 O 0.1738(3) 0.5433(5) 0.34056(12) 0.0542(14) Uani 1 d . . . O4 O 0.1702(3) 0.3199(5) 0.36095(12) 0.0432(12) Uani 1 d . . . O5 O 0.3288(3) 0.4325(5) 0.26649(12) 0.0451(12) Uani 1 d . . . O6 O 0.3270(3) 0.2082(5) 0.28766(12) 0.0552(14) Uani 1 d . . . O7 O 0.1710(3) 0.4324(5) 0.26659(12) 0.0447(12) Uani 1 d . . . O8 O 0.1732(3) 0.2087(5) 0.28777(12) 0.0561(14) Uani 1 d . . . O9 O 0.3858(3) 0.4078(5) 0.42559(12) 0.0477(13) Uani 1 d . . . O10 O 0.1144(3) 0.4074(5) 0.42549(12) 0.0482(13) Uani 1 d . . . O11 O 0.1146(3) 0.3386(6) 0.20209(12) 0.0492(13) Uani 1 d . . . O12 O 0.3856(3) 0.3389(6) 0.20201(12) 0.0483(13) Uani 1 d . . . C1 C 0.3464(4) 0.4490(8) 0.36283(19) 0.0439(18) Uani 1 d . . . C2 C 0.3949(4) 0.4959(8) 0.39428(18) 0.0468(18) Uani 1 d . . . C3 C 0.4769(5) 0.4700(10) 0.3836(2) 0.072(3) Uani 1 d . . . H3 H 0.4888 0.5255 0.3623 0.086 Uiso 1 calc R . . H3 H 0.4841 0.3707 0.3783 0.086 Uiso 1 calc R . . H3 H 0.5093 0.4975 0.4034 0.086 Uiso 1 calc R . . C4 C 0.3839(5) 0.6485(8) 0.4043(2) 0.062(2) Uani 1 d . . . H4 H 0.3900 0.7070 0.3830 0.075 Uiso 1 calc R . . H4 H 0.4204 0.6755 0.4224 0.075 Uiso 1 calc R . . H4 H 0.3340 0.6614 0.4140 0.075 Uiso 1 calc R . . C5 C 0.3170(4) 0.3717(7) 0.44018(18) 0.0399(17) Uani 1 d . . . C6 C 0.3191(4) 0.2803(8) 0.46983(17) 0.0420(18) Uani 1 d . . . C7 C 0.3924(5) 0.2217(9) 0.4853(2) 0.059(2) Uani 1 d . . . C8 C 0.4328(6) 0.1305(11) 0.4567(3) 0.096(4) Uani 1 d . . . H8A H 0.4787 0.0933 0.4669 0.116 Uiso 1 calc R . . H8B H 0.4444 0.1881 0.4357 0.116 Uiso 1 calc R . . H8C H 0.4007 0.0531 0.4494 0.116 Uiso 1 calc R . . C9 C 0.4427(6) 0.3426(12) 0.4983(3) 0.093(3) Uani 1 d . . . H9 H 0.4885 0.3042 0.5082 0.111 Uiso 1 calc R . . H9 H 0.4170 0.3965 0.5167 0.111 Uiso 1 calc R . . H9 H 0.4544 0.4037 0.4780 0.111 Uiso 1 calc R . . C10 C 0.3789(5) 0.1268(11) 0.5183(2) 0.084(3) Uani 1 d . . . H10 H 0.4263 0.0916 0.5273 0.101 Uiso 1 calc R . . H10 H 0.3475 0.0480 0.5114 0.101 Uiso 1 calc R . . H10 H 0.3544 0.1808 0.5372 0.101 Uiso 1 calc R . . C11 C 0.2500(4) 0.2400(8) 0.48334(18) 0.0461(17) Uiso 1 d . . . H11 H 0.2500 0.1804 0.5037 0.055 Uiso 1 calc R . . C12 C 0.1812(4) 0.2796(7) 0.46963(18) 0.0420(17) Uani 1 d . . . C13 C 0.1073(5) 0.2225(10) 0.4855(2) 0.061(2) Uani 1 d . . . C14 C 0.0563(6) 0.3425(12) 0.4982(3) 0.094(3) Uani 1 d . . . H14 H 0.0109 0.3031 0.5083 0.113 Uiso 1 calc R . . H14 H 0.0438 0.4025 0.4778 0.113 Uiso 1 calc R . . H14 H 0.0818 0.3977 0.5165 0.113 Uiso 1 calc R . . C15 C 0.1216(5) 0.1284(12) 0.5185(2) 0.086(3) Uani 1 d . . . H15 H 0.0745 0.0932 0.5277 0.103 Uiso 1 calc R . . H15 H 0.1464 0.1829 0.5372 0.103 Uiso 1 calc R . . H15 H 0.1530 0.0496 0.5116 0.103 Uiso 1 calc R . . C16 C 0.0667(6) 0.1320(12) 0.4573(3) 0.097(4) Uani 1 d . . . H16 H 0.0212 0.0945 0.4677 0.117 Uiso 1 calc R . . H16 H 0.0988 0.0547 0.4499 0.117 Uiso 1 calc R . . H16 H 0.0545 0.1895 0.4364 0.117 Uiso 1 calc R . . C17 C 0.1827(4) 0.3715(7) 0.44028(18) 0.0381(17) Uani 1 d . . . C18 C 0.2498(4) 0.4238(7) 0.42690(18) 0.0412(17) Uani 1 d . . . H18 H 0.2497 0.4941 0.4090 0.049 Uiso 1 calc R . . C19 C 0.1047(4) 0.4961(8) 0.39410(18) 0.0456(17) Uani 1 d . . . C20 C 0.1169(5) 0.6496(8) 0.4042(2) 0.063(2) Uani 1 d . . . H20 H 0.1104 0.7083 0.3829 0.075 Uiso 1 calc R . . H20 H 0.1670 0.6616 0.4136 0.075 Uiso 1 calc R . . H20 H 0.0809 0.6769 0.4225 0.075 Uiso 1 calc R . . C21 C 0.0229(5) 0.4703(10) 0.3838(2) 0.073(3) Uani 1 d . . . H21 H 0.0103 0.5262 0.3627 0.087 Uiso 1 calc R . . H21 H -0.0090 0.4972 0.4038 0.087 Uiso 1 calc R . . H21 H 0.0156 0.3711 0.3784 0.087 Uiso 1 calc R . . C22 C 0.1533(4) 0.4487(8) 0.36253(19) 0.0433(18) Uani 1 d . . . C23 C 0.1545(4) 0.3029(8) 0.26518(18) 0.0435(18) Uani 1 d . . . C24 C 0.1053(4) 0.2525(9) 0.23361(17) 0.0480(19) Uani 1 d . . . C25 C 0.1185(6) 0.0964(9) 0.2241(2) 0.075(3) Uani 1 d . . . H25 H 0.1119 0.0391 0.2456 0.090 Uiso 1 calc R . . H25 H 0.1688 0.0846 0.2150 0.090 Uiso 1 calc R . . H25 H 0.0830 0.0672 0.2057 0.090 Uiso 1 calc R . . C26 C 0.0252(5) 0.2786(12) 0.2444(2) 0.090(3) Uani 1 d . . . H26 H 0.0136 0.2237 0.2658 0.108 Uiso 1 calc R . . H26 H -0.0077 0.2507 0.2248 0.108 Uiso 1 calc R . . H26 H 0.0182 0.3781 0.2496 0.108 Uiso 1 calc R . . C27 C 0.1825(4) 0.3730(7) 0.18678(17) 0.0400(17) Uani 1 d . . . C28 C 0.1804(4) 0.4615(7) 0.15707(17) 0.0384(17) Uani 1 d . . . C29 C 0.1072(4) 0.5188(9) 0.14111(18) 0.053(2) Uani 1 d . . . C30 C 0.0676(5) 0.6120(10) 0.1689(2) 0.079(3) Uani 1 d . . . H30 H 0.0207 0.6451 0.1588 0.095 Uiso 1 calc R . . H30 H 0.0990 0.6922 0.1747 0.095 Uiso 1 calc R . . H30 H 0.0579 0.5577 0.1906 0.095 Uiso 1 calc R . . C31 C 0.1217(5) 0.6093(10) 0.1074(2) 0.072(3) Uani 1 d . . . H31 H 0.0745 0.6433 0.0979 0.086 Uiso 1 calc R . . H31 H 0.1467 0.5529 0.0892 0.086 Uiso 1 calc R . . H31 H 0.1529 0.6890 0.1139 0.086 Uiso 1 calc R . . C32 C 0.0550(5) 0.3971(10) 0.1295(2) 0.071(3) Uani 1 d . . . H32 H 0.0088 0.4358 0.1201 0.085 Uiso 1 calc R . . H32 H 0.0443 0.3378 0.1502 0.085 Uiso 1 calc R . . H32 H 0.0791 0.3413 0.1109 0.085 Uiso 1 calc R . . C33 C 0.2503(4) 0.4995(8) 0.14288(17) 0.0435(17) Uani 1 d . . . H33 H 0.2506 0.5561 0.1220 0.052 Uiso 1 calc R . . C34 C 0.3190(4) 0.4601(7) 0.15722(17) 0.0398(17) Uani 1 d . . . C35 C 0.3926(4) 0.5190(9) 0.14110(19) 0.053(2) Uani 1 d . . . C36 C 0.4448(5) 0.3974(10) 0.1296(2) 0.073(3) Uani 1 d . . . H36 H 0.4910 0.4362 0.1203 0.087 Uiso 1 calc R . . H36 H 0.4207 0.3417 0.1109 0.087 Uiso 1 calc R . . H36 H 0.4554 0.3380 0.1503 0.087 Uiso 1 calc R . . C37 C 0.3782(5) 0.6105(10) 0.1073(2) 0.075(3) Uani 1 d . . . H37 H 0.4255 0.6440 0.0978 0.090 Uiso 1 calc R . . H37 H 0.3473 0.6905 0.1138 0.090 Uiso 1 calc R . . H37 H 0.3530 0.5545 0.0890 0.090 Uiso 1 calc R . . C38 C 0.4317(5) 0.6122(11) 0.1688(2) 0.081(3) Uani 1 d . . . H38 H 0.4787 0.6452 0.1590 0.098 Uiso 1 calc R . . H38 H 0.4411 0.5583 0.1906 0.098 Uiso 1 calc R . . H38 H 0.4003 0.6924 0.1745 0.098 Uiso 1 calc R . . C39 C 0.3175(4) 0.3724(7) 0.18690(17) 0.0382(17) Uani 1 d . . . C40 C 0.2501(4) 0.3237(7) 0.20076(17) 0.0408(17) Uani 1 d . . . H40 H 0.2501 0.2573 0.2196 0.049 Uiso 1 calc R . . C41 C 0.3947(4) 0.2523(9) 0.23346(17) 0.0502(19) Uani 1 d . . . C42 C 0.4748(5) 0.2791(13) 0.2444(2) 0.090(4) Uani 1 d . . . H42 H 0.4864 0.2247 0.2659 0.108 Uiso 1 calc R . . H42 H 0.4816 0.3787 0.2495 0.108 Uiso 1 calc R . . H42 H 0.5078 0.2511 0.2249 0.108 Uiso 1 calc R . . C43 C 0.3817(6) 0.0970(9) 0.2242(2) 0.075(3) Uani 1 d . . . H43 H 0.3885 0.0400 0.2457 0.090 Uiso 1 calc R . . H43 H 0.4171 0.0676 0.2059 0.090 Uiso 1 calc R . . H43 H 0.3313 0.0848 0.2151 0.090 Uiso 1 calc R . . C44 C 0.3452(4) 0.3029(9) 0.26511(18) 0.0456(19) Uani 1 d . . . N1 N 0.2514(5) 0.0296(7) 0.34824(19) 0.079(2) Uani 1 d . . . C45 C 0.2500(5) -0.0709(7) 0.3196(2) 0.0490(19) Uani 1 d . . . C46 C 0.1852(6) -0.1219(11) 0.3058(3) 0.089(3) Uani 1 d . . . H46 H 0.1393 -0.0917 0.3154 0.107 Uiso 1 calc R . . C47 C 0.1863(6) -0.2210(11) 0.2770(3) 0.087(3) Uani 1 d . . . H47 H 0.1412 -0.2559 0.2676 0.104 Uiso 1 calc R . . C48 C 0.2506(6) -0.2648(9) 0.2631(2) 0.069(2) Uani 1 d . . . H48 H 0.2508 -0.3274 0.2434 0.082 Uiso 1 calc R . . C49 C 0.3135(6) -0.2206(11) 0.2770(3) 0.084(3) Uani 1 d . . . H49 H 0.3588 -0.2553 0.2677 0.101 Uiso 1 calc R . . C50 C 0.3150(6) -0.1212(10) 0.3057(3) 0.086(3) Uani 1 d . . . H50 H 0.3609 -0.0902 0.3151 0.104 Uiso 1 calc R . . C51 C 0.3125(12) 0.0232(11) 0.3711(4) 0.229(12) Uani 1 d . . . H51 H 0.3078 0.0947 0.3898 0.275 Uiso 1 calc R . . H51 H 0.3577 0.0397 0.3574 0.275 Uiso 1 calc R . . H51 H 0.3148 -0.0693 0.3823 0.275 Uiso 1 calc R . . C52 C 0.1839(8) 0.0212(16) 0.3701(4) 0.142(5) Uiso 1 d . . . H52A H 0.1860 0.0914 0.3891 0.170 Uiso 1 calc R . . H52B H 0.1801 -0.0721 0.3807 0.170 Uiso 1 calc R . . H52C H 0.1406 0.0386 0.3549 0.170 Uiso 1 calc R . . C53 C 0.2496(7) -0.3150(15) 0.4994(3) 0.116(4) Uiso 1 d . . . H53 H 0.2496 -0.3982 0.4833 0.139 Uiso 1 calc R A 1 Cl1 Cl 0.2623(6) -0.1728(9) 0.4701(2) 0.129(3) Uiso 0.597(12) d PU B 1 Cl2 Cl 0.3434(6) -0.3099(9) 0.5171(3) 0.160(4) Uiso 0.597(12) d PU B 1 Cl3 Cl 0.1560(5) -0.3102(9) 0.5171(3) 0.157(4) Uiso 0.597(12) d PU B 1 Cl1' Cl 0.2327(8) -0.1733(12) 0.4699(3) 0.111(4) Uiso 0.403(12) d PU B 2 Cl2' Cl 0.3041(8) -0.3043(14) 0.5364(4) 0.163(5) Uiso 0.403(12) d PU B 2 Cl3' Cl 0.1964(8) -0.3062(13) 0.5363(4) 0.154(5) Uiso 0.403(12) d PU B 2 C54 C -0.2503(8) 0.5976(15) 0.3759(3) 0.120(4) Uiso 1 d . . . H54 H -0.2486 0.6811 0.3598 0.144 Uiso 1 calc R C 1 Cl4 Cl -0.1658(6) 0.5650(11) 0.3918(3) 0.171(4) Uiso 0.538(7) d PU D 1 Cl5 Cl -0.3307(5) 0.5189(11) 0.3717(3) 0.163(3) Uiso 0.538(7) d PU D 1 Cl6 Cl -0.2522(6) 0.4210(12) 0.3459(3) 0.201(5) Uiso 0.538(7) d P D 1 Cl4' Cl -0.2477(7) 0.6601(14) 0.4226(3) 0.197(5) Uiso 0.462(7) d P D 2 Cl5' Cl -0.3304(7) 0.5760(14) 0.3973(4) 0.180(5) Uiso 0.462(7) d PU D 2 Cl6' Cl -0.1747(6) 0.5057(12) 0.3673(3) 0.160(4) Uiso 0.462(7) d PU D 2 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 Rh1 0.0627(4) 0.0253(3) 0.0396(3) 0.0061(3) 0.0015(2) -0.0001(3) Rh2 0.0654(4) 0.0247(3) 0.0375(3) 0.0050(2) 0.0015(2) -0.0001(3) O1 0.083(4) 0.034(3) 0.047(3) 0.011(2) -0.010(3) -0.002(3) O2 0.053(3) 0.031(3) 0.049(3) 0.006(2) 0.008(2) 0.003(2) O3 0.086(4) 0.031(3) 0.046(3) 0.008(2) 0.012(3) 0.001(3) O4 0.051(3) 0.030(3) 0.048(3) 0.006(2) -0.004(2) 0.000(2) O5 0.056(3) 0.031(3) 0.049(3) 0.010(2) -0.003(2) -0.001(2) O6 0.089(4) 0.035(3) 0.041(3) 0.008(2) 0.006(3) 0.008(3) O7 0.053(3) 0.035(3) 0.046(3) 0.009(2) 0.007(2) 0.002(2) O8 0.091(4) 0.036(3) 0.041(3) 0.009(2) -0.004(3) -0.008(3) O9 0.037(3) 0.056(3) 0.050(3) 0.017(2) 0.001(2) -0.002(2) O10 0.038(3) 0.056(3) 0.051(3) 0.014(2) 0.001(2) 0.003(2) O11 0.034(3) 0.066(4) 0.047(3) 0.015(3) 0.004(2) -0.003(3) O12 0.033(3) 0.068(4) 0.044(3) 0.014(2) -0.004(2) 0.003(3) C1 0.047(5) 0.040(5) 0.045(4) 0.003(3) 0.007(3) 0.001(4) C2 0.048(5) 0.043(5) 0.049(4) 0.010(4) 0.002(3) -0.001(4) C3 0.054(5) 0.086(7) 0.076(6) 0.012(5) 0.008(5) 0.000(5) C4 0.071(6) 0.050(5) 0.066(5) 0.004(4) -0.007(5) -0.014(4) C5 0.031(4) 0.039(4) 0.050(4) 0.001(3) 0.001(3) -0.002(3) C6 0.035(4) 0.048(5) 0.042(4) 0.009(3) -0.005(3) 0.005(3) C7 0.055(5) 0.067(6) 0.054(5) 0.023(4) -0.002(4) 0.013(4) C8 0.076(7) 0.101(9) 0.113(8) 0.029(7) 0.014(6) 0.052(6) C9 0.079(7) 0.105(9) 0.093(7) 0.021(6) -0.038(6) -0.017(6) C10 0.068(7) 0.107(9) 0.077(6) 0.042(6) -0.002(5) 0.026(6) C12 0.037(4) 0.043(5) 0.046(4) 0.010(3) 0.004(3) -0.002(3) C13 0.054(5) 0.070(6) 0.061(5) 0.021(4) 0.009(4) -0.010(5) C14 0.083(8) 0.106(9) 0.094(7) 0.019(6) 0.043(6) 0.013(7) C15 0.061(6) 0.118(9) 0.078(6) 0.046(6) 0.002(5) -0.017(6) C16 0.076(7) 0.107(9) 0.108(8) 0.036(7) -0.014(6) -0.052(7) C17 0.030(4) 0.039(4) 0.045(4) -0.001(3) 0.001(3) 0.002(3) C18 0.050(5) 0.036(4) 0.037(4) 0.002(3) 0.001(3) -0.001(4) C19 0.044(4) 0.045(5) 0.048(4) 0.007(4) -0.004(3) 0.000(4) C20 0.072(6) 0.046(5) 0.070(5) 0.003(4) 0.007(5) 0.018(4) C21 0.054(6) 0.083(7) 0.081(6) 0.019(5) -0.012(5) 0.003(5) C22 0.049(5) 0.037(5) 0.044(4) 0.000(3) -0.002(3) 0.000(3) C23 0.040(4) 0.053(5) 0.037(4) 0.005(3) 0.000(3) -0.008(4) C24 0.045(5) 0.060(5) 0.039(4) 0.013(4) 0.001(3) -0.008(4) C25 0.098(8) 0.061(6) 0.067(6) 0.004(5) -0.014(5) -0.034(5) C26 0.046(5) 0.147(11) 0.077(6) 0.030(6) 0.016(5) -0.009(6) C27 0.036(5) 0.046(5) 0.038(4) 0.000(3) -0.004(3) -0.006(3) C28 0.039(4) 0.039(4) 0.037(4) -0.002(3) -0.002(3) 0.003(3) C29 0.054(5) 0.061(5) 0.043(4) 0.005(4) -0.004(4) 0.011(4) C30 0.079(7) 0.087(8) 0.072(6) 0.007(5) 0.006(5) 0.041(6) C31 0.067(6) 0.089(7) 0.060(5) 0.030(5) -0.018(5) 0.017(5) C32 0.050(5) 0.096(8) 0.068(5) 0.005(5) -0.014(4) -0.002(5) C33 0.055(5) 0.039(4) 0.037(3) 0.010(3) 0.000(3) -0.003(4) C34 0.044(5) 0.040(4) 0.035(4) -0.001(3) 0.003(3) -0.003(3) C35 0.053(5) 0.060(5) 0.047(4) 0.007(4) 0.008(4) -0.008(4) C36 0.047(5) 0.104(8) 0.068(6) 0.009(5) 0.017(4) 0.006(5) C37 0.069(6) 0.096(8) 0.061(5) 0.027(5) 0.026(5) -0.022(5) C38 0.078(7) 0.093(8) 0.073(6) 0.003(5) -0.004(5) -0.040(6) C39 0.036(4) 0.040(4) 0.039(4) 0.002(3) 0.003(3) 0.003(3) C40 0.050(5) 0.040(4) 0.032(3) 0.008(3) 0.003(3) -0.001(4) C41 0.052(5) 0.060(5) 0.039(4) 0.014(4) 0.002(3) 0.008(4) C42 0.049(6) 0.149(11) 0.071(6) 0.031(6) -0.011(5) 0.011(6) C43 0.099(8) 0.066(7) 0.060(5) 0.005(5) 0.016(5) 0.032(6) C44 0.041(5) 0.063(6) 0.033(4) 0.004(4) 0.002(3) 0.006(4) N1 0.142(8) 0.040(4) 0.056(4) 0.008(3) 0.005(5) -0.001(4) C45 0.065(6) 0.027(4) 0.055(5) 0.009(3) 0.004(4) 0.002(4) C46 0.075(7) 0.060(7) 0.132(9) -0.012(6) -0.001(7) 0.004(6) C47 0.082(8) 0.068(8) 0.109(8) -0.001(6) -0.029(7) -0.009(6) C48 0.090(8) 0.037(5) 0.079(6) 0.010(4) -0.003(6) 0.004(5) C49 0.072(7) 0.065(7) 0.116(8) -0.004(6) 0.031(6) 0.003(6) C50 0.076(7) 0.053(6) 0.131(9) -0.013(6) -0.008(7) -0.007(5) C51 0.52(3) 0.024(6) 0.146(11) 0.003(6) -0.214(18) 0.010(11) _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 Rh1 O1 2.008(5) . ? Rh1 O3 2.015(5) . ? Rh1 O7 2.028(5) . ? Rh1 O5 2.031(5) . ? Rh1 Rh2 2.4052(8) . ? Rh2 O8 2.004(5) . ? Rh2 O6 2.014(5) . ? Rh2 O2 2.030(5) . ? Rh2 O4 2.037(5) . ? O1 C1 1.265(8) . ? O2 C1 1.263(8) . ? O3 C22 1.265(8) . ? O4 C22 1.259(8) . ? O5 C44 1.264(9) . ? O6 C44 1.268(9) . ? O7 C23 1.264(9) . ? O8 C23 1.268(8) . ? O9 C5 1.390(8) . ? O9 C2 1.437(8) . ? O10 C17 1.382(8) . ? O10 C19 1.444(8) . ? O11 C27 1.382(8) . ? O11 C24 1.433(8) . ? O12 C39 1.377(8) . ? O12 C41 1.432(8) . ? C1 C2 1.517(10) . ? C2 C4 1.507(11) . ? C2 C3 1.541(11) . ? C5 C18 1.390(10) . ? C5 C6 1.397(9) . ? C6 C11 1.390(10) . ? C6 C7 1.536(10) . ? C7 C9 1.534(13) . ? C7 C10 1.535(11) . ? C7 C8 1.549(12) . ? C11 C12 1.385(10) . ? C12 C17 1.392(9) . ? C12 C13 1.546(10) . ? C13 C15 1.534(11) . ? C13 C14 1.534(13) . ? C13 C16 1.534(12) . ? C17 C18 1.392(10) . ? C19 C20 1.518(11) . ? C19 C22 1.525(10) . ? C19 C21 1.534(11) . ? C23 C24 1.537(10) . ? C24 C26 1.512(11) . ? C24 C25 1.539(11) . ? C27 C28 1.382(9) . ? C27 C40 1.397(10) . ? C28 C33 1.406(9) . ? C28 C29 1.536(10) . ? C29 C30 1.530(11) . ? C29 C31 1.535(10) . ? C29 C32 1.546(11) . ? C33 C34 1.391(10) . ? C34 C39 1.378(9) . ? C34 C35 1.552(10) . ? C35 C38 1.523(11) . ? C35 C37 1.542(10) . ? C35 C36 1.545(11) . ? C39 C40 1.392(9) . ? C41 C42 1.513(11) . ? C41 C43 1.530(11) . ? C41 C44 1.546(10) . ? N1 C51 1.383(16) . ? N1 C45 1.424(10) . ? N1 C52 1.458(15) . ? C45 C46 1.356(12) . ? C45 C50 1.361(12) . ? C46 C47 1.422(14) . ? C47 C48 1.328(13) . ? C48 C49 1.306(13) . ? C49 C50 1.421(13) . ? C53 Cl3' 1.667(16) . ? C53 Cl2' 1.681(16) . ? C53 Cl1 1.746(15) . ? C53 Cl1' 1.756(17) . ? C53 Cl3 1.802(15) . ? C53 Cl2 1.804(15) . ? Cl1 Cl2 2.613(12) . ? Cl2' Cl3' 1.93(2) . ? C54 Cl5 1.630(15) . ? C54 Cl6' 1.641(16) . ? C54 Cl4 1.653(16) . ? C54 Cl5' 1.655(17) . ? C54 Cl4' 1.828(17) . ? C54 Cl6 2.009(16) . ? Cl4 Cl6 2.672(16) . ? Cl5 Cl6 1.938(14) . ? Cl4' Cl5' 1.923(17) . ? 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 Rh1 O3 85.5(2) . . ? O1 Rh1 O7 175.54(19) . . ? O3 Rh1 O7 92.9(2) . . ? O1 Rh1 O5 92.9(2) . . ? O3 Rh1 O5 175.75(19) . . ? O7 Rh1 O5 88.34(19) . . ? O1 Rh1 Rh2 88.25(14) . . ? O3 Rh1 Rh2 88.35(13) . . ? O7 Rh1 Rh2 87.53(13) . . ? O5 Rh1 Rh2 87.65(13) . . ? O8 Rh2 O6 86.6(2) . . ? O8 Rh2 O2 175.33(19) . . ? O6 Rh2 O2 91.9(2) . . ? O8 Rh2 O4 91.9(2) . . ? O6 Rh2 O4 175.40(19) . . ? O2 Rh2 O4 89.21(18) . . ? O8 Rh2 Rh1 88.39(14) . . ? O6 Rh2 Rh1 88.41(14) . . ? O2 Rh2 Rh1 87.13(13) . . ? O4 Rh2 Rh1 87.20(13) . . ? C1 O1 Rh1 119.4(5) . . ? C1 O2 Rh2 119.3(5) . . ? C22 O3 Rh1 118.9(5) . . ? C22 O4 Rh2 118.9(4) . . ? C44 O5 Rh1 118.0(4) . . ? C44 O6 Rh2 118.0(5) . . ? C23 O7 Rh1 118.2(4) . . ? C23 O8 Rh2 118.4(5) . . ? C5 O9 C2 123.9(5) . . ? C17 O10 C19 124.5(5) . . ? C27 O11 C24 124.8(5) . . ? C39 O12 C41 124.1(5) . . ? O2 C1 O1 125.1(7) . . ? O2 C1 C2 117.6(6) . . ? O1 C1 C2 117.3(7) . . ? O9 C2 C4 110.1(6) . . ? O9 C2 C1 112.5(6) . . ? C4 C2 C1 113.2(6) . . ? O9 C2 C3 102.9(6) . . ? C4 C2 C3 110.0(7) . . ? C1 C2 C3 107.6(6) . . ? O9 C5 C18 122.9(6) . . ? O9 C5 C6 115.7(6) . . ? C18 C5 C6 121.3(6) . . ? C11 C6 C5 115.4(6) . . ? C11 C6 C7 121.9(6) . . ? C5 C6 C7 122.6(6) . . ? C9 C7 C10 106.5(7) . . ? C9 C7 C6 110.3(7) . . ? C10 C7 C6 111.9(7) . . ? C9 C7 C8 110.8(8) . . ? C10 C7 C8 107.0(8) . . ? C6 C7 C8 110.3(7) . . ? C12 C11 C6 126.0(7) . . ? C11 C12 C17 115.9(6) . . ? C11 C12 C13 121.9(6) . . ? C17 C12 C13 122.2(6) . . ? C15 C13 C14 106.6(7) . . ? C15 C13 C16 107.1(8) . . ? C14 C13 C16 109.9(8) . . ? C15 C13 C12 111.3(7) . . ? C14 C13 C12 111.6(7) . . ? C16 C13 C12 110.1(7) . . ? O10 C17 C12 116.3(6) . . ? O10 C17 C18 122.5(6) . . ? C12 C17 C18 121.2(6) . . ? C5 C18 C17 119.7(6) . . ? O10 C19 C20 110.1(6) . . ? O10 C19 C22 112.1(6) . . ? C20 C19 C22 112.9(6) . . ? O10 C19 C21 102.7(6) . . ? C20 C19 C21 110.5(7) . . ? C22 C19 C21 108.0(6) . . ? O4 C22 O3 126.0(7) . . ? O4 C22 C19 117.3(6) . . ? O3 C22 C19 116.7(6) . . ? O7 C23 O8 126.6(6) . . ? O7 C23 C24 117.8(6) . . ? O8 C23 C24 115.6(7) . . ? O11 C24 C26 103.5(6) . . ? O11 C24 C23 111.9(6) . . ? C26 C24 C23 106.9(6) . . ? O11 C24 C25 110.1(6) . . ? C26 C24 C25 111.3(7) . . ? C23 C24 C25 112.6(6) . . ? O11 C27 C28 116.5(6) . . ? O11 C27 C40 122.2(6) . . ? C28 C27 C40 121.3(6) . . ? C27 C28 C33 115.4(6) . . ? C27 C28 C29 122.8(6) . . ? C33 C28 C29 121.7(6) . . ? C30 C29 C31 107.5(7) . . ? C30 C29 C28 110.1(6) . . ? C31 C29 C28 111.4(6) . . ? C30 C29 C32 109.6(7) . . ? C31 C29 C32 107.1(6) . . ? C28 C29 C32 111.0(7) . . ? C34 C33 C28 125.3(6) . . ? C39 C34 C33 116.6(6) . . ? C39 C34 C35 122.7(6) . . ? C33 C34 C35 120.6(6) . . ? C38 C35 C37 107.1(7) . . ? C38 C35 C36 109.9(7) . . ? C37 C35 C36 107.2(6) . . ? C38 C35 C34 109.9(6) . . ? C37 C35 C34 111.9(6) . . ? C36 C35 C34 110.7(7) . . ? O12 C39 C34 116.4(6) . . ? O12 C39 C40 122.9(6) . . ? C34 C39 C40 120.7(6) . . ? C39 C40 C27 120.4(6) . . ? O12 C41 C42 103.2(6) . . ? O12 C41 C43 110.6(6) . . ? C42 C41 C43 111.4(8) . . ? O12 C41 C44 111.9(6) . . ? C42 C41 C44 106.9(7) . . ? C43 C41 C44 112.4(7) . . ? O5 C44 O6 127.0(6) . . ? O5 C44 C41 117.7(6) . . ? O6 C44 C41 115.3(7) . . ? C51 N1 C45 116.0(9) . . ? C51 N1 C52 108.4(11) . . ? C45 N1 C52 111.1(9) . . ? C46 C45 C50 117.8(8) . . ? C46 C45 N1 122.1(9) . . ? C50 C45 N1 120.1(9) . . ? C45 C46 C47 120.2(10) . . ? C48 C47 C46 120.7(10) . . ? C49 C48 C47 119.8(10) . . ? C48 C49 C50 121.4(10) . . ? C45 C50 C49 120.0(9) . . ? Cl3' C53 Cl2' 70.4(10) . . ? Cl3' C53 Cl1 123.0(10) . . ? Cl2' C53 Cl1 112.6(10) . . ? Cl3' C53 Cl1' 111.7(9) . . ? Cl2' C53 Cl1' 123.9(11) . . ? Cl1 C53 Cl1' 17.4(5) . . ? Cl3' C53 Cl3 33.6(5) . . ? Cl2' C53 Cl3 104.0(10) . . ? Cl1 C53 Cl3 109.2(8) . . ? Cl1' C53 Cl3 92.7(8) . . ? Cl3' C53 Cl2 103.7(10) . . ? Cl2' C53 Cl2 33.3(5) . . ? Cl1 C53 Cl2 94.8(8) . . ? Cl1' C53 Cl2 111.4(9) . . ? Cl3 C53 Cl2 137.3(9) . . ? C53 Cl1 Cl2 43.5(5) . . ? C53 Cl2 Cl1 41.7(5) . . ? C53 Cl2' Cl3' 54.5(7) . . ? C53 Cl3' Cl2' 55.1(7) . . ? Cl5 C54 Cl6' 117.9(10) . . ? Cl5 C54 Cl4 139.2(11) . . ? Cl6' C54 Cl4 38.2(5) . . ? Cl5 C54 Cl5' 38.9(5) . . ? Cl6' C54 Cl5' 138.0(11) . . ? Cl4 C54 Cl5' 126.9(10) . . ? Cl5 C54 Cl4' 105.0(9) . . ? Cl6' C54 Cl4' 109.6(9) . . ? Cl4 C54 Cl4' 72.7(8) . . ? Cl5' C54 Cl4' 66.8(8) . . ? Cl5 C54 Cl6 63.4(7) . . ? Cl6' C54 Cl6 57.6(7) . . ? Cl4 C54 Cl6 93.2(8) . . ? Cl5' C54 Cl6 98.5(9) . . ? Cl4' C54 Cl6 142.5(9) . . ? C54 Cl4 Cl6 48.7(6) . . ? C54 Cl5 Cl6 67.9(7) . . ? Cl5 Cl6 C54 48.7(5) . . ? Cl5 Cl6 Cl4 82.1(5) . . ? C54 Cl6 Cl4 38.1(5) . . ? C54 Cl4' Cl5' 52.3(6) . . ? C54 Cl5' Cl4' 60.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Rh1 Rh2 O8 179.5(2) . . . . ? O3 Rh1 Rh2 O8 94.0(2) . . . . ? O7 Rh1 Rh2 O8 1.0(2) . . . . ? O5 Rh1 Rh2 O8 -87.5(2) . . . . ? O1 Rh1 Rh2 O6 -93.9(2) . . . . ? O3 Rh1 Rh2 O6 -179.4(2) . . . . ? O7 Rh1 Rh2 O6 87.6(2) . . . . ? O5 Rh1 Rh2 O6 -0.8(2) . . . . ? O1 Rh1 Rh2 O2 -1.8(2) . . . . ? O3 Rh1 Rh2 O2 -87.4(2) . . . . ? O7 Rh1 Rh2 O2 179.62(19) . . . . ? O5 Rh1 Rh2 O2 91.18(19) . . . . ? O1 Rh1 Rh2 O4 87.5(2) . . . . ? O3 Rh1 Rh2 O4 2.0(2) . . . . ? O7 Rh1 Rh2 O4 -91.03(19) . . . . ? O5 Rh1 Rh2 O4 -179.46(19) . . . . ? O3 Rh1 O1 C1 85.9(5) . . . . ? O7 Rh1 O1 C1 16(3) . . . . ? O5 Rh1 O1 C1 -90.2(5) . . . . ? Rh2 Rh1 O1 C1 -2.6(5) . . . . ? O8 Rh2 O2 C1 24(3) . . . . ? O6 Rh2 O2 C1 95.3(5) . . . . ? O4 Rh2 O2 C1 -80.3(5) . . . . ? Rh1 Rh2 O2 C1 7.0(5) . . . . ? O1 Rh1 O3 C22 -86.6(5) . . . . ? O7 Rh1 O3 C22 89.2(5) . . . . ? O5 Rh1 O3 C22 -18(3) . . . . ? Rh2 Rh1 O3 C22 1.8(5) . . . . ? O8 Rh2 O4 C22 -94.7(5) . . . . ? O6 Rh2 O4 C22 -24(3) . . . . ? O2 Rh2 O4 C22 80.7(5) . . . . ? Rh1 Rh2 O4 C22 -6.4(5) . . . . ? O1 Rh1 O5 C44 94.4(5) . . . . ? O3 Rh1 O5 C44 26(3) . . . . ? O7 Rh1 O5 C44 -81.4(5) . . . . ? Rh2 Rh1 O5 C44 6.2(5) . . . . ? O8 Rh2 O6 C44 84.2(5) . . . . ? O2 Rh2 O6 C44 -91.4(5) . . . . ? O4 Rh2 O6 C44 13(3) . . . . ? Rh1 Rh2 O6 C44 -4.3(5) . . . . ? O1 Rh1 O7 C23 -25(3) . . . . ? O3 Rh1 O7 C23 -94.5(5) . . . . ? O5 Rh1 O7 C23 81.4(5) . . . . ? Rh2 Rh1 O7 C23 -6.3(5) . . . . ? O6 Rh2 O8 C23 -84.5(5) . . . . ? O2 Rh2 O8 C23 -13(3) . . . . ? O4 Rh2 O8 C23 91.2(5) . . . . ? Rh1 Rh2 O8 C23 4.0(5) . . . . ? Rh2 O2 C1 O1 -11.6(9) . . . . ? Rh2 O2 C1 C2 168.7(4) . . . . ? Rh1 O1 C1 O2 9.3(10) . . . . ? Rh1 O1 C1 C2 -171.0(5) . . . . ? C5 O9 C2 C4 77.5(8) . . . . ? C5 O9 C2 C1 -49.8(9) . . . . ? C5 O9 C2 C3 -165.2(6) . . . . ? O2 C1 C2 O9 -28.2(9) . . . . ? O1 C1 C2 O9 152.1(6) . . . . ? O2 C1 C2 C4 -153.8(6) . . . . ? O1 C1 C2 C4 26.5(9) . . . . ? O2 C1 C2 C3 84.5(8) . . . . ? O1 C1 C2 C3 -95.2(8) . . . . ? C2 O9 C5 C18 -3.6(10) . . . . ? C2 O9 C5 C6 177.5(6) . . . . ? O9 C5 C6 C11 -177.5(6) . . . . ? C18 C5 C6 C11 3.6(10) . . . . ? O9 C5 C6 C7 -0.6(10) . . . . ? C18 C5 C6 C7 -179.6(7) . . . . ? C11 C6 C7 C9 -123.0(8) . . . . ? C5 C6 C7 C9 60.4(10) . . . . ? C11 C6 C7 C10 -4.6(11) . . . . ? C5 C6 C7 C10 178.7(8) . . . . ? C11 C6 C7 C8 114.3(8) . . . . ? C5 C6 C7 C8 -62.4(10) . . . . ? C5 C6 C11 C12 1.5(11) . . . . ? C7 C6 C11 C12 -175.4(7) . . . . ? C6 C11 C12 C17 -2.0(11) . . . . ? C6 C11 C12 C13 176.7(7) . . . . ? C11 C12 C13 C15 3.6(11) . . . . ? C17 C12 C13 C15 -177.7(8) . . . . ? C11 C12 C13 C14 122.6(8) . . . . ? C17 C12 C13 C14 -58.7(10) . . . . ? C11 C12 C13 C16 -115.0(8) . . . . ? C17 C12 C13 C16 63.6(10) . . . . ? C19 O10 C17 C12 -177.2(6) . . . . ? C19 O10 C17 C18 2.9(10) . . . . ? C11 C12 C17 O10 177.5(6) . . . . ? C13 C12 C17 O10 -1.2(10) . . . . ? C11 C12 C17 C18 -2.6(10) . . . . ? C13 C12 C17 C18 178.7(7) . . . . ? O9 C5 C18 C17 173.1(6) . . . . ? C6 C5 C18 C17 -8.0(10) . . . . ? O10 C17 C18 C5 -172.7(6) . . . . ? C12 C17 C18 C5 7.4(10) . . . . ? C17 O10 C19 C20 -76.4(8) . . . . ? C17 O10 C19 C22 50.2(9) . . . . ? C17 O10 C19 C21 165.9(6) . . . . ? Rh2 O4 C22 O3 10.3(10) . . . . ? Rh2 O4 C22 C19 -168.7(4) . . . . ? Rh1 O3 C22 O4 -7.9(10) . . . . ? Rh1 O3 C22 C19 171.1(5) . . . . ? O10 C19 C22 O4 27.8(9) . . . . ? C20 C19 C22 O4 152.8(7) . . . . ? C21 C19 C22 O4 -84.7(8) . . . . ? O10 C19 C22 O3 -151.3(6) . . . . ? C20 C19 C22 O3 -26.2(9) . . . . ? C21 C19 C22 O3 96.3(8) . . . . ? Rh1 O7 C23 O8 12.1(10) . . . . ? Rh1 O7 C23 C24 -169.4(4) . . . . ? Rh2 O8 C23 O7 -11.0(10) . . . . ? Rh2 O8 C23 C24 170.5(4) . . . . ? C27 O11 C24 C26 165.8(7) . . . . ? C27 O11 C24 C23 51.0(9) . . . . ? C27 O11 C24 C25 -75.0(9) . . . . ? O7 C23 C24 O11 28.4(9) . . . . ? O8 C23 C24 O11 -152.9(6) . . . . ? O7 C23 C24 C26 -84.4(8) . . . . ? O8 C23 C24 C26 94.3(8) . . . . ? O7 C23 C24 C25 153.1(7) . . . . ? O8 C23 C24 C25 -28.2(9) . . . . ? C24 O11 C27 C28 -177.9(6) . . . . ? C24 O11 C27 C40 1.0(10) . . . . ? O11 C27 C28 C33 177.5(6) . . . . ? C40 C27 C28 C33 -1.4(10) . . . . ? O11 C27 C28 C29 -0.6(10) . . . . ? C40 C27 C28 C29 -179.5(6) . . . . ? C27 C28 C29 C30 63.1(10) . . . . ? C33 C28 C29 C30 -114.9(8) . . . . ? C27 C28 C29 C31 -177.8(7) . . . . ? C33 C28 C29 C31 4.2(10) . . . . ? C27 C28 C29 C32 -58.5(9) . . . . ? C33 C28 C29 C32 123.5(7) . . . . ? C27 C28 C33 C34 -2.8(10) . . . . ? C29 C28 C33 C34 175.4(7) . . . . ? C28 C33 C34 C39 2.6(11) . . . . ? C28 C33 C34 C35 -174.8(7) . . . . ? C39 C34 C35 C38 -62.9(10) . . . . ? C33 C34 C35 C38 114.4(8) . . . . ? C39 C34 C35 C37 178.2(7) . . . . ? C33 C34 C35 C37 -4.6(10) . . . . ? C39 C34 C35 C36 58.7(9) . . . . ? C33 C34 C35 C36 -124.1(7) . . . . ? C41 O12 C39 C34 178.3(6) . . . . ? C41 O12 C39 C40 -0.5(10) . . . . ? C33 C34 C39 O12 -177.1(6) . . . . ? C35 C34 C39 O12 0.2(10) . . . . ? C33 C34 C39 C40 1.7(10) . . . . ? C35 C34 C39 C40 179.1(6) . . . . ? O12 C39 C40 C27 173.1(6) . . . . ? C34 C39 C40 C27 -5.7(10) . . . . ? O11 C27 C40 C39 -173.3(6) . . . . ? C28 C27 C40 C39 5.5(11) . . . . ? C39 O12 C41 C42 -165.7(7) . . . . ? C39 O12 C41 C43 75.0(9) . . . . ? C39 O12 C41 C44 -51.1(9) . . . . ? Rh1 O5 C44 O6 -12.3(10) . . . . ? Rh1 O5 C44 C41 169.7(5) . . . . ? Rh2 O6 C44 O5 11.3(10) . . . . ? Rh2 O6 C44 C41 -170.7(5) . . . . ? O12 C41 C44 O5 -28.3(9) . . . . ? C42 C41 C44 O5 84.0(8) . . . . ? C43 C41 C44 O5 -153.5(7) . . . . ? O12 C41 C44 O6 153.5(6) . . . . ? C42 C41 C44 O6 -94.2(8) . . . . ? C43 C41 C44 O6 28.3(9) . . . . ? C51 N1 C45 C46 149.6(11) . . . . ? C52 N1 C45 C46 25.3(12) . . . . ? C51 N1 C45 C50 -29.0(13) . . . . ? C52 N1 C45 C50 -153.3(10) . . . . ? C50 C45 C46 C47 -2.1(14) . . . . ? N1 C45 C46 C47 179.3(8) . . . . ? C45 C46 C47 C48 -0.1(16) . . . . ? C46 C47 C48 C49 2.6(15) . . . . ? C47 C48 C49 C50 -2.8(15) . . . . ? C46 C45 C50 C49 1.9(14) . . . . ? N1 C45 C50 C49 -179.5(8) . . . . ? C48 C49 C50 C45 0.6(16) . . . . ? Cl3' C53 Cl1 Cl2 109.7(13) . . . . ? Cl2' C53 Cl1 Cl2 29.1(7) . . . . ? Cl1' C53 Cl1 Cl2 163(2) . . . . ? Cl3 C53 Cl1 Cl2 144.1(12) . . . . ? Cl3' C53 Cl2 Cl1 -125.7(11) . . . . ? Cl2' C53 Cl2 Cl1 -125.0(12) . . . . ? Cl1' C53 Cl2 Cl1 -5.3(6) . . . . ? Cl3 C53 Cl2 Cl1 -125.3(16) . . . . ? Cl1 C53 Cl2' Cl3' 118.6(11) . . . . ? Cl1' C53 Cl2' Cl3' 103.5(13) . . . . ? Cl3 C53 Cl2' Cl3' 0.5(7) . . . . ? Cl2 C53 Cl2' Cl3' -179.3(12) . . . . ? Cl1 C53 Cl3' Cl2' -104.7(12) . . . . ? Cl1' C53 Cl3' Cl2' -119.8(11) . . . . ? Cl3 C53 Cl3' Cl2' -179.1(12) . . . . ? Cl2 C53 Cl3' Cl2' 0.4(7) . . . . ? Cl5 C54 Cl4 Cl6 51.4(13) . . . . ? Cl6' C54 Cl4 Cl6 -20.1(9) . . . . ? Cl5' C54 Cl4 Cl6 103.1(14) . . . . ? Cl4' C54 Cl4 Cl6 144.5(9) . . . . ? Cl6' C54 Cl5 Cl6 -19.3(9) . . . . ? Cl4 C54 Cl5 Cl6 -60.9(14) . . . . ? Cl5' C54 Cl5 Cl6 -152.4(11) . . . . ? Cl4' C54 Cl5 Cl6 -141.6(9) . . . . ? C54 Cl5 Cl6 Cl4 20.9(6) . . . . ? Cl6' C54 Cl6 Cl5 159.8(10) . . . . ? Cl4 C54 Cl6 Cl5 145.2(10) . . . . ? Cl5' C54 Cl6 Cl5 17.1(6) . . . . ? Cl4' C54 Cl6 Cl5 79.8(15) . . . . ? Cl5 C54 Cl6 Cl4 -145.2(10) . . . . ? Cl6' C54 Cl6 Cl4 14.6(7) . . . . ? Cl5' C54 Cl6 Cl4 -128.1(11) . . . . ? Cl4' C54 Cl6 Cl4 -65.4(14) . . . . ? C54 Cl4 Cl6 Cl5 -25.7(8) . . . . ? Cl5 C54 Cl4' Cl5' -7.3(8) . . . . ? Cl6' C54 Cl4' Cl5' -134.9(12) . . . . ? Cl4 C54 Cl4' Cl5' -144.9(10) . . . . ? Cl6 C54 Cl4' Cl5' -73.0(15) . . . . ? Cl5 C54 Cl5' Cl4' 168.7(12) . . . . ? Cl6' C54 Cl5' Cl4' 94.0(16) . . . . ? Cl4 C54 Cl5' Cl4' 43.4(11) . . . . ? Cl6 C54 Cl5' Cl4' 143.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 24.13 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.164 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.090 data_r31 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 N2 O10 Rh2' _chemical_formula_weight 874.58 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_cell_setting 'rhombohedral' _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 31.600(4) _cell_length_b 31.600(4) _cell_length_c 12.700(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10983(3) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type 'STOE IPDS' _diffrn_measurement_method 'IMAGE PLATE' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19768 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 22.48 _reflns_number_total 6376 _reflns_number_gt 5500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+98.6359P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(12) _refine_ls_number_reflns 6376 _refine_ls_number_parameters 421 _refine_ls_number_restraints 574 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 4.489 _refine_ls_shift/su_mean 0.408 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 Rh1 Rh 0.46190(7) 0.00012(8) 0.8030(3) 0.0430(6) Uani 1 d D . . Rh2 Rh 0.53809(7) 0.00007(8) 0.8036(3) 0.0408(6) Uani 1 d D . . O1 O 0.4773(4) 0.0256(6) 0.6513(6) 0.050(3) Uani 1 d DU . . O2 O 0.5482(4) 0.0249(6) 0.6510(6) 0.055(3) Uani 1 d DU . . C1 C 0.5187(3) 0.0371(4) 0.6142(5) 0.062(3) Uani 1 d DU . . C2 C 0.5343(4) 0.0670(3) 0.5104(6) 0.073(3) Uani 1 d DU . . C3 C 0.5150(7) 0.0321(4) 0.4142(8) 0.082(4) Uani 1 d DU . . H3A H 0.5272 0.0097 0.4172 0.124 Uiso 1 calc R . . H3B H 0.5259 0.0508 0.3504 0.124 Uiso 1 calc R . . H3C H 0.4799 0.0141 0.4155 0.124 Uiso 1 calc R . . C4 C 0.5110(6) 0.1000(6) 0.4980(11) 0.059(4) Uani 1 d DU . . H4A H 0.5234 0.1246 0.5518 0.088 Uiso 1 calc R . . H4B H 0.4762 0.0804 0.5044 0.088 Uiso 1 calc R . . H4C H 0.5192 0.1153 0.4300 0.088 Uiso 1 calc R . . O5 O 0.5870(5) 0.1012(4) 0.4841(9) 0.084(3) Uani 1 d DU . . C6 C 0.6166(4) 0.1310(3) 0.5664(6) 0.082(3) Uani 1 d DU . . O3 O 0.4998(2) 0.0707(2) 0.8566(12) 0.051(3) Uani 1 d DU . . O4 O 0.5712(2) 0.0714(2) 0.8523(13) 0.055(3) Uani 1 d DU . . C14 C 0.5459(2) 0.0923(2) 0.8579(8) 0.052(2) Uani 1 d DU . . C11 C 0.5738(4) 0.1482(2) 0.8763(6) 0.059(2) Uani 1 d DU . . C12 C 0.5788(7) 0.1613(4) 0.9956(7) 0.070(3) Uani 1 d DU . . H12A H 0.5960 0.1475 1.0305 0.105 Uiso 1 calc R . . H12B H 0.5469 0.1484 1.0261 0.105 Uiso 1 calc R . . H12C H 0.5966 0.1962 1.0037 0.105 Uiso 1 calc R . . C13 C 0.5470(5) 0.1741(4) 0.8309(14) 0.049(3) Uani 1 d DU . . H13A H 0.5449 0.1706 0.7557 0.073 Uiso 1 calc R . . H13B H 0.5649 0.2082 0.8488 0.073 Uiso 1 calc R . . H13C H 0.5147 0.1595 0.8602 0.073 Uiso 1 calc R . . O6 O 0.6251(5) 0.1803(4) 0.8372(9) 0.077(3) Uani 1 d DU . . C10 C 0.6348(4) 0.1690(3) 0.7368(7) 0.083(3) Uani 1 d DU . . C5 C 0.6009(4) 0.1385(4) 0.6630(6) 0.083(3) Uani 1 d DU . . H5 H 0.5677 0.1230 0.6783 0.099 Uiso 1 calc R . . C7 C 0.6662(4) 0.1541(4) 0.5441(7) 0.095(3) Uani 1 d DU . . H7 H 0.6768 0.1492 0.4794 0.114 Uiso 1 calc R . . C8 C 0.7001(4) 0.1847(5) 0.6179(8) 0.094(3) Uani 1 d DU . . H8 H 0.7333 0.2002 0.6027 0.113 Uiso 1 calc R . . C9 C 0.6843(4) 0.1921(4) 0.7146(8) 0.087(3) Uani 1 d DU . . H9 H 0.7070 0.2125 0.7643 0.105 Uiso 1 calc R . . O7 O 0.4287(2) -0.0711(3) 0.7545(14) 0.051(3) Uani 1 d DU . . O8 O 0.5002(3) -0.0713(2) 0.7577(13) 0.051(3) Uani 1 d DU . . C15 C 0.4549(3) -0.0904(2) 0.7397(4) 0.055(3) Uani 1 d DU . . C16 C 0.4294(5) -0.1429(3) 0.6950(12) 0.089(4) Uani 1 d DU . . H16A H 0.4522 -0.1546 0.6929 0.133 Uiso 1 calc R . . H16B H 0.4179 -0.1429 0.6250 0.133 Uiso 1 calc R . . H16C H 0.4022 -0.1639 0.7391 0.133 Uiso 1 calc R . . O9 O 0.4521(4) -0.0242(7) 0.9552(7) 0.055(3) Uani 1 d DU . . O10 O 0.5229(4) -0.0255(6) 0.9547(6) 0.054(3) Uani 1 d DU . . C17 C 0.4839(3) -0.0318(3) 0.9972(5) 0.056(3) Uani 1 d DU . . C18 C 0.4740(5) -0.0509(6) 1.1121(6) 0.082(4) Uani 1 d DU . . H18A H 0.4986 -0.0584 1.1336 0.123 Uiso 1 calc R . . H18B H 0.4424 -0.0798 1.1162 0.123 Uiso 1 calc R . . H18C H 0.4748 -0.0262 1.1576 0.123 Uiso 1 calc R . . N1 N 0.3914(4) -0.0002(7) 0.812(2) 0.054(3) Uani 1 d DU . . C21 C 0.3856(6) 0.0366(8) 0.773(2) 0.058(4) Uani 1 d DU . . H21 H 0.4141 0.0652 0.7551 0.069 Uiso 1 calc R . . C22 C 0.3431(6) 0.0364(7) 0.7568(18) 0.056(3) Uani 1 d DU . . H22 H 0.3416 0.0599 0.7155 0.067 Uiso 1 calc R . . C23 C 0.3015(5) -0.0013(7) 0.806(2) 0.050(3) Uani 1 d DU . . C24 C 0.3065(6) -0.0390(7) 0.837(2) 0.054(3) Uani 1 d DU . . H24 H 0.2783 -0.0684 0.8520 0.065 Uiso 1 calc R . . C25 C 0.3502(6) -0.0369(7) 0.8468(18) 0.051(3) Uani 1 d DU . . H25 H 0.3511 -0.0627 0.8799 0.061 Uiso 1 calc R . . C26 C 0.2507(5) -0.0068(5) 0.8012(12) 0.057(3) Uani 1 d DU . . C27 C 0.2492(6) 0.0241(7) 0.7135(13) 0.068(4) Uiso 1 d DU . . H27A H 0.2174 0.0209 0.7105 0.102 Uiso 1 calc R . . H27B H 0.2560 0.0135 0.6479 0.102 Uiso 1 calc R . . H27C H 0.2734 0.0576 0.7257 0.102 Uiso 1 calc R . . C28 C 0.2419(7) 0.0132(8) 0.9063(13) 0.080(4) Uiso 1 d DU . . H28A H 0.2106 0.0111 0.9041 0.120 Uiso 1 calc R . . H28B H 0.2670 0.0467 0.9153 0.120 Uiso 1 calc R . . H28C H 0.2429 -0.0058 0.9642 0.120 Uiso 1 calc R . . C29 C 0.2067(5) -0.0595(5) 0.7923(16) 0.068(4) Uiso 1 d DU . . H29A H 0.1769 -0.0585 0.7890 0.102 Uiso 1 calc R . . H29B H 0.2061 -0.0781 0.8528 0.102 Uiso 1 calc R . . H29C H 0.2100 -0.0746 0.7297 0.102 Uiso 1 calc R . . N2 N 0.6087(4) 0.0005(7) 0.8029(18) 0.046(3) Uani 1 d DU . . C31 C 0.6501(6) 0.0399(8) 0.775(2) 0.050(3) Uani 1 d DU . . H31 H 0.6492 0.0680 0.7572 0.060 Uiso 1 calc R . . C32 C 0.6953(6) 0.0415(7) 0.7719(19) 0.056(3) Uani 1 d DU . . H32 H 0.7234 0.0697 0.7509 0.067 Uiso 1 calc R . . C33 C 0.6969(5) -0.0005(7) 0.801(2) 0.049(3) Uani 1 d DU . . C34 C 0.6536(6) -0.0397(7) 0.836(2) 0.052(3) Uani 1 d DU . . H34 H 0.6534 -0.0678 0.8589 0.062 Uiso 1 calc R . . C35 C 0.6105(6) -0.0381(8) 0.840(2) 0.052(3) Uani 1 d DU . . H35 H 0.5825 -0.0644 0.8679 0.062 Uiso 1 calc R . . C36 C 0.7460(5) 0.0009(6) 0.8021(13) 0.051(3) Uani 1 d DU . . C37 C 0.7873(6) 0.0451(7) 0.7540(16) 0.079(4) Uiso 1 d DU . . H37A H 0.8168 0.0436 0.7613 0.118 Uiso 1 calc R . . H37B H 0.7911 0.0737 0.7889 0.118 Uiso 1 calc R . . H37C H 0.7807 0.0464 0.6807 0.118 Uiso 1 calc R . . C38 C 0.7408(8) -0.0440(7) 0.7435(17) 0.094(4) Uiso 1 d DU . . H38A H 0.7717 -0.0429 0.7428 0.141 Uiso 1 calc R . . H38B H 0.7305 -0.0440 0.6724 0.141 Uiso 1 calc R . . H38C H 0.7170 -0.0732 0.7786 0.141 Uiso 1 calc R . . C39 C 0.7591(6) -0.0022(7) 0.9168(11) 0.062(4) Uiso 1 d DU . . H39A H 0.7910 0.0010 0.9198 0.094 Uiso 1 calc R . . H39B H 0.7355 -0.0332 0.9458 0.094 Uiso 1 calc R . . H39C H 0.7592 0.0236 0.9567 0.094 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0392(13) 0.0717(15) 0.0277(12) -0.0058(9) -0.0028(9) 0.0350(12) Rh2 0.0370(14) 0.0667(15) 0.0269(12) -0.0051(9) -0.0010(8) 0.0319(12) O1 0.057(7) 0.090(6) 0.028(5) -0.012(5) -0.011(6) 0.055(6) O2 0.061(7) 0.090(6) 0.036(5) -0.010(5) -0.012(6) 0.054(6) C1 0.065(6) 0.098(5) 0.034(4) -0.008(4) -0.010(5) 0.049(6) C2 0.066(5) 0.115(5) 0.042(4) -0.006(4) 0.000(5) 0.048(5) C3 0.070(8) 0.121(8) 0.042(6) -0.014(6) 0.016(9) 0.036(9) C4 0.058(8) 0.109(8) 0.028(6) 0.031(6) 0.007(6) 0.056(7) O5 0.072(5) 0.119(5) 0.058(4) -0.003(4) 0.004(4) 0.046(5) C6 0.070(5) 0.111(5) 0.070(4) -0.002(4) 0.009(4) 0.050(4) O3 0.052(6) 0.076(6) 0.045(5) -0.021(5) -0.007(6) 0.046(6) O4 0.055(7) 0.074(6) 0.049(5) -0.017(5) -0.011(6) 0.042(6) C14 0.054(5) 0.073(5) 0.045(4) -0.020(4) -0.012(6) 0.044(5) C11 0.058(5) 0.074(4) 0.057(4) -0.030(3) -0.009(5) 0.041(5) C12 0.075(8) 0.074(6) 0.054(6) -0.022(5) -0.029(9) 0.032(8) C13 0.046(7) 0.022(5) 0.063(7) -0.021(5) -0.008(7) 0.006(5) O6 0.073(5) 0.085(5) 0.075(4) -0.017(4) -0.001(5) 0.041(4) C10 0.072(4) 0.096(5) 0.084(4) -0.007(4) 0.002(4) 0.043(4) C5 0.073(5) 0.104(5) 0.077(5) -0.004(4) -0.001(4) 0.049(4) C7 0.077(5) 0.114(6) 0.082(5) -0.002(5) 0.011(5) 0.038(5) C8 0.079(5) 0.107(6) 0.092(5) -0.007(5) 0.011(5) 0.043(5) C9 0.068(5) 0.103(6) 0.090(5) -0.007(5) 0.011(5) 0.043(5) O7 0.036(8) 0.069(6) 0.046(5) -0.008(5) 0.008(7) 0.025(7) O8 0.044(8) 0.067(6) 0.045(5) -0.011(5) 0.011(7) 0.030(7) C15 0.043(8) 0.073(5) 0.046(5) -0.016(4) 0.007(7) 0.025(7) C16 0.059(10) 0.104(8) 0.094(8) -0.055(7) -0.001(11) 0.033(10) O9 0.042(8) 0.100(6) 0.025(5) 0.006(5) 0.002(6) 0.038(7) O10 0.037(8) 0.099(6) 0.029(5) 0.006(5) -0.011(6) 0.037(7) C17 0.042(8) 0.105(6) 0.024(4) 0.007(4) -0.001(6) 0.037(7) C18 0.052(10) 0.150(9) 0.031(6) 0.016(7) 0.012(10) 0.040(10) N1 0.054(6) 0.067(6) 0.046(6) 0.005(5) 0.000(6) 0.035(5) C21 0.055(6) 0.068(6) 0.054(6) 0.008(5) 0.006(6) 0.034(6) C22 0.056(6) 0.070(5) 0.052(6) 0.012(5) 0.011(5) 0.040(5) C23 0.052(5) 0.071(5) 0.042(5) 0.011(4) 0.010(5) 0.042(5) C24 0.054(6) 0.069(5) 0.046(6) 0.011(5) 0.006(5) 0.037(5) C25 0.052(6) 0.067(6) 0.048(6) 0.012(5) 0.004(5) 0.040(5) C26 0.056(5) 0.076(5) 0.047(4) 0.017(4) 0.008(4) 0.039(4) N2 0.042(6) 0.082(6) 0.027(5) -0.004(5) 0.003(5) 0.040(5) C31 0.045(6) 0.080(6) 0.033(5) 0.004(5) 0.001(5) 0.037(5) C32 0.048(6) 0.084(6) 0.034(5) 0.010(5) 0.004(5) 0.031(5) C33 0.049(5) 0.081(5) 0.028(4) 0.011(4) 0.008(5) 0.042(5) C34 0.051(6) 0.080(6) 0.033(5) 0.009(5) 0.007(5) 0.040(5) C35 0.045(6) 0.082(6) 0.033(5) 0.006(5) 0.002(5) 0.035(5) C36 0.053(4) 0.079(5) 0.042(4) 0.019(4) 0.004(5) 0.049(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 Rh1 O9 2.045(4) . ? Rh1 O7 2.046(4) . ? Rh1 O3 2.049(4) . ? Rh1 O1 2.051(4) . ? Rh1 N1 2.225(5) . ? Rh1 Rh2 2.4083(8) . ? Rh2 O8 2.040(4) . ? Rh2 O10 2.044(4) . ? Rh2 O4 2.049(4) . ? Rh2 O2 2.055(4) . ? Rh2 N2 2.223(5) . ? O1 C1 1.262(4) . ? O2 C1 1.263(4) . ? C1 C2 1.551(7) . ? C2 O5 1.501(14) . ? C2 C3 1.552(9) . ? C2 C4 1.554(9) . ? O5 C6 1.405(13) . ? C6 C7 1.387(8) . ? C6 C5 1.388(8) . ? O3 C14 1.263(4) . ? O4 C14 1.267(4) . ? C14 C11 1.549(7) . ? C11 O6 1.503(14) . ? C11 C13 1.552(9) . ? C11 C12 1.558(9) . ? O6 C10 1.399(13) . ? C10 C9 1.386(8) . ? C10 C5 1.387(8) . ? C7 C8 1.386(8) . ? C8 C9 1.387(8) . ? O7 C15 1.263(4) . ? O8 C15 1.264(4) . ? C15 C16 1.546(7) . ? O9 C17 1.265(4) . ? O10 C17 1.266(4) . ? C17 C18 1.549(7) . ? N1 C25 1.313(12) . ? N1 C21 1.359(12) . ? C21 C22 1.357(13) . ? C22 C23 1.403(12) . ? C23 C24 1.335(12) . ? C23 C26 1.529(12) . ? C24 C25 1.357(12) . ? C26 C27 1.496(13) . ? C26 C29 1.551(13) . ? C26 C28 1.560(13) . ? N2 C31 1.325(12) . ? N2 C35 1.336(12) . ? C31 C32 1.403(13) . ? C32 C33 1.405(13) . ? C33 C34 1.384(12) . ? C33 C36 1.530(11) . ? C34 C35 1.388(13) . ? C36 C37 1.483(13) . ? C36 C39 1.531(13) . ? C36 C38 1.537(14) . ? 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 O9 Rh1 O7 88.5(8) . . ? O9 Rh1 O3 89.5(7) . . ? O7 Rh1 O3 175.1(4) . . ? O9 Rh1 O1 175.5(3) . . ? O7 Rh1 O1 92.2(7) . . ? O3 Rh1 O1 89.4(7) . . ? O9 Rh1 N1 89.1(6) . . ? O7 Rh1 N1 92.8(6) . . ? O3 Rh1 N1 91.5(6) . . ? O1 Rh1 N1 95.2(6) . . ? O9 Rh1 Rh2 87.80(17) . . ? O7 Rh1 Rh2 87.86(18) . . ? O3 Rh1 Rh2 87.65(18) . . ? O1 Rh1 Rh2 87.83(17) . . ? N1 Rh1 Rh2 176.8(6) . . ? O8 Rh2 O10 86.5(7) . . ? O8 Rh2 O4 175.7(3) . . ? O10 Rh2 O4 92.4(7) . . ? O8 Rh2 O2 92.6(7) . . ? O10 Rh2 O2 175.8(3) . . ? O4 Rh2 O2 88.2(8) . . ? O8 Rh2 N2 92.2(6) . . ? O10 Rh2 N2 92.5(6) . . ? O4 Rh2 N2 92.0(6) . . ? O2 Rh2 N2 91.7(5) . . ? O8 Rh2 Rh1 88.01(18) . . ? O10 Rh2 Rh1 88.02(18) . . ? O4 Rh2 Rh1 87.76(18) . . ? O2 Rh2 Rh1 87.81(18) . . ? N2 Rh2 Rh1 179.5(5) . . ? C1 O1 Rh1 118.2(3) . . ? C1 O2 Rh2 117.9(4) . . ? O1 C1 O2 126.2(5) . . ? O1 C1 C2 117.4(5) . . ? O2 C1 C2 116.3(5) . . ? O5 C2 C1 121.8(7) . . ? O5 C2 C3 103.7(6) . . ? C1 C2 C3 110.1(6) . . ? O5 C2 C4 102.7(6) . . ? C1 C2 C4 112.5(6) . . ? C3 C2 C4 104.3(10) . . ? C6 O5 C2 116.5(9) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 O5 113.7(8) . . ? C5 C6 O5 126.5(8) . . ? C14 O3 Rh1 118.7(4) . . ? C14 O4 Rh2 118.8(4) . . ? O3 C14 O4 125.1(5) . . ? O3 C14 C11 117.5(5) . . ? O4 C14 C11 117.2(4) . . ? O6 C11 C14 121.8(7) . . ? O6 C11 C13 102.1(6) . . ? C14 C11 C13 113.4(6) . . ? O6 C11 C12 102.1(7) . . ? C14 C11 C12 112.0(6) . . ? C13 C11 C12 103.3(10) . . ? C10 O6 C11 115.4(9) . . ? C9 C10 C5 120.3(3) . . ? C9 C10 O6 112.7(8) . . ? C5 C10 O6 127.0(8) . . ? C10 C5 C6 119.9(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 120.0(3) . . ? C10 C9 C8 119.8(3) . . ? C15 O7 Rh1 118.4(4) . . ? C15 O8 Rh2 118.5(4) . . ? O7 C15 O8 127.0(5) . . ? O7 C15 C16 117.1(5) . . ? O8 C15 C16 115.9(5) . . ? C17 O9 Rh1 118.9(3) . . ? C17 O10 Rh2 118.7(3) . . ? O9 C17 O10 126.5(5) . . ? O9 C17 C18 116.5(5) . . ? O10 C17 C18 117.0(5) . . ? C25 N1 C21 112.4(9) . . ? C25 N1 Rh1 124.7(11) . . ? C21 N1 Rh1 122.7(11) . . ? N1 C21 C22 127.5(14) . . ? C21 C22 C23 116.2(14) . . ? C24 C23 C22 114.3(10) . . ? C24 C23 C26 119.7(12) . . ? C22 C23 C26 124.2(12) . . ? C23 C24 C25 123.7(14) . . ? N1 C25 C24 123.2(14) . . ? C27 C26 C23 109.2(11) . . ? C27 C26 C29 110.1(12) . . ? C23 C26 C29 116.7(11) . . ? C27 C26 C28 107.7(12) . . ? C23 C26 C28 108.1(13) . . ? C29 C26 C28 104.6(11) . . ? C31 N2 C35 118.5(9) . . ? C31 N2 Rh2 121.6(11) . . ? C35 N2 Rh2 119.6(11) . . ? N2 C31 C32 123.5(13) . . ? C31 C32 C33 118.5(13) . . ? C34 C33 C32 116.3(10) . . ? C34 C33 C36 123.9(12) . . ? C32 C33 C36 119.5(12) . . ? C33 C34 C35 121.8(14) . . ? N2 C35 C34 120.9(13) . . ? C37 C36 C33 115.2(12) . . ? C37 C36 C39 108.3(12) . . ? C33 C36 C39 108.1(12) . . ? C37 C36 C38 107.9(12) . . ? C33 C36 C38 109.2(13) . . ? C39 C36 C38 108.0(12) . . ? _diffrn_measured_fraction_theta_max 0.333 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.333 _refine_diff_density_max 1.186 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.122