Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Satoshi Takamizawa' _publ_contact_author_address ;International Graduate School of Arts and Sciences Yokohama City University 22-2 Seto, Kanazawa-ku, Yokohama 236-0027 (Japan) ; _publ_contact_author_email staka@yokohama-cu.ac.jp _publ_contact_author_phone (+81)45-787-2187 _publ_contact_author_fax (+81)45-787-2187 _publ_section_title ; Closed-pore Crystal Capable of Adsorbing CO2 onto Isolated Cavities Generated by Disorderly Mixing of Substituents on Host Skeleton ; loop_ _publ_author_name 'Satoshi Takamizawa' 'Masa-aki Kohbara' data_51019k1 _database_code_depnum_ccdc_archive 'CCDC 642578' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H30 N2 O8 Rh2' _chemical_formula_weight 812.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5247(16) _cell_length_b 10.5607(16) _cell_length_c 15.696(2) _cell_angle_alpha 80.483(3) _cell_angle_beta 80.585(3) _cell_angle_gamma 88.619(3) _cell_volume 1697.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5783 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12611 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8279 _reflns_number_gt 6518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.6179P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8279 _refine_ls_number_parameters 456 _refine_ls_number_restraints 607 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.045 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3725(3) 1.2140(3) 0.0104(2) 0.0381(7) Uani 1 1 d U . . C2 C 0.3019(4) 1.3353(3) 0.0185(2) 0.0459(8) Uani 1 1 d U . . C3 C 0.1833(5) 1.3360(5) 0.0721(3) 0.0727(13) Uani 1 1 d U . . H3 H 0.1467 1.2588 0.1022 0.087 Uiso 1 1 calc R . . C4 C 0.1189(6) 1.4493(6) 0.0812(4) 0.0945(17) Uani 1 1 d U . . H4 H 0.0386 1.4483 0.1164 0.113 Uiso 1 1 calc R . . C5 C 0.1733(6) 1.5630(5) 0.0384(4) 0.0927(16) Uani 1 1 d U . . H5 H 0.1314 1.6398 0.0461 0.111 Uiso 1 1 calc R . . C6 C 0.2873(6) 1.5645(5) -0.0148(4) 0.0908(16) Uani 1 1 d U . . H6 H 0.3226 1.6423 -0.0448 0.109 Uiso 1 1 calc R . . C7 C 0.3527(5) 1.4515(4) -0.0254(3) 0.0720(13) Uani 1 1 d U . . H7 H 0.4316 1.4540 -0.0624 0.086 Uiso 1 1 calc R . . C8 C 0.6132(3) 1.0423(3) 0.1293(2) 0.0382(8) Uani 1 1 d U . . C9 C 0.6761(4) 1.0730(3) 0.2014(2) 0.0419(8) Uani 1 1 d U . . C10 C 0.7881(4) 1.1447(4) 0.1823(3) 0.0541(10) Uani 1 1 d U . . H10 H 0.8241 1.1725 0.1242 0.065 Uiso 1 1 calc R . . C11 C 0.8474(5) 1.1754(5) 0.2484(3) 0.0656(12) Uani 1 1 d U . . H11 H 0.9229 1.2237 0.2350 0.079 Uiso 1 1 calc R . . C12 C 0.7940(5) 1.1341(5) 0.3346(3) 0.0715(13) Uani 1 1 d U . . H12 H 0.8335 1.1540 0.3796 0.086 Uiso 1 1 calc R . . C13 C 0.6828(5) 1.0637(5) 0.3534(3) 0.0720(13) Uani 1 1 d U . . H13 H 0.6464 1.0365 0.4115 0.086 Uiso 1 1 calc R . . C14 C 0.6243(4) 1.0329(4) 0.2876(2) 0.0591(11) Uani 1 1 d U . . H14 H 0.5490 0.9844 0.3014 0.071 Uiso 1 1 calc R . . C15 C 0.2201(3) 0.5513(3) 0.5430(2) 0.0426(8) Uani 1 1 d U . . C16 C 0.3418(4) 0.5889(4) 0.5697(3) 0.0537(10) Uani 1 1 d U . . C17 C 0.4357(4) 0.6557(5) 0.5098(4) 0.0722(13) Uani 1 1 d U . . H17 H 0.4249 0.6778 0.4515 0.087 Uiso 1 1 calc R . . C18 C 0.5475(5) 0.6904(6) 0.5367(5) 0.0947(17) Uani 1 1 d U . . H18 H 0.6126 0.7350 0.4965 0.114 Uiso 1 1 calc R . . C19 C 0.5608(6) 0.6584(6) 0.6227(5) 0.1072(19) Uani 1 1 d U . . H19 H 0.6357 0.6822 0.6403 0.129 Uiso 1 1 calc R . . C20 C 0.4686(6) 0.5930(6) 0.6834(4) 0.1037(18) Uani 1 1 d U . . H20 H 0.4791 0.5730 0.7418 0.124 Uiso 1 1 calc R . . C21 C 0.3585(5) 0.5570(5) 0.6561(4) 0.0799(14) Uani 1 1 d U . . H21 H 0.2947 0.5105 0.6964 0.096 Uiso 1 1 calc R . . C22 C -0.0902(3) 0.7048(3) 0.5614(2) 0.0374(7) Uani 1 1 d U . . C23 C -0.1404(3) 0.8217(3) 0.5973(2) 0.0385(8) Uani 1 1 d U . . C24 C -0.1846(4) 0.8152(4) 0.6861(2) 0.0471(9) Uani 1 1 d U . . H24 H -0.1764 0.7391 0.7242 0.057 Uiso 1 1 calc R . . C25 C -0.2404(4) 0.9203(4) 0.7184(3) 0.0574(10) Uani 1 1 d U . . H25 H -0.2713 0.9147 0.7779 0.069 Uiso 1 1 calc R . . C26 C -0.2502(4) 1.0327(4) 0.6631(3) 0.0604(11) Uani 1 1 d U . . H26 H -0.2887 1.1033 0.6851 0.073 Uiso 1 1 calc R . . C27 C -0.2039(4) 1.0426(4) 0.5751(3) 0.0600(11) Uani 1 1 d U . . H27 H -0.2093 1.1202 0.5380 0.072 Uiso 1 1 calc R . . C28 C -0.1492(4) 0.9369(4) 0.5419(2) 0.0495(9) Uani 1 1 d U . . H28 H -0.1183 0.9432 0.4824 0.059 Uiso 1 1 calc R . . C29 C 0.3146(3) 0.7219(3) 0.2012(2) 0.0393(8) Uani 1 1 d U . . H29 H 0.4018 0.7035 0.1884 0.047 Uiso 1 1 calc R . . C30 C 0.2402(3) 0.6500(3) 0.2711(2) 0.0397(8) Uani 1 1 d U . . H30 H 0.2777 0.5825 0.3042 0.048 Uiso 1 1 calc R . . C31 C 0.0616(3) 0.7674(3) 0.2417(2) 0.0412(8) Uani 1 1 d U . . C32 C 0.1377(3) 0.8392(3) 0.1681(2) 0.0384(8) Uani 1 1 d U . . C33A C -0.0826(6) 0.7891(7) 0.2607(4) 0.0563(17) Uani 0.870(6) 1 d PU . . H33A H -0.0991 0.8807 0.2512 0.068 Uiso 0.870(6) 1 calc PR . . H33B H -0.1133 0.7564 0.3220 0.068 Uiso 0.870(6) 1 calc PR . . C34A C -0.1590(6) 0.7255(7) 0.2051(4) 0.094(2) Uani 0.870(6) 1 d PU . . H34A H -0.1372 0.7648 0.1449 0.141 Uiso 0.870(6) 1 calc PR . . H34B H -0.2495 0.7358 0.2244 0.141 Uiso 0.870(6) 1 calc PR . . H34C H -0.1387 0.6357 0.2108 0.141 Uiso 0.870(6) 1 calc PR . . C35A C 0.0809(7) 0.9397(10) 0.1059(5) 0.0546(19) Uani 0.870(6) 1 d PU . . H35A H 0.1411 0.9601 0.0526 0.082 Uiso 0.870(6) 1 calc PR . . H35B H 0.0628 1.0155 0.1320 0.082 Uiso 0.870(6) 1 calc PR . . H35C H 0.0026 0.9076 0.0933 0.082 Uiso 0.870(6) 1 calc PR . . C33B C 0.058(5) 0.939(7) 0.120(4) 0.043(5) Uani 0.130(6) 1 d PDU . . H33C H 0.1131 0.9981 0.0769 0.052 Uiso 0.130(6) 1 calc PR . . H33D H 0.0069 0.9873 0.1612 0.052 Uiso 0.130(6) 1 calc PR . . C34B C -0.033(3) 0.861(3) 0.075(2) 0.060(7) Uani 0.130(6) 1 d PDU . . H34D H 0.0114 0.8478 0.0185 0.090 Uiso 0.130(6) 1 calc PR . . H34E H -0.1103 0.9090 0.0677 0.090 Uiso 0.130(6) 1 calc PR . . H34F H -0.0549 0.7793 0.1108 0.090 Uiso 0.130(6) 1 calc PR . . C35B C -0.065(4) 0.807(4) 0.287(2) 0.035(6) Uani 0.130(6) 1 d PU . . H35D H -0.1263 0.7383 0.2956 0.053 Uiso 0.130(6) 1 calc PR . . H35E H -0.0962 0.8814 0.2526 0.053 Uiso 0.130(6) 1 calc PR . . H35F H -0.0554 0.8275 0.3433 0.053 Uiso 0.130(6) 1 calc PR . . N1 N 0.2641(3) 0.8188(3) 0.15046(17) 0.0366(6) Uani 1 1 d U . . N2 N 0.1142(3) 0.6743(3) 0.29356(18) 0.0404(7) Uani 1 1 d U . . O1 O 0.3232(2) 1.1117(2) 0.05585(15) 0.0416(6) Uani 1 1 d U . . O2 O 0.4792(2) 1.2211(2) -0.04101(15) 0.0433(6) Uani 1 1 d U . . O3 O 0.6665(2) 1.0874(2) 0.05200(14) 0.0432(6) Uani 1 1 d U . . O4 O 0.5114(2) 0.9754(2) 0.14859(14) 0.0425(6) Uani 1 1 d U . . O5 O 0.2018(2) 0.5968(2) 0.46575(16) 0.0462(6) Uani 1 1 d U . . O6 O 0.1437(2) 0.4794(2) 0.59966(16) 0.0458(6) Uani 1 1 d U . . O7 O -0.0999(2) 0.6005(2) 0.61436(15) 0.0441(6) Uani 1 1 d U . . O8 O -0.0424(2) 0.7182(2) 0.48055(15) 0.0444(6) Uani 1 1 d U . . Rh1 Rh 0.41634(2) 0.94114(2) 0.051355(15) 0.03235(8) Uani 1 1 d U . . Rh2 Rh 0.03132(2) 0.56237(2) 0.428668(16) 0.03433(8) Uani 1 1 d U . . 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 0.0446(19) 0.0362(17) 0.0302(16) -0.0028(13) 0.0006(14) 0.0018(14) C2 0.054(2) 0.0354(18) 0.0475(19) -0.0077(15) -0.0060(16) 0.0082(16) C3 0.075(3) 0.057(3) 0.074(3) -0.005(2) 0.015(2) 0.021(2) C4 0.089(3) 0.082(3) 0.100(4) -0.015(3) 0.018(3) 0.034(3) C5 0.103(4) 0.057(3) 0.119(4) -0.025(3) -0.013(3) 0.028(3) C6 0.092(3) 0.045(2) 0.130(4) -0.004(3) -0.013(3) 0.005(2) C7 0.065(3) 0.044(2) 0.099(3) 0.000(2) -0.005(2) 0.006(2) C8 0.0435(19) 0.0384(18) 0.0295(15) -0.0038(13) 0.0009(14) 0.0050(15) C9 0.0479(19) 0.0396(18) 0.0356(17) -0.0031(14) -0.0037(15) 0.0086(15) C10 0.058(2) 0.055(2) 0.049(2) -0.0048(18) -0.0084(18) -0.0010(19) C11 0.068(3) 0.068(3) 0.062(2) -0.005(2) -0.017(2) -0.009(2) C12 0.081(3) 0.083(3) 0.058(2) -0.017(2) -0.027(2) 0.000(3) C13 0.076(3) 0.098(3) 0.042(2) -0.010(2) -0.011(2) -0.002(3) C14 0.061(2) 0.077(3) 0.0383(19) -0.0087(19) -0.0049(18) -0.006(2) C15 0.0375(18) 0.0382(18) 0.0486(19) -0.0081(16) 0.0046(15) 0.0009(15) C16 0.041(2) 0.051(2) 0.069(2) -0.0166(19) -0.0034(18) -0.0008(17) C17 0.049(2) 0.071(3) 0.094(3) -0.019(2) 0.005(2) -0.016(2) C18 0.061(3) 0.095(4) 0.124(4) -0.017(3) -0.001(3) -0.026(3) C19 0.070(3) 0.122(4) 0.135(4) -0.024(4) -0.028(3) -0.023(3) C20 0.083(3) 0.125(4) 0.110(4) -0.015(3) -0.039(3) -0.012(3) C21 0.064(3) 0.092(3) 0.087(3) -0.012(3) -0.023(2) -0.011(3) C22 0.0339(17) 0.0371(17) 0.0374(17) -0.0037(14) 0.0035(13) -0.0029(14) C23 0.0364(17) 0.0392(18) 0.0381(17) -0.0084(14) 0.0013(14) -0.0017(14) C24 0.058(2) 0.046(2) 0.0364(18) -0.0072(16) -0.0019(16) -0.0026(17) C25 0.075(3) 0.058(2) 0.040(2) -0.0209(18) 0.0016(18) 0.002(2) C26 0.075(3) 0.053(2) 0.057(2) -0.028(2) -0.003(2) 0.008(2) C27 0.081(3) 0.039(2) 0.058(2) -0.0096(18) -0.003(2) 0.006(2) C28 0.064(2) 0.0394(19) 0.0405(19) -0.0065(16) 0.0054(17) 0.0030(17) C29 0.0384(18) 0.0401(18) 0.0315(16) 0.0025(14) 0.0085(13) 0.0039(14) C30 0.0392(18) 0.0349(17) 0.0366(17) 0.0042(14) 0.0083(14) 0.0024(14) C31 0.0439(19) 0.0357(17) 0.0377(17) 0.0000(14) 0.0066(14) -0.0024(15) C32 0.0426(18) 0.0352(17) 0.0322(16) 0.0010(13) 0.0025(14) -0.0024(14) C33A 0.045(3) 0.058(3) 0.054(4) 0.011(3) 0.006(3) 0.004(2) C34A 0.063(4) 0.109(5) 0.105(5) 0.006(4) -0.020(3) -0.020(3) C35A 0.046(4) 0.058(3) 0.049(4) 0.014(3) 0.000(3) 0.008(3) C33B 0.045(7) 0.045(7) 0.037(7) -0.002(6) -0.003(6) 0.000(6) C34B 0.061(9) 0.065(9) 0.053(9) -0.003(7) -0.011(7) 0.005(8) C35B 0.031(9) 0.037(9) 0.034(9) -0.001(7) -0.002(7) 0.003(7) N1 0.0405(16) 0.0346(15) 0.0284(13) 0.0018(11) 0.0063(11) -0.0015(12) N2 0.0429(16) 0.0348(15) 0.0344(14) 0.0034(12) 0.0115(12) -0.0024(13) O1 0.0466(14) 0.0334(12) 0.0361(12) 0.0009(10) 0.0113(10) 0.0054(10) O2 0.0496(14) 0.0317(12) 0.0394(13) 0.0027(10) 0.0109(11) 0.0020(11) O3 0.0494(14) 0.0485(14) 0.0275(11) -0.0016(10) 0.0033(10) -0.0084(12) O4 0.0474(14) 0.0496(15) 0.0255(11) 0.0009(10) 0.0022(10) -0.0052(12) O5 0.0393(14) 0.0480(15) 0.0446(14) -0.0012(12) 0.0084(11) -0.0105(11) O6 0.0422(14) 0.0474(15) 0.0423(13) 0.0043(11) -0.0014(11) -0.0076(11) O7 0.0522(15) 0.0370(13) 0.0347(12) -0.0015(10) 0.0128(11) 0.0004(11) O8 0.0538(15) 0.0343(13) 0.0368(13) -0.0024(10) 0.0134(11) 0.0010(11) Rh1 0.03909(15) 0.02928(14) 0.02224(13) 0.00267(10) 0.00711(10) -0.00079(11) Rh2 0.03551(15) 0.03085(14) 0.02951(14) 0.00072(10) 0.01043(10) -0.00333(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 C1 O1 1.263(4) . ? C1 O2 1.267(4) . ? C1 C2 1.478(5) . ? C2 C7 1.377(5) . ? C2 C3 1.387(5) . ? C3 C4 1.377(6) . ? C4 C5 1.365(7) . ? C5 C6 1.343(7) . ? C6 C7 1.383(6) . ? C8 O4 1.265(4) . ? C8 O3 1.270(4) . ? C8 C9 1.482(5) . ? C9 C14 1.375(5) . ? C9 C10 1.380(5) . ? C10 C11 1.380(6) . ? C11 C12 1.380(6) . ? C12 C13 1.366(6) . ? C13 C14 1.372(6) . ? C15 O6 1.259(4) . ? C15 O5 1.272(4) . ? C15 C16 1.493(5) . ? C16 C17 1.368(6) . ? C16 C21 1.381(6) . ? C17 C18 1.390(7) . ? C18 C19 1.366(8) . ? C19 C20 1.356(8) . ? C20 C21 1.382(7) . ? C22 O7 1.261(4) . ? C22 O8 1.273(4) . ? C22 C23 1.491(5) . ? C23 C28 1.383(5) . ? C23 C24 1.387(5) . ? C24 C25 1.375(5) . ? C25 C26 1.362(6) . ? C26 C27 1.375(6) . ? C27 C28 1.383(5) . ? C29 N1 1.344(4) . ? C29 C30 1.367(4) . ? C30 N2 1.344(4) . ? C31 N2 1.339(5) . ? C31 C32 1.409(4) . ? C31 C35B 1.50(4) . ? C31 C33A 1.518(8) . ? C32 N1 1.334(4) . ? C32 C35A 1.502(11) . ? C32 C33B 1.51(8) . ? C33A C34A 1.520(9) . ? C33B C34B 1.60(2) . ? N1 Rh1 2.297(2) . ? N2 Rh2 2.296(3) . ? O1 Rh1 2.036(2) . ? O2 Rh1 2.028(2) 2_675 ? O3 Rh1 2.030(2) 2_675 ? O4 Rh1 2.040(2) . ? O5 Rh2 2.033(3) . ? O6 Rh2 2.039(2) 2_566 ? O7 Rh2 2.025(2) 2_566 ? O8 Rh2 2.037(2) . ? Rh1 O2 2.028(2) 2_675 ? Rh1 O3 2.030(2) 2_675 ? Rh1 Rh1 2.3999(5) 2_675 ? Rh2 O7 2.025(2) 2_566 ? Rh2 O6 2.039(2) 2_566 ? Rh2 Rh2 2.4016(6) 2_566 ? 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 C1 O2 124.9(3) . . ? O1 C1 C2 117.9(3) . . ? O2 C1 C2 117.2(3) . . ? C7 C2 C3 117.8(4) . . ? C7 C2 C1 121.3(4) . . ? C3 C2 C1 121.0(4) . . ? C4 C3 C2 121.0(5) . . ? C5 C4 C3 119.8(5) . . ? C6 C5 C4 120.3(5) . . ? C5 C6 C7 120.7(5) . . ? C2 C7 C6 120.5(5) . . ? O4 C8 O3 124.9(3) . . ? O4 C8 C9 118.6(3) . . ? O3 C8 C9 116.5(3) . . ? C14 C9 C10 118.8(4) . . ? C14 C9 C8 121.4(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 120.7(4) . . ? C12 C11 C10 119.7(4) . . ? C13 C12 C11 119.6(4) . . ? C12 C13 C14 120.7(4) . . ? C13 C14 C9 120.6(4) . . ? O6 C15 O5 125.9(3) . . ? O6 C15 C16 117.0(4) . . ? O5 C15 C16 117.1(3) . . ? C17 C16 C21 119.9(4) . . ? C17 C16 C15 120.7(4) . . ? C21 C16 C15 119.4(4) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 119.4(5) . . ? C20 C19 C18 122.3(6) . . ? C19 C20 C21 118.1(6) . . ? C16 C21 C20 120.9(5) . . ? O7 C22 O8 125.7(3) . . ? O7 C22 C23 116.6(3) . . ? O8 C22 C23 117.7(3) . . ? C28 C23 C24 119.0(3) . . ? C28 C23 C22 120.5(3) . . ? C24 C23 C22 120.5(3) . . ? C25 C24 C23 120.6(4) . . ? C26 C25 C24 119.9(4) . . ? C25 C26 C27 120.6(4) . . ? C26 C27 C28 119.8(4) . . ? C27 C28 C23 120.1(3) . . ? N1 C29 C30 121.2(3) . . ? N2 C30 C29 121.8(3) . . ? N2 C31 C32 120.5(3) . . ? N2 C31 C35B 110.6(16) . . ? C32 C31 C35B 126.1(16) . . ? N2 C31 C33A 118.7(4) . . ? C32 C31 C33A 120.7(4) . . ? C35B C31 C33A 20.8(14) . . ? N1 C32 C31 120.8(3) . . ? N1 C32 C35A 117.2(3) . . ? C31 C32 C35A 122.1(4) . . ? N1 C32 C33B 128(2) . . ? C31 C32 C33B 111(2) . . ? C35A C32 C33B 12(2) . . ? C31 C33A C34A 114.0(5) . . ? C32 C33B C34B 106(4) . . ? C32 N1 C29 117.9(3) . . ? C32 N1 Rh1 128.4(2) . . ? C29 N1 Rh1 113.4(2) . . ? C31 N2 C30 117.5(3) . . ? C31 N2 Rh2 130.1(2) . . ? C30 N2 Rh2 111.7(2) . . ? C1 O1 Rh1 120.5(2) . . ? C1 O2 Rh1 119.0(2) . 2_675 ? C8 O3 Rh1 119.8(2) . 2_675 ? C8 O4 Rh1 119.5(2) . . ? C15 O5 Rh2 119.1(2) . . ? C15 O6 Rh2 119.0(2) . 2_566 ? C22 O7 Rh2 119.1(2) . 2_566 ? C22 O8 Rh2 119.3(2) . . ? O2 Rh1 O3 89.32(10) 2_675 2_675 ? O2 Rh1 O1 175.57(8) 2_675 . ? O3 Rh1 O1 90.98(10) 2_675 . ? O2 Rh1 O4 89.92(11) 2_675 . ? O3 Rh1 O4 175.66(8) 2_675 . ? O1 Rh1 O4 89.45(10) . . ? O2 Rh1 N1 88.17(9) 2_675 . ? O3 Rh1 N1 92.78(10) 2_675 . ? O1 Rh1 N1 96.22(9) . . ? O4 Rh1 N1 91.47(9) . . ? O2 Rh1 Rh1 88.65(6) 2_675 2_675 ? O3 Rh1 Rh1 87.92(6) 2_675 2_675 ? O1 Rh1 Rh1 86.94(6) . 2_675 ? O4 Rh1 Rh1 87.78(6) . 2_675 ? N1 Rh1 Rh1 176.74(7) . 2_675 ? O7 Rh2 O5 91.76(11) 2_566 . ? O7 Rh2 O8 175.83(9) 2_566 . ? O5 Rh2 O8 88.38(11) . . ? O7 Rh2 O6 88.26(10) 2_566 2_566 ? O5 Rh2 O6 175.86(9) . 2_566 ? O8 Rh2 O6 91.30(10) . 2_566 ? O7 Rh2 N2 88.30(9) 2_566 . ? O5 Rh2 N2 86.73(10) . . ? O8 Rh2 N2 95.87(10) . . ? O6 Rh2 N2 97.41(10) 2_566 . ? O7 Rh2 Rh2 88.48(6) 2_566 2_566 ? O5 Rh2 Rh2 87.87(7) . 2_566 ? O8 Rh2 Rh2 87.36(7) . 2_566 ? O6 Rh2 Rh2 87.99(7) 2_566 2_566 ? N2 Rh2 Rh2 173.62(8) . 2_566 ? 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 C1 C2 C7 176.5(4) . . . . ? O2 C1 C2 C7 -2.6(6) . . . . ? O1 C1 C2 C3 -2.1(6) . . . . ? O2 C1 C2 C3 178.7(4) . . . . ? C7 C2 C3 C4 -0.3(8) . . . . ? C1 C2 C3 C4 178.5(5) . . . . ? C2 C3 C4 C5 -1.3(9) . . . . ? C3 C4 C5 C6 2.2(10) . . . . ? C4 C5 C6 C7 -1.6(10) . . . . ? C3 C2 C7 C6 0.9(8) . . . . ? C1 C2 C7 C6 -177.9(5) . . . . ? C5 C6 C7 C2 0.1(9) . . . . ? O4 C8 C9 C14 -1.5(5) . . . . ? O3 C8 C9 C14 177.8(4) . . . . ? O4 C8 C9 C10 179.3(3) . . . . ? O3 C8 C9 C10 -1.5(5) . . . . ? C14 C9 C10 C11 0.1(6) . . . . ? C8 C9 C10 C11 179.3(4) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C10 C11 C12 C13 -0.3(8) . . . . ? C11 C12 C13 C14 0.5(8) . . . . ? C12 C13 C14 C9 -0.5(8) . . . . ? C10 C9 C14 C13 0.2(7) . . . . ? C8 C9 C14 C13 -179.1(4) . . . . ? O6 C15 C16 C17 173.3(4) . . . . ? O5 C15 C16 C17 -8.1(6) . . . . ? O6 C15 C16 C21 -7.5(6) . . . . ? O5 C15 C16 C21 171.2(4) . . . . ? C21 C16 C17 C18 0.2(7) . . . . ? C15 C16 C17 C18 179.4(4) . . . . ? C16 C17 C18 C19 -0.7(9) . . . . ? C17 C18 C19 C20 0.2(11) . . . . ? C18 C19 C20 C21 0.8(11) . . . . ? C17 C16 C21 C20 0.8(8) . . . . ? C15 C16 C21 C20 -178.4(5) . . . . ? C19 C20 C21 C16 -1.3(9) . . . . ? O7 C22 C23 C28 -171.5(3) . . . . ? O8 C22 C23 C28 8.0(5) . . . . ? O7 C22 C23 C24 5.4(5) . . . . ? O8 C22 C23 C24 -175.0(3) . . . . ? C28 C23 C24 C25 2.2(6) . . . . ? C22 C23 C24 C25 -174.8(3) . . . . ? C23 C24 C25 C26 -1.3(6) . . . . ? C24 C25 C26 C27 -0.5(7) . . . . ? C25 C26 C27 C28 1.4(7) . . . . ? C26 C27 C28 C23 -0.4(7) . . . . ? C24 C23 C28 C27 -1.4(6) . . . . ? C22 C23 C28 C27 175.6(4) . . . . ? N1 C29 C30 N2 -1.4(5) . . . . ? N2 C31 C32 N1 -2.3(5) . . . . ? C35B C31 C32 N1 157.0(18) . . . . ? C33A C31 C32 N1 -178.9(4) . . . . ? N2 C31 C32 C35A 176.8(5) . . . . ? C35B C31 C32 C35A -23.9(19) . . . . ? C33A C31 C32 C35A 0.2(7) . . . . ? N2 C31 C32 C33B -179.4(18) . . . . ? C35B C31 C32 C33B -20(3) . . . . ? C33A C31 C32 C33B 4.0(18) . . . . ? N2 C31 C33A C34A -97.9(6) . . . . ? C32 C31 C33A C34A 78.8(6) . . . . ? C35B C31 C33A C34A -170(5) . . . . ? N1 C32 C33B C34B 112(3) . . . . ? C31 C32 C33B C34B -71(3) . . . . ? C35A C32 C33B C34B 93(9) . . . . ? C31 C32 N1 C29 4.7(5) . . . . ? C35A C32 N1 C29 -174.5(4) . . . . ? C33B C32 N1 C29 -179(2) . . . . ? C31 C32 N1 Rh1 -168.5(2) . . . . ? C35A C32 N1 Rh1 12.4(6) . . . . ? C33B C32 N1 Rh1 8(2) . . . . ? C30 C29 N1 C32 -2.9(5) . . . . ? C30 C29 N1 Rh1 171.3(3) . . . . ? C32 C31 N2 C30 -2.0(5) . . . . ? C35B C31 N2 C30 -164.2(16) . . . . ? C33A C31 N2 C30 174.7(4) . . . . ? C32 C31 N2 Rh2 168.6(2) . . . . ? C35B C31 N2 Rh2 6.4(17) . . . . ? C33A C31 N2 Rh2 -14.8(6) . . . . ? C29 C30 N2 C31 3.8(5) . . . . ? C29 C30 N2 Rh2 -168.4(3) . . . . ? O2 C1 O1 Rh1 0.8(5) . . . . ? C2 C1 O1 Rh1 -178.3(2) . . . . ? O1 C1 O2 Rh1 -1.3(5) . . . 2_675 ? C2 C1 O2 Rh1 177.7(2) . . . 2_675 ? O4 C8 O3 Rh1 2.3(5) . . . 2_675 ? C9 C8 O3 Rh1 -176.9(2) . . . 2_675 ? O3 C8 O4 Rh1 -3.1(5) . . . . ? C9 C8 O4 Rh1 176.1(2) . . . . ? O6 C15 O5 Rh2 3.9(5) . . . . ? C16 C15 O5 Rh2 -174.6(2) . . . . ? O5 C15 O6 Rh2 -4.0(5) . . . 2_566 ? C16 C15 O6 Rh2 174.5(2) . . . 2_566 ? O8 C22 O7 Rh2 1.5(5) . . . 2_566 ? C23 C22 O7 Rh2 -179.0(2) . . . 2_566 ? O7 C22 O8 Rh2 -1.9(5) . . . . ? C23 C22 O8 Rh2 178.6(2) . . . . ? C1 O1 Rh1 O2 6.1(14) . . . 2_675 ? C1 O1 Rh1 O3 -87.8(3) . . . 2_675 ? C1 O1 Rh1 O4 87.9(3) . . . . ? C1 O1 Rh1 N1 179.3(3) . . . . ? C1 O1 Rh1 Rh1 0.1(3) . . . 2_675 ? C8 O4 Rh1 O2 90.7(3) . . . 2_675 ? C8 O4 Rh1 O3 10.8(14) . . . 2_675 ? C8 O4 Rh1 O1 -84.9(3) . . . . ? C8 O4 Rh1 N1 178.8(3) . . . . ? C8 O4 Rh1 Rh1 2.0(2) . . . 2_675 ? C32 N1 Rh1 O2 -151.9(3) . . . 2_675 ? C29 N1 Rh1 O2 34.7(2) . . . 2_675 ? C32 N1 Rh1 O3 -62.7(3) . . . 2_675 ? C29 N1 Rh1 O3 123.9(2) . . . 2_675 ? C32 N1 Rh1 O1 28.6(3) . . . . ? C29 N1 Rh1 O1 -144.8(2) . . . . ? C32 N1 Rh1 O4 118.2(3) . . . . ? C29 N1 Rh1 O4 -55.2(2) . . . . ? C32 N1 Rh1 Rh1 -165.1(11) . . . 2_675 ? C29 N1 Rh1 Rh1 21.5(14) . . . 2_675 ? C15 O5 Rh2 O7 -90.0(3) . . . 2_566 ? C15 O5 Rh2 O8 85.8(3) . . . . ? C15 O5 Rh2 O6 0.2(15) . . . 2_566 ? C15 O5 Rh2 N2 -178.2(3) . . . . ? C15 O5 Rh2 Rh2 -1.6(3) . . . 2_566 ? C22 O8 Rh2 O7 5.1(16) . . . 2_566 ? C22 O8 Rh2 O5 -86.8(3) . . . . ? C22 O8 Rh2 O6 89.0(3) . . . 2_566 ? C22 O8 Rh2 N2 -173.4(3) . . . . ? C22 O8 Rh2 Rh2 1.1(2) . . . 2_566 ? C31 N2 Rh2 O7 135.1(3) . . . 2_566 ? C30 N2 Rh2 O7 -54.0(2) . . . 2_566 ? C31 N2 Rh2 O5 -133.1(3) . . . . ? C30 N2 Rh2 O5 37.9(2) . . . . ? C31 N2 Rh2 O8 -45.0(3) . . . . ? C30 N2 Rh2 O8 125.9(2) . . . . ? C31 N2 Rh2 O6 47.0(3) . . . 2_566 ? C30 N2 Rh2 O6 -142.0(2) . . . 2_566 ? C31 N2 Rh2 Rh2 -165.3(5) . . . 2_566 ? C30 N2 Rh2 Rh2 5.7(8) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.920 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.094 #===END data_51005k1 _database_code_depnum_ccdc_archive 'CCDC 642579' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H30 N2 O8 Rh2' _chemical_formula_weight 812.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3271(10) _cell_length_b 10.4903(10) _cell_length_c 15.6507(15) _cell_angle_alpha 80.105(2) _cell_angle_beta 80.621(2) _cell_angle_gamma 86.903(2) _cell_volume 1647.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5698 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12077 _diffrn_reflns_av_R_equivalents 0.0136 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8052 _reflns_number_gt 7240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.7358P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8052 _refine_ls_number_parameters 456 _refine_ls_number_restraints 618 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.048 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.36501(19) 1.21596(18) 0.01257(11) 0.0170(4) Uani 1 1 d U . . C2 C 0.2899(2) 1.33903(19) 0.02338(12) 0.0190(4) Uani 1 1 d U . . C3 C 0.1667(2) 1.3365(2) 0.07596(14) 0.0272(4) Uani 1 1 d U . . H3 H 0.1293 1.2560 0.1033 0.033 Uiso 1 1 calc R . . C4 C 0.0991(2) 1.4511(2) 0.08835(16) 0.0343(5) Uani 1 1 d U . . H4 H 0.0149 1.4492 0.1237 0.041 Uiso 1 1 calc R . . C5 C 0.1540(2) 1.5686(2) 0.04927(17) 0.0331(5) Uani 1 1 d U . . H5 H 0.1077 1.6471 0.0582 0.040 Uiso 1 1 calc R . . C6 C 0.2761(2) 1.5720(2) -0.00269(17) 0.0320(5) Uani 1 1 d U . . H6 H 0.3139 1.6528 -0.0289 0.038 Uiso 1 1 calc R . . C7 C 0.3433(2) 1.4575(2) -0.01641(15) 0.0268(4) Uani 1 1 d U . . H7 H 0.4262 1.4599 -0.0532 0.032 Uiso 1 1 calc R . . C8 C 0.61378(19) 1.04163(18) 0.12992(12) 0.0170(4) Uani 1 1 d U . . C9 C 0.67577(19) 1.07469(19) 0.20239(12) 0.0183(4) Uani 1 1 d U . . C10 C 0.7876(2) 1.1494(2) 0.18318(13) 0.0218(4) Uani 1 1 d U . . H10 H 0.8242 1.1787 0.1237 0.026 Uiso 1 1 calc R . . C11 C 0.8459(2) 1.1812(2) 0.25010(14) 0.0255(4) Uani 1 1 d U . . H11 H 0.9223 1.2319 0.2365 0.031 Uiso 1 1 calc R . . C12 C 0.7923(2) 1.1389(2) 0.33719(13) 0.0260(4) Uani 1 1 d U . . H12 H 0.8323 1.1606 0.3832 0.031 Uiso 1 1 calc R . . C13 C 0.6809(2) 1.0654(2) 0.35689(13) 0.0277(5) Uani 1 1 d U . . H13 H 0.6444 1.0367 0.4164 0.033 Uiso 1 1 calc R . . C14 C 0.6221(2) 1.0331(2) 0.28988(13) 0.0229(4) Uani 1 1 d U . . H14 H 0.5455 0.9827 0.3037 0.027 Uiso 1 1 calc R . . C15 C 0.2230(2) 0.54714(19) 0.54421(14) 0.0225(4) Uani 1 1 d U . . C16 C 0.3439(2) 0.5855(2) 0.57346(15) 0.0264(4) Uani 1 1 d U . . C17 C 0.4401(2) 0.6537(2) 0.51342(17) 0.0321(5) Uani 1 1 d U . . H17 H 0.4308 0.6744 0.4532 0.039 Uiso 1 1 calc R . . C18 C 0.5502(3) 0.6916(3) 0.5423(2) 0.0419(6) Uani 1 1 d U . . H18 H 0.6169 0.7378 0.5016 0.050 Uiso 1 1 calc R . . C19 C 0.5627(3) 0.6622(3) 0.6296(2) 0.0480(7) Uani 1 1 d U . . H19 H 0.6382 0.6886 0.6489 0.058 Uiso 1 1 calc R . . C20 C 0.4670(3) 0.5949(3) 0.6897(2) 0.0450(6) Uani 1 1 d U . . H20 H 0.4762 0.5756 0.7500 0.054 Uiso 1 1 calc R . . C21 C 0.3580(2) 0.5556(2) 0.66188(17) 0.0349(5) Uani 1 1 d U . . H21 H 0.2924 0.5083 0.7029 0.042 Uiso 1 1 calc R . . C22 C -0.08995(19) 0.70887(19) 0.56117(12) 0.0190(4) Uani 1 1 d U . . C23 C -0.14031(19) 0.82788(19) 0.59717(12) 0.0183(4) Uani 1 1 d U . . C24 C -0.1826(2) 0.8208(2) 0.68732(12) 0.0215(4) Uani 1 1 d U . . H24 H -0.1730 0.7418 0.7261 0.026 Uiso 1 1 calc R . . C25 C -0.2385(2) 0.9288(2) 0.71997(13) 0.0248(4) Uani 1 1 d U . . H25 H -0.2680 0.9240 0.7812 0.030 Uiso 1 1 calc R . . C26 C -0.2513(2) 1.0440(2) 0.66337(14) 0.0253(4) Uani 1 1 d U . . H26 H -0.2915 1.1176 0.6858 0.030 Uiso 1 1 calc R . . C27 C -0.2060(2) 1.0528(2) 0.57417(14) 0.0251(4) Uani 1 1 d U . . H27 H -0.2127 1.1329 0.5360 0.030 Uiso 1 1 calc R . . C28 C -0.1508(2) 0.94456(19) 0.54067(13) 0.0219(4) Uani 1 1 d U . . H28 H -0.1204 0.9501 0.4795 0.026 Uiso 1 1 calc R . . C29 C 0.31815(19) 0.71657(19) 0.19972(12) 0.0185(4) Uani 1 1 d U . . H29 H 0.4089 0.6952 0.1861 0.022 Uiso 1 1 calc R . . C30 C 0.2432(2) 0.64445(19) 0.27056(12) 0.0198(4) Uani 1 1 d U . . H30 H 0.2828 0.5729 0.3037 0.024 Uiso 1 1 calc R . . C31 C 0.0600(2) 0.76973(19) 0.24269(13) 0.0208(4) Uani 1 1 d U . . C32 C 0.13610(19) 0.84075(19) 0.16828(12) 0.0182(4) Uani 1 1 d U . . C33A C -0.0864(3) 0.7973(3) 0.2631(2) 0.0234(6) Uani 0.859(5) 1 d PU . . H33A H -0.1033 0.8920 0.2509 0.028 Uiso 0.859(5) 1 calc PR . . H33B H -0.1165 0.7674 0.3264 0.028 Uiso 0.859(5) 1 calc PR . . C34A C -0.1658(3) 0.7311(3) 0.20953(19) 0.0354(7) Uani 0.859(5) 1 d PU . . H34A H -0.1431 0.7671 0.1471 0.053 Uiso 0.859(5) 1 calc PR . . H34B H -0.2598 0.7460 0.2287 0.053 Uiso 0.859(5) 1 calc PR . . H34C H -0.1455 0.6379 0.2185 0.053 Uiso 0.859(5) 1 calc PR . . C35A C 0.0764(5) 0.9485(5) 0.1104(4) 0.0241(9) Uani 0.859(5) 1 d PU . . H35A H 0.0624 1.0249 0.1393 0.036 Uiso 0.859(5) 1 calc PR . . H35B H -0.0079 0.9216 0.0993 0.036 Uiso 0.859(5) 1 calc PR . . H35C H 0.1357 0.9695 0.0545 0.036 Uiso 0.859(5) 1 calc PR . . C33B C 0.063(4) 0.932(4) 0.102(3) 0.018(4) Uani 0.141(5) 1 d PU . . H33C H 0.0282 1.0089 0.1273 0.022 Uiso 0.141(5) 1 calc PR . . H33D H 0.1260 0.9614 0.0478 0.022 Uiso 0.141(5) 1 calc PR . . C34B C -0.0393(18) 0.8707(17) 0.0793(11) 0.033(4) Uani 0.141(5) 1 d PU . . H34D H -0.0090 0.8358 0.0251 0.049 Uiso 0.141(5) 1 calc PR . . H34E H -0.1119 0.9332 0.0704 0.049 Uiso 0.141(5) 1 calc PR . . H34F H -0.0695 0.7998 0.1268 0.049 Uiso 0.141(5) 1 calc PR . . C35B C -0.0714(19) 0.8087(19) 0.2913(13) 0.022(4) Uani 0.141(5) 1 d PU . . H35D H -0.1362 0.7436 0.2915 0.033 Uiso 0.141(5) 1 calc PR . . H35E H -0.1005 0.8929 0.2619 0.033 Uiso 0.141(5) 1 calc PR . . H35F H -0.0624 0.8146 0.3518 0.033 Uiso 0.141(5) 1 calc PR . . N1 N 0.26542(16) 0.81685(16) 0.14927(10) 0.0171(3) Uani 1 1 d U . . N2 N 0.11465(17) 0.67329(16) 0.29391(11) 0.0206(3) Uani 1 1 d U . . O1 O 0.31655(14) 1.11205(13) 0.05685(8) 0.0185(3) Uani 1 1 d U . . O2 O 0.47333(14) 1.22422(13) -0.03978(9) 0.0196(3) Uani 1 1 d U . . O3 O 0.66745(13) 1.08734(13) 0.05222(8) 0.0184(3) Uani 1 1 d U . . O4 O 0.51236(13) 0.97317(13) 0.14943(8) 0.0185(3) Uani 1 1 d U . . O5 O 0.20552(14) 0.59197(14) 0.46631(9) 0.0229(3) Uani 1 1 d U . . O6 O 0.14545(14) 0.47435(14) 0.60097(9) 0.0235(3) Uani 1 1 d U . . O7 O -0.10114(14) 0.60276(13) 0.61466(9) 0.0218(3) Uani 1 1 d U . . O8 O -0.04222(15) 0.72190(14) 0.47995(9) 0.0230(3) Uani 1 1 d U . . Rh1 Rh 0.416550(14) 0.939842(13) 0.051339(8) 0.01407(5) Uani 1 1 d U . . Rh2 Rh 0.031933(15) 0.562575(14) 0.428364(9) 0.01776(5) Uani 1 1 d U . . 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 0.0209(9) 0.0172(9) 0.0119(8) -0.0022(7) 0.0001(7) -0.0001(7) C2 0.0229(10) 0.0171(9) 0.0168(8) -0.0041(7) -0.0020(7) 0.0019(7) C3 0.0274(11) 0.0238(10) 0.0272(10) -0.0053(8) 0.0056(8) 0.0020(8) C4 0.0321(12) 0.0323(12) 0.0355(12) -0.0086(10) 0.0042(10) 0.0075(10) C5 0.0354(12) 0.0237(11) 0.0429(13) -0.0136(10) -0.0086(10) 0.0090(9) C6 0.0338(12) 0.0175(10) 0.0447(13) -0.0037(9) -0.0081(10) 0.0000(9) C7 0.0254(10) 0.0207(10) 0.0327(11) -0.0028(8) -0.0016(9) -0.0002(8) C8 0.0196(9) 0.0151(8) 0.0144(8) -0.0020(7) 0.0016(7) 0.0038(7) C9 0.0201(9) 0.0194(9) 0.0140(8) -0.0027(7) 0.0003(7) 0.0032(7) C10 0.0241(10) 0.0215(10) 0.0179(9) -0.0015(7) 0.0001(7) 0.0010(8) C11 0.0257(11) 0.0259(10) 0.0246(10) -0.0038(8) -0.0029(8) -0.0022(8) C12 0.0284(11) 0.0309(11) 0.0202(9) -0.0067(8) -0.0064(8) 0.0014(9) C13 0.0292(11) 0.0369(12) 0.0155(9) -0.0032(8) -0.0012(8) 0.0006(9) C14 0.0223(10) 0.0283(11) 0.0162(9) -0.0022(8) 0.0010(7) -0.0008(8) C15 0.0221(10) 0.0171(9) 0.0267(10) -0.0080(8) 0.0053(8) 0.0016(8) C16 0.0232(10) 0.0213(10) 0.0346(11) -0.0095(8) 0.0009(8) 0.0003(8) C17 0.0265(11) 0.0272(11) 0.0417(13) -0.0123(10) 0.0053(10) -0.0036(9) C18 0.0268(12) 0.0371(14) 0.0621(17) -0.0166(12) 0.0027(11) -0.0065(10) C19 0.0295(13) 0.0462(16) 0.0738(19) -0.0209(14) -0.0124(13) -0.0017(11) C20 0.0374(14) 0.0492(16) 0.0519(15) -0.0094(13) -0.0171(12) 0.0006(12) C21 0.0311(12) 0.0336(13) 0.0398(13) -0.0053(10) -0.0057(10) -0.0010(10) C22 0.0186(9) 0.0167(9) 0.0193(9) -0.0030(7) 0.0049(7) -0.0027(7) C23 0.0173(9) 0.0186(9) 0.0179(8) -0.0049(7) 0.0023(7) -0.0017(7) C24 0.0247(10) 0.0211(10) 0.0180(9) -0.0045(7) 0.0004(8) -0.0026(8) C25 0.0287(11) 0.0281(11) 0.0179(9) -0.0093(8) 0.0020(8) -0.0017(9) C26 0.0292(11) 0.0229(10) 0.0246(10) -0.0107(8) 0.0001(8) 0.0010(8) C27 0.0338(11) 0.0174(9) 0.0224(10) -0.0032(8) -0.0001(8) -0.0003(8) C28 0.0279(10) 0.0196(9) 0.0168(9) -0.0041(7) 0.0025(7) -0.0021(8) C29 0.0191(9) 0.0181(9) 0.0158(8) -0.0021(7) 0.0032(7) 0.0005(7) C30 0.0220(10) 0.0165(9) 0.0185(9) -0.0031(7) 0.0042(7) -0.0004(7) C31 0.0206(10) 0.0171(9) 0.0216(9) -0.0032(7) 0.0060(7) -0.0016(7) C32 0.0204(9) 0.0165(9) 0.0169(8) -0.0038(7) 0.0011(7) -0.0018(7) C33A 0.0203(13) 0.0222(13) 0.0232(14) 0.0008(11) 0.0051(11) 0.0008(10) C34A 0.0274(14) 0.0375(16) 0.0394(15) -0.0005(12) -0.0037(11) -0.0072(12) C35A 0.0223(18) 0.025(2) 0.0245(19) -0.0021(13) -0.0033(13) -0.0002(14) C33B 0.018(4) 0.018(4) 0.018(4) -0.0029(11) -0.0030(11) -0.0005(10) C34B 0.039(7) 0.029(6) 0.029(6) -0.004(5) -0.005(5) 0.003(5) C35B 0.022(4) 0.022(4) 0.022(4) -0.0035(11) -0.0032(11) -0.0005(10) N1 0.0196(8) 0.0177(8) 0.0127(7) -0.0023(6) 0.0020(6) -0.0021(6) N2 0.0211(8) 0.0163(8) 0.0207(8) -0.0024(6) 0.0076(6) -0.0020(6) O1 0.0216(7) 0.0155(6) 0.0152(6) -0.0013(5) 0.0050(5) 0.0006(5) O2 0.0224(7) 0.0159(6) 0.0172(6) -0.0010(5) 0.0051(5) 0.0000(5) O3 0.0214(7) 0.0202(7) 0.0116(6) -0.0009(5) 0.0029(5) -0.0038(5) O4 0.0204(7) 0.0209(7) 0.0119(6) -0.0005(5) 0.0024(5) -0.0030(5) O5 0.0236(7) 0.0205(7) 0.0210(7) -0.0030(6) 0.0084(6) -0.0056(6) O6 0.0233(7) 0.0222(7) 0.0219(7) -0.0007(6) 0.0035(6) -0.0034(6) O7 0.0276(8) 0.0168(7) 0.0170(6) -0.0022(5) 0.0076(5) -0.0006(6) O8 0.0296(8) 0.0162(7) 0.0184(6) -0.0022(5) 0.0100(6) -0.0009(6) Rh1 0.01692(8) 0.01356(8) 0.00925(7) -0.00014(5) 0.00357(5) -0.00088(5) Rh2 0.02008(8) 0.01360(8) 0.01562(8) -0.00135(5) 0.00829(6) -0.00211(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 C1 O1 1.267(2) . ? C1 O2 1.272(2) . ? C1 C2 1.490(3) . ? C2 C7 1.390(3) . ? C2 C3 1.397(3) . ? C3 C4 1.384(3) . ? C4 C5 1.385(3) . ? C5 C6 1.383(3) . ? C6 C7 1.386(3) . ? C8 O4 1.268(2) . ? C8 O3 1.275(2) . ? C8 C9 1.487(3) . ? C9 C10 1.394(3) . ? C9 C14 1.395(3) . ? C10 C11 1.385(3) . ? C11 C12 1.390(3) . ? C12 C13 1.383(3) . ? C13 C14 1.391(3) . ? C15 O5 1.267(3) . ? C15 O6 1.271(2) . ? C15 C16 1.495(3) . ? C16 C17 1.387(3) . ? C16 C21 1.395(3) . ? C17 C18 1.391(4) . ? C18 C19 1.375(4) . ? C19 C20 1.380(4) . ? C20 C21 1.378(4) . ? C22 O7 1.271(2) . ? C22 O8 1.273(2) . ? C22 C23 1.491(3) . ? C23 C28 1.392(3) . ? C23 C24 1.398(3) . ? C24 C25 1.382(3) . ? C25 C26 1.384(3) . ? C26 C27 1.387(3) . ? C27 C28 1.388(3) . ? C29 N1 1.349(2) . ? C29 C30 1.377(2) . ? C30 N2 1.351(3) . ? C31 N2 1.339(3) . ? C31 C32 1.413(3) . ? C31 C35B 1.52(2) . ? C31 C33A 1.515(3) . ? C32 N1 1.340(3) . ? C32 C35A 1.494(6) . ? C32 C33B 1.55(4) . ? C33A C34A 1.531(4) . ? C33B C34B 1.39(3) . ? N1 Rh1 2.2822(15) . ? N2 Rh2 2.2777(16) . ? O1 Rh1 2.0397(14) . ? O2 Rh1 2.0289(14) 2_675 ? O3 Rh1 2.0260(14) 2_675 ? O4 Rh1 2.0433(14) . ? O5 Rh2 2.0325(15) . ? O6 Rh2 2.0318(15) 2_566 ? O7 Rh2 2.0206(14) 2_566 ? O8 Rh2 2.0385(14) . ? Rh1 O3 2.0260(14) 2_675 ? Rh1 O2 2.0289(14) 2_675 ? Rh1 Rh1 2.4045(3) 2_675 ? Rh2 O7 2.0206(14) 2_566 ? Rh2 O6 2.0318(15) 2_566 ? Rh2 Rh2 2.4055(3) 2_566 ? 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 C1 O2 125.40(18) . . ? O1 C1 C2 117.46(16) . . ? O2 C1 C2 117.14(16) . . ? C7 C2 C3 119.33(19) . . ? C7 C2 C1 120.45(18) . . ? C3 C2 C1 120.19(18) . . ? C4 C3 C2 120.1(2) . . ? C3 C4 C5 120.0(2) . . ? C6 C5 C4 120.3(2) . . ? C5 C6 C7 119.9(2) . . ? C6 C7 C2 120.3(2) . . ? O4 C8 O3 125.33(18) . . ? O4 C8 C9 118.55(16) . . ? O3 C8 C9 116.12(17) . . ? C10 C9 C14 119.34(18) . . ? C10 C9 C8 119.99(16) . . ? C14 C9 C8 120.67(18) . . ? C11 C10 C9 120.49(18) . . ? C10 C11 C12 119.9(2) . . ? C13 C12 C11 120.0(2) . . ? C12 C13 C14 120.28(19) . . ? C13 C14 C9 119.97(19) . . ? O5 C15 O6 126.0(2) . . ? O5 C15 C16 117.54(18) . . ? O6 C15 C16 116.49(19) . . ? C17 C16 C21 120.1(2) . . ? C17 C16 C15 120.2(2) . . ? C21 C16 C15 119.7(2) . . ? C16 C17 C18 119.3(2) . . ? C19 C18 C17 120.1(3) . . ? C18 C19 C20 120.8(3) . . ? C21 C20 C19 119.7(3) . . ? C20 C21 C16 120.0(2) . . ? O7 C22 O8 125.94(18) . . ? O7 C22 C23 116.45(16) . . ? O8 C22 C23 117.59(17) . . ? C28 C23 C24 120.03(18) . . ? C28 C23 C22 120.03(17) . . ? C24 C23 C22 119.87(18) . . ? C25 C24 C23 119.91(19) . . ? C24 C25 C26 119.88(18) . . ? C25 C26 C27 120.5(2) . . ? C26 C27 C28 120.0(2) . . ? C27 C28 C23 119.61(18) . . ? N1 C29 C30 121.39(18) . . ? N2 C30 C29 121.42(19) . . ? N2 C31 C32 120.60(18) . . ? N2 C31 C35B 109.2(8) . . ? C32 C31 C35B 127.9(8) . . ? N2 C31 C33A 118.96(18) . . ? C32 C31 C33A 120.4(2) . . ? C35B C31 C33A 19.9(7) . . ? N1 C32 C31 120.95(18) . . ? N1 C32 C35A 117.8(3) . . ? C31 C32 C35A 121.2(3) . . ? N1 C32 C33B 120.4(15) . . ? C31 C32 C33B 118.0(14) . . ? C35A C32 C33B 10.8(12) . . ? C31 C33A C34A 112.8(2) . . ? C34B C33B C32 112(3) . . ? C32 N1 C29 117.63(16) . . ? C32 N1 Rh1 127.94(13) . . ? C29 N1 Rh1 113.99(13) . . ? C31 N2 C30 117.78(16) . . ? C31 N2 Rh2 129.68(13) . . ? C30 N2 Rh2 111.98(13) . . ? C1 O1 Rh1 120.34(12) . . ? C1 O2 Rh1 118.40(12) . 2_675 ? C8 O3 Rh1 119.56(12) . 2_675 ? C8 O4 Rh1 119.12(11) . . ? C15 O5 Rh2 119.05(13) . . ? C15 O6 Rh2 118.79(14) . 2_566 ? C22 O7 Rh2 118.91(12) . 2_566 ? C22 O8 Rh2 119.03(13) . . ? O3 Rh1 O2 88.97(6) 2_675 2_675 ? O3 Rh1 O1 91.04(6) 2_675 . ? O2 Rh1 O1 175.82(5) 2_675 . ? O3 Rh1 O4 175.86(5) 2_675 . ? O2 Rh1 O4 90.48(6) 2_675 . ? O1 Rh1 O4 89.22(6) . . ? O3 Rh1 N1 92.45(5) 2_675 . ? O2 Rh1 N1 88.13(6) 2_675 . ? O1 Rh1 N1 96.05(6) . . ? O4 Rh1 N1 91.63(5) . . ? O3 Rh1 Rh1 88.08(4) 2_675 2_675 ? O2 Rh1 Rh1 89.02(4) 2_675 2_675 ? O1 Rh1 Rh1 86.80(4) . 2_675 ? O4 Rh1 Rh1 87.81(4) . 2_675 ? N1 Rh1 Rh1 177.09(4) . 2_675 ? O7 Rh2 O6 87.80(6) 2_566 2_566 ? O7 Rh2 O5 92.09(6) 2_566 . ? O6 Rh2 O5 175.92(5) 2_566 . ? O7 Rh2 O8 176.06(5) 2_566 . ? O6 Rh2 O8 91.85(6) 2_566 . ? O5 Rh2 O8 87.98(6) . . ? O7 Rh2 N2 88.36(6) 2_566 . ? O6 Rh2 N2 97.06(6) 2_566 . ? O5 Rh2 N2 87.01(6) . . ? O8 Rh2 N2 95.57(6) . . ? O7 Rh2 Rh2 88.54(4) 2_566 2_566 ? O6 Rh2 Rh2 88.06(4) 2_566 2_566 ? O5 Rh2 Rh2 87.86(4) . 2_566 ? O8 Rh2 Rh2 87.53(4) . 2_566 ? N2 Rh2 Rh2 173.90(5) . 2_566 ? 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 C1 C2 C7 173.65(19) . . . . ? O2 C1 C2 C7 -5.6(3) . . . . ? O1 C1 C2 C3 -4.3(3) . . . . ? O2 C1 C2 C3 176.38(19) . . . . ? C7 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C4 177.8(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C5 C6 C7 C2 -1.5(4) . . . . ? C3 C2 C7 C6 1.3(3) . . . . ? C1 C2 C7 C6 -176.8(2) . . . . ? O4 C8 C9 C10 179.79(18) . . . . ? O3 C8 C9 C10 -1.3(3) . . . . ? O4 C8 C9 C14 -1.1(3) . . . . ? O3 C8 C9 C14 177.88(18) . . . . ? C14 C9 C10 C11 0.6(3) . . . . ? C8 C9 C10 C11 179.73(19) . . . . ? C9 C10 C11 C12 -0.3(3) . . . . ? C10 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 C9 0.2(3) . . . . ? C10 C9 C14 C13 -0.5(3) . . . . ? C8 C9 C14 C13 -179.7(2) . . . . ? O5 C15 C16 C17 -8.0(3) . . . . ? O6 C15 C16 C17 173.48(19) . . . . ? O5 C15 C16 C21 170.1(2) . . . . ? O6 C15 C16 C21 -8.4(3) . . . . ? C21 C16 C17 C18 0.1(3) . . . . ? C15 C16 C17 C18 178.3(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C19 C20 C21 C16 -0.8(4) . . . . ? C17 C16 C21 C20 0.5(4) . . . . ? C15 C16 C21 C20 -177.6(2) . . . . ? O7 C22 C23 C28 -169.92(19) . . . . ? O8 C22 C23 C28 8.8(3) . . . . ? O7 C22 C23 C24 7.1(3) . . . . ? O8 C22 C23 C24 -174.18(19) . . . . ? C28 C23 C24 C25 1.9(3) . . . . ? C22 C23 C24 C25 -175.12(19) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C24 C25 C26 C27 -1.4(3) . . . . ? C25 C26 C27 C28 2.0(3) . . . . ? C26 C27 C28 C23 -0.6(3) . . . . ? C24 C23 C28 C27 -1.3(3) . . . . ? C22 C23 C28 C27 175.70(19) . . . . ? N1 C29 C30 N2 -1.8(3) . . . . ? N2 C31 C32 N1 -2.7(3) . . . . ? C35B C31 C32 N1 158.0(9) . . . . ? C33A C31 C32 N1 -179.7(2) . . . . ? N2 C31 C32 C35A 179.9(3) . . . . ? C35B C31 C32 C35A -19.5(10) . . . . ? C33A C31 C32 C35A 2.9(4) . . . . ? N2 C31 C32 C33B 168.0(14) . . . . ? C35B C31 C32 C33B -31.4(17) . . . . ? C33A C31 C32 C33B -9.0(14) . . . . ? N2 C31 C33A C34A -95.5(3) . . . . ? C32 C31 C33A C34A 81.5(3) . . . . ? C35B C31 C33A C34A -160(2) . . . . ? N1 C32 C33B C34B 123(2) . . . . ? C31 C32 C33B C34B -48(3) . . . . ? C35A C32 C33B C34B -158(11) . . . . ? C31 C32 N1 C29 4.9(3) . . . . ? C35A C32 N1 C29 -177.6(2) . . . . ? C33B C32 N1 C29 -165.6(14) . . . . ? C31 C32 N1 Rh1 -166.94(14) . . . . ? C35A C32 N1 Rh1 10.6(3) . . . . ? C33B C32 N1 Rh1 22.6(14) . . . . ? C30 C29 N1 C32 -2.7(3) . . . . ? C30 C29 N1 Rh1 170.25(15) . . . . ? C32 C31 N2 C30 -1.8(3) . . . . ? C35B C31 N2 C30 -165.8(8) . . . . ? C33A C31 N2 C30 175.2(2) . . . . ? C32 C31 N2 Rh2 168.87(14) . . . . ? C35B C31 N2 Rh2 4.9(8) . . . . ? C33A C31 N2 Rh2 -14.1(3) . . . . ? C29 C30 N2 C31 4.0(3) . . . . ? C29 C30 N2 Rh2 -168.26(15) . . . . ? O2 C1 O1 Rh1 2.4(3) . . . . ? C2 C1 O1 Rh1 -176.83(12) . . . . ? O1 C1 O2 Rh1 -2.5(3) . . . 2_675 ? C2 C1 O2 Rh1 176.70(12) . . . 2_675 ? O4 C8 O3 Rh1 3.5(3) . . . 2_675 ? C9 C8 O3 Rh1 -175.35(12) . . . 2_675 ? O3 C8 O4 Rh1 -4.1(3) . . . . ? C9 C8 O4 Rh1 174.75(13) . . . . ? O6 C15 O5 Rh2 6.3(3) . . . . ? C16 C15 O5 Rh2 -171.98(13) . . . . ? O5 C15 O6 Rh2 -6.3(3) . . . 2_566 ? C16 C15 O6 Rh2 172.02(13) . . . 2_566 ? O8 C22 O7 Rh2 2.6(3) . . . 2_566 ? C23 C22 O7 Rh2 -178.77(13) . . . 2_566 ? O7 C22 O8 Rh2 -2.9(3) . . . . ? C23 C22 O8 Rh2 178.53(13) . . . . ? C1 O1 Rh1 O3 -88.99(14) . . . 2_675 ? C1 O1 Rh1 O2 1.0(8) . . . 2_675 ? C1 O1 Rh1 O4 86.88(14) . . . . ? C1 O1 Rh1 N1 178.43(14) . . . . ? C1 O1 Rh1 Rh1 -0.97(14) . . . 2_675 ? C8 O4 Rh1 O3 9.1(8) . . . 2_675 ? C8 O4 Rh1 O2 91.32(14) . . . 2_675 ? C8 O4 Rh1 O1 -84.51(14) . . . . ? C8 O4 Rh1 N1 179.47(14) . . . . ? C8 O4 Rh1 Rh1 2.32(13) . . . 2_675 ? C32 N1 Rh1 O3 -64.78(16) . . . 2_675 ? C29 N1 Rh1 O3 123.17(13) . . . 2_675 ? C32 N1 Rh1 O2 -153.67(16) . . . 2_675 ? C29 N1 Rh1 O2 34.29(13) . . . 2_675 ? C32 N1 Rh1 O1 26.52(16) . . . . ? C29 N1 Rh1 O1 -145.53(13) . . . . ? C32 N1 Rh1 O4 115.91(16) . . . . ? C29 N1 Rh1 O4 -56.14(13) . . . . ? C32 N1 Rh1 Rh1 -165.4(7) . . . 2_675 ? C29 N1 Rh1 Rh1 22.6(9) . . . 2_675 ? C15 O5 Rh2 O7 -91.35(15) . . . 2_566 ? C15 O5 Rh2 O6 -3.0(9) . . . 2_566 ? C15 O5 Rh2 O8 84.71(15) . . . . ? C15 O5 Rh2 N2 -179.59(15) . . . . ? C15 O5 Rh2 Rh2 -2.89(14) . . . 2_566 ? C22 O8 Rh2 O7 4.6(10) . . . 2_566 ? C22 O8 Rh2 O6 89.49(16) . . . 2_566 ? C22 O8 Rh2 O5 -86.44(15) . . . . ? C22 O8 Rh2 N2 -173.23(15) . . . . ? C22 O8 Rh2 Rh2 1.51(15) . . . 2_566 ? C31 N2 Rh2 O7 135.54(18) . . . 2_566 ? C30 N2 Rh2 O7 -53.35(14) . . . 2_566 ? C31 N2 Rh2 O6 47.96(18) . . . 2_566 ? C30 N2 Rh2 O6 -140.93(13) . . . 2_566 ? C31 N2 Rh2 O5 -132.28(18) . . . . ? C30 N2 Rh2 O5 38.83(14) . . . . ? C31 N2 Rh2 O8 -44.60(18) . . . . ? C30 N2 Rh2 O8 126.50(14) . . . . ? C31 N2 Rh2 Rh2 -165.0(3) . . . 2_566 ? C30 N2 Rh2 Rh2 6.1(5) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.592 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.088 #===END data_50919k1 _database_code_depnum_ccdc_archive 'CCDC 642580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H30 N2 O8 Rh2' _chemical_formula_weight 812.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5480(7) _cell_length_b 10.5517(8) _cell_length_c 15.6898(11) _cell_angle_alpha 80.607(2) _cell_angle_beta 80.563(2) _cell_angle_gamma 88.756(2) _cell_volume 1699.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5786 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; The measurement was carried out in a pressurized CO2 atmosphere (ca. 6.4MPa at room temperature). ; _diffrn_ambient_temperature 298 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12601 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8316 _reflns_number_gt 6499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.8971P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8316 _refine_ls_number_parameters 456 _refine_ls_number_restraints 608 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.036 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3734(3) 1.2137(3) 0.01055(19) 0.0384(7) Uani 1 1 d U . . C2 C 0.3019(3) 1.3356(3) 0.0182(2) 0.0469(8) Uani 1 1 d U . . C3 C 0.1841(4) 1.3347(4) 0.0720(3) 0.0713(12) Uani 1 1 d U . . H3 H 0.1482 1.2573 0.1024 0.086 Uiso 1 1 calc R . . C4 C 0.1195(5) 1.4483(5) 0.0807(4) 0.0930(16) Uani 1 1 d U . . H4 H 0.0394 1.4471 0.1160 0.112 Uiso 1 1 calc R . . C5 C 0.1727(5) 1.5625(5) 0.0376(4) 0.0928(15) Uani 1 1 d U . . H5 H 0.1296 1.6389 0.0446 0.111 Uiso 1 1 calc R . . C6 C 0.2885(5) 1.5648(4) -0.0155(4) 0.0929(15) Uani 1 1 d U . . H6 H 0.3244 1.6427 -0.0450 0.111 Uiso 1 1 calc R . . C7 C 0.3531(4) 1.4513(4) -0.0257(3) 0.0734(12) Uani 1 1 d U . . H7 H 0.4319 1.4534 -0.0626 0.088 Uiso 1 1 calc R . . C8 C 0.6133(3) 1.0428(3) 0.12869(19) 0.0382(7) Uani 1 1 d U . . C9 C 0.6772(3) 1.0734(3) 0.2010(2) 0.0441(7) Uani 1 1 d U . . C10 C 0.7895(4) 1.1451(4) 0.1817(2) 0.0545(9) Uani 1 1 d U . . H10 H 0.8256 1.1730 0.1236 0.065 Uiso 1 1 calc R . . C11 C 0.8482(4) 1.1756(4) 0.2481(3) 0.0668(11) Uani 1 1 d U . . H11 H 0.9236 1.2240 0.2348 0.080 Uiso 1 1 calc R . . C12 C 0.7952(4) 1.1344(5) 0.3337(3) 0.0711(11) Uani 1 1 d U . . H12 H 0.8352 1.1543 0.3785 0.085 Uiso 1 1 calc R . . C13 C 0.6842(4) 1.0645(5) 0.3533(3) 0.0738(12) Uani 1 1 d U . . H13 H 0.6481 1.0378 0.4115 0.089 Uiso 1 1 calc R . . C14 C 0.6251(4) 1.0330(4) 0.2872(2) 0.0605(10) Uani 1 1 d U . . H14 H 0.5499 0.9844 0.3010 0.073 Uiso 1 1 calc R . . C15 C 0.2193(3) 0.5517(3) 0.5428(2) 0.0434(7) Uani 1 1 d U . . C16 C 0.3409(3) 0.5899(4) 0.5695(3) 0.0543(9) Uani 1 1 d U . . C17 C 0.4348(4) 0.6563(4) 0.5094(3) 0.0713(12) Uani 1 1 d U . . H17 H 0.4236 0.6789 0.4513 0.086 Uiso 1 1 calc R . . C18 C 0.5475(5) 0.6897(5) 0.5362(4) 0.0969(16) Uani 1 1 d U . . H18 H 0.6131 0.7336 0.4961 0.116 Uiso 1 1 calc R . . C19 C 0.5600(5) 0.6569(6) 0.6223(5) 0.1106(18) Uani 1 1 d U . . H19 H 0.6352 0.6798 0.6398 0.133 Uiso 1 1 calc R . . C20 C 0.4687(5) 0.5932(6) 0.6828(4) 0.1085(18) Uani 1 1 d U . . H20 H 0.4796 0.5730 0.7411 0.130 Uiso 1 1 calc R . . C21 C 0.3577(4) 0.5583(5) 0.6559(3) 0.0816(13) Uani 1 1 d U . . H21 H 0.2935 0.5130 0.6964 0.098 Uiso 1 1 calc R . . C22 C -0.0902(3) 0.7052(3) 0.56109(19) 0.0369(6) Uani 1 1 d U . . C23 C -0.1412(3) 0.8216(3) 0.5970(2) 0.0376(7) Uani 1 1 d U . . C24 C -0.1856(3) 0.8151(3) 0.6859(2) 0.0464(8) Uani 1 1 d U . . H24 H -0.1781 0.7390 0.7240 0.056 Uiso 1 1 calc R . . C25 C -0.2409(4) 0.9207(4) 0.7179(2) 0.0576(9) Uani 1 1 d U . . H25 H -0.2717 0.9157 0.7774 0.069 Uiso 1 1 calc R . . C26 C -0.2506(4) 1.0335(4) 0.6620(3) 0.0606(10) Uani 1 1 d U . . H26 H -0.2892 1.1044 0.6836 0.073 Uiso 1 1 calc R . . C27 C -0.2040(4) 1.0424(4) 0.5747(3) 0.0610(10) Uani 1 1 d U . . H27 H -0.2092 1.1198 0.5374 0.073 Uiso 1 1 calc R . . C28 C -0.1492(3) 0.9370(3) 0.5418(2) 0.0497(8) Uani 1 1 d U . . H28 H -0.1175 0.9434 0.4824 0.060 Uiso 1 1 calc R . . C29 C 0.3137(3) 0.7229(3) 0.20111(18) 0.0387(7) Uani 1 1 d U . . H29 H 0.4009 0.7050 0.1887 0.046 Uiso 1 1 calc R . . C30 C 0.2397(3) 0.6501(3) 0.2710(2) 0.0396(7) Uani 1 1 d U . . H30 H 0.2772 0.5825 0.3039 0.048 Uiso 1 1 calc R . . C31 C 0.0621(3) 0.7675(3) 0.2419(2) 0.0412(7) Uani 1 1 d U . . C32 C 0.1376(3) 0.8388(3) 0.16857(19) 0.0385(7) Uani 1 1 d DU . . C33A C -0.0816(5) 0.7876(6) 0.2608(4) 0.0545(14) Uani 0.854(7) 1 d PU . . H33A H -0.0985 0.8791 0.2515 0.065 Uiso 0.854(7) 1 calc PR . . H33B H -0.1119 0.7548 0.3221 0.065 Uiso 0.854(7) 1 calc PR . . C34A C -0.1581(5) 0.7235(6) 0.2056(4) 0.093(2) Uani 0.854(7) 1 d PU . . H34A H -0.1340 0.7603 0.1450 0.140 Uiso 0.854(7) 1 calc PR . . H34B H -0.2482 0.7367 0.2236 0.140 Uiso 0.854(7) 1 calc PR . . H34C H -0.1404 0.6331 0.2131 0.140 Uiso 0.854(7) 1 calc PR . . C35A C 0.0815(11) 0.9401(7) 0.1069(8) 0.061(2) Uani 0.854(7) 1 d PU . . H35A H 0.1364 0.9528 0.0510 0.091 Uiso 0.854(7) 1 calc PR . . H35B H 0.0745 1.0192 0.1301 0.091 Uiso 0.854(7) 1 calc PR . . H35C H -0.0021 0.9133 0.1003 0.091 Uiso 0.854(7) 1 calc PR . . C33B C 0.068(7) 0.937(3) 0.113(5) 0.048(5) Uani 0.146(7) 1 d PDU . . H33C H 0.1281 0.9877 0.0678 0.058 Uiso 0.146(7) 1 calc PR . . H33D H 0.0184 0.9933 0.1484 0.058 Uiso 0.146(7) 1 calc PR . . C34B C -0.020(3) 0.862(3) 0.0722(18) 0.066(6) Uani 0.146(7) 1 d PDU . . H34D H -0.0359 0.7785 0.1065 0.099 Uiso 0.146(7) 1 calc PR . . H34E H 0.0194 0.8540 0.0138 0.099 Uiso 0.146(7) 1 calc PR . . H34F H -0.1002 0.9071 0.0704 0.099 Uiso 0.146(7) 1 calc PR . . C35B C -0.067(3) 0.812(3) 0.2901(19) 0.040(5) Uani 0.146(7) 1 d PU . . H35D H -0.1362 0.7639 0.2778 0.060 Uiso 0.146(7) 1 calc PR . . H35E H -0.0785 0.9017 0.2706 0.060 Uiso 0.146(7) 1 calc PR . . H35F H -0.0660 0.7971 0.3521 0.060 Uiso 0.146(7) 1 calc PR . . N1 N 0.2642(2) 0.8190(2) 0.15014(15) 0.0366(6) Uani 1 1 d U . . N2 N 0.1141(2) 0.6741(2) 0.29323(16) 0.0397(6) Uani 1 1 d U . . O1 O 0.3238(2) 1.1116(2) 0.05618(13) 0.0420(5) Uani 1 1 d U . . O2 O 0.4798(2) 1.22108(19) -0.04097(14) 0.0437(5) Uani 1 1 d U . . O3 O 0.6667(2) 1.0877(2) 0.05144(13) 0.0429(5) Uani 1 1 d U . . O4 O 0.5118(2) 0.9758(2) 0.14864(13) 0.0410(5) Uani 1 1 d U . . O5 O 0.2009(2) 0.5971(2) 0.46600(15) 0.0457(5) Uani 1 1 d U . . O6 O 0.1425(2) 0.4804(2) 0.59974(15) 0.0473(6) Uani 1 1 d U . . O7 O -0.1005(2) 0.6004(2) 0.61411(13) 0.0433(5) Uani 1 1 d U . . O8 O -0.0423(2) 0.7185(2) 0.48056(14) 0.0441(5) Uani 1 1 d U . . Rh1 Rh 0.41647(2) 0.94109(2) 0.051424(13) 0.03250(7) Uani 1 1 d U . . Rh2 Rh 0.03130(2) 0.56222(2) 0.428682(14) 0.03407(7) Uani 1 1 d U . . 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 0.0457(16) 0.0348(15) 0.0313(14) -0.0031(11) 0.0009(12) 0.0024(12) C2 0.0552(19) 0.0367(16) 0.0469(18) -0.0066(13) -0.0039(15) 0.0055(14) C3 0.076(3) 0.053(2) 0.072(2) -0.0016(19) 0.017(2) 0.0171(19) C4 0.093(3) 0.074(3) 0.102(3) -0.017(3) 0.014(3) 0.033(2) C5 0.101(3) 0.056(3) 0.123(4) -0.026(3) -0.014(3) 0.030(2) C6 0.095(3) 0.043(2) 0.135(4) -0.005(2) -0.012(3) 0.006(2) C7 0.066(2) 0.044(2) 0.103(3) -0.002(2) -0.002(2) 0.0045(18) C8 0.0434(16) 0.0359(15) 0.0318(14) -0.0034(12) 0.0019(12) 0.0046(13) C9 0.0484(18) 0.0454(17) 0.0363(15) -0.0051(13) -0.0030(13) 0.0064(14) C10 0.057(2) 0.055(2) 0.0479(19) -0.0023(16) -0.0061(16) -0.0031(17) C11 0.065(2) 0.071(3) 0.065(2) -0.005(2) -0.017(2) -0.009(2) C12 0.077(3) 0.088(3) 0.056(2) -0.018(2) -0.026(2) 0.000(2) C13 0.079(3) 0.103(3) 0.0386(19) -0.011(2) -0.0081(19) -0.005(2) C14 0.061(2) 0.080(3) 0.0373(18) -0.0049(17) -0.0026(16) -0.0076(19) C15 0.0362(16) 0.0379(16) 0.0529(18) -0.0078(14) 0.0031(14) -0.0008(13) C16 0.0419(18) 0.0500(19) 0.072(2) -0.0150(17) -0.0054(17) -0.0021(15) C17 0.047(2) 0.068(3) 0.096(3) -0.018(2) 0.003(2) -0.0127(18) C18 0.059(3) 0.096(3) 0.132(4) -0.020(3) 0.003(3) -0.025(2) C19 0.072(3) 0.126(4) 0.141(4) -0.027(4) -0.029(3) -0.027(3) C20 0.084(3) 0.131(4) 0.120(4) -0.018(3) -0.041(3) -0.017(3) C21 0.064(3) 0.096(3) 0.089(3) -0.012(3) -0.025(2) -0.012(2) C22 0.0334(15) 0.0361(15) 0.0376(15) -0.0045(12) 0.0034(12) -0.0037(12) C23 0.0373(15) 0.0360(15) 0.0373(15) -0.0080(12) 0.0033(12) -0.0050(12) C24 0.0543(19) 0.0464(18) 0.0372(16) -0.0086(13) -0.0018(14) -0.0018(15) C25 0.074(2) 0.061(2) 0.0391(17) -0.0215(16) 0.0015(17) -0.0006(18) C26 0.076(2) 0.051(2) 0.058(2) -0.0262(17) -0.0055(19) 0.0090(18) C27 0.085(3) 0.0402(19) 0.055(2) -0.0095(16) -0.0020(19) 0.0057(18) C28 0.063(2) 0.0391(17) 0.0421(17) -0.0063(14) 0.0058(15) -0.0001(15) C29 0.0368(15) 0.0393(16) 0.0318(14) 0.0028(12) 0.0096(12) 0.0023(12) C30 0.0417(16) 0.0317(15) 0.0371(15) 0.0035(12) 0.0086(13) 0.0038(12) C31 0.0410(16) 0.0353(15) 0.0402(16) -0.0007(12) 0.0095(13) -0.0019(12) C32 0.0421(16) 0.0355(15) 0.0331(14) -0.0002(12) 0.0029(12) -0.0021(12) C33A 0.045(3) 0.059(3) 0.049(3) 0.007(2) 0.006(2) 0.003(2) C34A 0.067(3) 0.108(5) 0.098(4) 0.009(3) -0.017(3) -0.019(3) C35A 0.051(4) 0.064(3) 0.056(3) 0.018(2) -0.001(3) 0.002(2) C33B 0.047(7) 0.047(7) 0.045(7) 0.003(6) -0.003(6) -0.003(6) C34B 0.069(9) 0.068(9) 0.060(9) 0.000(7) -0.018(7) 0.008(7) C35B 0.037(8) 0.041(8) 0.038(8) -0.008(7) 0.003(7) 0.005(7) N1 0.0425(14) 0.0348(13) 0.0261(11) 0.0014(9) 0.0069(10) -0.0009(10) N2 0.0405(14) 0.0319(13) 0.0382(13) 0.0015(10) 0.0120(11) -0.0024(10) O1 0.0469(12) 0.0345(11) 0.0368(11) -0.0002(9) 0.0106(9) 0.0017(9) O2 0.0522(13) 0.0291(11) 0.0402(11) 0.0029(9) 0.0119(10) 0.0004(9) O3 0.0479(13) 0.0464(13) 0.0303(10) -0.0006(9) 0.0015(9) -0.0098(10) O4 0.0456(12) 0.0471(13) 0.0262(10) 0.0000(9) 0.0012(9) -0.0046(10) O5 0.0371(12) 0.0490(13) 0.0438(12) 0.0015(10) 0.0069(10) -0.0128(10) O6 0.0395(12) 0.0519(14) 0.0453(13) 0.0028(10) -0.0015(10) -0.0092(10) O7 0.0506(13) 0.0347(11) 0.0363(11) -0.0010(9) 0.0122(10) 0.0020(9) O8 0.0538(13) 0.0327(11) 0.0366(11) -0.0008(9) 0.0154(10) -0.0007(9) Rh1 0.03923(13) 0.02926(12) 0.02266(11) 0.00212(8) 0.00749(9) -0.00157(9) Rh2 0.03499(13) 0.03045(12) 0.02969(12) 0.00059(9) 0.01060(9) -0.00389(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.264(3) . ? C1 O2 1.267(3) . ? C1 C2 1.488(4) . ? C2 C7 1.374(5) . ? C2 C3 1.383(5) . ? C3 C4 1.381(6) . ? C4 C5 1.365(7) . ? C5 C6 1.359(7) . ? C6 C7 1.384(6) . ? C8 O4 1.263(4) . ? C8 O3 1.269(3) . ? C8 C9 1.491(5) . ? C9 C14 1.376(4) . ? C9 C10 1.383(5) . ? C10 C11 1.379(6) . ? C11 C12 1.370(6) . ? C12 C13 1.362(6) . ? C13 C14 1.382(6) . ? C15 O6 1.261(4) . ? C15 O5 1.266(4) . ? C15 C16 1.496(5) . ? C16 C17 1.367(5) . ? C16 C21 1.381(6) . ? C17 C18 1.395(6) . ? C18 C19 1.366(8) . ? C19 C20 1.342(8) . ? C20 C21 1.385(6) . ? C22 O7 1.266(3) . ? C22 O8 1.268(3) . ? C22 C23 1.487(4) . ? C23 C28 1.384(4) . ? C23 C24 1.387(4) . ? C24 C25 1.376(5) . ? C25 C26 1.370(5) . ? C26 C27 1.365(5) . ? C27 C28 1.379(5) . ? C29 N1 1.338(4) . ? C29 C30 1.369(4) . ? C30 N2 1.343(4) . ? C31 N2 1.336(4) . ? C31 C32 1.403(4) . ? C31 C33A 1.513(6) . ? C31 C35B 1.55(3) . ? C32 N1 1.338(4) . ? C32 C35A 1.500(6) . ? C32 C33B 1.50(2) . ? C33A C34A 1.518(8) . ? C33B C34B 1.51(2) . ? N1 Rh1 2.293(2) . ? N2 Rh2 2.300(2) . ? O1 Rh1 2.035(2) . ? O2 Rh1 2.026(2) 2_675 ? O3 Rh1 2.026(2) 2_675 ? O4 Rh1 2.043(2) . ? O5 Rh2 2.030(2) . ? O6 Rh2 2.033(2) 2_566 ? O7 Rh2 2.022(2) 2_566 ? O8 Rh2 2.039(2) . ? Rh1 O2 2.026(2) 2_675 ? Rh1 O3 2.026(2) 2_675 ? Rh1 Rh1 2.4005(4) 2_675 ? Rh2 O7 2.022(2) 2_566 ? Rh2 O6 2.033(2) 2_566 ? Rh2 Rh2 2.4005(4) 2_566 ? 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 C1 O2 125.2(3) . . ? O1 C1 C2 117.7(3) . . ? O2 C1 C2 117.1(3) . . ? C7 C2 C3 118.7(3) . . ? C7 C2 C1 120.9(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 120.2(4) . . ? C5 C4 C3 120.2(5) . . ? C6 C5 C4 120.1(4) . . ? C5 C6 C7 120.0(5) . . ? C2 C7 C6 120.6(4) . . ? O4 C8 O3 125.5(3) . . ? O4 C8 C9 118.3(3) . . ? O3 C8 C9 116.2(3) . . ? C14 C9 C10 119.0(3) . . ? C14 C9 C8 121.0(3) . . ? C10 C9 C8 120.0(3) . . ? C11 C10 C9 120.4(4) . . ? C12 C11 C10 119.9(4) . . ? C13 C12 C11 120.2(4) . . ? C12 C13 C14 120.3(4) . . ? C9 C14 C13 120.2(4) . . ? O6 C15 O5 125.9(3) . . ? O6 C15 C16 117.0(3) . . ? O5 C15 C16 117.1(3) . . ? C17 C16 C21 119.9(4) . . ? C17 C16 C15 120.6(4) . . ? C21 C16 C15 119.5(4) . . ? C16 C17 C18 119.2(5) . . ? C19 C18 C17 118.9(5) . . ? C20 C19 C18 123.0(6) . . ? C19 C20 C21 118.0(6) . . ? C16 C21 C20 120.8(5) . . ? O7 C22 O8 125.6(3) . . ? O7 C22 C23 116.5(3) . . ? O8 C22 C23 117.9(3) . . ? C28 C23 C24 118.9(3) . . ? C28 C23 C22 120.5(3) . . ? C24 C23 C22 120.6(3) . . ? C25 C24 C23 120.3(3) . . ? C26 C25 C24 119.9(3) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C28 120.1(4) . . ? C27 C28 C23 120.2(3) . . ? N1 C29 C30 121.9(3) . . ? N2 C30 C29 121.4(3) . . ? N2 C31 C32 120.6(3) . . ? N2 C31 C33A 118.3(3) . . ? C32 C31 C33A 120.9(3) . . ? N2 C31 C35B 110.8(12) . . ? C32 C31 C35B 125.4(12) . . ? C33A C31 C35B 22.7(11) . . ? N1 C32 C31 121.2(3) . . ? N1 C32 C35A 116.7(6) . . ? C31 C32 C35A 122.2(6) . . ? N1 C32 C33B 123(3) . . ? C31 C32 C33B 116(3) . . ? C35A C32 C33B 6(4) . . ? C31 C33A C34A 114.5(5) . . ? C32 C33B C34B 106(2) . . ? C29 N1 C32 117.1(2) . . ? C29 N1 Rh1 113.53(19) . . ? C32 N1 Rh1 128.96(19) . . ? C31 N2 C30 117.6(2) . . ? C31 N2 Rh2 130.11(19) . . ? C30 N2 Rh2 111.60(19) . . ? C1 O1 Rh1 120.28(19) . . ? C1 O2 Rh1 118.80(18) . 2_675 ? C8 O3 Rh1 119.5(2) . 2_675 ? C8 O4 Rh1 119.13(19) . . ? C15 O5 Rh2 119.26(19) . . ? C15 O6 Rh2 119.0(2) . 2_566 ? C22 O7 Rh2 119.15(19) . 2_566 ? C22 O8 Rh2 119.36(19) . . ? O2 Rh1 O3 89.40(9) 2_675 2_675 ? O2 Rh1 O1 175.66(8) 2_675 . ? O3 Rh1 O1 90.93(9) 2_675 . ? O2 Rh1 O4 89.94(9) 2_675 . ? O3 Rh1 O4 175.76(8) 2_675 . ? O1 Rh1 O4 89.42(9) . . ? O2 Rh1 N1 88.21(8) 2_675 . ? O3 Rh1 N1 92.45(9) 2_675 . ? O1 Rh1 N1 96.10(8) . . ? O4 Rh1 N1 91.71(9) . . ? O2 Rh1 Rh1 88.71(6) 2_675 2_675 ? O3 Rh1 Rh1 88.08(6) 2_675 2_675 ? O1 Rh1 Rh1 86.97(6) . 2_675 ? O4 Rh1 Rh1 87.72(6) . 2_675 ? N1 Rh1 Rh1 176.87(6) . 2_675 ? O7 Rh2 O5 91.55(10) 2_566 . ? O7 Rh2 O6 88.36(10) 2_566 2_566 ? O5 Rh2 O6 175.77(8) . 2_566 ? O7 Rh2 O8 175.86(8) 2_566 . ? O5 Rh2 O8 88.29(10) . . ? O6 Rh2 O8 91.49(10) 2_566 . ? O7 Rh2 N2 88.26(8) 2_566 . ? O5 Rh2 N2 86.91(9) . . ? O6 Rh2 N2 97.32(9) 2_566 . ? O8 Rh2 N2 95.86(8) . . ? O7 Rh2 Rh2 88.47(6) 2_566 2_566 ? O5 Rh2 Rh2 87.75(6) . 2_566 ? O6 Rh2 Rh2 88.02(6) 2_566 2_566 ? O8 Rh2 Rh2 87.40(6) . 2_566 ? N2 Rh2 Rh2 173.66(7) . 2_566 ? 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 C1 C2 C7 176.4(4) . . . . ? O2 C1 C2 C7 -3.1(5) . . . . ? O1 C1 C2 C3 -1.6(5) . . . . ? O2 C1 C2 C3 178.9(4) . . . . ? C7 C2 C3 C4 0.3(7) . . . . ? C1 C2 C3 C4 178.3(4) . . . . ? C2 C3 C4 C5 -1.3(8) . . . . ? C3 C4 C5 C6 1.3(9) . . . . ? C4 C5 C6 C7 -0.3(9) . . . . ? C3 C2 C7 C6 0.7(7) . . . . ? C1 C2 C7 C6 -177.3(4) . . . . ? C5 C6 C7 C2 -0.7(8) . . . . ? O4 C8 C9 C14 -1.9(5) . . . . ? O3 C8 C9 C14 177.9(3) . . . . ? O4 C8 C9 C10 179.2(3) . . . . ? O3 C8 C9 C10 -1.1(5) . . . . ? C14 C9 C10 C11 0.0(6) . . . . ? C8 C9 C10 C11 179.0(3) . . . . ? C9 C10 C11 C12 0.1(6) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C11 C12 C13 C14 0.9(8) . . . . ? C10 C9 C14 C13 0.3(6) . . . . ? C8 C9 C14 C13 -178.7(4) . . . . ? C12 C13 C14 C9 -0.7(7) . . . . ? O6 C15 C16 C17 173.5(3) . . . . ? O5 C15 C16 C17 -8.7(5) . . . . ? O6 C15 C16 C21 -6.9(5) . . . . ? O5 C15 C16 C21 170.9(4) . . . . ? C21 C16 C17 C18 0.9(7) . . . . ? C15 C16 C17 C18 -179.5(4) . . . . ? C16 C17 C18 C19 -1.1(8) . . . . ? C17 C18 C19 C20 0.3(10) . . . . ? C18 C19 C20 C21 0.7(10) . . . . ? C17 C16 C21 C20 0.1(7) . . . . ? C15 C16 C21 C20 -179.5(5) . . . . ? C19 C20 C21 C16 -0.9(9) . . . . ? O7 C22 C23 C28 -171.7(3) . . . . ? O8 C22 C23 C28 7.3(5) . . . . ? O7 C22 C23 C24 6.0(5) . . . . ? O8 C22 C23 C24 -175.0(3) . . . . ? C28 C23 C24 C25 2.3(5) . . . . ? C22 C23 C24 C25 -175.4(3) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C24 C25 C26 C27 -1.0(7) . . . . ? C25 C26 C27 C28 1.4(7) . . . . ? C26 C27 C28 C23 0.0(6) . . . . ? C24 C23 C28 C27 -1.9(5) . . . . ? C22 C23 C28 C27 175.9(3) . . . . ? N1 C29 C30 N2 -1.8(5) . . . . ? N2 C31 C32 N1 -2.8(5) . . . . ? C33A C31 C32 N1 -178.1(4) . . . . ? C35B C31 C32 N1 155.2(14) . . . . ? N2 C31 C32 C35A 177.0(5) . . . . ? C33A C31 C32 C35A 1.7(7) . . . . ? C35B C31 C32 C35A -25.0(16) . . . . ? N2 C31 C32 C33B 177(2) . . . . ? C33A C31 C32 C33B 1(2) . . . . ? C35B C31 C32 C33B -25(2) . . . . ? N2 C31 C33A C34A -97.1(5) . . . . ? C32 C31 C33A C34A 78.4(6) . . . . ? C35B C31 C33A C34A -173(4) . . . . ? N1 C32 C33B C34B 113(4) . . . . ? C31 C32 C33B C34B -67(6) . . . . ? C35A C32 C33B C34B 115(24) . . . . ? C30 C29 N1 C32 -2.1(5) . . . . ? C30 C29 N1 Rh1 171.5(3) . . . . ? C31 C32 N1 C29 4.3(5) . . . . ? C35A C32 N1 C29 -175.5(5) . . . . ? C33B C32 N1 C29 -175(2) . . . . ? C31 C32 N1 Rh1 -168.2(2) . . . . ? C35A C32 N1 Rh1 12.0(6) . . . . ? C33B C32 N1 Rh1 12(2) . . . . ? C32 C31 N2 C30 -1.2(5) . . . . ? C33A C31 N2 C30 174.3(4) . . . . ? C35B C31 N2 C30 -162.1(13) . . . . ? C32 C31 N2 Rh2 168.5(2) . . . . ? C33A C31 N2 Rh2 -16.1(5) . . . . ? C35B C31 N2 Rh2 7.5(13) . . . . ? C29 C30 N2 C31 3.4(5) . . . . ? C29 C30 N2 Rh2 -168.1(3) . . . . ? O2 C1 O1 Rh1 0.6(5) . . . . ? C2 C1 O1 Rh1 -178.9(2) . . . . ? O1 C1 O2 Rh1 -1.1(5) . . . 2_675 ? C2 C1 O2 Rh1 178.3(2) . . . 2_675 ? O4 C8 O3 Rh1 2.6(4) . . . 2_675 ? C9 C8 O3 Rh1 -177.2(2) . . . 2_675 ? O3 C8 O4 Rh1 -3.2(4) . . . . ? C9 C8 O4 Rh1 176.5(2) . . . . ? O6 C15 O5 Rh2 2.8(5) . . . . ? C16 C15 O5 Rh2 -174.7(2) . . . . ? O5 C15 O6 Rh2 -2.9(5) . . . 2_566 ? C16 C15 O6 Rh2 174.7(2) . . . 2_566 ? O8 C22 O7 Rh2 2.0(4) . . . 2_566 ? C23 C22 O7 Rh2 -179.1(2) . . . 2_566 ? O7 C22 O8 Rh2 -2.1(4) . . . . ? C23 C22 O8 Rh2 179.1(2) . . . . ? C1 O1 Rh1 O2 6.4(14) . . . 2_675 ? C1 O1 Rh1 O3 -87.9(2) . . . 2_675 ? C1 O1 Rh1 O4 87.9(2) . . . . ? C1 O1 Rh1 N1 179.6(2) . . . . ? C1 O1 Rh1 Rh1 0.2(2) . . . 2_675 ? C8 O4 Rh1 O2 90.7(2) . . . 2_675 ? C8 O4 Rh1 O3 9.7(13) . . . 2_675 ? C8 O4 Rh1 O1 -85.0(2) . . . . ? C8 O4 Rh1 N1 178.9(2) . . . . ? C8 O4 Rh1 Rh1 2.0(2) . . . 2_675 ? C29 N1 Rh1 O2 35.1(2) . . . 2_675 ? C32 N1 Rh1 O2 -152.1(3) . . . 2_675 ? C29 N1 Rh1 O3 124.4(2) . . . 2_675 ? C32 N1 Rh1 O3 -62.8(3) . . . 2_675 ? C29 N1 Rh1 O1 -144.4(2) . . . . ? C32 N1 Rh1 O1 28.4(3) . . . . ? C29 N1 Rh1 O4 -54.8(2) . . . . ? C32 N1 Rh1 O4 118.0(3) . . . . ? C29 N1 Rh1 Rh1 24.7(14) . . . 2_675 ? C32 N1 Rh1 Rh1 -162.5(11) . . . 2_675 ? C15 O5 Rh2 O7 -89.7(2) . . . 2_566 ? C15 O5 Rh2 O6 -0.9(14) . . . 2_566 ? C15 O5 Rh2 O8 86.2(2) . . . . ? C15 O5 Rh2 N2 -177.8(2) . . . . ? C15 O5 Rh2 Rh2 -1.3(2) . . . 2_566 ? C22 O8 Rh2 O7 1.1(14) . . . 2_566 ? C22 O8 Rh2 O5 -86.9(2) . . . . ? C22 O8 Rh2 O6 88.9(2) . . . 2_566 ? C22 O8 Rh2 N2 -173.6(2) . . . . ? C22 O8 Rh2 Rh2 1.0(2) . . . 2_566 ? C31 N2 Rh2 O7 136.1(3) . . . 2_566 ? C30 N2 Rh2 O7 -53.8(2) . . . 2_566 ? C31 N2 Rh2 O5 -132.3(3) . . . . ? C30 N2 Rh2 O5 37.8(2) . . . . ? C31 N2 Rh2 O6 47.9(3) . . . 2_566 ? C30 N2 Rh2 O6 -142.0(2) . . . 2_566 ? C31 N2 Rh2 O8 -44.3(3) . . . . ? C30 N2 Rh2 O8 125.8(2) . . . . ? C31 N2 Rh2 Rh2 -165.0(5) . . . 2_566 ? C30 N2 Rh2 Rh2 5.1(8) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.957 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.082 #===END data_50927k1 _database_code_depnum_ccdc_archive 'CCDC 642581' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.11 H30 N2 O8.23 Rh2' _chemical_formula_weight 817.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3535(8) _cell_length_b 10.4929(8) _cell_length_c 15.6133(12) _cell_angle_alpha 80.184(2) _cell_angle_beta 80.752(2) _cell_angle_gamma 87.0850(10) _cell_volume 1649.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 821 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5698 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; The measurement was carried out in a pressurized CO2 atmosphere (ca. 6.4MPa at room temperature). ; _diffrn_ambient_temperature 90 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12065 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8032 _reflns_number_gt 6704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.9600P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8032 _refine_ls_number_parameters 484 _refine_ls_number_restraints 666 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.009 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3664(2) 1.2159(2) 0.01222(15) 0.0172(5) Uani 1 1 d U . . C2 C 0.2912(3) 1.3392(2) 0.02298(16) 0.0196(5) Uani 1 1 d U . . C3 C 0.1690(3) 1.3365(3) 0.07561(18) 0.0272(6) Uani 1 1 d U . . H3 H 0.1322 1.2560 0.1035 0.033 Uiso 1 1 calc R . . C4 C 0.1010(3) 1.4513(3) 0.0874(2) 0.0359(7) Uani 1 1 d U . . H4 H 0.0170 1.4493 0.1225 0.043 Uiso 1 1 calc R . . C5 C 0.1556(3) 1.5685(3) 0.0479(2) 0.0349(7) Uani 1 1 d U . . H5 H 0.1093 1.6469 0.0565 0.042 Uiso 1 1 calc R . . C6 C 0.2769(3) 1.5721(3) -0.0039(2) 0.0347(7) Uani 1 1 d U . . H6 H 0.3143 1.6528 -0.0306 0.042 Uiso 1 1 calc R . . C7 C 0.3443(3) 1.4573(3) -0.0172(2) 0.0278(6) Uani 1 1 d U . . H7 H 0.4270 1.4598 -0.0539 0.033 Uiso 1 1 calc R . . C8 C 0.6143(2) 1.0423(2) 0.12947(15) 0.0173(5) Uani 1 1 d U . . C9 C 0.6768(2) 1.0754(2) 0.20226(16) 0.0185(5) Uani 1 1 d U . . C10 C 0.7891(3) 1.1489(3) 0.18239(17) 0.0220(5) Uani 1 1 d U . . H10 H 0.8256 1.1773 0.1228 0.026 Uiso 1 1 calc R . . C11 C 0.8475(3) 1.1807(3) 0.24934(18) 0.0262(6) Uani 1 1 d U . . H11 H 0.9244 1.2305 0.2356 0.031 Uiso 1 1 calc R . . C12 C 0.7943(3) 1.1399(3) 0.33632(18) 0.0273(6) Uani 1 1 d U . . H12 H 0.8347 1.1616 0.3822 0.033 Uiso 1 1 calc R . . C13 C 0.6817(3) 1.0673(3) 0.35647(18) 0.0288(6) Uani 1 1 d U . . H13 H 0.6449 1.0394 0.4161 0.035 Uiso 1 1 calc R . . C14 C 0.6231(3) 1.0354(3) 0.28964(16) 0.0232(5) Uani 1 1 d U . . H14 H 0.5459 0.9861 0.3035 0.028 Uiso 1 1 calc R . . C15 C 0.2223(3) 0.5469(2) 0.54517(17) 0.0226(5) Uani 1 1 d U . . C16 C 0.3433(3) 0.5857(3) 0.5740(2) 0.0271(6) Uani 1 1 d U . . C17 C 0.4399(3) 0.6528(3) 0.5136(2) 0.0335(7) Uani 1 1 d U . . H17 H 0.4307 0.6732 0.4532 0.040 Uiso 1 1 calc R . . C18 C 0.5500(3) 0.6897(3) 0.5428(3) 0.0433(8) Uani 1 1 d U . . H18 H 0.6169 0.7354 0.5021 0.052 Uiso 1 1 calc R . . C19 C 0.5624(3) 0.6601(4) 0.6306(3) 0.0482(8) Uani 1 1 d U . . H19 H 0.6383 0.6854 0.6498 0.058 Uiso 1 1 calc R . . C20 C 0.4664(4) 0.5945(4) 0.6907(3) 0.0481(8) Uani 1 1 d U . . H20 H 0.4753 0.5756 0.7512 0.058 Uiso 1 1 calc R . . C21 C 0.3566(3) 0.5564(3) 0.6623(2) 0.0373(7) Uani 1 1 d U . . H21 H 0.2904 0.5101 0.7033 0.045 Uiso 1 1 calc R . . C22 C -0.0904(2) 0.7088(2) 0.56099(16) 0.0182(5) Uani 1 1 d U . . C23 C -0.1408(2) 0.8275(2) 0.59700(16) 0.0176(5) Uani 1 1 d U . . C24 C -0.1836(2) 0.8205(2) 0.68680(16) 0.0212(5) Uani 1 1 d U . . H24 H -0.1743 0.7416 0.7257 0.025 Uiso 1 1 calc R . . C25 C -0.2400(3) 0.9288(3) 0.71959(17) 0.0250(5) Uani 1 1 d U . . H25 H -0.2698 0.9238 0.7809 0.030 Uiso 1 1 calc R . . C26 C -0.2529(3) 1.0435(3) 0.66317(18) 0.0258(6) Uani 1 1 d U . . H26 H -0.2934 1.1169 0.6856 0.031 Uiso 1 1 calc R . . C27 C -0.2071(3) 1.0525(3) 0.57405(18) 0.0260(6) Uani 1 1 d U . . H27 H -0.2138 1.1325 0.5358 0.031 Uiso 1 1 calc R . . C28 C -0.1511(3) 0.9442(2) 0.54058(16) 0.0213(5) Uani 1 1 d U . . H28 H -0.1201 0.9499 0.4794 0.026 Uiso 1 1 calc R . . C29 C 0.3177(2) 0.7169(2) 0.19997(15) 0.0186(5) Uani 1 1 d U . . H29 H 0.4082 0.6958 0.1865 0.022 Uiso 1 1 calc R . . C30 C 0.2430(2) 0.6446(2) 0.27057(16) 0.0208(5) Uani 1 1 d U . . H30 H 0.2823 0.5727 0.3035 0.025 Uiso 1 1 calc R . . C31 C 0.0607(3) 0.7696(2) 0.24281(17) 0.0218(5) Uani 1 1 d DU . . C32 C 0.1370(2) 0.8411(2) 0.16877(16) 0.0185(5) Uani 1 1 d DU . . C33A C -0.0850(3) 0.7972(4) 0.2632(3) 0.0251(8) Uani 0.868(6) 1 d PDU . . H33A H -0.1016 0.8919 0.2511 0.030 Uiso 0.868(6) 1 calc PR . . H33B H -0.1151 0.7673 0.3266 0.030 Uiso 0.868(6) 1 calc PR . . C34A C -0.1647(4) 0.7309(4) 0.2092(3) 0.0376(9) Uani 0.868(6) 1 d PDU . . H34A H -0.1420 0.7669 0.1467 0.056 Uiso 0.868(6) 1 calc PR . . H34B H -0.2584 0.7458 0.2283 0.056 Uiso 0.868(6) 1 calc PR . . H34C H -0.1447 0.6378 0.2181 0.056 Uiso 0.868(6) 1 calc PR . . C35A C 0.0777(7) 0.9465(5) 0.1086(6) 0.0262(14) Uani 0.868(6) 1 d PDU . . H35A H 0.0640 1.0246 0.1358 0.039 Uiso 0.868(6) 1 calc PR . . H35B H -0.0065 0.9186 0.0981 0.039 Uiso 0.868(6) 1 calc PR . . H35C H 0.1367 0.9652 0.0526 0.039 Uiso 0.868(6) 1 calc PR . . C33B C 0.064(5) 0.947(3) 0.116(4) 0.021(3) Uani 0.132(6) 1 d PDU . . H33C H 0.1248 0.9964 0.0677 0.026 Uiso 0.132(6) 1 calc PR . . H33D H 0.0181 1.0068 0.1537 0.026 Uiso 0.132(6) 1 calc PR . . C34B C -0.034(2) 0.874(2) 0.0788(14) 0.027(4) Uani 0.132(6) 1 d PDU . . H34D H 0.0096 0.8432 0.0254 0.040 Uiso 0.132(6) 1 calc PR . . H34E H -0.1072 0.9327 0.0646 0.040 Uiso 0.132(6) 1 calc PR . . H34F H -0.0672 0.8002 0.1228 0.040 Uiso 0.132(6) 1 calc PR . . C35B C -0.0669(19) 0.812(2) 0.2935(16) 0.022(4) Uani 0.132(6) 1 d PDU . . H35D H -0.1312 0.7443 0.3017 0.033 Uiso 0.132(6) 1 calc PR . . H35E H -0.1000 0.8919 0.2606 0.033 Uiso 0.132(6) 1 calc PR . . H35F H -0.0519 0.8285 0.3511 0.033 Uiso 0.132(6) 1 calc PR . . N1 N 0.2657(2) 0.8171(2) 0.14937(13) 0.0181(4) Uani 1 1 d U . . N2 N 0.1149(2) 0.6735(2) 0.29419(14) 0.0206(4) Uani 1 1 d U . . O1 O 0.31728(17) 1.11256(16) 0.05711(11) 0.0185(4) Uani 1 1 d U . . O2 O 0.47376(17) 1.22398(16) -0.03996(11) 0.0195(4) Uani 1 1 d U . . O3 O 0.66744(17) 1.08805(17) 0.05174(11) 0.0187(4) Uani 1 1 d U . . O4 O 0.51316(17) 0.97373(17) 0.14950(11) 0.0186(4) Uani 1 1 d U . . O5 O 0.20509(18) 0.59261(17) 0.46661(12) 0.0235(4) Uani 1 1 d U . . O6 O 0.14452(18) 0.47493(18) 0.60122(12) 0.0241(4) Uani 1 1 d U . . O7 O -0.10155(18) 0.60274(17) 0.61470(11) 0.0218(4) Uani 1 1 d U . . O8 O -0.04201(18) 0.72150(17) 0.48042(11) 0.0220(4) Uani 1 1 d U . . Rh1 Rh 0.416806(18) 0.939984(17) 0.051499(11) 0.01412(5) Uani 1 1 d U . . Rh2 Rh 0.032143(19) 0.562453(18) 0.428420(12) 0.01767(6) Uani 1 1 d U . . O2S O -0.436(2) 0.743(3) 0.3164(16) 0.074(5) Uani 0.111(5) 1 d PDU . . O1S O -0.300(2) 0.720(3) 0.1861(16) 0.073(5) Uani 0.111(5) 1 d PDU . . C1S C -0.371(2) 0.731(5) 0.2502(17) 0.074(5) Uani 0.111(5) 1 d PDU . . 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 0.0208(11) 0.0156(11) 0.0138(10) -0.0003(8) -0.0014(9) 0.0001(9) C2 0.0224(12) 0.0176(11) 0.0184(11) -0.0032(9) -0.0026(9) 0.0022(9) C3 0.0271(14) 0.0232(13) 0.0282(13) -0.0025(10) 0.0025(11) 0.0031(11) C4 0.0339(15) 0.0322(15) 0.0389(15) -0.0097(13) 0.0029(13) 0.0098(12) C5 0.0371(16) 0.0248(14) 0.0447(16) -0.0105(12) -0.0105(13) 0.0109(12) C6 0.0362(16) 0.0191(13) 0.0486(17) -0.0023(12) -0.0091(13) 0.0001(11) C7 0.0255(13) 0.0200(13) 0.0361(14) -0.0018(11) -0.0030(11) 0.0012(10) C8 0.0202(11) 0.0159(11) 0.0141(10) -0.0021(8) 0.0005(9) 0.0031(9) C9 0.0196(11) 0.0189(11) 0.0157(10) -0.0021(9) -0.0007(9) 0.0044(9) C10 0.0231(12) 0.0226(12) 0.0182(11) 0.0001(9) -0.0008(9) 0.0000(10) C11 0.0260(13) 0.0269(13) 0.0253(13) -0.0021(10) -0.0036(10) -0.0047(11) C12 0.0289(14) 0.0339(14) 0.0206(12) -0.0063(11) -0.0071(10) 0.0019(11) C13 0.0302(14) 0.0384(15) 0.0164(11) -0.0019(11) -0.0026(10) -0.0001(12) C14 0.0205(12) 0.0296(13) 0.0173(11) -0.0006(10) 0.0008(9) -0.0021(10) C15 0.0211(12) 0.0183(11) 0.0258(12) -0.0048(10) 0.0046(10) 0.0016(9) C16 0.0246(13) 0.0189(12) 0.0373(14) -0.0079(11) 0.0001(11) 0.0004(10) C17 0.0258(14) 0.0290(14) 0.0450(16) -0.0120(12) 0.0043(12) -0.0047(11) C18 0.0264(15) 0.0393(17) 0.064(2) -0.0152(15) 0.0012(14) -0.0067(13) C19 0.0333(17) 0.0448(18) 0.071(2) -0.0144(17) -0.0160(16) -0.0037(14) C20 0.0425(18) 0.0468(19) 0.058(2) -0.0058(16) -0.0185(16) -0.0021(15) C21 0.0349(16) 0.0316(15) 0.0455(17) -0.0039(13) -0.0085(13) -0.0028(13) C22 0.0187(11) 0.0160(11) 0.0172(11) -0.0008(9) 0.0034(9) -0.0027(9) C23 0.0163(11) 0.0163(11) 0.0190(11) -0.0024(9) 0.0014(9) -0.0023(9) C24 0.0229(12) 0.0205(12) 0.0189(11) -0.0012(9) -0.0010(9) -0.0024(10) C25 0.0302(14) 0.0265(13) 0.0181(11) -0.0073(10) 0.0012(10) -0.0018(11) C26 0.0317(14) 0.0203(12) 0.0258(12) -0.0103(10) 0.0004(11) 0.0016(10) C27 0.0361(15) 0.0171(12) 0.0232(12) -0.0019(10) -0.0014(11) 0.0003(11) C28 0.0281(13) 0.0166(11) 0.0167(11) -0.0011(9) 0.0019(10) -0.0003(10) C29 0.0187(11) 0.0181(11) 0.0156(10) 0.0002(9) 0.0033(9) 0.0012(9) C30 0.0213(12) 0.0169(11) 0.0201(11) -0.0001(9) 0.0051(9) 0.0010(9) C31 0.0222(12) 0.0174(11) 0.0225(12) -0.0015(9) 0.0046(10) -0.0015(9) C32 0.0205(12) 0.0163(11) 0.0172(11) -0.0024(9) 0.0022(9) -0.0028(9) C33A 0.0201(16) 0.0248(16) 0.0254(18) 0.0024(14) 0.0040(13) 0.0030(12) C34A 0.0292(18) 0.040(2) 0.041(2) 0.0019(15) -0.0055(15) -0.0056(15) C35A 0.021(2) 0.0276(17) 0.026(2) 0.0037(14) 0.000(2) 0.0019(14) C33B 0.021(5) 0.021(5) 0.021(5) -0.001(4) 0.000(4) -0.002(4) C34B 0.025(6) 0.030(6) 0.025(6) -0.001(5) -0.007(5) 0.002(5) C35B 0.019(6) 0.022(6) 0.022(6) 0.001(5) 0.000(5) 0.000(5) N1 0.0213(10) 0.0160(10) 0.0145(9) -0.0012(7) 0.0034(8) -0.0019(8) N2 0.0213(11) 0.0161(10) 0.0199(10) -0.0002(8) 0.0072(8) -0.0002(8) O1 0.0202(9) 0.0152(8) 0.0161(8) 0.0010(6) 0.0051(7) 0.0020(7) O2 0.0221(9) 0.0149(8) 0.0182(8) -0.0010(6) 0.0052(7) 0.0002(7) O3 0.0213(9) 0.0200(9) 0.0127(8) 0.0002(6) 0.0020(6) -0.0042(7) O4 0.0201(9) 0.0214(9) 0.0122(8) 0.0004(6) 0.0012(6) -0.0026(7) O5 0.0213(9) 0.0202(9) 0.0247(9) -0.0011(7) 0.0080(7) -0.0051(7) O6 0.0238(10) 0.0219(9) 0.0235(9) 0.0005(7) 0.0024(7) -0.0039(7) O7 0.0272(10) 0.0165(8) 0.0174(8) -0.0012(7) 0.0073(7) 0.0000(7) O8 0.0269(10) 0.0160(8) 0.0184(8) -0.0010(7) 0.0084(7) -0.0005(7) Rh1 0.01715(10) 0.01304(9) 0.00936(9) 0.00148(6) 0.00305(6) -0.00100(7) Rh2 0.01989(11) 0.01305(10) 0.01569(9) 0.00040(7) 0.00778(7) -0.00165(7) O2S 0.074(5) 0.074(5) 0.074(5) -0.0121(12) -0.0114(12) -0.0017(9) O1S 0.073(5) 0.073(5) 0.073(5) -0.0119(12) -0.0113(12) -0.0016(9) C1S 0.074(5) 0.074(5) 0.074(5) -0.0121(12) -0.0114(11) -0.0017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.266(3) . ? C1 O1 1.268(3) . ? C1 C2 1.496(3) . ? C2 C7 1.387(4) . ? C2 C3 1.392(4) . ? C3 C4 1.388(4) . ? C4 C5 1.383(4) . ? C5 C6 1.378(4) . ? C6 C7 1.390(4) . ? C8 O4 1.267(3) . ? C8 O3 1.273(3) . ? C8 C9 1.492(3) . ? C9 C14 1.390(3) . ? C9 C10 1.391(4) . ? C10 C11 1.383(4) . ? C11 C12 1.384(4) . ? C12 C13 1.389(4) . ? C13 C14 1.382(4) . ? C15 O6 1.263(3) . ? C15 O5 1.276(3) . ? C15 C16 1.495(4) . ? C16 C21 1.388(4) . ? C16 C17 1.388(4) . ? C17 C18 1.388(5) . ? C18 C19 1.379(5) . ? C19 C20 1.376(5) . ? C20 C21 1.384(5) . ? C22 O8 1.264(3) . ? C22 O7 1.272(3) . ? C22 C23 1.489(3) . ? C23 C28 1.391(3) . ? C23 C24 1.392(3) . ? C24 C25 1.389(3) . ? C25 C26 1.380(4) . ? C26 C27 1.385(4) . ? C27 C28 1.393(3) . ? C29 N1 1.347(3) . ? C29 C30 1.375(3) . ? C30 N2 1.352(3) . ? C31 N2 1.337(3) . ? C31 C32 1.412(3) . ? C31 C33A 1.514(4) . ? C31 C35B 1.516(16) . ? C32 N1 1.339(3) . ? C32 C35A 1.498(5) . ? C32 C33B 1.51(2) . ? C33A C34A 1.536(6) . ? C33B C34B 1.54(2) . ? N1 Rh1 2.283(2) . ? N2 Rh2 2.275(2) . ? O1 Rh1 2.0455(17) . ? O2 Rh1 2.0293(17) 2_675 ? O3 Rh1 2.0212(17) 2_675 ? O4 Rh1 2.0429(17) . ? O5 Rh2 2.032(2) . ? O6 Rh2 2.0299(19) 2_566 ? O7 Rh2 2.0224(17) 2_566 ? O8 Rh2 2.0408(17) . ? Rh1 O3 2.0212(17) 2_675 ? Rh1 O2 2.0293(17) 2_675 ? Rh1 Rh1 2.4041(4) 2_675 ? Rh2 O7 2.0224(17) 2_566 ? Rh2 O6 2.0299(19) 2_566 ? Rh2 Rh2 2.4018(4) 2_566 ? O2S C1S 1.1604(10) . ? O1S C1S 1.1604(10) . ? 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 125.8(2) . . ? O2 C1 C2 117.3(2) . . ? O1 C1 C2 116.9(2) . . ? C7 C2 C3 119.5(2) . . ? C7 C2 C1 120.4(2) . . ? C3 C2 C1 120.2(2) . . ? C4 C3 C2 120.1(3) . . ? C5 C4 C3 120.0(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C7 119.9(3) . . ? C2 C7 C6 120.3(3) . . ? O4 C8 O3 125.7(2) . . ? O4 C8 C9 118.2(2) . . ? O3 C8 C9 116.1(2) . . ? C14 C9 C10 119.6(2) . . ? C14 C9 C8 120.8(2) . . ? C10 C9 C8 119.6(2) . . ? C11 C10 C9 120.1(2) . . ? C10 C11 C12 120.1(3) . . ? C11 C12 C13 120.0(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C9 120.2(3) . . ? O6 C15 O5 125.8(3) . . ? O6 C15 C16 117.3(2) . . ? O5 C15 C16 116.9(2) . . ? C21 C16 C17 120.4(3) . . ? C21 C16 C15 119.2(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 119.1(3) . . ? C19 C18 C17 120.2(3) . . ? C20 C19 C18 120.9(3) . . ? C19 C20 C21 119.4(4) . . ? C20 C21 C16 120.1(3) . . ? O8 C22 O7 125.8(2) . . ? O8 C22 C23 117.8(2) . . ? O7 C22 C23 116.4(2) . . ? C28 C23 C24 119.8(2) . . ? C28 C23 C22 120.1(2) . . ? C24 C23 C22 120.0(2) . . ? C25 C24 C23 120.0(2) . . ? C26 C25 C24 120.0(2) . . ? C25 C26 C27 120.4(2) . . ? C26 C27 C28 120.0(2) . . ? C23 C28 C27 119.8(2) . . ? N1 C29 C30 121.6(2) . . ? N2 C30 C29 121.4(2) . . ? N2 C31 C32 120.6(2) . . ? N2 C31 C33A 118.9(2) . . ? C32 C31 C33A 120.5(3) . . ? N2 C31 C35B 108.8(10) . . ? C32 C31 C35B 127.3(10) . . ? C33A C31 C35B 22.2(9) . . ? N1 C32 C31 121.2(2) . . ? N1 C32 C35A 117.2(4) . . ? C31 C32 C35A 121.6(4) . . ? N1 C32 C33B 123(3) . . ? C31 C32 C33B 115(3) . . ? C35A C32 C33B 6(3) . . ? C31 C33A C34A 112.7(3) . . ? C32 C33B C34B 104.4(18) . . ? C32 N1 C29 117.3(2) . . ? C32 N1 Rh1 128.11(17) . . ? C29 N1 Rh1 114.06(16) . . ? C31 N2 C30 117.6(2) . . ? C31 N2 Rh2 129.73(16) . . ? C30 N2 Rh2 112.15(17) . . ? C1 O1 Rh1 119.85(15) . . ? C1 O2 Rh1 118.45(15) . 2_675 ? C8 O3 Rh1 119.38(16) . 2_675 ? C8 O4 Rh1 118.92(15) . . ? C15 O5 Rh2 118.71(16) . . ? C15 O6 Rh2 119.29(18) . 2_566 ? C22 O7 Rh2 118.82(15) . 2_566 ? C22 O8 Rh2 119.37(16) . . ? O3 Rh1 O2 88.87(7) 2_675 2_675 ? O3 Rh1 O4 175.88(6) 2_675 . ? O2 Rh1 O4 90.44(7) 2_675 . ? O3 Rh1 O1 91.21(7) 2_675 . ? O2 Rh1 O1 175.82(6) 2_675 . ? O4 Rh1 O1 89.19(7) . . ? O3 Rh1 N1 92.10(7) 2_675 . ? O2 Rh1 N1 88.17(7) 2_675 . ? O4 Rh1 N1 91.93(7) . . ? O1 Rh1 N1 96.00(7) . . ? O3 Rh1 Rh1 88.22(5) 2_675 2_675 ? O2 Rh1 Rh1 88.98(5) 2_675 2_675 ? O4 Rh1 Rh1 87.71(5) . 2_675 ? O1 Rh1 Rh1 86.85(5) . 2_675 ? N1 Rh1 Rh1 177.12(5) . 2_675 ? O7 Rh2 O6 87.90(8) 2_566 2_566 ? O7 Rh2 O5 92.05(8) 2_566 . ? O6 Rh2 O5 175.98(7) 2_566 . ? O7 Rh2 O8 175.96(7) 2_566 . ? O6 Rh2 O8 91.85(8) 2_566 . ? O5 Rh2 O8 87.92(7) . . ? O7 Rh2 N2 88.43(7) 2_566 . ? O6 Rh2 N2 97.21(8) 2_566 . ? O5 Rh2 N2 86.80(8) . . ? O8 Rh2 N2 95.60(7) . . ? O7 Rh2 Rh2 88.59(5) 2_566 2_566 ? O6 Rh2 Rh2 87.90(5) 2_566 2_566 ? O5 Rh2 Rh2 88.08(5) . 2_566 ? O8 Rh2 Rh2 87.37(5) . 2_566 ? N2 Rh2 Rh2 173.99(6) . 2_566 ? O2S C1S O1S 176(2) . . ? 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 C1 C2 C7 -5.5(4) . . . . ? O1 C1 C2 C7 173.7(2) . . . . ? O2 C1 C2 C3 176.5(2) . . . . ? O1 C1 C2 C3 -4.3(4) . . . . ? C7 C2 C3 C4 0.2(4) . . . . ? C1 C2 C3 C4 178.3(3) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C3 C4 C5 C6 0.7(5) . . . . ? C4 C5 C6 C7 0.5(5) . . . . ? C3 C2 C7 C6 0.9(4) . . . . ? C1 C2 C7 C6 -177.1(3) . . . . ? C5 C6 C7 C2 -1.3(5) . . . . ? O4 C8 C9 C14 -2.0(4) . . . . ? O3 C8 C9 C14 177.0(2) . . . . ? O4 C8 C9 C10 179.0(2) . . . . ? O3 C8 C9 C10 -2.0(3) . . . . ? C14 C9 C10 C11 0.7(4) . . . . ? C8 C9 C10 C11 179.7(2) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 C9 0.3(4) . . . . ? C10 C9 C14 C13 -0.7(4) . . . . ? C8 C9 C14 C13 -179.7(2) . . . . ? O6 C15 C16 C21 -8.5(4) . . . . ? O5 C15 C16 C21 169.6(3) . . . . ? O6 C15 C16 C17 173.0(2) . . . . ? O5 C15 C16 C17 -8.9(4) . . . . ? C21 C16 C17 C18 0.3(4) . . . . ? C15 C16 C17 C18 178.7(3) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 -0.3(6) . . . . ? C18 C19 C20 C21 0.8(6) . . . . ? C19 C20 C21 C16 -0.8(5) . . . . ? C17 C16 C21 C20 0.2(5) . . . . ? C15 C16 C21 C20 -178.2(3) . . . . ? O8 C22 C23 C28 9.2(4) . . . . ? O7 C22 C23 C28 -170.1(2) . . . . ? O8 C22 C23 C24 -174.0(2) . . . . ? O7 C22 C23 C24 6.7(4) . . . . ? C28 C23 C24 C25 1.9(4) . . . . ? C22 C23 C24 C25 -175.0(2) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? C24 C25 C26 C27 -1.5(4) . . . . ? C25 C26 C27 C28 1.9(4) . . . . ? C24 C23 C28 C27 -1.5(4) . . . . ? C22 C23 C28 C27 175.4(2) . . . . ? C26 C27 C28 C23 -0.4(4) . . . . ? N1 C29 C30 N2 -2.3(4) . . . . ? N2 C31 C32 N1 -1.9(4) . . . . ? C33A C31 C32 N1 -179.4(3) . . . . ? C35B C31 C32 N1 155.0(13) . . . . ? N2 C31 C32 C35A 178.1(4) . . . . ? C33A C31 C32 C35A 0.5(5) . . . . ? C35B C31 C32 C35A -25.1(14) . . . . ? N2 C31 C32 C33B 179.7(17) . . . . ? C33A C31 C32 C33B 2.2(18) . . . . ? C35B C31 C32 C33B -23(2) . . . . ? N2 C31 C33A C34A -95.7(4) . . . . ? C32 C31 C33A C34A 81.9(4) . . . . ? C35B C31 C33A C34A -163(3) . . . . ? N1 C32 C33B C34B 117(3) . . . . ? C31 C32 C33B C34B -65(4) . . . . ? C35A C32 C33B C34B 102(15) . . . . ? C31 C32 N1 C29 4.1(3) . . . . ? C35A C32 N1 C29 -175.8(4) . . . . ? C33B C32 N1 C29 -177.6(19) . . . . ? C31 C32 N1 Rh1 -167.25(18) . . . . ? C35A C32 N1 Rh1 12.8(4) . . . . ? C33B C32 N1 Rh1 11(2) . . . . ? C30 C29 N1 C32 -2.1(4) . . . . ? C30 C29 N1 Rh1 170.4(2) . . . . ? C32 C31 N2 C30 -2.5(4) . . . . ? C33A C31 N2 C30 175.1(3) . . . . ? C35B C31 N2 C30 -163.2(11) . . . . ? C32 C31 N2 Rh2 168.70(18) . . . . ? C33A C31 N2 Rh2 -13.7(4) . . . . ? C35B C31 N2 Rh2 8.0(11) . . . . ? C29 C30 N2 C31 4.5(4) . . . . ? C29 C30 N2 Rh2 -168.2(2) . . . . ? O2 C1 O1 Rh1 2.1(3) . . . . ? C2 C1 O1 Rh1 -177.06(16) . . . . ? O1 C1 O2 Rh1 -2.3(3) . . . 2_675 ? C2 C1 O2 Rh1 176.83(16) . . . 2_675 ? O4 C8 O3 Rh1 3.3(3) . . . 2_675 ? C9 C8 O3 Rh1 -175.63(15) . . . 2_675 ? O3 C8 O4 Rh1 -4.0(3) . . . . ? C9 C8 O4 Rh1 174.86(16) . . . . ? O6 C15 O5 Rh2 5.6(3) . . . . ? C16 C15 O5 Rh2 -172.30(16) . . . . ? O5 C15 O6 Rh2 -5.7(4) . . . 2_566 ? C16 C15 O6 Rh2 172.20(16) . . . 2_566 ? O8 C22 O7 Rh2 2.0(4) . . . 2_566 ? C23 C22 O7 Rh2 -178.76(16) . . . 2_566 ? O7 C22 O8 Rh2 -2.2(4) . . . . ? C23 C22 O8 Rh2 178.64(17) . . . . ? C8 O4 Rh1 O3 11.1(10) . . . 2_675 ? C8 O4 Rh1 O2 91.36(18) . . . 2_675 ? C8 O4 Rh1 O1 -84.47(18) . . . . ? C8 O4 Rh1 N1 179.55(18) . . . . ? C8 O4 Rh1 Rh1 2.40(17) . . . 2_675 ? C1 O1 Rh1 O3 -88.90(19) . . . 2_675 ? C1 O1 Rh1 O2 2.1(11) . . . 2_675 ? C1 O1 Rh1 O4 87.00(18) . . . . ? C1 O1 Rh1 N1 178.86(18) . . . . ? C1 O1 Rh1 Rh1 -0.75(18) . . . 2_675 ? C32 N1 Rh1 O3 -65.3(2) . . . 2_675 ? C29 N1 Rh1 O3 123.08(17) . . . 2_675 ? C32 N1 Rh1 O2 -154.1(2) . . . 2_675 ? C29 N1 Rh1 O2 34.28(17) . . . 2_675 ? C32 N1 Rh1 O4 115.5(2) . . . . ? C29 N1 Rh1 O4 -56.09(17) . . . . ? C32 N1 Rh1 O1 26.1(2) . . . . ? C29 N1 Rh1 O1 -145.48(17) . . . . ? C32 N1 Rh1 Rh1 -161.7(10) . . . 2_675 ? C29 N1 Rh1 Rh1 26.7(12) . . . 2_675 ? C15 O5 Rh2 O7 -91.02(18) . . . 2_566 ? C15 O5 Rh2 O6 -1.8(11) . . . 2_566 ? C15 O5 Rh2 O8 84.93(18) . . . . ? C15 O5 Rh2 N2 -179.34(19) . . . . ? C15 O5 Rh2 Rh2 -2.50(18) . . . 2_566 ? C22 O8 Rh2 O7 2.5(12) . . . 2_566 ? C22 O8 Rh2 O6 88.9(2) . . . 2_566 ? C22 O8 Rh2 O5 -87.1(2) . . . . ? C22 O8 Rh2 N2 -173.67(19) . . . . ? C22 O8 Rh2 Rh2 1.08(19) . . . 2_566 ? C31 N2 Rh2 O7 135.6(2) . . . 2_566 ? C30 N2 Rh2 O7 -52.85(18) . . . 2_566 ? C31 N2 Rh2 O6 47.9(2) . . . 2_566 ? C30 N2 Rh2 O6 -140.53(17) . . . 2_566 ? C31 N2 Rh2 O5 -132.3(2) . . . . ? C30 N2 Rh2 O5 39.29(18) . . . . ? C31 N2 Rh2 O8 -44.7(2) . . . . ? C30 N2 Rh2 O8 126.88(18) . . . . ? C31 N2 Rh2 Rh2 -164.1(4) . . . 2_566 ? C30 N2 Rh2 Rh2 7.5(6) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.042 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.097