Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2000 CCDC reference number 182/1852 #----------------------------------------------------------------------- # CIF data for Ms. No. B007347O # # "Supramolecular Structures Based on Dimetal Units: Simultaneous # Utilization of Equatorial and Axial Connections" # Authors: F. Albert Cotton, Chun Lin, Carlos A. Murillo # # Chem. Commun. #----------------------------------------------------------------------- data_cmpd_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Rh2(DAniF)2]2[O2CCH2CO2]2[NC5H4CHCHC5H4N]2(3CH2Cl2)(0.5Et2O)' _chemical_formula_sum 'C95 H95 Cl6 N12 O16.50 Rh4' _chemical_formula_weight 2293.17 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 56.521(4) _cell_length_b 19.016(2) _cell_length_c 19.564(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.053(2) _cell_angle_gamma 90.00 _cell_volume 20484(3) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4195 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 21.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9304 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43133 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_sigmaI/netI 0.1517 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 22.56 _reflns_number_total 13458 _reflns_number_gt 6882 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13458 _refine_ls_number_parameters 613 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1707 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2227 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _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 Rh1 Rh 0.127477(18) 0.40000(6) 0.25618(6) 0.0314(3) Uani 1 1 d . . . Rh2 Rh 0.167755(18) 0.41043(6) 0.22856(6) 0.0308(3) Uani 1 1 d . . . Rh3 Rh 0.085100(18) 0.17744(6) 0.06187(6) 0.0334(3) Uani 1 1 d . . . Rh4 Rh 0.119153(18) 0.14736(6) 0.01034(5) 0.0310(3) Uani 1 1 d . . . N1 N 0.14354(18) 0.4091(5) 0.3595(5) 0.027(2) Uiso 1 1 d . . . N2 N 0.18174(18) 0.4168(5) 0.3339(5) 0.028(3) Uiso 1 1 d . . . N3 N 0.12362(19) 0.5044(6) 0.2445(5) 0.036(3) Uiso 1 1 d . . . N4 N 0.16197(18) 0.5143(5) 0.2194(5) 0.031(3) Uiso 1 1 d . . . N5 N 0.06306(19) 0.1566(5) -0.0342(5) 0.033(3) Uiso 1 1 d . . . N6 N 0.09619(19) 0.1591(5) -0.0854(5) 0.035(3) Uiso 1 1 d . . . N7 N 0.08475(19) 0.0767(5) 0.0930(5) 0.034(3) Uiso 1 1 d . . . N8 N 0.10971(18) 0.0458(5) 0.0178(5) 0.030(3) Uiso 1 1 d . . . N301 N 0.09113(18) 0.3722(5) 0.2780(5) 0.033(3) Uiso 1 1 d . . . N302 N 0.20359(19) 0.4080(6) 0.1953(5) 0.037(3) Uiso 1 1 d . . . N303 N 0.05340(19) 0.2237(6) 0.1048(5) 0.037(3) Uiso 1 1 d . . . N304 N 0.15497(18) 0.1319(5) -0.0232(5) 0.031(3) Uiso 1 1 d . . . O1 O 0.0993(3) 0.3666(10) 0.5857(9) 0.142(6) Uiso 1 1 d . . . O2 O 0.2812(2) 0.4096(6) 0.4514(6) 0.076(3) Uiso 1 1 d . . . O3 O 0.0366(3) 0.6541(8) 0.2207(7) 0.104(5) Uiso 1 1 d . . . O4 O 0.22145(19) 0.6983(6) 0.1100(6) 0.065(3) Uiso 1 1 d . . . O6 O 0.1283(2) 0.1878(6) -0.3335(6) 0.080(4) Uiso 1 1 d . . . O7 O 0.0380(3) -0.0071(8) 0.3042(8) 0.112(5) Uiso 1 1 d . . . O8 O 0.15352(17) -0.1717(5) -0.1002(5) 0.053(3) Uiso 1 1 d . . . O201 O 0.11392(14) 0.3887(4) 0.1479(4) 0.029(2) Uiso 1 1 d . . . O202 O 0.15052(15) 0.3985(4) 0.1230(4) 0.032(2) Uiso 1 1 d . . . O203 O 0.13414(15) 0.2938(4) 0.2639(4) 0.034(2) Uiso 1 1 d . . . O204 O 0.16982(14) 0.3003(4) 0.2315(4) 0.030(2) Uiso 1 1 d . . . O205 O 0.11124(15) 0.1992(4) 0.1535(4) 0.032(2) Uiso 1 1 d . . . O206 O 0.14001(14) 0.1433(4) 0.1130(4) 0.0255(19) Uiso 1 1 d . . . O207 O 0.08975(16) 0.2789(4) 0.0304(4) 0.038(2) Uiso 1 1 d . . . O208 O 0.12705(15) 0.2546(4) 0.0139(4) 0.036(2) Uiso 1 1 d . . . C1 C 0.1674(2) 0.4136(7) 0.3781(7) 0.036(3) Uiso 1 1 d . . . H1A H 0.1746 0.4145 0.4263 0.043 Uiso 1 1 calc R . . C2 C 0.1413(2) 0.5423(8) 0.2273(7) 0.041(4) Uiso 1 1 d . . . H2A H 0.1390 0.5909 0.2204 0.049 Uiso 1 1 calc R . . C3 C 0.0729(3) 0.1578(7) -0.0878(8) 0.046(4) Uiso 1 1 d . . . H3A H 0.0623 0.1579 -0.1325 0.056 Uiso 1 1 calc R . . C4 C 0.0957(2) 0.0274(7) 0.0625(7) 0.036(3) Uiso 1 1 d . . . H4A H 0.0937 -0.0204 0.0722 0.043 Uiso 1 1 calc R . . C201 C 0.1283(2) 0.3884(7) 0.1057(7) 0.032(3) Uiso 1 1 d . . . C202 C 0.1172(2) 0.3729(6) 0.0312(6) 0.032(3) Uiso 1 1 d . . . H20A H 0.1286 0.3849 0.0020 0.039 Uiso 1 1 calc R . . H20B H 0.1025 0.4015 0.0156 0.039 Uiso 1 1 calc R . . C203 C 0.1107(2) 0.2966(7) 0.0227(7) 0.034(3) Uiso 1 1 d . . . C204 C 0.1324(2) 0.1761(7) 0.1587(6) 0.028(3) Uiso 1 1 d . . . C205 C 0.1502(2) 0.1893(6) 0.2271(6) 0.026(3) Uiso 1 1 d . . . H20C H 0.1662 0.1716 0.2245 0.032 Uiso 1 1 calc R . . H20D H 0.1450 0.1642 0.2649 0.032 Uiso 1 1 calc R . . C206 C 0.1517(2) 0.2669(7) 0.2430(7) 0.032(3) Uiso 1 1 d . . . C301 C 0.0828(2) 0.3075(7) 0.2576(7) 0.042(4) Uiso 1 1 d . . . H30A H 0.0908 0.2815 0.2287 0.051 Uiso 1 1 calc R . . C302 C 0.0632(3) 0.2777(8) 0.2770(7) 0.045(4) Uiso 1 1 d . . . H30B H 0.0588 0.2310 0.2645 0.054 Uiso 1 1 calc R . . C303 C 0.0501(3) 0.3169(8) 0.3152(8) 0.050(4) Uiso 1 1 d . . . C304 C 0.0580(2) 0.3848(7) 0.3341(7) 0.038(4) Uiso 1 1 d . . . H30C H 0.0496 0.4133 0.3601 0.045 Uiso 1 1 calc R . . C305 C 0.0780(2) 0.4093(7) 0.3147(7) 0.040(4) Uiso 1 1 d . . . H30D H 0.0830 0.4555 0.3278 0.048 Uiso 1 1 calc R . . C306 C 0.0276(3) 0.2843(8) 0.3310(8) 0.051(4) Uiso 1 1 d . . . H30E H 0.0250 0.2361 0.3215 0.061 Uiso 1 1 calc R . . C311 C 0.2077(2) 0.3576(7) 0.1519(7) 0.038(3) Uiso 1 1 d . . . H31A H 0.1955 0.3242 0.1361 0.046 Uiso 1 1 calc R . . C312 C 0.2291(3) 0.3521(8) 0.1292(8) 0.049(4) Uiso 1 1 d . . . H31B H 0.2311 0.3158 0.0985 0.059 Uiso 1 1 calc R . . C313 C 0.2473(2) 0.4004(7) 0.1520(7) 0.033(3) Uiso 1 1 d . . . C314 C 0.2434(2) 0.4521(7) 0.1974(7) 0.038(4) Uiso 1 1 d . . . H31C H 0.2557 0.4852 0.2141 0.046 Uiso 1 1 calc R . . C315 C 0.2221(2) 0.4562(7) 0.2185(7) 0.037(3) Uiso 1 1 d . . . H31D H 0.2199 0.4923 0.2493 0.044 Uiso 1 1 calc R . . C316 C 0.2708(3) 0.4001(8) 0.1312(7) 0.049(4) Uiso 1 1 d . . . H31E H 0.2829 0.4294 0.1572 0.058 Uiso 1 1 calc R . . C331 C 0.0509(3) 0.2929(8) 0.1035(7) 0.047(4) Uiso 1 1 d . . . H33A H 0.0638 0.3209 0.0960 0.057 Uiso 1 1 calc R . . C332 C 0.0294(3) 0.3263(8) 0.1129(7) 0.051(4) Uiso 1 1 d . . . H33B H 0.0277 0.3755 0.1096 0.061 Uiso 1 1 calc R . . C333 C 0.0102(3) 0.2835(8) 0.1275(8) 0.053(4) Uiso 1 1 d . . . C334 C 0.0138(3) 0.2132(8) 0.1314(7) 0.047(4) Uiso 1 1 d . . . H33C H 0.0021 0.1837 0.1435 0.057 Uiso 1 1 calc R . . C335 C 0.0350(3) 0.1843(8) 0.1175(7) 0.052(4) Uiso 1 1 d . . . H33D H 0.0365 0.1351 0.1171 0.062 Uiso 1 1 calc R . . C336 C -0.0113(3) 0.3190(9) 0.1425(8) 0.062(5) Uiso 1 1 d . . . H33E H -0.0136 0.3674 0.1331 0.075 Uiso 1 1 calc R . . C341 C 0.1745(3) 0.1617(7) 0.0154(8) 0.044(4) Uiso 1 1 d . . . H34A H 0.1730 0.1833 0.0574 0.053 Uiso 1 1 calc R . . C342 C 0.1968(2) 0.1639(7) -0.0008(7) 0.040(4) Uiso 1 1 d . . . H34B H 0.2100 0.1860 0.0297 0.048 Uiso 1 1 calc R . . C343 C 0.1998(2) 0.1341(7) -0.0606(7) 0.040(4) Uiso 1 1 d . . . C344 C 0.1797(2) 0.1018(7) -0.1033(7) 0.042(4) Uiso 1 1 d . . . H34C H 0.1811 0.0805 -0.1456 0.051 Uiso 1 1 calc R . . C345 C 0.1579(3) 0.1011(7) -0.0833(7) 0.043(4) Uiso 1 1 d . . . H34D H 0.1445 0.0784 -0.1123 0.052 Uiso 1 1 calc R . . C346 C 0.2234(3) 0.1366(7) -0.0802(7) 0.043(4) Uiso 1 1 d . . . H34E H 0.2352 0.1668 -0.0544 0.051 Uiso 1 1 calc R . . C11 C 0.1316(2) 0.3975(7) 0.4147(7) 0.033(3) Uiso 1 1 d . . . C12 C 0.1216(3) 0.3308(8) 0.4205(8) 0.050(4) Uiso 1 1 d . . . H12A H 0.1224 0.2958 0.3872 0.060 Uiso 1 1 calc R . . C13 C 0.1104(3) 0.3165(9) 0.4754(8) 0.064(5) Uiso 1 1 d . . . H13A H 0.1037 0.2721 0.4807 0.076 Uiso 1 1 calc R . . C14 C 0.1097(3) 0.3693(11) 0.5208(10) 0.078(6) Uiso 1 1 d . . . C15 C 0.1186(3) 0.4336(10) 0.5190(10) 0.080(6) Uiso 1 1 d . . . H15A H 0.1175 0.4678 0.5528 0.096 Uiso 1 1 calc R . . C16 C 0.1299(3) 0.4473(9) 0.4632(8) 0.058(4) Uiso 1 1 d . . . H16A H 0.1365 0.4921 0.4593 0.070 Uiso 1 1 calc R . . C17 C 0.0873(5) 0.3077(15) 0.5845(14) 0.161(11) Uiso 1 1 d . . . H17A H 0.0805 0.3049 0.6256 0.241 Uiso 1 1 calc R . . H17B H 0.0983 0.2684 0.5845 0.241 Uiso 1 1 calc R . . H17C H 0.0744 0.3059 0.5425 0.241 Uiso 1 1 calc R . . C21 C 0.2070(2) 0.4176(7) 0.3638(7) 0.035(3) Uiso 1 1 d . . . C22 C 0.2179(3) 0.4731(8) 0.4049(7) 0.046(4) Uiso 1 1 d . . . H22A H 0.2084 0.5117 0.4125 0.056 Uiso 1 1 calc R . . C23 C 0.2426(3) 0.4731(9) 0.4349(8) 0.059(5) Uiso 1 1 d . . . H23A H 0.2497 0.5112 0.4628 0.071 Uiso 1 1 calc R . . C24 C 0.2568(3) 0.4163(8) 0.4236(8) 0.057(4) Uiso 1 1 d . . . C25 C 0.2464(3) 0.3599(8) 0.3836(7) 0.044(4) Uiso 1 1 d . . . H25A H 0.2558 0.3213 0.3760 0.052 Uiso 1 1 calc R . . C26 C 0.2219(2) 0.3614(7) 0.3550(7) 0.040(4) Uiso 1 1 d . . . H26A H 0.2148 0.3226 0.3282 0.048 Uiso 1 1 calc R . . C27 C 0.2932(4) 0.4716(11) 0.4892(11) 0.102(7) Uiso 1 1 d . . . H27A H 0.3103 0.4618 0.5068 0.153 Uiso 1 1 calc R . . H27B H 0.2858 0.4823 0.5282 0.153 Uiso 1 1 calc R . . H27C H 0.2913 0.5115 0.4576 0.153 Uiso 1 1 calc R . . C31 C 0.1013(3) 0.5417(7) 0.2432(7) 0.042(4) Uiso 1 1 d . . . C32 C 0.1008(3) 0.5995(8) 0.2841(8) 0.052(4) Uiso 1 1 d . . . H32A H 0.1150 0.6134 0.3163 0.062 Uiso 1 1 calc R . . C33 C 0.0795(3) 0.6387(9) 0.2791(9) 0.065(5) Uiso 1 1 d . . . H33F H 0.0790 0.6787 0.3071 0.078 Uiso 1 1 calc R . . C34 C 0.0594(3) 0.6161(10) 0.2317(9) 0.070(5) Uiso 1 1 d . . . C35 C 0.0591(3) 0.5568(9) 0.1928(9) 0.069(5) Uiso 1 1 d . . . H35A H 0.0446 0.5408 0.1634 0.083 Uiso 1 1 calc R . . C36 C 0.0803(3) 0.5208(8) 0.1973(8) 0.047(4) Uiso 1 1 d . . . H36A H 0.0805 0.4812 0.1686 0.057 Uiso 1 1 calc R . . C37 C 0.0367(5) 0.7217(14) 0.2556(13) 0.142(10) Uiso 1 1 d . . . H37A H 0.0205 0.7417 0.2441 0.213 Uiso 1 1 calc R . . H37B H 0.0479 0.7533 0.2401 0.213 Uiso 1 1 calc R . . H37C H 0.0418 0.7152 0.3060 0.213 Uiso 1 1 calc R . . C41 C 0.1773(2) 0.5624(7) 0.1906(7) 0.039(4) Uiso 1 1 d . . . C42 C 0.1809(2) 0.5507(7) 0.1257(7) 0.037(3) Uiso 1 1 d . . . H42A H 0.1730 0.5128 0.0991 0.044 Uiso 1 1 calc R . . C43 C 0.1962(2) 0.5945(7) 0.0977(7) 0.044(4) Uiso 1 1 d . . . H43A H 0.1994 0.5843 0.0537 0.053 Uiso 1 1 calc R . . C44 C 0.2063(2) 0.6509(7) 0.1338(7) 0.040(4) Uiso 1 1 d . . . C45 C 0.2029(3) 0.6632(8) 0.1991(8) 0.057(4) Uiso 1 1 d . . . H45A H 0.2104 0.7022 0.2245 0.068 Uiso 1 1 calc R . . C46 C 0.1884(2) 0.6187(7) 0.2293(8) 0.045(4) Uiso 1 1 d . . . H46A H 0.1862 0.6270 0.2749 0.054 Uiso 1 1 calc R . . C47 C 0.2252(3) 0.6858(9) 0.0428(9) 0.071(5) Uiso 1 1 d . . . H47A H 0.2360 0.7216 0.0314 0.106 Uiso 1 1 calc R . . H47B H 0.2098 0.6874 0.0088 0.106 Uiso 1 1 calc R . . H47C H 0.2326 0.6399 0.0415 0.106 Uiso 1 1 calc R . . C51 C 0.0374(3) 0.1562(8) -0.0439(7) 0.043(4) Uiso 1 1 d . A . C52 C 0.0243(3) 0.2147(10) -0.0653(9) 0.072(5) Uiso 1 1 d . . . H52A H 0.0321 0.2550 -0.0776 0.087 Uiso 1 1 calc R . . C53 C -0.0010(4) 0.2160(11) -0.0695(10) 0.093(6) Uiso 1 1 d . A . H53A H -0.0104 0.2560 -0.0859 0.111 Uiso 1 1 calc R . . C54 C -0.0116(5) 0.1553(13) -0.0483(12) 0.111(8) Uiso 1 1 d . . . C55 C 0.0011(4) 0.0969(13) -0.0292(12) 0.111(8) Uiso 1 1 d . A . H55A H -0.0064 0.0562 -0.0172 0.133 Uiso 1 1 calc R . . C56 C 0.0265(3) 0.0971(10) -0.0274(9) 0.073(5) Uiso 1 1 d . . . H56A H 0.0356 0.0560 -0.0146 0.087 Uiso 1 1 calc R A . O5 O -0.0368(7) 0.146(2) -0.019(3) 0.125(8) Uiso 0.47(2) 1 d PD A 1 C57 C -0.0458(13) 0.128(4) 0.041(3) 0.20(2) Uiso 0.47(2) 1 d PD A 1 H57A H -0.0634 0.1298 0.0289 0.305 Uiso 0.47(2) 1 calc PR A 1 H57B H -0.0396 0.1619 0.0780 0.305 Uiso 0.47(2) 1 calc PR A 1 H57C H -0.0404 0.0814 0.0565 0.305 Uiso 0.47(2) 1 calc PR A 1 O5' O -0.0376(6) 0.1538(17) -0.073(2) 0.125(8) Uiso 0.53(2) 1 d PD A 2 C57' C -0.0504(11) 0.205(3) -0.045(3) 0.20(2) Uiso 0.53(2) 1 d PD A 2 H57D H -0.0676 0.2000 -0.0646 0.305 Uiso 0.53(2) 1 calc PR A 2 H57E H -0.0451 0.2513 -0.0554 0.305 Uiso 0.53(2) 1 calc PR A 2 H57F H -0.0473 0.1992 0.0060 0.305 Uiso 0.53(2) 1 calc PR A 2 C61 C 0.1039(2) 0.1682(7) -0.1497(7) 0.039(4) Uiso 1 1 d . . . C62 C 0.0950(3) 0.1274(8) -0.2075(8) 0.050(4) Uiso 1 1 d . . . H62A H 0.0833 0.0927 -0.2054 0.060 Uiso 1 1 calc R . . C63 C 0.1030(3) 0.1364(8) -0.2696(8) 0.056(4) Uiso 1 1 d . . . H63A H 0.0962 0.1102 -0.3100 0.067 Uiso 1 1 calc R . . C64 C 0.1209(3) 0.1842(9) -0.2701(8) 0.057(4) Uiso 1 1 d . . . C65 C 0.1301(3) 0.2268(8) -0.2138(7) 0.047(4) Uiso 1 1 d . . . H65A H 0.1419 0.2609 -0.2156 0.056 Uiso 1 1 calc R . . C66 C 0.1211(2) 0.2176(7) -0.1546(7) 0.042(4) Uiso 1 1 d . . . H66A H 0.1272 0.2464 -0.1155 0.051 Uiso 1 1 calc R . . C67 C 0.1476(4) 0.2348(11) -0.3360(11) 0.099(7) Uiso 1 1 d . . . H67A H 0.1512 0.2329 -0.3821 0.148 Uiso 1 1 calc R . . H67B H 0.1619 0.2213 -0.3008 0.148 Uiso 1 1 calc R . . H67C H 0.1428 0.2822 -0.3266 0.148 Uiso 1 1 calc R . . C71 C 0.0732(2) 0.0515(7) 0.1472(7) 0.039(4) Uiso 1 1 d . . . C72 C 0.0780(3) 0.0865(8) 0.2098(8) 0.052(4) Uiso 1 1 d . B . H72A H 0.0895 0.1230 0.2169 0.063 Uiso 1 1 calc R . . C73 C 0.0664(3) 0.0699(9) 0.2634(10) 0.072(5) Uiso 1 1 d . . . H73A H 0.0688 0.0952 0.3057 0.086 Uiso 1 1 calc R B . C74 C 0.0514(3) 0.0144(10) 0.2490(10) 0.075(5) Uiso 1 1 d . B . C75 C 0.0458(3) -0.0219(9) 0.1893(9) 0.068(5) Uiso 1 1 d . . . H75A H 0.0345 -0.0592 0.1838 0.082 Uiso 1 1 calc R B . C76 C 0.0569(3) -0.0035(8) 0.1355(9) 0.057(4) Uiso 1 1 d . B . H76A H 0.0534 -0.0277 0.0924 0.069 Uiso 1 1 calc R . . C77 C 0.0393(7) 0.044(2) 0.367(2) 0.128(12) Uiso 0.61(2) 1 d P B 1 H77A H 0.0301 0.0251 0.3985 0.192 Uiso 0.61(2) 1 calc PR B 1 H77B H 0.0326 0.0894 0.3490 0.192 Uiso 0.61(2) 1 calc PR B 1 H77C H 0.0562 0.0502 0.3912 0.192 Uiso 0.61(2) 1 calc PR B 1 C77' C 0.0193(10) -0.074(3) 0.279(3) 0.128(12) Uiso 0.39(2) 1 d P B 2 H77D H 0.0111 -0.0859 0.3164 0.192 Uiso 0.39(2) 1 calc PR B 2 H77E H 0.0285 -0.1147 0.2695 0.192 Uiso 0.39(2) 1 calc PR B 2 H77F H 0.0073 -0.0616 0.2372 0.192 Uiso 0.39(2) 1 calc PR B 2 C81 C 0.1204(2) -0.0110(7) -0.0101(7) 0.034(3) Uiso 1 1 d . . . C82 C 0.1361(3) -0.0563(8) 0.0303(8) 0.053(4) Uiso 1 1 d . . . H82A H 0.1395 -0.0508 0.0793 0.064 Uiso 1 1 calc R . . C83 C 0.1477(3) -0.1119(8) 0.0016(8) 0.049(4) Uiso 1 1 d . . . H83A H 0.1586 -0.1423 0.0314 0.059 Uiso 1 1 calc R . . C84 C 0.1432(2) -0.1204(7) -0.0670(7) 0.039(4) Uiso 1 1 d . . . C85 C 0.1271(3) -0.0763(8) -0.1101(8) 0.055(4) Uiso 1 1 d . . . H85A H 0.1237 -0.0830 -0.1590 0.066 Uiso 1 1 calc R . . C86 C 0.1158(3) -0.0222(7) -0.0823(7) 0.044(4) Uiso 1 1 d . . . H86A H 0.1050 0.0075 -0.1126 0.053 Uiso 1 1 calc R . . C87 C 0.1708(3) -0.2177(9) -0.0589(9) 0.069(5) Uiso 1 1 d . . . H87A H 0.1765 -0.2509 -0.0893 0.103 Uiso 1 1 calc R . . H87B H 0.1632 -0.2432 -0.0264 0.103 Uiso 1 1 calc R . . H87C H 0.1844 -0.1906 -0.0328 0.103 Uiso 1 1 calc R . . C1S C 0.1811(4) 0.6591(12) 0.4597(12) 0.107(7) Uiso 1 1 d . . . Cl1 Cl 0.20986(10) 0.6715(3) 0.4375(3) 0.107(2) Uani 1 1 d . . . Cl2 Cl 0.16322(8) 0.6034(3) 0.4012(3) 0.0816(15) Uani 1 1 d . . . C2S C 0.3267(4) 0.5190(11) 0.3052(11) 0.094(7) Uiso 1 1 d . . . Cl3 Cl 0.30969(12) 0.4433(4) 0.3172(4) 0.144(3) Uani 1 1 d . . . Cl4 Cl 0.35096(14) 0.4955(3) 0.2689(3) 0.128(2) Uani 1 1 d . . . C3S C 0.2266(6) 0.1834(16) 0.2587(16) 0.060(7) Uiso 0.48(2) 1 d PD C 1 Cl5 Cl 0.2168(5) 0.1528(16) 0.3219(12) 0.187(5) Uiso 0.48(2) 1 d PD C 1 Cl6 Cl 0.2322(7) 0.141(2) 0.1919(14) 0.238(7) Uiso 0.48(2) 1 d PD C 1 C3S' C 0.2224(6) 0.1120(16) 0.2702(15) 0.060(7) Uiso 0.52(2) 1 d PD C 2 Cl5' Cl 0.2149(4) 0.1264(13) 0.3409(12) 0.187(5) Uiso 0.52(2) 1 d PD C 2 Cl6' Cl 0.2227(6) 0.1398(19) 0.1948(13) 0.238(7) Uiso 0.52(2) 1 d PD C 2 O1S O -0.0220(6) 0.4923(16) -0.4000(17) 0.117(10) Uiso 0.50 1 d P . . C4S C -0.0138(8) 0.462(2) -0.332(3) 0.109(15) Uiso 0.50 1 d P D . C5S C 0.0001(11) 0.509(2) -0.271(2) 0.108(16) Uiso 0.50 1 d P . . C6S C -0.0458(9) 0.443(3) -0.441(3) 0.047(12) Uiso 0.296(16) 1 d PD D 1 C7S C -0.0530(7) 0.478(2) -0.498(2) 0.024(8) Uiso 0.296(16) 1 d PD D 1 C6S' C -0.0374(16) 0.471(4) -0.457(4) 0.047(12) Uiso 0.204(16) 1 d PD D 2 C7S' C -0.0362(10) 0.519(3) -0.500(3) 0.024(8) Uiso 0.204(16) 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0200(6) 0.0399(7) 0.0392(7) -0.0065(6) 0.0174(5) -0.0046(5) Rh2 0.0196(6) 0.0378(7) 0.0393(7) -0.0051(5) 0.0156(5) -0.0048(5) Rh3 0.0158(6) 0.0481(8) 0.0384(7) -0.0088(6) 0.0108(5) 0.0006(5) Rh4 0.0178(6) 0.0450(7) 0.0327(6) -0.0058(5) 0.0110(5) 0.0017(5) Cl1 0.077(4) 0.093(4) 0.154(6) -0.047(4) 0.033(4) -0.016(3) Cl2 0.061(3) 0.104(4) 0.082(3) -0.019(3) 0.023(3) -0.006(3) Cl3 0.109(6) 0.148(6) 0.146(6) 0.027(5) -0.032(4) -0.042(4) Cl4 0.191(7) 0.110(5) 0.085(4) -0.012(4) 0.034(4) -0.028(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 Rh2 2.4637(13) . Y Rh1 N3 2.004(11) . Y Rh1 N1 2.027(10) . Y Rh1 O203 2.054(8) . Y Rh1 O201 2.095(8) . Y Rh1 N301 2.253(10) . Y Rh2 N4 2.004(10) . Y Rh2 N2 2.037(10) . Y Rh2 O202 2.088(8) . Y Rh2 O204 2.098(8) . Y Rh2 N302 2.264(10) . Y Rh3 Rh4 2.4340(13) . Y Rh3 N7 2.012(10) . Y Rh3 N5 2.046(10) . Y Rh3 O207 2.060(9) . Y Rh3 O205 2.091(8) . Y Rh3 N303 2.317(10) . Y Rh4 N8 2.018(10) . Y Rh4 N6 2.036(11) . Y Rh4 O208 2.086(9) . Y Rh4 O206 2.088(8) . Y Rh4 N304 2.284(10) . Y N1 C1 1.316(14) . ? N1 C11 1.416(14) . ? N2 C1 1.315(14) . ? N2 C21 1.415(15) . ? N3 C2 1.337(16) . ? N3 C31 1.441(16) . ? N4 C2 1.322(15) . ? N4 C41 1.458(16) . ? N5 C3 1.293(15) . ? N5 C51 1.417(16) . ? N6 C3 1.308(15) . ? N6 C61 1.431(15) . ? N7 C4 1.337(15) . ? N7 C71 1.446(15) . ? N8 C4 1.350(15) . ? N8 C81 1.406(15) . ? N301 C305 1.345(15) . ? N301 C301 1.345(16) . ? N302 C311 1.335(15) . ? N302 C315 1.389(16) . ? N303 C331 1.324(16) . ? N303 C335 1.349(17) . ? N304 C341 1.317(16) . ? N304 C345 1.357(16) . ? O1 C17 1.30(3) . ? O1 C14 1.52(2) . ? O2 C24 1.369(18) . ? O2 C27 1.47(2) . ? O3 C34 1.45(2) . ? O3 C37 1.46(2) . ? O4 C44 1.393(16) . ? O4 C47 1.400(17) . ? O6 C64 1.398(17) . ? O6 C67 1.42(2) . ? O7 C74 1.51(2) . ? O7 C77 1.55(4) . ? O7 C77' 1.66(6) . ? O8 C84 1.373(15) . ? O8 C87 1.419(17) . ? O201 C201 1.282(14) . ? O202 C201 1.241(13) . ? O203 C206 1.266(14) . ? O204 C206 1.266(14) . ? O205 C204 1.257(13) . ? O206 C204 1.244(13) . ? O207 C203 1.272(14) . ? O208 C203 1.261(14) . ? C201 C202 1.481(17) . ? C202 C203 1.496(17) . ? C204 C205 1.502(16) . ? C205 C206 1.505(16) . ? C301 C302 1.372(18) . ? C302 C303 1.385(18) . ? C303 C304 1.389(18) . ? C303 C306 1.505(19) . ? C304 C305 1.352(17) . ? C306 C336 1.331(19) 2 ? C311 C312 1.380(18) . ? C312 C313 1.378(18) . ? C313 C314 1.375(17) . ? C313 C316 1.472(18) . ? C314 C315 1.356(17) . ? C316 C346 1.321(18) 7 ? C331 C332 1.422(19) . ? C332 C333 1.436(19) . ? C333 C334 1.352(19) . ? C333 C336 1.48(2) . ? C334 C335 1.398(19) . ? C336 C306 1.330(19) 2 ? C341 C342 1.369(18) . ? C342 C343 1.344(17) . ? C343 C344 1.391(18) . ? C343 C346 1.469(18) . ? C344 C345 1.376(18) . ? C346 C316 1.321(18) 7 ? C11 C16 1.358(18) . ? C11 C12 1.403(18) . ? C12 C13 1.390(19) . ? C13 C14 1.35(2) . ? C14 C15 1.33(2) . ? C15 C16 1.41(2) . ? C21 C22 1.386(18) . ? C21 C26 1.396(17) . ? C22 C23 1.385(19) . ? C23 C24 1.39(2) . ? C24 C25 1.379(19) . ? C25 C26 1.369(17) . ? C31 C32 1.365(18) . ? C31 C36 1.376(19) . ? C32 C33 1.40(2) . ? C33 C34 1.36(2) . ? C34 C35 1.36(2) . ? C35 C36 1.36(2) . ? C41 C42 1.348(17) . ? C41 C46 1.377(18) . ? C42 C43 1.400(18) . ? C43 C44 1.339(18) . ? C44 C45 1.354(18) . ? C45 C46 1.400(19) . ? C51 C52 1.35(2) . ? C51 C56 1.36(2) . ? C52 C53 1.41(2) . ? C53 C54 1.41(3) . ? C54 C55 1.33(3) . ? C54 O5' 1.44(3) . ? C54 O5 1.66(5) . ? C55 C56 1.42(3) . ? O5 C57 1.42(5) . ? O5' C57' 1.39(5) . ? C61 C62 1.370(18) . ? C61 C66 1.373(18) . ? C62 C63 1.400(19) . ? C63 C64 1.36(2) . ? C64 C65 1.37(2) . ? C65 C66 1.376(17) . ? C71 C72 1.366(18) . ? C71 C76 1.379(19) . ? C72 C73 1.39(2) . ? C73 C74 1.34(2) . ? C74 C75 1.33(2) . ? C75 C76 1.39(2) . ? C81 C82 1.357(18) . ? C81 C86 1.394(18) . ? C82 C83 1.424(19) . ? C83 C84 1.319(18) . ? C84 C85 1.377(19) . ? C85 C86 1.384(19) . ? C1S Cl2 1.71(2) . ? C1S Cl1 1.79(2) . ? C2S Cl4 1.74(2) . ? C2S Cl3 1.78(2) . ? C3S Cl5 1.57(3) . ? C3S Cl6 1.62(3) . ? C3S' Cl6' 1.57(3) . ? C3S' Cl5' 1.56(3) . ? O1S C6S' 1.31(8) . ? O1S C4S 1.43(5) . ? O1S C6S 1.69(6) . ? C4S C5S 1.56(6) . ? C6S C7S 1.26(5) . ? C6S' C7S' 1.26(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh1 N1 92.4(4) . . Y N3 Rh1 O203 174.7(4) . . Y N1 Rh1 O203 88.7(4) . . Y N3 Rh1 O201 88.9(4) . . Y N1 Rh1 O201 174.9(3) . . Y O203 Rh1 O201 89.6(3) . . Y N3 Rh1 N301 100.0(4) . . Y N1 Rh1 N301 93.0(4) . . Y O203 Rh1 N301 85.1(3) . . Y O201 Rh1 N301 91.5(3) . . Y N3 Rh1 Rh2 88.7(3) . . Y N1 Rh1 Rh2 89.1(3) . . Y O203 Rh1 Rh2 86.1(2) . . Y O201 Rh1 Rh2 86.1(2) . . Y N301 Rh1 Rh2 170.9(3) . . Y N4 Rh2 N2 92.8(4) . . Y N4 Rh2 O202 89.3(4) . . Y N2 Rh2 O202 174.3(4) . . Y N4 Rh2 O204 173.6(4) . . Y N2 Rh2 O204 91.5(4) . . Y O202 Rh2 O204 85.9(3) . . Y N4 Rh2 N302 97.6(4) . . Y N2 Rh2 N302 97.1(4) . . Y O202 Rh2 N302 87.8(3) . . Y O204 Rh2 N302 86.6(3) . . Y N4 Rh2 Rh1 87.6(3) . . Y N2 Rh2 Rh1 87.1(3) . . Y O202 Rh2 Rh1 87.7(2) . . Y O204 Rh2 Rh1 87.8(2) . . Y N302 Rh2 Rh1 173.0(3) . . Y N7 Rh3 N5 92.8(4) . . Y N7 Rh3 O207 173.2(4) . . Y N5 Rh3 O207 89.9(4) . . Y N7 Rh3 O205 89.0(4) . . Y N5 Rh3 O205 172.7(4) . . Y O207 Rh3 O205 87.6(3) . . Y N7 Rh3 N303 101.0(4) . . Y N5 Rh3 N303 92.7(4) . . Y O207 Rh3 N303 85.1(4) . . Y O205 Rh3 N303 93.9(3) . . Y N7 Rh3 Rh4 88.0(3) . . Y N5 Rh3 Rh4 87.0(3) . . Y O207 Rh3 Rh4 86.0(2) . . Y O205 Rh3 Rh4 86.0(2) . . Y N303 Rh3 Rh4 171.1(3) . . Y N8 Rh4 N6 92.7(4) . . Y N8 Rh4 O208 172.6(4) . . Y N6 Rh4 O208 90.6(4) . . Y N8 Rh4 O206 89.8(4) . . Y N6 Rh4 O206 173.3(4) . . Y O208 Rh4 O206 86.2(3) . . Y N8 Rh4 N304 99.4(4) . . Y N6 Rh4 N304 99.9(4) . . Y O208 Rh4 N304 86.5(3) . . Y O206 Rh4 N304 85.8(3) . . Y N8 Rh4 Rh3 87.0(3) . . Y N6 Rh4 Rh3 87.5(3) . . Y O208 Rh4 Rh3 86.5(2) . . Y O206 Rh4 Rh3 86.4(2) . . Y N304 Rh4 Rh3 169.9(3) . . Y C1 N1 C11 115.8(10) . . ? C1 N1 Rh1 118.8(8) . . ? C11 N1 Rh1 124.3(8) . . ? C1 N2 C21 116.3(11) . . ? C1 N2 Rh2 120.4(9) . . ? C21 N2 Rh2 122.9(7) . . ? C2 N3 C31 115.5(11) . . ? C2 N3 Rh1 119.6(9) . . ? C31 N3 Rh1 124.2(9) . . ? C2 N4 C41 114.2(11) . . ? C2 N4 Rh2 121.1(9) . . ? C41 N4 Rh2 123.6(8) . . ? C3 N5 C51 120.3(12) . . ? C3 N5 Rh3 117.2(10) . . ? C51 N5 Rh3 121.0(8) . . ? C3 N6 C61 118.3(12) . . ? C3 N6 Rh4 117.3(9) . . ? C61 N6 Rh4 124.4(9) . . ? C4 N7 C71 115.3(11) . . ? C4 N7 Rh3 119.7(9) . . ? C71 N7 Rh3 125.0(8) . . ? C4 N8 C81 114.7(11) . . ? C4 N8 Rh4 119.8(8) . . ? C81 N8 Rh4 124.3(8) . . ? C305 N301 C301 116.2(11) . . ? C305 N301 Rh1 128.0(9) . . ? C301 N301 Rh1 115.5(8) . . ? C311 N302 C315 117.0(11) . . ? C311 N302 Rh2 119.6(9) . . ? C315 N302 Rh2 123.4(9) . . ? C331 N303 C335 118.3(12) . . ? C331 N303 Rh3 117.2(9) . . ? C335 N303 Rh3 123.2(10) . . ? C341 N304 C345 115.7(11) . . ? C341 N304 Rh4 117.6(9) . . ? C345 N304 Rh4 126.4(9) . . ? C17 O1 C14 108(2) . . ? C24 O2 C27 115.6(14) . . ? C34 O3 C37 117.5(16) . . ? C44 O4 C47 116.2(12) . . ? C64 O6 C67 116.6(14) . . ? C74 O7 C77 116.7(19) . . ? C74 O7 C77' 113(2) . . ? C77 O7 C77' 129(3) . . ? C84 O8 C87 118.7(12) . . ? C201 O201 Rh1 120.8(8) . . ? C201 O202 Rh2 120.3(7) . . ? C206 O203 Rh1 121.2(8) . . ? C206 O204 Rh2 117.6(8) . . ? C204 O205 Rh3 118.5(8) . . ? C204 O206 Rh4 117.5(8) . . ? C203 O207 Rh3 117.9(8) . . ? C203 O208 Rh4 117.7(8) . . ? N2 C1 N1 124.5(12) . . ? N4 C2 N3 122.9(13) . . ? N5 C3 N6 125.8(14) . . ? N7 C4 N8 120.4(12) . . ? O202 C201 O201 125.0(12) . . ? O202 C201 C202 118.6(11) . . ? O201 C201 C202 116.4(12) . . ? C201 C202 C203 109.9(10) . . ? O208 C203 O207 125.3(12) . . ? O208 C203 C202 117.5(12) . . ? O207 C203 C202 117.0(11) . . ? O206 C204 O205 126.4(12) . . ? O206 C204 C205 117.1(11) . . ? O205 C204 C205 116.5(11) . . ? C204 C205 C206 110.1(10) . . ? O204 C206 O203 125.5(12) . . ? O204 C206 C205 117.8(11) . . ? O203 C206 C205 116.7(11) . . ? N301 C301 C302 123.1(13) . . ? C301 C302 C303 119.5(14) . . ? C302 C303 C304 117.6(14) . . ? C302 C303 C306 117.9(14) . . ? C304 C303 C306 124.4(13) . . ? C305 C304 C303 119.0(13) . . ? N301 C305 C304 124.5(13) . . ? C336 C306 C303 124.4(15) 2 . ? N302 C311 C312 123.4(13) . . ? C313 C312 C311 119.3(14) . . ? C314 C313 C312 117.8(13) . . ? C314 C313 C316 117.9(12) . . ? C312 C313 C316 124.3(13) . . ? C315 C314 C313 121.4(13) . . ? C314 C315 N302 121.1(13) . . ? C346 C316 C313 127.4(14) 7 . ? N303 C331 C332 122.1(14) . . ? C331 C332 C333 118.7(15) . . ? C334 C333 C332 117.4(14) . . ? C334 C333 C336 124.2(14) . . ? C332 C333 C336 118.3(14) . . ? C333 C334 C335 120.2(14) . . ? N303 C335 C334 123.1(15) . . ? C306 C336 C333 121.6(16) 2 . ? N304 C341 C342 125.3(14) . . ? C343 C342 C341 119.3(14) . . ? C342 C343 C344 117.7(13) . . ? C342 C343 C346 120.8(13) . . ? C344 C343 C346 121.5(13) . . ? C345 C344 C343 119.8(14) . . ? N304 C345 C344 122.2(13) . . ? C316 C346 C343 125.3(14) 7 . ? C16 C11 C12 118.8(13) . . ? C16 C11 N1 123.0(13) . . ? C12 C11 N1 118.2(12) . . ? C13 C12 C11 120.0(14) . . ? C14 C13 C12 116.7(17) . . ? C15 C14 C13 127.1(19) . . ? C15 C14 O1 106.0(18) . . ? C13 C14 O1 126.9(18) . . ? C14 C15 C16 115.6(18) . . ? C11 C16 C15 121.8(16) . . ? C22 C21 C26 116.9(13) . . ? C22 C21 N2 121.6(12) . . ? C26 C21 N2 121.5(12) . . ? C21 C22 C23 121.4(14) . . ? C22 C23 C24 119.6(16) . . ? O2 C24 C25 114.6(14) . . ? O2 C24 C23 125.0(15) . . ? C25 C24 C23 120.4(16) . . ? C26 C25 C24 118.6(14) . . ? C25 C26 C21 123.2(14) . . ? C32 C31 C36 119.0(14) . . ? C32 C31 N3 121.4(13) . . ? C36 C31 N3 119.5(13) . . ? C31 C32 C33 121.3(15) . . ? C34 C33 C32 116.8(17) . . ? C35 C34 C33 123.1(18) . . ? C35 C34 O3 115.7(17) . . ? C33 C34 O3 121.3(17) . . ? C34 C35 C36 118.8(17) . . ? C35 C36 C31 120.9(16) . . ? C42 C41 C46 120.0(13) . . ? C42 C41 N4 119.3(12) . . ? C46 C41 N4 120.7(12) . . ? C41 C42 C43 120.6(13) . . ? C44 C43 C42 119.8(13) . . ? C43 C44 C45 120.1(14) . . ? C43 C44 O4 124.2(13) . . ? C45 C44 O4 115.6(13) . . ? C44 C45 C46 121.1(15) . . ? C41 C46 C45 118.3(14) . . ? C52 C51 C56 120.4(16) . . ? C52 C51 N5 120.7(14) . . ? C56 C51 N5 118.8(14) . . ? C51 C52 C53 120.7(18) . . ? C54 C53 C52 117(2) . . ? C55 C54 C53 122(3) . . ? C55 C54 O5' 122(3) . . ? C53 C54 O5' 113(3) . . ? C55 C54 O5 105(2) . . ? C53 C54 O5 130(2) . . ? O5' C54 O5 38.6(17) . . ? C54 C55 C56 119(2) . . ? C51 C56 C55 120.5(19) . . ? C57 O5 C54 143(5) . . ? C57' O5' C54 116(4) . . ? C62 C61 C66 117.6(13) . . ? C62 C61 N6 122.0(12) . . ? C66 C61 N6 120.4(12) . . ? C61 C62 C63 121.1(15) . . ? C64 C63 C62 118.3(16) . . ? C63 C64 C65 122.4(15) . . ? C63 C64 O6 114.2(15) . . ? C65 C64 O6 123.3(15) . . ? C64 C65 C66 117.2(14) . . ? C61 C66 C65 123.2(14) . . ? C72 C71 C76 120.6(14) . . ? C72 C71 N7 117.7(12) . . ? C76 C71 N7 121.7(13) . . ? C71 C72 C73 122.2(15) . . ? C74 C73 C72 113.8(17) . . ? C75 C74 C73 127.3(19) . . ? C75 C74 O7 115.3(17) . . ? C73 C74 O7 117.3(17) . . ? C74 C75 C76 118.3(18) . . ? C71 C76 C75 117.8(16) . . ? C82 C81 C86 116.1(13) . . ? C82 C81 N8 123.0(13) . . ? C86 C81 N8 120.9(12) . . ? C81 C82 C83 122.8(15) . . ? C84 C83 C82 119.4(15) . . ? C83 C84 O8 124.2(14) . . ? C83 C84 C85 120.0(14) . . ? O8 C84 C85 115.8(13) . . ? C84 C85 C86 120.7(15) . . ? C85 C86 C81 121.1(14) . . ? Cl2 C1S Cl1 110.6(12) . . ? Cl4 C2S Cl3 110.2(12) . . ? Cl5 C3S Cl6 128(2) . . ? Cl6' C3S' Cl5' 147(3) . . ? C6S' O1S C4S 132(4) . . ? C4S O1S C6S 106(3) . . ? O1S C4S C5S 119(4) . . ? C5S C5S C4S 131(7) 2_554 . ? C7S C6S O1S 101(4) . . ? C7S' C6S' O1S 102(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.346 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.160 #===END data_cmpd_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Rh2(DAniF)2]2(O2CCH2CO2)2(NCC6H4CN)2(4CH2Cl2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C86 H80 Cl8 N12 O16 Rh4' _chemical_formula_weight 2232.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.708(2) _cell_length_b 14.378(2) _cell_length_c 14.997(3) _cell_angle_alpha 65.810(3) _cell_angle_beta 72.693(3) _cell_angle_gamma 74.766(3) _cell_volume 2355.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3714 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 22.52 _exptl_crystal_description 'Triangular plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type 'Analytical (face index)' _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.975 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10596 _diffrn_reflns_av_R_equivalents 0.1285 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 22.60 _reflns_number_total 6163 _reflns_number_observed 4202 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6162 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_obs 0.0508 _refine_ls_wR_factor_all 0.1402 _refine_ls_wR_factor_obs 0.1193 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 1.06593(4) 1.14018(5) 0.75278(4) 0.0301(2) Uani 1 d . . Rh2 Rh 0.89628(4) 1.22556(4) 0.83564(4) 0.0294(2) Uani 1 d . . N1 N 1.1180(6) 1.2784(5) 0.6822(5) 0.044(2) Uani 1 d . . N2 N 0.9590(5) 1.3579(5) 0.7619(5) 0.042(2) Uani 1 d . . N3 N 0.9878(5) 1.1694(5) 0.6431(4) 0.0352(15) Uani 1 d . . N4 N 0.8264(5) 1.2522(5) 0.7204(4) 0.037(2) Uani 1 d . . N5 N 1.2243(5) 1.0574(5) 0.6881(5) 0.0341(15) Uani 1 d . . N6 N 0.7466(5) 1.2987(5) 0.9194(5) 0.0320(14) Uani 1 d . . O1 O 1.5499(4) 1.2849(5) 0.4454(4) 0.061(2) Uani 1 d . . O2 O 0.7363(6) 1.6918(6) 0.8820(6) 0.091(2) Uani 1 d . . O3 O 1.2095(5) 0.9851(5) 0.3588(5) 0.066(2) Uani 1 d . . O4 O 0.3696(5) 1.4045(5) 0.7642(5) 0.069(2) Uani 1 d . . O201 O 1.0003(4) 1.0037(4) 0.8342(4) 0.0343(12) Uani 1 d . . O202 O 0.8436(4) 1.0820(4) 0.9092(3) 0.0322(12) Uani 1 d . . O203 O 1.1350(4) 1.1108(4) 0.8733(3) 0.0327(12) Uani 1 d . . O204 O 0.9781(4) 1.1902(4) 0.9494(3) 0.0321(11) Uani 1 d . . C1 C 1.0608(7) 1.3601(6) 0.7045(5) 0.039(2) Uani 1 d . . H1A H 1.0927(7) 1.4204(6) 0.6792(5) 0.046 Uiso 1 calc R . C2 C 0.8844(6) 1.2172(6) 0.6479(6) 0.039(2) Uani 1 d . . H2A H 0.8492(6) 1.2274(6) 0.5969(6) 0.047 Uiso 1 calc R . C3 C 1.0759(6) 1.1381(5) 0.9451(5) 0.028(2) Uani 1 d . . C4 C 1.1239(6) 1.1010(5) 1.0361(5) 0.030(2) Uani 1 d . . H4A H 1.0949(6) 1.1502(5) 1.0710(5) 0.036 Uiso 1 calc R . H4B H 1.2055(6) 1.0953(5) 1.0166(5) 0.036 Uiso 1 calc R . C5 C 0.9086(5) 1.0032(5) 0.8958(5) 0.027(2) Uani 1 d . . C11 C 1.2308(6) 1.2846(6) 0.6229(5) 0.035(2) Uani 1 d . . C12 C 1.3197(6) 1.2524(7) 0.6670(6) 0.048(2) Uani 1 d . . H12A H 1.3070(6) 1.2301(7) 0.7371(6) 0.057 Uiso 1 calc R . C13 C 1.4272(7) 1.2516(7) 0.6124(6) 0.049(2) Uani 1 d . . H13A H 1.4878(7) 1.2287(7) 0.6441(6) 0.059 Uiso 1 calc R . C14 C 1.4447(6) 1.2859(7) 0.5076(6) 0.045(2) Uani 1 d . . C15 C 1.3574(7) 1.3151(8) 0.4635(6) 0.057(3) Uani 1 d . . H15A H 1.3698(7) 1.3345(8) 0.3938(6) 0.068 Uiso 1 calc R . C16 C 1.2501(6) 1.3169(7) 0.5201(6) 0.050(2) Uani 1 d . . H16A H 1.1894(6) 1.3403(7) 0.4884(6) 0.060 Uiso 1 calc R . C17 C 1.6436(7) 1.2468(10) 0.4912(8) 0.082(3) Uani 1 d . . H17A H 1.7119(7) 1.2502(10) 0.4400(8) 0.122 Uiso 1 calc R . H17B H 1.6409(7) 1.1756(10) 0.5361(8) 0.122 Uiso 1 calc R . H17C H 1.6418(7) 1.2885(10) 0.5288(8) 0.122 Uiso 1 calc R . C21 C 0.9091(6) 1.4463(6) 0.7921(6) 0.038(2) Uani 1 d . . C22 C 0.8348(7) 1.5237(7) 0.7408(7) 0.056(2) Uani 1 d . . H22A H 0.8222(7) 1.5217(7) 0.6830(7) 0.067 Uiso 1 calc R . C23 C 0.7798(9) 1.6027(8) 0.7728(8) 0.075(3) Uani 1 d . . H23A H 0.7289(9) 1.6544(8) 0.7372(8) 0.090 Uiso 1 calc R . C24 C 0.7972(7) 1.6083(7) 0.8559(8) 0.058(3) Uani 1 d . . C25 C 0.8711(8) 1.5319(8) 0.9092(7) 0.062(3) Uani 1 d . . H25A H 0.8835(8) 1.5343(8) 0.9669(7) 0.074 Uiso 1 calc R . C26 C 0.9265(8) 1.4517(7) 0.8753(7) 0.059(2) Uani 1 d . . H26A H 0.9774(8) 1.3997(7) 0.9106(7) 0.071 Uiso 1 calc R . C27 C 0.7425(10) 1.6934(9) 0.9730(10) 0.096(4) Uani 1 d . . H27A H 0.6965(10) 1.7555(9) 0.9826(10) 0.145 Uiso 1 calc R . H27B H 0.8194(10) 1.6927(9) 0.9720(10) 0.145 Uiso 1 calc R . H27C H 0.7160(10) 1.6332(9) 1.0275(10) 0.145 Uiso 1 calc R . C31 C 1.0392(6) 1.1288(7) 0.5644(6) 0.039(2) Uani 1 d . . C32 C 1.0733(6) 1.0211(7) 0.5926(6) 0.048(2) Uani 1 d . . H32A H 1.0590(6) 0.9786(7) 0.6606(6) 0.057 Uiso 1 calc R . C33 C 1.1274(6) 0.9781(7) 0.5210(6) 0.051(2) Uani 1 d . . H33A H 1.1480(6) 0.9060(7) 0.5402(6) 0.061 Uiso 1 calc R . C34 C 1.1512(6) 1.0386(7) 0.4233(6) 0.045(2) Uani 1 d . . C35 C 1.1191(6) 1.1433(7) 0.3913(6) 0.048(2) Uani 1 d . . H35A H 1.1339(6) 1.1843(7) 0.3228(6) 0.058 Uiso 1 calc R . C36 C 1.0621(7) 1.1886(8) 0.4656(7) 0.055(2) Uani 1 d . . H36A H 1.0404(7) 1.2606(8) 0.4458(7) 0.066 Uiso 1 calc R . C37 C 1.2336(9) 1.0438(9) 0.2553(6) 0.078(3) Uani 1 d . . H37A H 1.2739(9) 0.9984(9) 0.2188(6) 0.117 Uiso 1 calc R . H37B H 1.2790(9) 1.0944(9) 0.2429(6) 0.117 Uiso 1 calc R . H37C H 1.1644(9) 1.0791(9) 0.2333(6) 0.117 Uiso 1 calc R . C41 C 0.7096(6) 1.2940(6) 0.7241(6) 0.039(2) Uani 1 d . . C42 C 0.6311(6) 1.2375(6) 0.8010(6) 0.042(2) Uani 1 d . . H42A H 0.6555(6) 1.1723(6) 0.8458(6) 0.050 Uiso 1 calc R . C43 C 0.5194(6) 1.2758(7) 0.8120(6) 0.048(2) Uani 1 d . . H43A H 0.4676(6) 1.2376(7) 0.8645(6) 0.057 Uiso 1 calc R . C44 C 0.4833(7) 1.3716(7) 0.7450(7) 0.051(2) Uani 1 d . . C45 C 0.5597(7) 1.4283(7) 0.6663(7) 0.055(2) Uani 1 d . . H45A H 0.5352(7) 1.4927(7) 0.6203(7) 0.066 Uiso 1 calc R . C46 C 0.6731(7) 1.3876(7) 0.6573(6) 0.046(2) Uani 1 d . . H46A H 0.7253(7) 1.4251(7) 0.6046(6) 0.056 Uiso 1 calc R . C47 C 0.3264(8) 1.4995(9) 0.6936(11) 0.098(4) Uani 1 d . . H47A H 0.2460(8) 1.5140(9) 0.7155(11) 0.147 Uiso 1 calc R . H47B H 0.3445(8) 1.4934(9) 0.6285(11) 0.147 Uiso 1 calc R . H47C H 0.3596(8) 1.5552(9) 0.6891(11) 0.147 Uiso 1 calc R . C51 C 1.3035(6) 1.0382(6) 0.6369(6) 0.039(2) Uani 1 d . . C52 C 1.4055(6) 1.0165(6) 0.5685(6) 0.036(2) Uani 1 d . . C53 C 1.5019(7) 0.9618(8) 0.6015(6) 0.057(2) Uani 1 d . . C54 C 1.5994(6) 0.9442(7) 0.5321(6) 0.049(2) Uani 1 d . . C61 C 0.6741(6) 1.3539(6) 0.9471(6) 0.039(2) Uani 1 d . . C62 C 0.5851(6) 1.4276(6) 0.9747(6) 0.040(2) Uani 1 d . . C63 C 0.5126(8) 1.4825(9) 0.9125(8) 0.076(4) Uani 1 d . . C64 C 0.5769(8) 1.4457(9) 1.0614(8) 0.078(4) Uani 1 d . . C1S C 0.6319(8) 1.0638(9) 1.1000(8) 0.073(3) Uani 1 d . . Cl1 Cl 0.5252(2) 1.1667(2) 1.1155(2) 0.0927(10) Uani 1 d . . Cl2 Cl 0.5717(6) 0.9606(10) 1.1235(30) 0.115(7) Uani 0.67(5) d P 1 Cl2' Cl 0.5703(13) 0.9936(30) 1.0563(36) 0.086(9) Uani 0.33(5) d P 2 C2S C 0.8440(7) 1.2160(8) 1.1602(7) 0.064(3) Uani 1 d . . Cl3 Cl 0.9313(3) 1.2855(3) 1.1709(3) 0.1059(11) Uani 1 d . . Cl4 Cl 0.7137(2) 1.2250(2) 1.2445(2) 0.0883(9) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0266(3) 0.0321(4) 0.0258(3) -0.0164(3) 0.0081(3) -0.0012(3) Rh2 0.0262(3) 0.0285(4) 0.0270(3) -0.0148(3) 0.0048(3) 0.0018(3) N1 0.059(4) 0.030(4) 0.035(4) -0.004(3) -0.001(3) -0.018(3) N2 0.044(4) 0.032(4) 0.040(4) 0.002(3) -0.010(3) -0.012(3) N3 0.034(4) 0.042(4) 0.027(3) -0.020(3) 0.002(3) 0.000(3) N4 0.038(4) 0.034(4) 0.031(4) -0.012(3) -0.006(3) 0.005(3) N5 0.031(4) 0.035(4) 0.037(4) -0.017(3) -0.002(3) -0.005(3) N6 0.031(3) 0.028(4) 0.039(4) -0.018(3) -0.004(3) -0.002(3) O1 0.031(3) 0.096(5) 0.051(4) -0.032(4) 0.013(3) -0.017(3) O2 0.103(6) 0.062(5) 0.108(6) -0.062(5) 0.007(5) 0.005(4) O3 0.063(4) 0.079(5) 0.060(4) -0.048(4) 0.005(3) -0.002(4) O4 0.036(3) 0.069(5) 0.102(5) -0.042(4) -0.012(3) 0.006(3) O201 0.024(3) 0.033(3) 0.037(3) -0.018(2) 0.009(2) 0.000(2) O202 0.028(3) 0.029(3) 0.031(3) -0.014(2) 0.009(2) -0.001(2) O203 0.025(2) 0.039(3) 0.030(3) -0.019(2) 0.004(2) 0.001(2) O204 0.032(3) 0.028(3) 0.031(3) -0.016(2) -0.001(2) 0.005(2) C1 0.060(6) 0.025(4) 0.029(4) -0.010(4) -0.006(4) -0.008(4) C2 0.046(5) 0.037(5) 0.028(4) -0.010(4) -0.002(4) -0.007(4) C3 0.028(4) 0.025(4) 0.026(4) -0.015(3) 0.007(3) -0.001(3) C4 0.030(4) 0.029(4) 0.027(4) -0.016(3) 0.006(3) -0.003(3) C5 0.021(4) 0.032(4) 0.028(4) -0.020(3) -0.002(3) 0.006(3) C11 0.031(4) 0.043(5) 0.025(4) -0.020(4) 0.016(3) -0.009(4) C12 0.037(5) 0.074(6) 0.031(4) -0.023(4) 0.001(4) -0.009(4) C13 0.041(5) 0.067(6) 0.046(5) -0.025(5) -0.007(4) -0.017(4) C14 0.037(5) 0.047(5) 0.046(5) -0.023(4) 0.006(4) -0.007(4) C15 0.043(5) 0.092(8) 0.032(5) -0.022(5) 0.007(4) -0.023(5) C16 0.031(4) 0.067(6) 0.044(5) -0.013(5) -0.003(4) -0.012(4) C17 0.040(5) 0.097(9) 0.086(8) -0.032(7) 0.007(5) -0.002(6) C21 0.040(4) 0.021(4) 0.044(5) -0.016(4) 0.002(4) 0.002(4) C22 0.068(6) 0.043(6) 0.061(6) -0.028(5) -0.017(5) 0.006(5) C23 0.091(8) 0.043(6) 0.083(8) -0.026(6) -0.034(6) 0.023(6) C24 0.055(6) 0.038(6) 0.076(7) -0.035(5) 0.012(5) -0.005(5) C25 0.081(7) 0.054(6) 0.057(6) -0.033(5) -0.006(5) -0.011(6) C26 0.068(6) 0.047(6) 0.068(6) -0.032(5) -0.018(5) 0.006(5) C27 0.109(9) 0.076(8) 0.116(10) -0.070(8) 0.020(8) -0.026(7) C31 0.030(4) 0.056(6) 0.031(5) -0.024(4) 0.007(3) -0.008(4) C32 0.042(5) 0.058(6) 0.047(5) -0.033(5) 0.004(4) -0.007(4) C33 0.042(5) 0.058(6) 0.051(6) -0.027(5) -0.003(4) 0.000(4) C34 0.039(5) 0.056(6) 0.043(5) -0.033(5) 0.002(4) -0.004(4) C35 0.044(5) 0.059(6) 0.038(5) -0.022(5) 0.002(4) -0.008(4) C36 0.049(5) 0.058(6) 0.055(6) -0.023(5) 0.000(4) -0.013(5) C37 0.082(7) 0.116(10) 0.032(5) -0.044(6) 0.008(5) -0.005(7) C41 0.035(4) 0.045(5) 0.038(5) -0.027(4) -0.007(4) 0.006(4) C42 0.039(5) 0.039(5) 0.046(5) -0.019(4) -0.007(4) 0.000(4) C43 0.040(5) 0.056(6) 0.051(5) -0.030(5) -0.002(4) -0.005(4) C44 0.039(5) 0.050(6) 0.071(6) -0.032(5) -0.009(5) -0.004(4) C45 0.055(6) 0.040(5) 0.063(6) -0.019(5) -0.010(5) 0.004(5) C46 0.042(5) 0.043(5) 0.044(5) -0.014(4) -0.003(4) -0.002(4) C47 0.050(6) 0.060(8) 0.171(13) -0.029(8) -0.048(8) 0.021(6) C51 0.029(4) 0.045(5) 0.043(5) -0.032(4) 0.010(4) 0.000(4) C52 0.022(4) 0.042(5) 0.043(5) -0.028(4) 0.014(4) -0.005(4) C53 0.037(5) 0.084(7) 0.043(5) -0.034(5) 0.008(4) -0.002(5) C54 0.029(4) 0.066(6) 0.044(5) -0.024(5) 0.006(4) 0.000(4) C61 0.036(4) 0.038(5) 0.037(5) -0.016(4) 0.000(4) -0.003(4) C62 0.030(4) 0.033(5) 0.052(5) -0.027(4) 0.013(4) -0.002(4) C63 0.071(6) 0.094(8) 0.071(7) -0.060(7) -0.038(6) 0.052(6) C64 0.074(7) 0.095(9) 0.073(7) -0.061(7) -0.038(6) 0.052(6) C1S 0.060(6) 0.071(8) 0.071(7) -0.027(6) -0.001(5) 0.002(6) Cl1 0.089(2) 0.077(2) 0.085(2) -0.036(2) 0.030(2) -0.014(2) Cl2 0.071(3) 0.068(5) 0.187(22) -0.038(8) -0.017(5) -0.006(3) Cl2' 0.057(6) 0.080(13) 0.112(21) -0.043(14) 0.006(7) -0.011(6) C2S 0.051(5) 0.081(8) 0.067(6) -0.046(6) 0.002(5) -0.005(5) Cl3 0.084(2) 0.130(3) 0.128(3) -0.088(3) 0.002(2) -0.018(2) Cl4 0.071(2) 0.076(2) 0.091(2) -0.035(2) 0.014(2) 0.0035(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 Rh2 2.4422(7) . Y Rh1 N1 2.014(6) . Y Rh1 N3 2.014(6) . Y Rh1 O201 2.081(5) . Y Rh1 O203 2.084(5) . Y Rh1 N5 2.221(6) . Y Rh2 N2 2.007(6) . Y Rh2 N4 2.028(6) . Y Rh2 O204 2.078(5) . Y Rh2 O202 2.085(5) . Y Rh2 N6 2.216(6) . Y N1 C1 1.323(9) . ? N1 C11 1.448(9) . ? N2 C1 1.324(9) . ? N2 C21 1.448(9) . ? N3 C2 1.309(9) . ? N3 C31 1.437(9) . ? N4 C2 1.325(9) . ? N4 C41 1.441(9) . ? N5 C51 1.117(8) . ? N6 C61 1.145(9) . ? O1 C14 1.385(9) . ? O1 C17 1.422(11) . ? O2 C24 1.383(10) . ? O2 C27 1.400(13) . ? O3 C34 1.400(9) . ? O3 C37 1.412(11) . ? O4 C44 1.378(10) . ? O4 C47 1.433(13) . ? O201 C5 1.253(8) . ? O202 C5 1.266(8) . ? O203 C3 1.260(7) . ? O204 C3 1.270(8) . ? C3 C4 1.499(9) . ? C4 C5 1.510(10) 2_777 ? C5 C4 1.510(10) 2_777 ? C11 C12 1.359(10) . ? C11 C16 1.379(11) . ? C12 C13 1.367(11) . ? C13 C14 1.407(11) . ? C14 C15 1.344(11) . ? C15 C16 1.376(11) . ? C21 C26 1.367(11) . ? C21 C22 1.378(11) . ? C22 C23 1.356(12) . ? C23 C24 1.365(13) . ? C24 C25 1.383(13) . ? C25 C26 1.387(12) . ? C31 C36 1.360(12) . ? C31 C32 1.408(12) . ? C32 C33 1.376(10) . ? C33 C34 1.351(12) . ? C34 C35 1.365(12) . ? C35 C36 1.435(11) . ? C41 C46 1.368(11) . ? C41 C42 1.400(11) . ? C42 C43 1.366(10) . ? C43 C44 1.388(12) . ? C44 C45 1.394(12) . ? C45 C46 1.393(11) . ? C51 C52 1.445(10) . ? C52 C53 1.379(11) . ? C52 C54 1.392(11) 2_876 ? C53 C54 1.402(10) . ? C54 C52 1.392(11) 2_876 ? C61 C62 1.423(10) . ? C62 C63 1.366(11) . ? C62 C64 1.398(11) . ? C63 C64 1.400(11) 2_687 ? C64 C63 1.400(11) 2_687 ? C1S Cl2 1.708(13) . ? C1S Cl1 1.767(10) . ? C1S Cl2' 1.82(2) . ? C2S Cl3 1.754(10) . ? C2S Cl4 1.770(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh1 N3 90.8(3) . . Y N1 Rh1 O201 174.6(2) . . Y N3 Rh1 O201 90.1(2) . . Y N1 Rh1 O203 90.7(2) . . Y N3 Rh1 O203 175.7(2) . . Y O201 Rh1 O203 88.0(2) . . Y N1 Rh1 N5 93.4(2) . . Y N3 Rh1 N5 95.5(2) . . Y O201 Rh1 N5 91.8(2) . . Y O203 Rh1 N5 88.4(2) . . Y N1 Rh1 Rh2 87.8(2) . . Y N3 Rh1 Rh2 88.5(2) . . Y O201 Rh1 Rh2 86.92(12) . . Y O203 Rh1 Rh2 87.56(12) . . Y N5 Rh1 Rh2 175.8(2) . . Y N2 Rh2 N4 91.0(3) . . Y N2 Rh2 O204 89.8(2) . . Y N4 Rh2 O204 175.4(2) . . Y N2 Rh2 O202 175.6(2) . . Y N4 Rh2 O202 90.0(2) . . Y O204 Rh2 O202 88.8(2) . . Y N2 Rh2 N6 92.7(2) . . Y N4 Rh2 N6 95.3(2) . . Y O204 Rh2 N6 89.2(2) . . Y O202 Rh2 N6 91.5(2) . . Y N2 Rh2 Rh1 88.1(2) . . Y N4 Rh2 Rh1 88.1(2) . . Y O204 Rh2 Rh1 87.37(12) . . Y O202 Rh2 Rh1 87.57(12) . . Y N6 Rh2 Rh1 176.4(2) . . Y C1 N1 C11 117.7(6) . . ? C1 N1 Rh1 121.2(5) . . ? C11 N1 Rh1 119.6(5) . . ? C1 N2 C21 116.3(6) . . ? C1 N2 Rh2 121.3(5) . . ? C21 N2 Rh2 120.0(5) . . ? C2 N3 C31 118.6(6) . . ? C2 N3 Rh1 120.1(5) . . ? C31 N3 Rh1 121.0(5) . . ? C2 N4 C41 119.1(6) . . ? C2 N4 Rh2 119.4(5) . . ? C41 N4 Rh2 120.8(5) . . ? C51 N5 Rh1 163.0(7) . . ? C61 N6 Rh2 166.5(6) . . ? C14 O1 C17 117.6(7) . . ? C24 O2 C27 117.5(9) . . ? C34 O3 C37 117.3(8) . . ? C44 O4 C47 117.4(8) . . ? C5 O201 Rh1 120.3(4) . . ? C5 O202 Rh2 119.1(4) . . ? C3 O203 Rh1 119.1(4) . . ? C3 O204 Rh2 119.3(4) . . ? N1 C1 N2 120.7(7) . . ? N3 C2 N4 123.8(7) . . ? O203 C3 O204 126.4(6) . . ? O203 C3 C4 116.6(6) . . ? O204 C3 C4 117.0(5) . . ? C3 C4 C5 108.4(5) . 2_777 ? O201 C5 O202 125.7(7) . . ? O201 C5 C4 116.9(6) . 2_777 ? O202 C5 C4 117.3(6) . 2_777 ? C12 C11 C16 118.7(7) . . ? C12 C11 N1 121.2(6) . . ? C16 C11 N1 119.9(7) . . ? C11 C12 C13 122.0(7) . . ? C12 C13 C14 118.2(8) . . ? C15 C14 O1 116.6(7) . . ? C15 C14 C13 120.2(7) . . ? O1 C14 C13 123.0(8) . . ? C14 C15 C16 120.3(8) . . ? C15 C16 C11 120.5(8) . . ? C26 C21 C22 118.3(7) . . ? C26 C21 N2 121.8(7) . . ? C22 C21 N2 119.7(7) . . ? C23 C22 C21 120.8(9) . . ? C22 C23 C24 121.0(9) . . ? C23 C24 C25 119.8(8) . . ? C23 C24 O2 116.2(9) . . ? C25 C24 O2 124.0(9) . . ? C24 C25 C26 118.3(9) . . ? C21 C26 C25 121.8(9) . . ? C36 C31 C32 118.6(7) . . ? C36 C31 N3 123.8(8) . . ? C32 C31 N3 117.4(7) . . ? C33 C32 C31 120.2(8) . . ? C34 C33 C32 120.5(9) . . ? C33 C34 C35 122.0(7) . . ? C33 C34 O3 114.6(8) . . ? C35 C34 O3 123.4(8) . . ? C34 C35 C36 117.7(8) . . ? C31 C36 C35 120.9(9) . . ? C46 C41 C42 119.1(7) . . ? C46 C41 N4 122.6(7) . . ? C42 C41 N4 118.3(7) . . ? C43 C42 C41 121.1(8) . . ? C42 C43 C44 119.4(8) . . ? O4 C44 C43 114.9(8) . . ? O4 C44 C45 124.5(8) . . ? C43 C44 C45 120.5(8) . . ? C46 C45 C44 118.8(8) . . ? C41 C46 C45 121.1(8) . . ? N5 C51 C52 178.3(9) . . ? C53 C52 C54 122.5(6) . 2_876 ? C53 C52 C51 121.4(7) . . ? C54 C52 C51 116.0(7) 2_876 . ? C52 C53 C54 119.5(8) . . ? C52 C54 C53 118.0(7) 2_876 . ? N6 C61 C62 176.0(8) . . ? C63 C62 C64 121.7(7) . . ? C63 C62 C61 118.6(7) . . ? C64 C62 C61 119.6(7) . . ? C62 C63 C64 119.9(7) . 2_687 ? C62 C64 C63 118.3(8) . 2_687 ? Cl2 C1S Cl1 108.7(6) . . ? Cl1 C1S Cl2' 104.6(10) . . ? Cl3 C2S Cl4 109.5(5) . . ? _refine_diff_density_max 1.378 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.114 #===END data_cmpd_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Rh2(DAniF)2]4[O2CCO2]4[NCC6F4C6F4CN]4(12.36CH2Cl2)' _chemical_formula_sum 'C196.36 H144.72 Cl24.72 F32 N24 O32 Rh8' _chemical_formula_weight 5660.01 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 18.235(6) _cell_length_b 18.430(6) _cell_length_c 18.665(6) _cell_angle_alpha 81.839(7) _cell_angle_beta 81.775(6) _cell_angle_gamma 80.742(7) _cell_volume 6082(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1007 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 21.79 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2815 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean 'none (area detector data)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22643 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.2153 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 22.64 _reflns_number_total 15333 _reflns_number_gt 5965 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15333 _refine_ls_number_parameters 814 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.2231 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2625 _refine_ls_wR_factor_gt 0.2110 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.152 _refine_ls_shift/su_mean 0.010 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 Rh1 Rh -2.25002(8) 1.64766(8) -1.03980(7) 0.0333(4) Uani 1 1 d . . . Rh2 Rh -2.22764(8) 1.67401(8) -0.92215(7) 0.0352(4) Uani 1 1 d . . . Rh3 Rh -2.12892(8) 1.28386(8) -0.94933(7) 0.0317(4) Uani 1 1 d . . . Rh4 Rh -2.11013(8) 1.30982(8) -0.82906(7) 0.0340(4) Uani 1 1 d . . . N1 N -2.3519(8) 1.6256(8) -0.9919(8) 0.044(4) Uiso 1 1 d . . . N2 N -2.3346(7) 1.6680(7) -0.8851(7) 0.037(4) Uiso 1 1 d . . . N3 N -2.2864(8) 1.7556(8) -1.0626(8) 0.039(4) Uiso 1 1 d . . . N4 N -2.2526(7) 1.7821(8) -0.9579(8) 0.040(4) Uiso 1 1 d . . . N5 N -2.2338(7) 1.2683(7) -0.9098(7) 0.037(4) Uiso 1 1 d . . . N6 N -2.2194(8) 1.2951(8) -0.7977(8) 0.042(4) Uiso 1 1 d . . . N7 N -2.0934(7) 1.1765(8) -0.9189(8) 0.039(4) Uiso 1 1 d . . . N8 N -2.0760(8) 1.2018(8) -0.8051(8) 0.042(4) Uiso 1 1 d . . . C1 C -2.3739(10) 1.6389(10) -0.9245(10) 0.044(5) Uiso 1 1 d . . . H1 H -2.4209 1.6269 -0.9028 0.053 Uiso 1 1 calc R . . C2 C -2.2779(10) 1.8037(11) -1.0200(10) 0.049(5) Uiso 1 1 d . . . H2 H -2.2904 1.8546 -1.0348 0.058 Uiso 1 1 calc R . . C3 C -2.2590(10) 1.2762(9) -0.8424(9) 0.038(5) Uiso 1 1 d . . . H3 H -2.3083 1.2679 -0.8251 0.045 Uiso 1 1 calc R . . C4 C -2.0747(10) 1.1542(11) -0.8522(10) 0.044(5) Uiso 1 1 d . . . H4 H -2.0602 1.1035 -0.8382 0.053 Uiso 1 1 calc R . . C5 C -2.1925(9) 1.5167(10) -0.9445(9) 0.032(4) Uiso 1 1 d . . . C6 C -2.1651(9) 1.4381(10) -0.9265(9) 0.032(4) Uiso 1 1 d . . . C7 C -2.1007(9) 1.6788(9) -1.0330(9) 0.033(4) Uiso 1 1 d . . . C8 C -1.9792(9) 1.3130(8) -0.9375(8) 0.028(4) Uiso 1 1 d . . . O201 O -2.1425(6) 1.6704(6) -1.0787(6) 0.033(3) Uiso 1 1 d . . . O202 O -2.1170(6) 1.6772(6) -0.9647(6) 0.037(3) Uiso 1 1 d . . . O203 O -2.2088(6) 1.5389(6) -1.0103(6) 0.036(3) Uiso 1 1 d . . . O204 O -2.2006(6) 1.5610(6) -0.8956(6) 0.035(3) Uiso 1 1 d . . . O205 O -2.0195(6) 1.3008(6) -0.9827(6) 0.037(3) Uiso 1 1 d . . . O206 O -2.0000(6) 1.3231(6) -0.8715(6) 0.035(3) Uiso 1 1 d . . . O207 O -2.1654(6) 1.3958(6) -0.9731(6) 0.033(3) Uiso 1 1 d . . . O208 O -2.1458(6) 1.4211(6) -0.8626(6) 0.038(3) Uiso 1 1 d . . . O1 O -2.5544(7) 1.5178(7) -1.1337(7) 0.060(4) Uiso 1 1 d . . . O2 O -2.4202(13) 1.7048(13) -0.5913(13) 0.160(9) Uiso 1 1 d . . . O4 O -2.2379(12) 1.9972(12) -0.7792(12) 0.139(7) Uiso 1 1 d . . . O5 O -2.4467(9) 1.2264(9) -1.0809(8) 0.089(5) Uiso 1 1 d . . . O6 O -2.3583(11) 1.3417(12) -0.5152(11) 0.134(7) Uiso 1 1 d . . . O7 O -2.0715(7) 0.9570(7) -1.1024(7) 0.063(4) Uiso 1 1 d . . . C11 C -2.4050(10) 1.6025(10) -1.0313(9) 0.039(5) Uiso 1 1 d . . . C12 C -2.3828(10) 1.5365(10) -1.0660(9) 0.051(5) Uiso 1 1 d . . . H12 H -2.3337 1.5111 -1.0663 0.061 Uiso 1 1 calc R . . C13 C -2.4353(10) 1.5112(10) -1.0990(9) 0.046(5) Uiso 1 1 d . . . H13 H -2.4223 1.4675 -1.1213 0.055 Uiso 1 1 calc R . . C14 C -2.5074(10) 1.5501(10) -1.0995(10) 0.047(5) Uiso 1 1 d . . . C15 C -2.5257(12) 1.6122(11) -1.0683(11) 0.064(6) Uiso 1 1 d . . . H15 H -2.5740 1.6392 -1.0693 0.077 Uiso 1 1 calc R . . C16 C -2.4732(10) 1.6365(11) -1.0344(10) 0.052(5) Uiso 1 1 d . . . H16 H -2.4875 1.6802 -1.0122 0.063 Uiso 1 1 calc R . . C17 C -2.6294(10) 1.5474(10) -1.1289(10) 0.057(6) Uiso 1 1 d . . . H17A H -2.6557 1.5197 -1.1549 0.086 Uiso 1 1 calc R . . H17B H -2.6344 1.5988 -1.1502 0.086 Uiso 1 1 calc R . . H17C H -2.6507 1.5443 -1.0780 0.086 Uiso 1 1 calc R . . C21 C -2.3646(9) 1.6730(10) -0.8123(9) 0.038(5) Uiso 1 1 d . . . C22 C -2.3661(12) 1.7391(13) -0.7889(12) 0.076(7) Uiso 1 1 d . . . H22 H -2.3498 1.7784 -0.8220 0.091 Uiso 1 1 calc R . . C23 C -2.3928(12) 1.7514(14) -0.7119(13) 0.086(7) Uiso 1 1 d . . . H23 H -2.4028 1.7983 -0.6954 0.103 Uiso 1 1 calc R . . C24 C -2.4012(12) 1.6857(14) -0.6676(13) 0.078(7) Uiso 1 1 d . . . C25 C -2.4026(12) 1.6216(14) -0.6893(13) 0.083(7) Uiso 1 1 d . . . H25 H -2.4164 1.5812 -0.6562 0.100 Uiso 1 1 calc R . . C26 C -2.3822(12) 1.6154(13) -0.7651(12) 0.079(7) Uiso 1 1 d . . . H26 H -2.3813 1.5696 -0.7821 0.095 Uiso 1 1 calc R . . C27 C -2.4401(19) 1.649(2) -0.5471(19) 0.175(15) Uiso 1 1 d . . . H27A H -2.4522 1.6626 -0.4981 0.263 Uiso 1 1 calc R . . H27B H -2.3994 1.6079 -0.5480 0.263 Uiso 1 1 calc R . . H27C H -2.4838 1.6341 -0.5621 0.263 Uiso 1 1 calc R . . C31 C -2.2978(11) 1.7846(11) -1.1349(11) 0.057(6) Uiso 1 1 d . A . C32 C -2.2566(11) 1.8301(11) -1.1788(11) 0.061(6) Uiso 1 1 d . . . H32 H -2.2188 1.8475 -1.1594 0.073 Uiso 1 1 calc R . . C33 C -2.2661(16) 1.8540(15) -1.2527(15) 0.109(9) Uiso 1 1 d . A . H33 H -2.2321 1.8816 -1.2830 0.131 Uiso 1 1 calc R . . C34 C -2.3255(17) 1.8360(16) -1.2783(17) 0.108(9) Uiso 1 1 d . . . C35 C -2.3749(18) 1.7952(16) -1.2369(17) 0.132(11) Uiso 1 1 d . A . H35 H -2.4167 1.7855 -1.2561 0.158 Uiso 1 1 calc R . . C36 C -2.3619(13) 1.7654(13) -1.1589(13) 0.087(8) Uiso 1 1 d . . . H36 H -2.3942 1.7361 -1.1284 0.104 Uiso 1 1 calc R A . O3 O -2.300(5) 1.840(3) -1.371(5) 0.155(13) Uiso 0.32(3) 1 d PD A 1 C37 C -2.353(9) 1.825(10) -1.414(9) 0.36(5) Uiso 0.32(3) 1 d PD A 1 H37A H -2.3320 1.8298 -1.4651 0.544 Uiso 0.32(3) 1 calc PR A 1 H37B H -2.3986 1.8604 -1.4080 0.544 Uiso 0.32(3) 1 calc PR A 1 H37C H -2.3649 1.7753 -1.3993 0.544 Uiso 0.32(3) 1 calc PR A 1 O3' O -2.352(2) 1.863(2) -1.350(2) 0.155(13) Uiso 0.68(3) 1 d PD A 2 C37' C -2.303(5) 1.918(4) -1.378(5) 0.36(5) Uiso 0.68(3) 1 d PD A 2 H37D H -2.3146 1.9399 -1.4260 0.544 Uiso 0.68(3) 1 calc PR A 2 H37E H -2.2516 1.8937 -1.3810 0.544 Uiso 0.68(3) 1 calc PR A 2 H37F H -2.3106 1.9555 -1.3455 0.544 Uiso 0.68(3) 1 calc PR A 2 C41 C -2.2463(11) 1.8377(11) -0.9125(10) 0.046(5) Uiso 1 1 d . . . C42 C -2.1857(12) 1.8318(12) -0.8771(11) 0.065(6) Uiso 1 1 d . . . H42 H -2.1467 1.7926 -0.8851 0.078 Uiso 1 1 calc R . . C43 C -2.1779(12) 1.8812(12) -0.8289(11) 0.067(6) Uiso 1 1 d . . . H43 H -2.1370 1.8738 -0.8019 0.081 Uiso 1 1 calc R . . C44 C -2.2295(13) 1.9366(13) -0.8237(12) 0.074(7) Uiso 1 1 d . . . C45 C -2.2935(13) 1.9512(13) -0.8540(12) 0.082(7) Uiso 1 1 d . . . H45 H -2.3307 1.9917 -0.8452 0.098 Uiso 1 1 calc R . . C46 C -2.2989(13) 1.8947(13) -0.9040(13) 0.085(7) Uiso 1 1 d . . . H46 H -2.3408 1.9006 -0.9295 0.102 Uiso 1 1 calc R . . C47 C -2.1834(19) 1.9818(19) -0.7414(19) 0.170(15) Uiso 1 1 d . . . H47A H -2.1855 2.0202 -0.7103 0.256 Uiso 1 1 calc R . . H47B H -2.1366 1.9789 -0.7737 0.256 Uiso 1 1 calc R . . H47C H -2.1866 1.9346 -0.7115 0.256 Uiso 1 1 calc R . . C51 C -2.2862(9) 1.2526(9) -0.9518(9) 0.035(5) Uiso 1 1 d . . . C52 C -2.3267(10) 1.1944(11) -0.9307(11) 0.058(6) Uiso 1 1 d . . . H52 H -2.3174 1.1621 -0.8882 0.070 Uiso 1 1 calc R . . C53 C -2.3835(11) 1.1823(11) -0.9731(11) 0.063(6) Uiso 1 1 d . . . H53 H -2.4130 1.1443 -0.9576 0.075 Uiso 1 1 calc R . . C54 C -2.3919(12) 1.2259(12) -1.0333(12) 0.069(6) Uiso 1 1 d . . . C55 C -2.3515(11) 1.2841(12) -1.0564(12) 0.069(6) Uiso 1 1 d . . . H55 H -2.3601 1.3144 -1.1002 0.083 Uiso 1 1 calc R . . C56 C -2.2982(10) 1.2983(10) -1.0157(9) 0.048(5) Uiso 1 1 d . . . H56 H -2.2710 1.3380 -1.0314 0.057 Uiso 1 1 calc R . . C57 C -2.4963(14) 1.1751(14) -1.0547(14) 0.115(10) Uiso 1 1 d . . . H57A H -2.5322 1.1776 -1.0889 0.173 Uiso 1 1 calc R . . H57B H -2.5225 1.1865 -1.0077 0.173 Uiso 1 1 calc R . . H57C H -2.4684 1.1256 -1.0493 0.173 Uiso 1 1 calc R . . C61 C -2.2554(11) 1.3091(11) -0.7245(11) 0.055(6) Uiso 1 1 d . . . C62 C -2.2579(11) 1.3768(11) -0.7018(11) 0.064(6) Uiso 1 1 d . . . H62 H -2.2349 1.4133 -0.7333 0.076 Uiso 1 1 calc R . . C63 C -2.2927(12) 1.3936(13) -0.6343(12) 0.074(7) Uiso 1 1 d . . . H63 H -2.2943 1.4403 -0.6191 0.089 Uiso 1 1 calc R . . C64 C -2.3248(13) 1.3381(14) -0.5912(14) 0.086(7) Uiso 1 1 d . . . C65 C -2.3273(12) 1.2676(12) -0.6114(12) 0.075(7) Uiso 1 1 d . . . H65 H -2.3540 1.2331 -0.5810 0.090 Uiso 1 1 calc R . . C66 C -2.2872(12) 1.2512(13) -0.6803(12) 0.077(7) Uiso 1 1 d . . . H66 H -2.2824 1.2039 -0.6952 0.092 Uiso 1 1 calc R . . C67 C -2.3595(19) 1.410(2) -0.5017(19) 0.176(15) Uiso 1 1 d . . . H67A H -2.3815 1.4153 -0.4518 0.264 Uiso 1 1 calc R . . H67B H -2.3891 1.4444 -0.5348 0.264 Uiso 1 1 calc R . . H67C H -2.3088 1.4222 -0.5085 0.264 Uiso 1 1 calc R . . C71 C -2.0902(9) 1.1203(9) -0.9652(9) 0.033(4) Uiso 1 1 d . . . C72 C -2.0449(9) 1.1223(10) -1.0301(9) 0.044(5) Uiso 1 1 d . . . H72 H -2.0160 1.1610 -1.0443 0.053 Uiso 1 1 calc R . . C73 C -2.0410(10) 1.0671(10) -1.0757(10) 0.047(5) Uiso 1 1 d . . . H73 H -2.0107 1.0689 -1.1209 0.056 Uiso 1 1 calc R . . C74 C -2.0824(10) 1.0109(10) -1.0527(9) 0.044(5) Uiso 1 1 d . . . C75 C -2.1301(11) 1.0091(11) -0.9886(10) 0.060(6) Uiso 1 1 d . . . H75 H -2.1587 0.9703 -0.9739 0.072 Uiso 1 1 calc R . . C76 C -2.1349(9) 1.0660(9) -0.9464(9) 0.043(5) Uiso 1 1 d . . . H76 H -2.1695 1.0673 -0.9040 0.051 Uiso 1 1 calc R . . C77 C -2.1104(10) 0.8921(10) -1.0781(10) 0.060(6) Uiso 1 1 d . . . H77A H -2.0997 0.8588 -1.1153 0.091 Uiso 1 1 calc R . . H77B H -2.1639 0.9082 -1.0698 0.091 Uiso 1 1 calc R . . H77C H -2.0931 0.8666 -1.0331 0.091 Uiso 1 1 calc R . . C81 C -2.0472(10) 1.1745(10) -0.7370(10) 0.044(5) Uiso 1 1 d . B . C82 C -1.9803(13) 1.1884(13) -0.7255(13) 0.083(7) Uiso 1 1 d . . . H82 H -1.9518 1.2150 -0.7632 0.099 Uiso 1 1 calc R . . C83 C -1.9506(16) 1.1643(15) -0.6581(15) 0.113(10) Uiso 1 1 d . B . H83 H -1.9030 1.1719 -0.6497 0.135 Uiso 1 1 calc R . . C84 C -1.9962(15) 1.1307(14) -0.6096(15) 0.094(8) Uiso 1 1 d . . . C85 C -2.0628(15) 1.1088(14) -0.6180(15) 0.101(9) Uiso 1 1 d . B . H85 H -2.0894 1.0789 -0.5817 0.121 Uiso 1 1 calc R . . C86 C -2.0862(13) 1.1345(12) -0.6834(12) 0.080(7) Uiso 1 1 d . . . H86 H -2.1326 1.1237 -0.6920 0.097 Uiso 1 1 calc R B . O8 O -1.978(2) 1.099(2) -0.532(2) 0.117(10) Uiso 0.57(3) 1 d PD B 1 C87 C -1.932(6) 1.091(6) -0.463(6) 0.38(6) Uiso 0.57(3) 1 d PD B 1 H87A H -1.9526 1.0558 -0.4248 0.570 Uiso 0.57(3) 1 calc PR B 1 H87B H -1.9358 1.1384 -0.4460 0.570 Uiso 0.57(3) 1 calc PR B 1 H87C H -1.8798 1.0724 -0.4779 0.570 Uiso 0.57(3) 1 calc PR B 1 O8' O -1.933(3) 1.123(3) -0.541(3) 0.117(10) Uiso 0.43(3) 1 d PD B 2 C87' C -2.010(6) 1.109(9) -0.495(10) 0.38(6) Uiso 0.43(3) 1 d PD B 2 H87D H -2.0045 1.0998 -0.4437 0.570 Uiso 0.43(3) 1 calc PR B 2 H87E H -2.0269 1.0662 -0.5097 0.570 Uiso 0.43(3) 1 calc PR B 2 H87F H -2.0475 1.1522 -0.5038 0.570 Uiso 0.43(3) 1 calc PR B 2 N201 N -2.2526(10) 1.6163(10) -1.1539(10) 0.069(6) Uiso 1 1 d . . . N202 N -2.1974(11) 1.6788(11) -0.8058(12) 0.083(6) Uiso 1 1 d . . . N203 N -2.1317(7) 1.2775(7) -1.0637(7) 0.037(4) Uiso 1 1 d . . . N204 N -2.0864(8) 1.3386(8) -0.7224(9) 0.050(4) Uiso 1 1 d . . . C201 C -2.2440(11) 1.6127(11) -1.1994(12) 0.053(6) Uiso 1 1 d U . . C202 C -2.2373(15) 1.6254(15) -1.2834(15) 0.099(8) Uiso 1 1 d U . . C203 C -2.2825(17) 1.5842(17) -1.3186(18) 0.113(9) Uiso 1 1 d U . . C204 C -2.2737(17) 1.5930(17) -1.3944(18) 0.115(9) Uiso 1 1 d U . . C205 C -2.2230(17) 1.6331(17) -1.4387(17) 0.111(9) Uiso 1 1 d U . . C206 C -2.1827(19) 1.6752(19) -1.4057(19) 0.128(10) Uiso 1 1 d U . . C207 C -2.1869(16) 1.6673(15) -1.3279(16) 0.094(8) Uiso 1 1 d U . . C208 C -2.2141(15) 1.6455(18) -1.5205(17) 0.107(9) Uiso 1 1 d U . . C209 C -2.2211(18) 1.715(2) -1.558(2) 0.124(10) Uiso 1 1 d U . . C210 C -2.219(2) 1.721(2) -1.634(2) 0.150(12) Uiso 1 1 d U . . C211 C -2.2034(15) 1.6549(18) -1.6734(17) 0.110(9) Uiso 1 1 d U . . C212 C -2.1937(17) 1.5839(19) -1.6371(18) 0.110(9) Uiso 1 1 d U . . C213 C -2.2084(19) 1.586(2) -1.557(2) 0.141(11) Uiso 1 1 d U . . C214 C -2.1966(17) 1.6667(16) -0.7499(17) 0.044(8) Uiso 0.63(3) 1 d P . 1 C215 C -2.1421(17) 1.6533(16) -0.7765(16) 0.044(8) Uiso 0.63(3) 1 d P . 2 C221 C -2.0834(11) 1.3422(11) -0.6647(12) 0.057(6) Uiso 1 1 d . . . C222 C -2.0848(11) 1.3365(12) -0.5865(11) 0.061(6) Uiso 1 1 d . . . C223 C -2.1240(11) 1.2903(12) -0.5421(12) 0.060(6) Uiso 1 1 d . . . C224 C -2.1281(14) 1.2832(14) -0.4666(14) 0.082(7) Uiso 1 1 d . . . C225 C -2.0908(13) 1.3331(13) -0.4388(13) 0.082(7) Uiso 1 1 d . . . C226 C -2.0400(15) 1.3693(15) -0.4856(16) 0.097(8) Uiso 1 1 d . . . C227 C -2.0350(15) 1.3726(15) -0.5574(16) 0.099(9) Uiso 1 1 d . . . C228 C -2.0955(13) 1.3194(13) -0.3547(12) 0.069(6) Uiso 1 1 d . . . C229 C -2.1554(19) 1.3570(18) -0.3157(19) 0.127(11) Uiso 1 1 d . . . C230 C -2.1625(17) 1.3383(15) -0.2408(16) 0.101(9) Uiso 1 1 d . . . C231 C -2.1095(13) 1.2992(12) -0.2038(12) 0.067(6) Uiso 1 1 d . . . C232 C -2.0437(15) 1.2713(14) -0.2416(14) 0.079(7) Uiso 1 1 d . . . C233 C -2.0360(16) 1.2836(15) -0.3168(16) 0.095(8) Uiso 1 1 d . . . C241 C -2.1214(9) 1.2883(10) -1.1238(10) 0.041(5) Uiso 1 1 d . . . F3 F -2.3254(11) 1.5382(13) -1.2815(9) 0.194(10) Uani 1 1 d . . . F4 F -2.3162(13) 1.5571(13) -1.4252(10) 0.208(11) Uani 1 1 d . . . F6 F -2.1301(12) 1.7119(11) -1.4467(9) 0.173(8) Uani 1 1 d . . . F7 F -2.1461(11) 1.6953(14) -1.2979(8) 0.186(10) Uani 1 1 d . . . F9 F -2.2403(16) 1.7719(11) -1.5265(10) 0.220(12) Uani 1 1 d . . . F10 F -2.2242(13) 1.7890(11) -1.6698(11) 0.194(9) Uani 1 1 d . . . F12 F -2.1786(10) 1.5315(8) -1.6650(6) 0.129(7) Uani 1 1 d . . . F13 F -2.1900(13) 1.5122(11) -1.5190(10) 0.181(8) Uani 1 1 d . . . F23 F -2.1655(9) 1.2505(8) -0.5689(7) 0.110(5) Uani 1 1 d . . . F24 F -2.1706(9) 1.2403(10) -0.4243(7) 0.137(7) Uani 1 1 d . . . F26 F -1.9984(14) 1.4063(14) -0.4557(8) 0.228(13) Uani 1 1 d . . . F27 F -1.9998(12) 1.4220(12) -0.5989(7) 0.194(11) Uani 1 1 d . . . F29 F -2.2113(9) 1.3943(18) -0.3512(8) 0.270(17) Uani 1 1 d . . . F30 F -2.2302(9) 1.3725(14) -0.2038(7) 0.211(12) Uani 1 1 d . . . F32 F -1.9919(9) 1.2326(9) -0.2082(7) 0.135(7) Uani 1 1 d . . . F33 F -1.9737(10) 1.2524(10) -0.3536(7) 0.158(8) Uani 1 1 d . . . C1S C -1.7672(17) 1.8765(17) -0.8827(17) 0.132(11) Uiso 1 1 d . . . Cl1 Cl -1.7648(7) 1.8313(7) -0.8022(7) 0.213(5) Uiso 1 1 d . . . Cl2 Cl -1.7165(7) 1.9553(7) -0.8982(7) 0.216(5) Uiso 1 1 d . . . C2S C -1.4820(19) 1.416(2) -0.702(2) 0.159(13) Uiso 1 1 d . . . Cl3 Cl -1.5314(13) 1.3299(13) -0.6652(14) 0.249(11) Uiso 0.65 1 d P C 1 Cl3' Cl -1.498(2) 1.339(2) -0.717(2) 0.182(13) Uiso 0.35 1 d P C 2 Cl4 Cl -1.5068(8) 1.4568(8) -0.6243(8) 0.234(6) Uiso 1 1 d . C . C3S C -2.081(2) 1.007(2) -1.269(2) 0.173(15) Uiso 1 1 d . . . Cl5 Cl -2.1529(9) 1.0312(9) -1.3348(9) 0.298(8) Uiso 1 1 d . . . Cl6 Cl -2.0229(9) 1.0797(9) -1.2909(9) 0.274(7) Uiso 1 1 d . . . C4S C -1.578(2) 1.719(2) -0.755(2) 0.138(14) Uiso 0.853(11) 1 d PD D 1 Cl7 Cl -1.6183(9) 1.7488(11) -0.6671(9) 0.246(8) Uiso 0.853(11) 1 d PD D 1 Cl8 Cl -1.5983(7) 1.6225(8) -0.7458(7) 0.177(5) Uiso 0.853(11) 1 d PD D 1 C4S' C -1.631(12) 1.789(6) -0.778(5) 0.138(14) Uiso 0.147(11) 1 d PD D 2 Cl7' Cl -1.611(5) 1.826(5) -0.699(6) 0.246(8) Uiso 0.147(11) 1 d PD D 2 Cl8' Cl -1.643(5) 1.692(4) -0.742(4) 0.177(5) Uiso 0.147(11) 1 d PD D 2 C5S C -1.553(4) 2.016(4) -0.817(4) 0.15(2) Uiso 0.50 1 d P . . Cl9 Cl -1.5278(13) 1.9226(13) -0.7700(13) 0.204(9) Uiso 0.50 1 d P . . Cl10 Cl -1.5261(10) 2.0298(10) -0.8959(10) 0.143(6) Uiso 0.50 1 d P . . C6S C -2.387(2) 1.066(2) -0.672(3) 0.07(3) Uiso 0.25 1 d PG . . Cl11 Cl -1.4156(14) 2.1199(14) -0.7338(14) 0.090(8) Uiso 0.25 1 d PG . . Cl12 Cl -2.414(2) 0.983(2) -0.649(3) 0.29(3) Uiso 0.25 1 d PG . . C7S C -2.254(3) 1.098(3) -0.471(3) 0.035(17) Uiso 0.25 1 d PD . . Cl13 Cl -2.353(3) 1.113(6) -0.465(5) 0.45(5) Uiso 0.25 1 d PD . . Cl14 Cl -2.235(3) 1.034(3) -0.535(3) 0.23(2) Uiso 0.25 1 d PD . . C8S C -2.016(2) 1.558(2) -0.7608(19) 0.056(10) Uiso 0.53 1 d P . . Cl15 Cl -1.935(2) 1.488(2) -0.762(2) 0.234(15) Uiso 0.38 1 d P . . Cl16 Cl -2.073(3) 1.512(3) -0.806(3) 0.26(3) Uiso 0.25 1 d P . . C9S C -1.933(6) 1.483(6) -0.857(6) 0.10(3) Uiso 0.28 1 d P . . Cl17 Cl -1.8626(19) 1.5362(19) -0.8697(19) 0.231(14) Uiso 0.40 1 d P . . Cl18 Cl -1.920(2) 1.406(3) -0.794(2) 0.261(19) Uiso 0.35 1 d P . . C10S C -2.004(5) 1.560(5) -0.887(4) 0.09(3) Uiso 0.37 1 d P . . Cl19 Cl -2.0086(19) 1.631(2) -0.864(2) 0.168(13) Uiso 0.29 1 d P . . Cl20 Cl -1.996(2) 1.5067(19) -0.9732(15) 0.139(11) Uiso 0.30 1 d P . . Cl21 Cl -1.968(2) 1.532(2) -0.898(2) 0.200(16) Uiso 0.39 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0359(9) 0.0406(10) 0.0260(8) -0.0116(7) -0.0030(7) -0.0079(8) Rh2 0.0398(10) 0.0433(10) 0.0271(8) -0.0158(8) -0.0002(7) -0.0125(8) Rh3 0.0412(10) 0.0387(10) 0.0185(8) -0.0083(7) -0.0014(7) -0.0130(8) Rh4 0.0430(10) 0.0427(10) 0.0182(8) -0.0079(7) 0.0001(7) -0.0119(8) F3 0.23(2) 0.29(3) 0.100(13) -0.030(14) 0.036(13) -0.18(2) F4 0.27(2) 0.29(3) 0.125(14) -0.070(16) -0.036(16) -0.18(2) F6 0.23(2) 0.21(2) 0.100(12) 0.014(13) -0.002(13) -0.147(17) F7 0.166(17) 0.35(3) 0.076(11) -0.010(14) -0.027(11) -0.149(19) F9 0.42(4) 0.135(16) 0.127(15) -0.093(13) -0.019(19) -0.067(19) F10 0.29(3) 0.121(16) 0.174(19) 0.004(14) -0.033(18) -0.068(16) F12 0.25(2) 0.078(10) 0.044(8) -0.031(7) 0.030(10) -0.003(11) F13 0.28(3) 0.124(16) 0.135(15) -0.021(13) -0.038(16) 0.002(16) F23 0.161(14) 0.122(12) 0.064(8) -0.013(8) -0.021(9) -0.064(11) F24 0.184(16) 0.202(18) 0.047(8) 0.006(9) -0.001(9) -0.119(14) F26 0.34(3) 0.35(3) 0.071(11) -0.028(14) -0.039(14) -0.26(3) F27 0.30(2) 0.30(2) 0.052(9) 0.002(12) -0.044(12) -0.24(2) F29 0.097(13) 0.60(5) 0.044(9) 0.021(17) -0.015(9) 0.10(2) F30 0.108(13) 0.43(3) 0.043(9) 0.002(14) 0.008(9) 0.069(17) F32 0.135(13) 0.166(16) 0.073(10) -0.029(10) -0.007(10) 0.081(12) F33 0.171(17) 0.200(18) 0.065(10) -0.032(11) 0.017(11) 0.070(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N3 1.998(14) . Y Rh1 N1 2.020(13) . Y Rh1 O203 2.051(11) . Y Rh1 O201 2.078(10) . Y Rh1 N201 2.29(2) . Y Rh1 Rh2 2.418(2) . Y Rh2 N2 1.989(13) . Y Rh2 N4 2.010(14) . Y Rh2 O204 2.067(11) . Y Rh2 O202 2.067(10) . Y Rh2 N202 2.33(2) . Y Rh3 N5 1.999(13) . Y Rh3 N7 2.009(14) . Y Rh3 O205 2.064(10) . Y Rh3 O207 2.068(11) . Y Rh3 N203 2.163(14) . Y Rh3 Rh4 2.442(2) . Y Rh4 N8 1.995(15) . Y Rh4 N6 2.044(14) . Y Rh4 O208 2.084(11) . Y Rh4 O206 2.090(10) . Y Rh4 N204 2.247(17) . Y N1 C1 1.31(2) . ? N1 C11 1.44(2) . ? N2 C1 1.31(2) . ? N2 C21 1.40(2) . ? N3 C2 1.31(2) . ? N3 C31 1.41(2) . ? N4 C2 1.30(2) . ? N4 C41 1.45(2) . ? N5 C3 1.298(19) . ? N5 C51 1.41(2) . ? N6 C3 1.29(2) . ? N6 C61 1.47(2) . ? N7 C4 1.33(2) . ? N7 C71 1.43(2) . ? N8 C4 1.32(2) . ? N8 C81 1.44(2) . ? C5 O204 1.287(18) . ? C5 O203 1.299(18) . ? C5 C6 1.46(2) . ? C6 O207 1.249(18) . ? C6 O208 1.274(18) . ? C7 O201 1.262(18) . ? C7 O202 1.264(18) . ? C7 C8 1.507(19) 2_183 ? C8 O205 1.259(17) . ? C8 O206 1.266(17) . ? C8 C7 1.507(19) 2_183 ? O1 C17 1.384(19) . ? O1 C14 1.39(2) . ? O2 C27 1.29(3) . ? O2 C24 1.49(3) . ? O4 C47 1.27(3) . ? O4 C44 1.46(3) . ? O5 C57 1.40(3) . ? O5 C54 1.43(2) . ? O6 C67 1.32(3) . ? O6 C64 1.47(3) . ? O7 C74 1.43(2) . ? O7 C77 1.47(2) . ? C11 C16 1.30(2) . ? C11 C12 1.43(2) . ? C12 C13 1.38(2) . ? C13 C14 1.39(2) . ? C14 C15 1.33(2) . ? C15 C16 1.38(2) . ? C21 C26 1.33(2) . ? C21 C22 1.35(3) . ? C22 C23 1.49(3) . ? C23 C24 1.38(3) . ? C24 C25 1.31(3) . ? C25 C26 1.43(3) . ? C31 C32 1.33(2) . ? C31 C36 1.42(3) . ? C32 C33 1.41(3) . ? C33 C34 1.35(3) . ? C34 C35 1.35(3) . ? C34 O3' 1.48(4) . ? C34 O3 1.71(9) . ? C35 C36 1.52(3) . ? O3 C37 1.43(2) . ? O3' C37' 1.44(3) . ? C41 C46 1.31(3) . ? C41 C42 1.35(2) . ? C42 C43 1.40(3) . ? C43 C44 1.28(3) . ? C44 C45 1.34(3) . ? C45 C46 1.52(3) . ? C51 C52 1.38(2) . ? C51 C56 1.38(2) . ? C52 C53 1.45(3) . ? C53 C54 1.30(3) . ? C54 C55 1.38(3) . ? C55 C56 1.39(2) . ? C61 C62 1.36(3) . ? C61 C66 1.40(2) . ? C62 C63 1.38(3) . ? C63 C64 1.36(3) . ? C64 C65 1.41(3) . ? C65 C66 1.43(3) . ? C71 C72 1.37(2) . ? C71 C76 1.37(2) . ? C72 C73 1.40(2) . ? C73 C74 1.36(2) . ? C74 C75 1.37(2) . ? C75 C76 1.38(2) . ? C81 C82 1.34(3) . ? C81 C86 1.34(2) . ? C82 C83 1.43(3) . ? C83 C84 1.30(3) . ? C84 C85 1.38(3) . ? C84 O8 1.55(4) . ? C84 O8' 1.82(6) . ? C85 C86 1.35(3) . ? O8 C87 1.59(8) . ? O8' C87' 1.59(8) . ? N201 C201 0.85(2) . ? N202 C214 1.04(3) . ? N202 C215 1.21(3) . ? N203 C241 1.106(18) . ? N204 C221 1.10(2) . ? C201 C202 1.54(3) . ? C202 C207 1.40(3) . ? C202 C203 1.48(4) . ? C203 F3 1.30(3) . ? C203 C204 1.39(4) . ? C204 F4 1.33(3) . ? C204 C205 1.38(3) . ? C205 C206 1.40(4) . ? C205 C208 1.50(4) . ? C206 F6 1.35(3) . ? C206 C207 1.43(4) . ? C207 F7 1.21(3) . ? C208 C213 1.35(4) . ? C208 C209 1.36(4) . ? C209 F9 1.25(4) . ? C209 C210 1.40(4) . ? C210 F10 1.34(4) . ? C210 C211 1.48(4) . ? C211 C212 1.38(3) . ? C211 C214 1.40(4) 1_554 ? C212 F12 1.14(3) . ? C212 C213 1.49(4) . ? C213 F13 1.45(4) . ? C214 C211 1.40(4) 1_556 ? C221 C222 1.45(3) . ? C222 C223 1.32(2) . ? C222 C227 1.41(3) . ? C223 F23 1.32(2) . ? C223 C224 1.39(3) . ? C224 F24 1.30(2) . ? C224 C225 1.42(3) . ? C225 C226 1.37(3) . ? C225 C228 1.55(3) . ? C226 F26 1.32(3) . ? C226 C227 1.32(3) . ? C227 F27 1.30(3) . ? C228 C229 1.37(3) . ? C228 C233 1.40(3) . ? C229 F29 1.34(3) . ? C229 C230 1.38(4) . ? C230 C231 1.32(3) . ? C230 F30 1.42(3) . ? C231 C232 1.37(3) . ? C231 C241 1.47(3) 1_556 ? C232 F32 1.27(3) . ? C232 C233 1.38(3) . ? C233 F33 1.33(3) . ? C241 C231 1.47(3) 1_554 ? C1S Cl1 1.61(3) . ? C1S Cl2 1.81(3) . ? C2S Cl3' 1.56(4) . ? C2S Cl4 1.70(4) . ? C2S Cl3 1.94(4) . ? C3S Cl6 1.81(4) . ? C3S Cl5 1.87(4) . ? C4S Cl7 1.82(4) . ? C4S Cl8 1.85(4) . ? C4S' Cl7' 1.82(4) . ? C4S' Cl8' 1.85(5) . ? C5S Cl10 1.49(6) . ? C5S Cl9 1.83(7) . ? C6S Cl11 1.5080 1_445 ? C6S Cl12 1.6606 . ? Cl11 C6S 1.51(5) 1_665 ? C7S Cl14 1.75(2) . ? C7S Cl13 1.76(2) . ? C8S Cl15 1.79(5) . ? C8S Cl16 1.82(7) . ? Cl15 C9S 1.79(10) . ? C9S Cl17 1.70(9) . ? C9S Cl18 1.73(11) . ? C10S Cl20 1.98(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh1 N1 92.9(6) . . Y N3 Rh1 O203 175.7(5) . . Y N1 Rh1 O203 88.3(5) . . Y N3 Rh1 O201 88.0(5) . . Y N1 Rh1 O201 174.3(5) . . Y O203 Rh1 O201 90.5(4) . . Y N3 Rh1 N201 96.6(6) . . Y N1 Rh1 N201 99.9(6) . . Y O203 Rh1 N201 87.2(6) . . Y O201 Rh1 N201 85.6(5) . . Y N3 Rh1 Rh2 87.7(4) . . Y N1 Rh1 Rh2 87.2(4) . . Y O203 Rh1 Rh2 88.3(3) . . Y O201 Rh1 Rh2 87.2(3) . . Y N201 Rh1 Rh2 171.5(5) . . Y N2 Rh2 N4 90.9(5) . . Y N2 Rh2 O204 90.6(5) . . Y N4 Rh2 O204 174.6(5) . . Y N2 Rh2 O202 177.1(5) . . Y N4 Rh2 O202 90.0(5) . . Y O204 Rh2 O202 88.2(4) . . Y N2 Rh2 N202 92.5(6) . . Y N4 Rh2 N202 101.6(6) . . Y O204 Rh2 N202 83.6(6) . . Y O202 Rh2 N202 90.0(6) . . Y N2 Rh2 Rh1 89.4(4) . . Y N4 Rh2 Rh1 87.7(4) . . Y O204 Rh2 Rh1 87.1(3) . . Y O202 Rh2 Rh1 87.9(3) . . Y N202 Rh2 Rh1 170.5(5) . . Y N5 Rh3 N7 89.9(5) . . Y N5 Rh3 O205 176.0(5) . . Y N7 Rh3 O205 89.7(5) . . Y N5 Rh3 O207 89.5(5) . . Y N7 Rh3 O207 175.9(5) . . Y O205 Rh3 O207 90.6(4) . . Y N5 Rh3 N203 100.0(5) . . Y N7 Rh3 N203 98.2(5) . . Y O205 Rh3 N203 84.0(5) . . Y O207 Rh3 N203 85.9(5) . . Y N5 Rh3 Rh4 89.1(4) . . Y N7 Rh3 Rh4 88.4(4) . . Y O205 Rh3 Rh4 86.9(3) . . Y O207 Rh3 Rh4 87.5(3) . . Y N203 Rh3 Rh4 168.7(3) . . Y N8 Rh4 N6 91.2(5) . . Y N8 Rh4 O208 175.5(5) . . Y N6 Rh4 O208 89.1(5) . . Y N8 Rh4 O206 88.8(5) . . Y N6 Rh4 O206 174.3(5) . . Y O208 Rh4 O206 90.4(4) . . Y N8 Rh4 N204 93.9(6) . . Y N6 Rh4 N204 97.4(6) . . Y O208 Rh4 N204 90.5(5) . . Y O206 Rh4 N204 88.3(5) . . Y N8 Rh4 Rh3 87.9(4) . . Y N6 Rh4 Rh3 86.3(4) . . Y O208 Rh4 Rh3 87.6(3) . . Y O206 Rh4 Rh3 88.0(3) . . Y N204 Rh4 Rh3 175.8(4) . . Y C1 N1 C11 117.9(15) . . ? C1 N1 Rh1 119.3(13) . . ? C11 N1 Rh1 122.4(11) . . ? C1 N2 C21 116.3(14) . . ? C1 N2 Rh2 117.9(12) . . ? C21 N2 Rh2 123.3(12) . . ? C2 N3 C31 115.9(16) . . ? C2 N3 Rh1 121.4(14) . . ? C31 N3 Rh1 119.3(13) . . ? C2 N4 C41 118.4(16) . . ? C2 N4 Rh2 121.3(14) . . ? C41 N4 Rh2 120.2(12) . . ? C3 N5 C51 115.3(15) . . ? C3 N5 Rh3 120.4(13) . . ? C51 N5 Rh3 124.2(11) . . ? C3 N6 C61 118.6(15) . . ? C3 N6 Rh4 121.2(12) . . ? C61 N6 Rh4 120.2(12) . . ? C4 N7 C71 116.8(15) . . ? C4 N7 Rh3 120.4(13) . . ? C71 N7 Rh3 122.7(11) . . ? C4 N8 C81 118.1(16) . . ? C4 N8 Rh4 121.7(13) . . ? C81 N8 Rh4 120.0(12) . . ? N1 C1 N2 124.4(17) . . ? N4 C2 N3 121.0(19) . . ? N6 C3 N5 123.0(17) . . ? N8 C4 N7 121.5(18) . . ? O204 C5 O203 122.3(16) . . ? O204 C5 C6 120.0(14) . . ? O203 C5 C6 117.7(15) . . ? O207 C6 O208 127.9(17) . . ? O207 C6 C5 117.8(15) . . ? O208 C6 C5 114.3(15) . . ? O201 C7 O202 127.6(15) . . ? O201 C7 C8 116.4(14) . 2_183 ? O202 C7 C8 115.9(15) . 2_183 ? O205 C8 O206 126.9(15) . . ? O205 C8 C7 116.0(13) . 2_183 ? O206 C8 C7 117.1(14) . 2_183 ? C7 O201 Rh1 118.0(10) . . ? C7 O202 Rh2 117.5(11) . . ? C5 O203 Rh1 120.4(11) . . ? C5 O204 Rh2 120.9(11) . . ? C8 O205 Rh3 120.3(10) . . ? C8 O206 Rh4 117.7(11) . . ? C6 O207 Rh3 119.2(11) . . ? C6 O208 Rh4 117.7(11) . . ? C17 O1 C14 118.0(15) . . ? C27 O2 C24 111(3) . . ? C47 O4 C44 105(3) . . ? C57 O5 C54 112.8(18) . . ? C67 O6 C64 107(2) . . ? C74 O7 C77 115.4(13) . . ? C16 C11 C12 118.0(18) . . ? C16 C11 N1 123.8(17) . . ? C12 C11 N1 118.1(16) . . ? C13 C12 C11 118.2(18) . . ? C12 C13 C14 120.4(18) . . ? C15 C14 O1 126.0(19) . . ? C15 C14 C13 119.9(19) . . ? O1 C14 C13 114.1(17) . . ? C14 C15 C16 119(2) . . ? C11 C16 C15 124(2) . . ? C26 C21 C22 120(2) . . ? C26 C21 N2 123.8(18) . . ? C22 C21 N2 115.7(16) . . ? C21 C22 C23 122(2) . . ? C24 C23 C22 112(2) . . ? C25 C24 C23 126(3) . . ? C25 C24 O2 127(2) . . ? C23 C24 O2 107(2) . . ? C24 C25 C26 117(2) . . ? C21 C26 C25 121(2) . . ? C32 C31 N3 126(2) . . ? C32 C31 C36 119(2) . . ? N3 C31 C36 114.9(18) . . ? C31 C32 C33 124(2) . . ? C34 C33 C32 118(3) . . ? C33 C34 C35 123(3) . . ? C33 C34 O3' 127(3) . . ? C35 C34 O3' 110(3) . . ? C33 C34 O3 104(4) . . ? C35 C34 O3 127(4) . . ? O3' C34 O3 36(3) . . ? C34 C35 C36 119(3) . . ? C31 C36 C35 116(2) . . ? C37 O3 C34 118(10) . . ? C37' O3' C34 101(5) . . ? C46 C41 C42 118(2) . . ? C46 C41 N4 121.6(19) . . ? C42 C41 N4 120.2(19) . . ? C41 C42 C43 123(2) . . ? C44 C43 C42 116(2) . . ? C43 C44 C45 128(3) . . ? C43 C44 O4 130(2) . . ? C45 C44 O4 102(2) . . ? C44 C45 C46 112(2) . . ? C41 C46 C45 121(2) . . ? C52 C51 C56 119.3(18) . . ? C52 C51 N5 122.3(16) . . ? C56 C51 N5 118.4(15) . . ? C51 C52 C53 120.9(19) . . ? C54 C53 C52 118(2) . . ? C53 C54 C55 123(2) . . ? C53 C54 O5 127(2) . . ? C55 C54 O5 110.2(19) . . ? C54 C55 C56 121(2) . . ? C51 C56 C55 118.5(17) . . ? C62 C61 C66 122(2) . . ? C62 C61 N6 120.2(17) . . ? C66 C61 N6 117.6(18) . . ? C61 C62 C63 123(2) . . ? C64 C63 C62 116(2) . . ? C63 C64 C65 125(2) . . ? C63 C64 O6 125(2) . . ? C65 C64 O6 110(2) . . ? C64 C65 C66 117(2) . . ? C61 C66 C65 117(2) . . ? C72 C71 C76 119.5(17) . . ? C72 C71 N7 120.1(14) . . ? C76 C71 N7 120.4(15) . . ? C71 C72 C73 120.5(16) . . ? C74 C73 C72 118.3(17) . . ? C73 C74 C75 122.0(18) . . ? C73 C74 O7 112.9(15) . . ? C75 C74 O7 125.1(16) . . ? C74 C75 C76 118.3(18) . . ? C71 C76 C75 121.2(17) . . ? C82 C81 C86 118(2) . . ? C82 C81 N8 120.5(18) . . ? C86 C81 N8 121.4(18) . . ? C81 C82 C83 122(2) . . ? C84 C83 C82 113(3) . . ? C83 C84 C85 129(3) . . ? C83 C84 O8 123(3) . . ? C85 C84 O8 108(3) . . ? C83 C84 O8' 91(3) . . ? C85 C84 O8' 140(3) . . ? O8 C84 O8' 32.3(17) . . ? C86 C85 C84 113(3) . . ? C81 C86 C85 124(2) . . ? C84 O8 C87 155(6) . . ? C87' O8' C84 76(8) . . ? C201 N201 Rh1 164(2) . . ? C214 N202 C215 55(2) . . ? C214 N202 Rh2 159(2) . . ? C215 N202 Rh2 132(2) . . ? C241 N203 Rh3 161.4(14) . . ? C221 N204 Rh4 166.0(17) . . ? N201 C201 C202 166(3) . . ? C207 C202 C203 118(3) . . ? C207 C202 C201 125(3) . . ? C203 C202 C201 117(2) . . ? F3 C203 C204 121(3) . . ? F3 C203 C202 122(3) . . ? C204 C203 C202 117(3) . . ? F4 C204 C205 119(3) . . ? F4 C204 C203 116(3) . . ? C205 C204 C203 125(4) . . ? C204 C205 C206 118(3) . . ? C204 C205 C208 126(3) . . ? C206 C205 C208 115(3) . . ? F6 C206 C205 120(3) . . ? F6 C206 C207 120(3) . . ? C205 C206 C207 120(3) . . ? F7 C207 C202 117(3) . . ? F7 C207 C206 121(3) . . ? C202 C207 C206 121(3) . . ? C213 C208 C209 120(4) . . ? C213 C208 C205 118(3) . . ? C209 C208 C205 122(3) . . ? F9 C209 C208 122(4) . . ? F9 C209 C210 119(4) . . ? C208 C209 C210 118(4) . . ? F10 C210 C209 117(4) . . ? F10 C210 C211 121(4) . . ? C209 C210 C211 122(4) . . ? C212 C211 C214 121(3) . 1_554 ? C212 C211 C210 122(3) . . ? C214 C211 C210 118(3) 1_554 . ? F12 C212 C211 125(3) . . ? F12 C212 C213 125(3) . . ? C211 C212 C213 110(3) . . ? C208 C213 F13 119(3) . . ? C208 C213 C212 127(4) . . ? F13 C213 C212 110(3) . . ? N202 C214 C211 174(4) . 1_556 ? N204 C221 C222 171(2) . . ? C223 C222 C227 119(2) . . ? C223 C222 C221 121(2) . . ? C227 C222 C221 119(2) . . ? C222 C223 F23 120(2) . . ? C222 C223 C224 124(2) . . ? F23 C223 C224 116.2(19) . . ? F24 C224 C223 122(2) . . ? F24 C224 C225 122(2) . . ? C223 C224 C225 115(2) . . ? C226 C225 C224 118(3) . . ? C226 C225 C228 127(2) . . ? C224 C225 C228 112(2) . . ? F26 C226 C227 120(3) . . ? F26 C226 C225 116(3) . . ? C227 C226 C225 123(3) . . ? F27 C227 C226 120(3) . . ? F27 C227 C222 120(2) . . ? C226 C227 C222 118(3) . . ? C229 C228 C233 117(3) . . ? C229 C228 C225 117(2) . . ? C233 C228 C225 124(2) . . ? F29 C229 C228 119(3) . . ? F29 C229 C230 123(3) . . ? C228 C229 C230 116(3) . . ? C231 C230 C229 125(3) . . ? C231 C230 F30 121(3) . . ? C229 C230 F30 114(3) . . ? C230 C231 C232 119(3) . . ? C230 C231 C241 120(2) . 1_556 ? C232 C231 C241 121(2) . 1_556 ? F32 C232 C231 121(2) . . ? F32 C232 C233 121(3) . . ? C231 C232 C233 118(3) . . ? F33 C233 C232 118(3) . . ? F33 C233 C228 119(3) . . ? C232 C233 C228 122(3) . . ? N203 C241 C231 177(2) . 1_554 ? Cl1 C1S Cl2 114(2) . . ? Cl3' C2S Cl4 128(3) . . ? Cl4 C2S Cl3 94.8(19) . . ? Cl6 C3S Cl5 105(2) . . ? Cl7 C4S Cl8 103(2) . . ? Cl7' C4S' Cl8' 103(3) . . ? Cl10 C5S Cl9 118(4) . . ? Cl11 C6S Cl12 122.3 1_445 . ? Cl14 C7S Cl13 99(5) . . ? Cl15 C8S Cl16 98(3) . . ? Cl15 C8S Cl19 109(2) . . ? Cl21 C9S Cl17 88(6) . . ? Cl21 C9S Cl18 157(8) . . ? Cl17 C9S Cl18 114(7) . . ? Cl21 C9S Cl15 123(8) . . ? Cl17 C9S Cl15 86(5) . . ? Cl17 C9S C10S 95(6) . . ? Cl18 C9S C10S 142(6) . . ? Cl15 C9S C10S 104(6) . . ? Cl21 C10S Cl19 129(10) . . ? Cl19 C10S C9S 121(6) . . ? Cl19 C10S Cl20 144(5) . . ? Cl21 C10S Cl16 111(9) . . ? Cl19 C10S Cl16 101(5) . . ? Cl20 C10S Cl16 108(4) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.64 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.137 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.157 #===END