# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_C46H60F9N6O9S3Cl6Rh _database_code_depnum_ccdc_archive 'CCDC 905662' #TrackingRef 'web_deposit_cif_file_0_MichalSabat_1349986668.Complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H54 N6 Rh, 3(C F3 O3 S), 3(C H2 Cl2)' _chemical_formula_sum 'C46 H60 Cl6 F9 N6 O9 Rh S3' _chemical_formula_weight 1423.79 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' S S 0.1246 0.1234 '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' 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 11.9286(4) _cell_length_b 13.9649(4) _cell_length_c 19.8273(6) _cell_angle_alpha 83.142(1) _cell_angle_beta 80.976(1) _cell_angle_gamma 67.371(1) _cell_volume 3004.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 31.41 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7667 _exptl_absorpt_correction_T_max 0.8544 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33458 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 32.18 _reflns_number_total 21018 _reflns_number_gt 14363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 17720 _refine_ls_number_parameters 735 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 1.352 _refine_ls_restrained_S_all 1.352 _refine_ls_shift/su_max 0.002 _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 Rh Rh 0.708050(19) 0.871075(16) 0.687891(10) 0.01623(8) Uani 1 1 d . . . Cl1 Cl 0.85125(15) 0.67726(13) 0.47748(10) 0.0785(5) Uani 1 1 d . . . Cl2 Cl 1.0268(2) 0.52507(16) 0.38370(12) 0.1085(8) Uani 1 1 d . . . Cl3 Cl 0.67577(19) 0.31259(11) 0.24157(9) 0.0790(5) Uani 1 1 d . . . Cl4 Cl 0.42436(18) 0.41242(11) 0.21309(8) 0.0732(4) Uani 1 1 d . . . Cl5 Cl 0.11706(15) 0.72861(11) 0.96128(7) 0.0631(4) Uani 1 1 d . . . Cl6 Cl -0.03792(16) 0.86654(13) 0.86196(8) 0.0774(4) Uani 1 1 d . . . S1 S 0.59206(7) 0.59189(6) 0.35755(4) 0.02428(16) Uani 1 1 d . . . S2 S 0.37130(7) 0.27683(6) 0.00424(4) 0.02340(15) Uani 1 1 d . . . S3 S 0.76623(9) 1.03261(7) 0.38098(4) 0.03150(18) Uani 1 1 d . . . F1 F 0.6404(3) 0.7506(2) 0.29635(17) 0.0624(8) Uani 1 1 d . . . F2 F 0.4500(3) 0.77879(19) 0.31636(12) 0.0543(7) Uani 1 1 d . . . F3 F 0.5608(3) 0.6843(2) 0.23440(12) 0.0592(8) Uani 1 1 d . . . F4 F 0.3439(3) 0.4524(2) 0.05301(14) 0.0515(7) Uani 1 1 d . . . F5 F 0.3995(3) 0.4457(2) -0.05562(13) 0.0528(7) Uani 1 1 d . . . F6 F 0.5287(3) 0.3628(2) 0.01427(14) 0.0543(7) Uani 1 1 d . . . F7 F 0.7247(3) 0.9834(2) 0.44223(13) 0.0541(7) Uani 1 1 d . . . F8 F 0.8866(3) 1.0337(3) 0.38084(16) 0.0707(9) Uani 1 1 d . . . F9 F 0.6729(4) 1.1254(2) 0.35612(19) 0.0797(11) Uani 1 1 d . . . O1 O 0.7136(2) 0.52503(19) 0.33150(12) 0.0322(5) Uani 1 1 d . . . O2 O 0.5847(3) 0.6346(2) 0.42162(12) 0.0360(6) Uani 1 1 d . . . O3 O 0.4963(3) 0.5557(2) 0.35187(17) 0.0441(7) Uani 1 1 d . . . O4 O 0.4109(3) 0.2190(2) 0.06695(12) 0.0374(6) Uani 1 1 d . . . O5 O 0.4394(2) 0.22805(19) -0.05796(12) 0.0312(5) Uani 1 1 d . . . O6 O 0.2402(2) 0.3230(2) 0.00428(13) 0.0338(5) Uani 1 1 d . . . O7 O 0.8762(3) 0.8498(2) 0.33244(17) 0.0486(8) Uani 1 1 d . . . O8 O 0.6880(3) 0.9287(2) 0.31105(14) 0.0390(6) Uani 1 1 d . . . O9 O 0.8292(3) 0.9759(3) 0.25553(12) 0.0432(7) Uani 1 1 d . . . N1 N 0.5643(2) 0.91272(18) 0.76283(12) 0.0184(4) Uani 1 1 d . . . N2 N 0.7469(2) 0.97454(19) 0.73151(12) 0.0184(4) Uani 1 1 d . . . N3 N 0.8636(2) 0.82903(18) 0.62110(11) 0.0174(4) Uani 1 1 d . . . N4 N 0.8173(2) 0.75189(19) 0.74346(12) 0.0183(4) Uani 1 1 d . . . N5 N 0.6061(2) 0.98717(19) 0.62517(12) 0.0197(5) Uani 1 1 d . . . N6 N 0.6598(2) 0.7681(2) 0.64694(12) 0.0222(5) Uani 1 1 d . . . C1 C 0.4769(3) 0.8732(2) 0.77601(15) 0.0221(5) Uani 1 1 d . . . H1 H 0.4777 0.8227 0.7476 0.026 Uiso 1 1 calc R . . C2 C 0.3854(3) 0.9041(2) 0.83010(15) 0.0224(6) Uani 1 1 d . . . H2 H 0.3258 0.8731 0.8391 0.027 Uiso 1 1 calc R . . C3 C 0.3794(3) 0.9799(2) 0.87144(14) 0.0189(5) Uani 1 1 d . . . C4 C 0.4696(3) 1.0221(2) 0.85648(14) 0.0195(5) Uani 1 1 d . . . H4 H 0.4680 1.0751 0.8830 0.023 Uiso 1 1 calc R . . C5 C 0.5622(3) 0.9866(2) 0.80264(13) 0.0171(5) Uani 1 1 d . . . C6 C 0.6633(2) 1.0237(2) 0.78391(13) 0.0170(5) Uani 1 1 d . . . C7 C 0.6750(3) 1.1027(2) 0.81481(14) 0.0188(5) Uani 1 1 d . . . H7A H 0.6162 1.1353 0.8515 0.023 Uiso 1 1 calc R . . C8 C 0.7722(3) 1.1346(2) 0.79241(14) 0.0195(5) Uani 1 1 d . . . C9 C 0.8590(3) 1.0815(2) 0.73929(15) 0.0230(6) Uani 1 1 d . . . H9A H 0.9281 1.0995 0.7234 0.028 Uiso 1 1 calc R . . C10 C 0.8432(3) 1.0034(2) 0.71065(15) 0.0221(5) Uani 1 1 d . . . H10 H 0.9023 0.9685 0.6748 0.026 Uiso 1 1 calc R . . C11 C 0.2772(3) 1.0194(2) 0.93035(15) 0.0224(6) Uani 1 1 d . . . C12 C 0.1931(4) 0.9582(3) 0.9419(2) 0.0363(8) Uani 1 1 d . . . H12A H 0.1522 0.9675 0.9011 0.054 Uiso 1 1 calc R . . H12B H 0.1316 0.9835 0.9813 0.054 Uiso 1 1 calc R . . H12C H 0.2416 0.8842 0.9508 0.054 Uiso 1 1 calc R . . C13 C 0.3339(3) 1.0109(3) 0.99648(16) 0.0293(7) Uani 1 1 d . . . H13A H 0.3854 0.9382 1.0069 0.044 Uiso 1 1 calc R . . H13B H 0.2685 1.0353 1.0343 0.044 Uiso 1 1 calc R . . H13C H 0.3838 1.0537 0.9903 0.044 Uiso 1 1 calc R . . C14 C 0.2030(3) 1.1346(3) 0.91084(18) 0.0294(7) Uani 1 1 d . . . H14A H 0.2558 1.1747 0.9069 0.044 Uiso 1 1 calc R . . H14B H 0.1339 1.1621 0.9463 0.044 Uiso 1 1 calc R . . H14C H 0.1724 1.1401 0.8669 0.044 Uiso 1 1 calc R . . C15 C 0.7880(3) 1.2246(2) 0.82193(17) 0.0256(6) Uani 1 1 d . . . C16 C 0.9083(4) 1.1813(4) 0.8538(2) 0.0410(9) Uani 1 1 d . . . H16A H 0.9201 1.2378 0.8730 0.061 Uiso 1 1 calc R . . H16B H 0.9766 1.1504 0.8186 0.061 Uiso 1 1 calc R . . H16C H 0.9051 1.1281 0.8903 0.061 Uiso 1 1 calc R . . C17 C 0.7962(4) 1.3047(3) 0.7631(2) 0.0418(9) Uani 1 1 d . . . H17A H 0.7200 1.3321 0.7420 0.063 Uiso 1 1 calc R . . H17B H 0.8650 1.2714 0.7288 0.063 Uiso 1 1 calc R . . H17C H 0.8087 1.3619 0.7810 0.063 Uiso 1 1 calc R . . C18 C 0.6846(4) 1.2754(3) 0.8766(2) 0.0416(9) Uani 1 1 d . . . H18A H 0.6070 1.3038 0.8569 0.062 Uiso 1 1 calc R . . H18B H 0.6990 1.3316 0.8944 0.062 Uiso 1 1 calc R . . H18C H 0.6808 1.2236 0.9139 0.062 Uiso 1 1 calc R . . C19 C 0.8787(3) 0.8763(2) 0.55903(14) 0.0215(5) Uani 1 1 d . . . H19 H 0.8115 0.9334 0.5434 0.026 Uiso 1 1 calc R . . C20 C 0.9884(3) 0.8443(2) 0.51755(14) 0.0234(6) Uani 1 1 d . . . H20 H 0.9956 0.8790 0.4738 0.028 Uiso 1 1 calc R . . C21 C 1.0889(3) 0.7615(2) 0.53921(14) 0.0217(5) Uani 1 1 d . . . C22 C 1.0715(3) 0.7126(2) 0.60383(14) 0.0210(5) Uani 1 1 d . . . H22 H 1.1375 0.6550 0.6202 0.025 Uiso 1 1 calc R . . C23 C 0.9594(3) 0.7473(2) 0.64396(13) 0.0180(5) Uani 1 1 d . . . C24 C 0.9318(3) 0.7013(2) 0.71223(13) 0.0181(5) Uani 1 1 d . . . C25 C 1.0111(3) 0.6119(2) 0.74266(14) 0.0210(5) Uani 1 1 d . . . H25 H 1.0914 0.5784 0.7204 0.025 Uiso 1 1 calc R . . C26 C 0.9741(3) 0.5699(2) 0.80624(14) 0.0213(5) Uani 1 1 d . . . C27 C 0.8579(3) 0.6252(3) 0.83716(15) 0.0252(6) Uani 1 1 d . . . H27 H 0.8298 0.6009 0.8808 0.030 Uiso 1 1 calc R . . C28 C 0.7817(3) 0.7160(2) 0.80525(14) 0.0232(6) Uani 1 1 d . . . H28 H 0.7029 0.7531 0.8278 0.028 Uiso 1 1 calc R . . C29 C 1.2092(3) 0.7233(3) 0.49297(16) 0.0273(6) Uani 1 1 d . . . C30 C 1.3142(6) 0.6622(11) 0.5309(4) 0.198(8) Uani 1 1 d . . . H30A H 1.3509 0.5912 0.5158 0.297 Uiso 1 1 calc R . . H30B H 1.2862 0.6603 0.5800 0.297 Uiso 1 1 calc R . . H30C H 1.3753 0.6946 0.5219 0.297 Uiso 1 1 calc R . . C31 C 1.2373(7) 0.8145(5) 0.4569(4) 0.097(3) Uani 1 1 d . . . H31A H 1.2330 0.8619 0.4908 0.145 Uiso 1 1 calc R . . H31B H 1.1774 0.8514 0.4248 0.145 Uiso 1 1 calc R . . H31C H 1.3197 0.7894 0.4318 0.145 Uiso 1 1 calc R . . C32 C 1.1963(8) 0.6655(9) 0.4398(6) 0.186(7) Uani 1 1 d . . . H32A H 1.2757 0.6338 0.4126 0.279 Uiso 1 1 calc R . . H32B H 1.1373 0.7130 0.4101 0.279 Uiso 1 1 calc R . . H32C H 1.1671 0.6110 0.4612 0.279 Uiso 1 1 calc R . . C33 C 1.0583(3) 0.4683(2) 0.83775(15) 0.0255(6) Uani 1 1 d . . . C34 C 1.1785(3) 0.4779(3) 0.84794(19) 0.0338(7) Uani 1 1 d . . . H34A H 1.2170 0.4973 0.8039 0.051 Uiso 1 1 calc R . . H34B H 1.2339 0.4111 0.8664 0.051 Uiso 1 1 calc R . . H34C H 1.1613 0.5315 0.8800 0.051 Uiso 1 1 calc R . . C35 C 1.0873(4) 0.3828(3) 0.78818(18) 0.0332(7) Uani 1 1 d . . . H35A H 1.0112 0.3763 0.7810 0.050 Uiso 1 1 calc R . . H35B H 1.1419 0.3165 0.8077 0.050 Uiso 1 1 calc R . . H35C H 1.1274 0.4011 0.7443 0.050 Uiso 1 1 calc R . . C36 C 0.9979(4) 0.4369(3) 0.90683(18) 0.0391(9) Uani 1 1 d . . . H36A H 0.9743 0.4928 0.9380 0.059 Uiso 1 1 calc R . . H36B H 1.0561 0.3731 0.9269 0.059 Uiso 1 1 calc R . . H36C H 0.9251 0.4250 0.8996 0.059 Uiso 1 1 calc R . . C37 C 0.5490(3) 1.0485(2) 0.58811(14) 0.0208(5) Uani 1 1 d . . . C38 C 0.4768(3) 1.1255(2) 0.54008(17) 0.0266(6) Uani 1 1 d . . . H38A H 0.5252 1.1211 0.4950 0.040 Uiso 1 1 calc R . . H38B H 0.4535 1.1951 0.5561 0.040 Uiso 1 1 calc R . . H38C H 0.4029 1.1124 0.5367 0.040 Uiso 1 1 calc R . . C39 C 0.6294(3) 0.7116(3) 0.62550(16) 0.0293(7) Uani 1 1 d . . . C40 C 0.5875(6) 0.6396(4) 0.5994(2) 0.0562(13) Uani 1 1 d . . . H40A H 0.6222 0.5708 0.6230 0.084 Uiso 1 1 calc R . . H40B H 0.6142 0.6348 0.5502 0.084 Uiso 1 1 calc R . . H40C H 0.4980 0.6648 0.6075 0.084 Uiso 1 1 calc R . . C41 C 0.5602(4) 0.7066(3) 0.29751(19) 0.0379(9) Uani 1 1 d . . . C42 C 0.4135(4) 0.3905(3) 0.00373(19) 0.0344(7) Uani 1 1 d . . . C43 C 0.7912(3) 0.9416(3) 0.31706(19) 0.0351(8) Uani 1 1 d . . . C44 C 0.8888(8) 0.5905(10) 0.4182(5) 0.151(5) Uani 1 1 d . . . H44A H 0.8540 0.5380 0.4383 0.181 Uiso 1 1 calc R . . H44B H 0.8421 0.6278 0.3797 0.181 Uiso 1 1 calc R . . C45 C 0.5689(7) 0.4238(4) 0.2076(3) 0.0694(17) Uani 1 1 d . . . H45A H 0.5980 0.4366 0.1590 0.083 Uiso 1 1 calc R . . H45B H 0.5601 0.4841 0.2326 0.083 Uiso 1 1 calc R . . C46 C -0.0018(5) 0.7499(4) 0.9128(3) 0.0556(12) Uani 1 1 d . . . H46A H -0.0755 0.7507 0.9441 0.067 Uiso 1 1 calc R . . H46B H 0.0219 0.6915 0.8830 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.01451(11) 0.01678(11) 0.01516(11) -0.00166(7) 0.00056(7) -0.00411(8) Cl1 0.0617(9) 0.0745(9) 0.1084(12) -0.0285(9) -0.0238(9) -0.0235(7) Cl2 0.1036(14) 0.0951(13) 0.1275(16) -0.0560(12) -0.0642(13) -0.0047(11) Cl3 0.1059(13) 0.0508(7) 0.0947(11) 0.0036(7) -0.0319(10) -0.0400(8) Cl4 0.1056(13) 0.0519(7) 0.0706(8) 0.0080(6) -0.0299(8) -0.0351(8) Cl5 0.0834(10) 0.0745(8) 0.0539(6) 0.0167(6) -0.0290(6) -0.0522(8) Cl6 0.0706(10) 0.0774(9) 0.0799(10) 0.0261(8) -0.0249(8) -0.0259(8) S1 0.0198(3) 0.0224(3) 0.0270(3) -0.0026(3) 0.0012(3) -0.0050(3) S2 0.0241(4) 0.0252(3) 0.0185(3) -0.0017(3) 0.0018(3) -0.0082(3) S3 0.0336(4) 0.0355(4) 0.0268(4) 0.0015(3) -0.0064(3) -0.0144(3) F1 0.068(2) 0.0420(14) 0.078(2) 0.0070(13) 0.0077(16) -0.0308(14) F2 0.0513(16) 0.0394(12) 0.0396(12) 0.0035(10) 0.0004(11) 0.0146(11) F3 0.072(2) 0.0549(15) 0.0258(11) -0.0008(10) -0.0059(11) 0.0025(14) F4 0.0578(17) 0.0492(14) 0.0523(14) -0.0286(12) 0.0186(12) -0.0276(13) F5 0.076(2) 0.0430(13) 0.0442(13) 0.0050(11) 0.0022(13) -0.0331(14) F6 0.0432(14) 0.0790(19) 0.0560(15) -0.0246(14) 0.0035(12) -0.0373(14) F7 0.0518(16) 0.0751(19) 0.0360(12) 0.0019(12) -0.0013(11) -0.0273(14) F8 0.068(2) 0.108(3) 0.0581(17) -0.0091(17) -0.0032(15) -0.058(2) F9 0.095(3) 0.0476(16) 0.081(2) 0.0029(16) -0.027(2) -0.0044(17) O1 0.0236(12) 0.0312(12) 0.0324(12) -0.0015(10) 0.0037(9) -0.0028(9) O2 0.0422(15) 0.0319(12) 0.0269(11) -0.0049(10) -0.0024(10) -0.0060(11) O3 0.0293(14) 0.0405(15) 0.0656(19) -0.0094(14) -0.0011(13) -0.0164(12) O4 0.0372(14) 0.0376(13) 0.0255(11) 0.0042(10) 0.0011(10) -0.0045(11) O5 0.0360(14) 0.0335(12) 0.0237(10) -0.0105(9) 0.0081(9) -0.0147(10) O6 0.0242(12) 0.0411(14) 0.0338(12) -0.0049(11) -0.0011(10) -0.0098(10) O7 0.0390(16) 0.0315(14) 0.0603(18) -0.0111(13) 0.0002(14) 0.0033(12) O8 0.0304(13) 0.0587(17) 0.0385(13) -0.0180(13) -0.0006(11) -0.0254(13) O9 0.0289(13) 0.079(2) 0.0186(10) -0.0082(12) 0.0023(9) -0.0176(13) N1 0.0159(11) 0.0181(10) 0.0194(10) -0.0015(8) 0.0006(8) -0.0053(8) N2 0.0139(10) 0.0237(11) 0.0156(10) -0.0005(8) 0.0027(8) -0.0067(9) N3 0.0162(11) 0.0173(10) 0.0144(9) -0.0001(8) 0.0019(8) -0.0032(8) N4 0.0164(11) 0.0198(10) 0.0163(10) 0.0000(8) 0.0011(8) -0.0055(9) N5 0.0168(11) 0.0194(11) 0.0206(10) -0.0020(9) -0.0014(9) -0.0044(9) N6 0.0232(12) 0.0217(11) 0.0194(11) -0.0035(9) -0.0007(9) -0.0060(9) C1 0.0188(13) 0.0216(13) 0.0262(13) -0.0043(11) -0.0007(11) -0.0080(10) C2 0.0185(13) 0.0238(13) 0.0261(13) -0.0018(11) 0.0019(11) -0.0111(11) C3 0.0149(12) 0.0217(12) 0.0190(11) -0.0002(10) 0.0010(10) -0.0071(10) C4 0.0186(13) 0.0218(12) 0.0184(11) -0.0028(10) 0.0015(10) -0.0088(10) C5 0.0166(12) 0.0189(12) 0.0160(11) -0.0012(9) -0.0003(9) -0.0074(10) C6 0.0137(11) 0.0195(12) 0.0167(11) -0.0004(9) 0.0000(9) -0.0060(9) C7 0.0162(12) 0.0204(12) 0.0189(11) -0.0027(10) 0.0008(10) -0.0066(10) C8 0.0172(12) 0.0235(13) 0.0194(12) -0.0017(10) -0.0009(10) -0.0096(10) C9 0.0167(13) 0.0304(15) 0.0236(13) -0.0045(11) 0.0046(10) -0.0124(11) C10 0.0181(13) 0.0276(14) 0.0209(12) -0.0037(11) 0.0034(10) -0.0105(11) C11 0.0165(13) 0.0262(14) 0.0239(13) -0.0047(11) 0.0063(10) -0.0096(11) C12 0.0294(17) 0.044(2) 0.0407(18) -0.0130(16) 0.0154(15) -0.0242(15) C13 0.0267(16) 0.0353(17) 0.0230(13) -0.0028(12) 0.0024(12) -0.0103(13) C14 0.0178(14) 0.0292(15) 0.0355(16) -0.0080(13) -0.0001(12) -0.0019(12) C15 0.0222(14) 0.0267(14) 0.0307(15) -0.0079(12) 0.0019(12) -0.0123(12) C16 0.035(2) 0.052(2) 0.044(2) -0.0171(18) -0.0055(16) -0.0199(17) C17 0.048(2) 0.0352(18) 0.048(2) -0.0016(17) -0.0012(18) -0.0238(17) C18 0.038(2) 0.044(2) 0.051(2) -0.0225(18) 0.0142(17) -0.0255(17) C19 0.0212(13) 0.0230(13) 0.0163(11) 0.0031(10) -0.0001(10) -0.0058(11) C20 0.0257(15) 0.0249(13) 0.0146(11) 0.0023(10) 0.0009(10) -0.0062(11) C21 0.0197(13) 0.0238(13) 0.0189(12) -0.0010(10) 0.0026(10) -0.0072(11) C22 0.0179(13) 0.0222(13) 0.0194(12) 0.0003(10) 0.0012(10) -0.0053(10) C23 0.0170(12) 0.0187(12) 0.0157(11) 0.0008(9) -0.0014(9) -0.0046(10) C24 0.0170(12) 0.0196(12) 0.0152(11) -0.0006(9) 0.0011(9) -0.0052(10) C25 0.0171(13) 0.0241(13) 0.0186(12) -0.0002(10) 0.0010(10) -0.0058(10) C26 0.0211(14) 0.0236(13) 0.0175(12) 0.0021(10) -0.0009(10) -0.0080(11) C27 0.0239(15) 0.0301(15) 0.0175(12) 0.0035(11) 0.0007(11) -0.0084(12) C28 0.0184(13) 0.0277(14) 0.0173(12) 0.0005(11) 0.0030(10) -0.0043(11) C29 0.0208(14) 0.0301(15) 0.0247(13) 0.0018(12) 0.0060(11) -0.0068(12) C30 0.026(3) 0.341(15) 0.080(4) 0.113(7) 0.027(3) 0.042(5) C31 0.075(4) 0.062(3) 0.129(6) -0.003(4) 0.071(4) -0.031(3) C32 0.109(6) 0.272(13) 0.245(12) -0.238(11) 0.142(8) -0.143(8) C33 0.0232(15) 0.0261(14) 0.0211(13) 0.0054(11) -0.0018(11) -0.0050(11) C34 0.0267(17) 0.0349(17) 0.0334(16) 0.0016(14) -0.0107(14) -0.0031(13) C35 0.040(2) 0.0254(15) 0.0312(16) 0.0022(13) -0.0024(14) -0.0109(14) C36 0.0350(19) 0.0377(18) 0.0296(16) 0.0121(14) 0.0021(14) -0.0038(15) C37 0.0188(13) 0.0212(12) 0.0207(12) -0.0026(10) 0.0024(10) -0.0071(10) C38 0.0224(14) 0.0245(14) 0.0287(14) 0.0031(12) -0.0057(12) -0.0044(11) C39 0.0393(19) 0.0266(15) 0.0239(14) -0.0026(12) -0.0040(13) -0.0141(13) C40 0.096(4) 0.061(3) 0.039(2) -0.008(2) -0.010(2) -0.058(3) C41 0.044(2) 0.0277(16) 0.0299(16) 0.0004(13) 0.0003(15) -0.0023(15) C42 0.0375(19) 0.0371(18) 0.0323(16) -0.0102(14) 0.0058(14) -0.0195(15) C43 0.0242(16) 0.045(2) 0.0341(17) -0.0072(15) 0.0022(13) -0.0122(15) C44 0.077(5) 0.271(14) 0.148(8) -0.147(9) 0.032(5) -0.092(7) C45 0.110(5) 0.049(3) 0.057(3) 0.010(2) -0.009(3) -0.043(3) C46 0.066(3) 0.050(3) 0.060(3) -0.003(2) -0.016(2) -0.028(2) _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 Rh N2 1.998(3) . ? Rh N4 2.006(2) . ? Rh N3 2.029(2) . ? Rh N6 2.030(3) . ? Rh N1 2.031(2) . ? Rh N5 2.032(2) . ? Cl1 C44 1.675(7) . ? Cl2 C44 1.628(8) . ? Cl3 C45 1.729(6) . ? Cl4 C45 1.778(7) . ? Cl5 C46 1.748(5) . ? Cl6 C46 1.749(5) . ? S1 O3 1.439(3) . ? S1 O1 1.442(2) . ? S1 O2 1.443(3) . ? S1 C41 1.829(4) . ? S2 O4 1.440(3) . ? S2 O6 1.444(3) . ? S2 O5 1.451(2) . ? S2 C42 1.840(4) . ? S3 F7 1.438(3) . ? S3 F9 1.439(3) . ? S3 F8 1.441(3) . ? S3 C43 1.813(4) . ? F1 C41 1.318(6) . ? F2 C41 1.342(4) . ? F3 C41 1.323(4) . ? F4 C42 1.336(4) . ? F5 C42 1.324(5) . ? F6 C42 1.320(5) . ? O7 C43 1.330(5) . ? O8 C43 1.335(5) . ? O9 C43 1.334(5) . ? N1 C1 1.335(4) . ? N1 C5 1.363(4) . ? N2 C10 1.349(4) . ? N2 C6 1.365(3) . ? N3 C19 1.346(3) . ? N3 C23 1.359(3) . ? N4 C28 1.337(4) . ? N4 C24 1.358(4) . ? N5 C37 1.138(4) . ? N6 C39 1.133(4) . ? C1 C2 1.382(4) . ? C2 C3 1.388(4) . ? C3 C4 1.393(4) . ? C3 C11 1.531(4) . ? C4 C5 1.393(4) . ? C5 C6 1.468(4) . ? C6 C7 1.386(4) . ? C7 C8 1.389(4) . ? C8 C9 1.409(4) . ? C8 C15 1.532(4) . ? C9 C10 1.373(4) . ? C11 C12 1.526(5) . ? C11 C13 1.539(4) . ? C11 C14 1.544(4) . ? C15 C18 1.514(5) . ? C15 C16 1.533(5) . ? C15 C17 1.536(5) . ? C19 C20 1.374(4) . ? C20 C21 1.391(4) . ? C21 C22 1.403(4) . ? C21 C29 1.516(4) . ? C22 C23 1.385(4) . ? C23 C24 1.473(4) . ? C24 C25 1.381(4) . ? C25 C26 1.405(4) . ? C26 C27 1.384(4) . ? C26 C33 1.517(4) . ? C27 C28 1.391(4) . ? C29 C32 1.461(7) . ? C29 C30 1.478(7) . ? C29 C31 1.510(6) . ? C33 C34 1.537(5) . ? C33 C35 1.538(5) . ? C33 C36 1.541(5) . ? C37 C38 1.451(4) . ? C39 C40 1.456(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 N2 Rh N4 92.08(10) . . ? N2 Rh N3 94.81(10) . . ? N4 Rh N3 80.25(9) . . ? N2 Rh N6 176.90(10) . . ? N4 Rh N6 88.55(10) . . ? N3 Rh N6 88.29(10) . . ? N2 Rh N1 80.46(10) . . ? N4 Rh N1 95.45(9) . . ? N3 Rh N1 173.54(10) . . ? N6 Rh N1 96.46(10) . . ? N2 Rh N5 89.81(10) . . ? N4 Rh N5 175.65(9) . . ? N3 Rh N5 95.69(9) . . ? N6 Rh N5 89.78(10) . . ? N1 Rh N5 88.73(10) . . ? O3 S1 O1 115.33(17) . . ? O3 S1 O2 115.67(19) . . ? O1 S1 O2 114.33(16) . . ? O3 S1 C41 103.2(2) . . ? O1 S1 C41 103.32(17) . . ? O2 S1 C41 102.39(17) . . ? O4 S2 O6 114.59(16) . . ? O4 S2 O5 115.22(15) . . ? O6 S2 O5 115.19(15) . . ? O4 S2 C42 102.90(18) . . ? O6 S2 C42 102.89(17) . . ? O5 S2 C42 103.58(16) . . ? F7 S3 F9 113.8(2) . . ? F7 S3 F8 113.66(19) . . ? F9 S3 F8 118.2(2) . . ? F7 S3 C43 102.73(18) . . ? F9 S3 C43 102.94(19) . . ? F8 S3 C43 102.75(19) . . ? C1 N1 C5 119.5(2) . . ? C1 N1 Rh 125.9(2) . . ? C5 N1 Rh 114.55(19) . . ? C10 N2 C6 118.6(3) . . ? C10 N2 Rh 125.48(19) . . ? C6 N2 Rh 115.79(19) . . ? C19 N3 C23 119.4(2) . . ? C19 N3 Rh 125.71(19) . . ? C23 N3 Rh 114.87(18) . . ? C28 N4 C24 119.5(2) . . ? C28 N4 Rh 124.5(2) . . ? C24 N4 Rh 115.76(18) . . ? C37 N5 Rh 176.6(2) . . ? C39 N6 Rh 177.7(3) . . ? N1 C1 C2 121.4(3) . . ? C1 C2 C3 120.8(3) . . ? C2 C3 C4 117.3(3) . . ? C2 C3 C11 122.7(3) . . ? C4 C3 C11 119.9(3) . . ? C5 C4 C3 120.0(3) . . ? N1 C5 C4 120.9(3) . . ? N1 C5 C6 114.8(2) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C7 121.3(3) . . ? N2 C6 C5 114.3(2) . . ? C7 C6 C5 124.4(2) . . ? C6 C7 C8 120.4(2) . . ? C7 C8 C9 117.5(3) . . ? C7 C8 C15 123.3(3) . . ? C9 C8 C15 119.2(3) . . ? C10 C9 C8 119.7(3) . . ? N2 C10 C9 122.5(3) . . ? C12 C11 C3 112.0(3) . . ? C12 C11 C13 109.2(3) . . ? C3 C11 C13 109.4(3) . . ? C12 C11 C14 109.7(3) . . ? C3 C11 C14 106.8(2) . . ? C13 C11 C14 109.8(3) . . ? C18 C15 C8 112.3(3) . . ? C18 C15 C16 108.5(3) . . ? C8 C15 C16 108.2(3) . . ? C18 C15 C17 110.3(3) . . ? C8 C15 C17 108.5(3) . . ? C16 C15 C17 108.9(3) . . ? N3 C19 C20 122.0(3) . . ? C19 C20 C21 120.4(3) . . ? C20 C21 C22 117.0(3) . . ? C20 C21 C29 120.9(3) . . ? C22 C21 C29 122.1(3) . . ? C23 C22 C21 120.7(3) . . ? N3 C23 C22 120.5(2) . . ? N3 C23 C24 114.6(2) . . ? C22 C23 C24 124.9(2) . . ? N4 C24 C25 121.0(2) . . ? N4 C24 C23 114.4(2) . . ? C25 C24 C23 124.5(2) . . ? C24 C25 C26 120.6(3) . . ? C27 C26 C25 116.6(3) . . ? C27 C26 C33 122.7(3) . . ? C25 C26 C33 120.7(3) . . ? C26 C27 C28 120.9(3) . . ? N4 C28 C27 121.3(3) . . ? C32 C29 C30 112.5(8) . . ? C32 C29 C31 106.7(7) . . ? C30 C29 C31 106.0(7) . . ? C32 C29 C21 108.5(4) . . ? C30 C29 C21 112.9(3) . . ? C31 C29 C21 110.2(3) . . ? C26 C33 C34 109.9(3) . . ? C26 C33 C35 108.4(3) . . ? C34 C33 C35 108.7(3) . . ? C26 C33 C36 111.6(3) . . ? C34 C33 C36 109.6(3) . . ? C35 C33 C36 108.7(3) . . ? N5 C37 C38 179.1(3) . . ? N6 C39 C40 178.5(4) . . ? F1 C41 F3 108.3(4) . . ? F1 C41 F2 106.5(3) . . ? F3 C41 F2 107.6(3) . . ? F1 C41 S1 111.4(3) . . ? F3 C41 S1 112.2(3) . . ? F2 C41 S1 110.6(3) . . ? F6 C42 F5 107.6(3) . . ? F6 C42 F4 107.5(3) . . ? F5 C42 F4 108.1(3) . . ? F6 C42 S2 111.6(3) . . ? F5 C42 S2 111.2(3) . . ? F4 C42 S2 110.6(3) . . ? O7 C43 O9 107.4(3) . . ? O7 C43 O8 109.2(4) . . ? O9 C43 O8 106.7(3) . . ? O7 C43 S3 111.0(3) . . ? O9 C43 S3 111.1(3) . . ? O8 C43 S3 111.3(3) . . ? Cl2 C44 Cl1 125.9(5) . . ? Cl3 C45 Cl4 111.3(3) . . ? Cl5 C46 Cl6 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 32.18 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.466 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.131 data_C52H65Cl6F9N7O9S3Rh _database_code_depnum_ccdc_archive 'CCDC 905663' #TrackingRef 'web_deposit_cif_file_1_MichalSabat_1349986668.Complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H59 N7 Rh, 3(C F3 O3 S), 3(C H2 Cl2)' _chemical_formula_sum 'C52 H65 Cl6 F9 N7 O9 Rh S3' _chemical_formula_weight 1514.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 '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' 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 13.0509(4) _cell_length_b 16.0965(5) _cell_length_c 17.8206(6) _cell_angle_alpha 69.599(1) _cell_angle_beta 87.830(1) _cell_angle_gamma 72.066(1) _cell_volume 3328.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6776 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 19.91 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7891 _exptl_absorpt_correction_T_max 0.8446 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19105 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.93 _reflns_number_total 12055 _reflns_number_gt 4681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 6047 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2201 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.672 _refine_ls_restrained_S_all 1.672 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Rh Rh 0.51479(6) 0.74969(5) 0.73173(4) 0.0264(4) Uani 1 1 d . . . Cl1 Cl 0.6158(4) 0.8823(3) 0.0755(2) 0.0949(14) Uani 1 1 d . . . Cl2 Cl 0.4633(3) 0.8456(2) -0.01130(18) 0.0667(10) Uani 1 1 d . . . Cl3 Cl 0.3259(7) 0.3358(5) 0.7237(4) 0.255(5) Uani 1 1 d . . . Cl4 Cl 0.2975(3) 0.4336(3) 0.5565(3) 0.0865(12) Uani 1 1 d . . . Cl5 Cl 0.7579(6) 0.7602(4) 0.9342(3) 0.134(2) Uani 1 1 d . . . Cl6 Cl 0.9571(4) 0.7334(4) 1.0206(4) 0.1327(19) Uani 1 1 d . . . S1 S 0.0088(2) 0.7862(2) 0.70459(17) 0.0399(8) Uani 1 1 d . . . S2 S 0.3714(3) 0.1114(2) 0.5927(2) 0.0656(11) Uani 1 1 d . . . S3 S 0.6042(3) 0.4050(2) 0.80837(19) 0.0519(9) Uani 1 1 d . . . F1 F -0.1007(7) 0.9507(5) 0.6028(4) 0.090(3) Uani 1 1 d . . . F2 F 0.0713(7) 0.9227(6) 0.6092(5) 0.105(3) Uani 1 1 d . . . F3 F -0.0019(7) 0.8599(7) 0.5481(4) 0.105(3) Uani 1 1 d . . . F4 F 0.1728(6) 0.2046(6) 0.5452(5) 0.085(2) Uani 1 1 d . . . F5 F 0.2069(7) 0.0562(6) 0.5867(5) 0.094(3) Uani 1 1 d . . . F6 F 0.2571(9) 0.1292(6) 0.4701(5) 0.107(3) Uani 1 1 d . . . F7 F 0.7944(6) 0.3705(5) 0.8755(6) 0.092(3) Uani 1 1 d . . . F8 F 0.6988(8) 0.2919(6) 0.9488(7) 0.127(4) Uani 1 1 d . . . F9 F 0.7726(7) 0.2571(6) 0.8498(9) 0.145(5) Uani 1 1 d . . . O1 O -0.0741(6) 0.7494(6) 0.6959(5) 0.062(2) Uani 1 1 d . . . O2 O 0.1180(6) 0.7293(5) 0.7051(5) 0.054(2) Uani 1 1 d . . . O3 O -0.0083(6) 0.8297(6) 0.7640(4) 0.052(2) Uani 1 1 d . . . O4 O 0.3395(8) 0.1164(6) 0.6742(4) 0.076(3) Uani 1 1 d . . . O5 O 0.4053(6) 0.1880(4) 0.5455(4) 0.0407(19) Uani 1 1 d . . . O6 O 0.4390(6) 0.0202(5) 0.5958(4) 0.049(2) Uani 1 1 d . . . O7 O 0.6447(9) 0.4417(7) 0.7328(5) 0.089(3) Uani 1 1 d . . . O8 O 0.5595(6) 0.4729(5) 0.8445(4) 0.051(2) Uani 1 1 d . . . O9 O 0.5411(7) 0.3465(6) 0.8109(7) 0.089(3) Uani 1 1 d . . . N1 N 0.4516(6) 0.8304(5) 0.6196(4) 0.027(2) Uani 1 1 d . . . N2 N 0.4485(7) 0.6567(5) 0.7227(5) 0.033(2) Uani 1 1 d . . . N3 N 0.3786(6) 0.7289(5) 0.5877(4) 0.029(2) Uani 1 1 d . . . N4 N 0.5851(7) 0.6637(5) 0.8440(4) 0.026(2) Uani 1 1 d . . . N5 N 0.6553(7) 0.6724(5) 0.7040(5) 0.031(2) Uani 1 1 d . . . N6 N 0.3846(6) 0.8288(5) 0.7689(4) 0.025(2) Uani 1 1 d . . . N7 N 0.5764(6) 0.8472(5) 0.7429(4) 0.024(2) Uani 1 1 d . . . C1 C 0.3968(8) 0.8133(7) 0.5711(6) 0.029(3) Uani 1 1 d . . . C2 C 0.4012(9) 0.6542(7) 0.6619(6) 0.034(3) Uani 1 1 d . . . C3 C 0.3473(9) 0.8887(7) 0.4916(6) 0.039(3) Uani 1 1 d . . . H3A H 0.3713 0.9430 0.4840 0.059 Uiso 1 1 calc R . . H3B H 0.2684 0.9072 0.4914 0.059 Uiso 1 1 calc R . . H3C H 0.3702 0.8650 0.4480 0.059 Uiso 1 1 calc R . . C4 C 0.3677(10) 0.5734(7) 0.6666(6) 0.045(3) Uani 1 1 d . . . H4A H 0.3942 0.5235 0.7187 0.067 Uiso 1 1 calc R . . H4B H 0.3978 0.5508 0.6235 0.067 Uiso 1 1 calc R . . H4C H 0.2886 0.5920 0.6607 0.067 Uiso 1 1 calc R . . C5 C 0.3368(9) 0.7107(7) 0.5212(6) 0.030(3) Uani 1 1 d . . . C6 C 0.2270(10) 0.7312(7) 0.5075(6) 0.044(3) Uani 1 1 d . . . H6 H 0.1776 0.7585 0.5393 0.052 Uiso 1 1 calc R . . C7 C 0.1903(11) 0.7104(9) 0.4451(8) 0.059(4) Uani 1 1 d . . . H7 H 0.1151 0.7246 0.4335 0.071 Uiso 1 1 calc R . . C8 C 0.2645(14) 0.6690(9) 0.4005(7) 0.061(4) Uani 1 1 d . . . H8 H 0.2397 0.6546 0.3585 0.073 Uiso 1 1 calc R . . C9 C 0.3705(13) 0.6494(8) 0.4159(7) 0.056(4) Uani 1 1 d . . . H9 H 0.4203 0.6202 0.3854 0.068 Uiso 1 1 calc R . . C10 C 0.4081(10) 0.6712(7) 0.4759(6) 0.039(3) Uani 1 1 d . . . H10 H 0.4834 0.6588 0.4855 0.047 Uiso 1 1 calc R . . C11 C 0.5374(8) 0.6584(7) 0.9138(6) 0.028(2) Uani 1 1 d . . . H11 H 0.4643 0.6953 0.9119 0.033 Uiso 1 1 calc R . . C12 C 0.5920(8) 0.6010(7) 0.9872(6) 0.031(3) Uani 1 1 d . . . H12 H 0.5562 0.5979 1.0350 0.037 Uiso 1 1 calc R . . C13 C 0.7003(8) 0.5470(7) 0.9913(5) 0.029(3) Uani 1 1 d . . . C14 C 0.7445(9) 0.5521(7) 0.9185(6) 0.033(3) Uani 1 1 d . . . H14 H 0.8168 0.5149 0.9184 0.040 Uiso 1 1 calc R . . C15 C 0.6870(8) 0.6090(6) 0.8470(5) 0.023(2) Uani 1 1 d . . . C16 C 0.7275(9) 0.6134(7) 0.7672(6) 0.028(3) Uani 1 1 d . . . C17 C 0.8274(9) 0.5611(7) 0.7561(6) 0.033(3) Uani 1 1 d . . . H17 H 0.8770 0.5212 0.8013 0.039 Uiso 1 1 calc R . . C18 C 0.8576(9) 0.5656(8) 0.6787(7) 0.040(3) Uani 1 1 d . . . C19 C 0.7810(10) 0.6238(8) 0.6167(6) 0.042(3) Uani 1 1 d . . . H19 H 0.7969 0.6278 0.5633 0.050 Uiso 1 1 calc R . . C20 C 0.6816(10) 0.6767(7) 0.6299(6) 0.036(3) Uani 1 1 d . . . H20 H 0.6309 0.7170 0.5855 0.043 Uiso 1 1 calc R . . C21 C 0.7625(9) 0.4844(8) 1.0719(6) 0.041(3) Uani 1 1 d . . . C22 C 0.7216(13) 0.4029(9) 1.1054(8) 0.093(6) Uani 1 1 d . . . H22A H 0.6428 0.4251 1.1056 0.139 Uiso 1 1 calc R . . H22B H 0.7535 0.3661 1.1605 0.139 Uiso 1 1 calc R . . H22C H 0.7417 0.3638 1.0723 0.139 Uiso 1 1 calc R . . C23 C 0.7393(10) 0.5392(11) 1.1312(7) 0.075(4) Uani 1 1 d . . . H23A H 0.6620 0.5565 1.1394 0.113 Uiso 1 1 calc R . . H23B H 0.7607 0.5957 1.1086 0.113 Uiso 1 1 calc R . . H23C H 0.7808 0.4996 1.1828 0.113 Uiso 1 1 calc R . . C24 C 0.8833(9) 0.4576(9) 1.0662(7) 0.061(4) Uani 1 1 d . . . H24A H 0.9196 0.4107 1.1175 0.091 Uiso 1 1 calc R . . H24B H 0.9064 0.5131 1.0541 0.091 Uiso 1 1 calc R . . H24C H 0.9022 0.4318 1.0234 0.091 Uiso 1 1 calc R . . C25 C 0.9687(9) 0.5081(9) 0.6647(7) 0.055(3) Uani 1 1 d . . . C26 C 1.0451(13) 0.475(3) 0.7343(14) 0.28(2) Uani 1 1 d . . . H26A H 1.0445 0.4131 0.7697 0.414 Uiso 1 1 calc R . . H26B H 1.0244 0.5186 0.7635 0.414 Uiso 1 1 calc R . . H26C H 1.1178 0.4714 0.7165 0.414 Uiso 1 1 calc R . . C27 C 0.9601(12) 0.4388(11) 0.6324(12) 0.108(6) Uani 1 1 d . . . H27A H 1.0290 0.4134 0.6120 0.162 Uiso 1 1 calc R . . H27B H 0.9029 0.4681 0.5886 0.162 Uiso 1 1 calc R . . H27C H 0.9426 0.3882 0.6749 0.162 Uiso 1 1 calc R . . C28 C 1.0199(19) 0.5747(17) 0.6013(19) 0.228(17) Uani 1 1 d . . . H28A H 0.9892 0.6380 0.6023 0.342 Uiso 1 1 calc R . . H28B H 1.0045 0.5749 0.5478 0.342 Uiso 1 1 calc R . . H28C H 1.0982 0.5532 0.6138 0.342 Uiso 1 1 calc R . . C29 C 0.2848(9) 0.8199(7) 0.7730(5) 0.034(3) Uani 1 1 d . . . H29 H 0.2709 0.7738 0.7568 0.041 Uiso 1 1 calc R . . C30 C 0.2032(8) 0.8770(8) 0.8005(6) 0.037(3) Uani 1 1 d . . . H30 H 0.1341 0.8684 0.8039 0.045 Uiso 1 1 calc R . . C31 C 0.2180(8) 0.9458(7) 0.8232(6) 0.034(3) Uani 1 1 d . . . C32 C 0.3203(8) 0.9552(7) 0.8167(6) 0.031(3) Uani 1 1 d . . . H32 H 0.3348 1.0019 0.8316 0.037 Uiso 1 1 calc R . . C33 C 0.4014(8) 0.8975(6) 0.7887(5) 0.024(2) Uani 1 1 d . . . C34 C 0.5115(8) 0.9066(6) 0.7751(5) 0.024(2) Uani 1 1 d . . . C35 C 0.5432(8) 0.9739(6) 0.7893(5) 0.027(2) Uani 1 1 d . . . H35 H 0.4974 1.0124 0.8150 0.032 Uiso 1 1 calc R . . C36 C 0.6438(8) 0.9861(7) 0.7658(5) 0.027(2) Uani 1 1 d . . . C37 C 0.7079(9) 0.9249(7) 0.7328(6) 0.035(3) Uani 1 1 d . . . H37 H 0.7769 0.9295 0.7169 0.042 Uiso 1 1 calc R . . C38 C 0.6730(8) 0.8570(7) 0.7226(5) 0.032(3) Uani 1 1 d . . . H38 H 0.7195 0.8151 0.7002 0.039 Uiso 1 1 calc R . . C39 C 0.1268(9) 1.0107(9) 0.8518(8) 0.052(3) Uani 1 1 d . . . C40 C 0.0416(12) 0.9648(12) 0.8891(10) 0.094(5) Uani 1 1 d . . . H40A H 0.0750 0.9089 0.9360 0.142 Uiso 1 1 calc R . . H40B H 0.0114 0.9473 0.8496 0.142 Uiso 1 1 calc R . . H40C H -0.0162 1.0089 0.9058 0.142 Uiso 1 1 calc R . . C41 C 0.0654(17) 1.0901(14) 0.7761(15) 0.198(14) Uani 1 1 d . . . H41A H -0.0043 1.1244 0.7898 0.297 Uiso 1 1 calc R . . H41B H 0.0533 1.0641 0.7363 0.297 Uiso 1 1 calc R . . H41C H 0.1079 1.1326 0.7538 0.297 Uiso 1 1 calc R . . C42 C 0.1653(19) 1.042(3) 0.911(3) 0.32(3) Uani 1 1 d . . . H42A H 0.1339 1.0194 0.9621 0.483 Uiso 1 1 calc R . . H42B H 0.1433 1.1102 0.8911 0.483 Uiso 1 1 calc R . . H42C H 0.2443 1.0165 0.9192 0.483 Uiso 1 1 calc R . . C43 C 0.6766(8) 1.0632(7) 0.7790(6) 0.036(3) Uani 1 1 d . . . C44 C 0.7799(9) 1.0721(8) 0.7384(7) 0.055(3) Uani 1 1 d . . . H44A H 0.8375 1.0121 0.7593 0.082 Uiso 1 1 calc R . . H44B H 0.8017 1.1199 0.7496 0.082 Uiso 1 1 calc R . . H44C H 0.7668 1.0899 0.6803 0.082 Uiso 1 1 calc R . . C45 C 0.6942(11) 1.0408(8) 0.8679(6) 0.057(4) Uani 1 1 d . . . H45A H 0.6263 1.0396 0.8930 0.086 Uiso 1 1 calc R . . H45B H 0.7187 1.0886 0.8769 0.086 Uiso 1 1 calc R . . H45C H 0.7491 0.9796 0.8918 0.086 Uiso 1 1 calc R . . C46 C 0.5848(9) 1.1557(7) 0.7422(7) 0.048(3) Uani 1 1 d . . . H46A H 0.5732 1.1697 0.6845 0.072 Uiso 1 1 calc R . . H46B H 0.6042 1.2061 0.7507 0.072 Uiso 1 1 calc R . . H46C H 0.5183 1.1503 0.7680 0.072 Uiso 1 1 calc R . . C47 C -0.0059(11) 0.8857(10) 0.6108(9) 0.067(4) Uani 1 1 d . . . C48 C 0.2457(14) 0.1251(11) 0.5504(12) 0.089(5) Uani 1 1 d . . . C49 C 0.7231(12) 0.3282(10) 0.8732(12) 0.080(5) Uani 1 1 d . . . C50 C 0.5586(10) 0.7982(9) 0.0725(7) 0.060(4) Uani 1 1 d . . . H50A H 0.5226 0.7776 0.1225 0.071 Uiso 1 1 calc R . . H50B H 0.6160 0.7431 0.0688 0.071 Uiso 1 1 calc R . . C51 C 0.3273(18) 0.3336(12) 0.6400(11) 0.132(8) Uani 1 1 d . . . H51A H 0.2765 0.3003 0.6362 0.158 Uiso 1 1 calc R . . H51B H 0.4004 0.2940 0.6353 0.158 Uiso 1 1 calc R . . C52 C 0.8700(16) 0.7502(19) 0.9297(10) 0.230(18) Uani 1 1 d . . . H52A H 0.8762 0.8062 0.8859 0.277 Uiso 1 1 calc R . . H52B H 0.9034 0.6962 0.9126 0.277 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0388(6) 0.0210(5) 0.0192(5) -0.0059(4) 0.0013(4) -0.0104(4) Cl1 0.133(4) 0.111(3) 0.086(3) -0.049(2) 0.027(3) -0.085(3) Cl2 0.086(3) 0.062(2) 0.047(2) -0.0196(16) -0.0027(18) -0.0159(19) Cl3 0.289(9) 0.220(7) 0.110(4) -0.106(5) -0.111(5) 0.189(7) Cl4 0.060(2) 0.071(3) 0.138(4) -0.063(3) -0.005(2) -0.002(2) Cl5 0.226(7) 0.153(5) 0.069(3) -0.022(3) 0.017(3) -0.144(5) Cl6 0.111(4) 0.127(4) 0.163(5) -0.080(4) 0.005(3) -0.008(3) S1 0.0340(19) 0.0443(18) 0.0430(18) -0.0154(14) 0.0007(14) -0.0142(16) S2 0.064(2) 0.033(2) 0.088(3) -0.0041(18) -0.012(2) -0.0174(18) S3 0.059(2) 0.0372(19) 0.070(2) -0.0273(17) 0.0211(18) -0.0217(17) F1 0.075(6) 0.078(6) 0.063(5) 0.000(4) 0.018(4) 0.018(5) F2 0.086(6) 0.099(7) 0.105(7) 0.008(5) 0.029(5) -0.050(6) F3 0.082(6) 0.148(8) 0.037(5) -0.025(5) 0.003(4) 0.020(6) F4 0.069(5) 0.077(6) 0.096(6) -0.017(5) -0.006(5) -0.018(5) F5 0.099(6) 0.078(6) 0.105(6) -0.005(5) -0.003(5) -0.059(5) F6 0.174(10) 0.089(6) 0.060(6) -0.017(5) -0.023(6) -0.053(6) F7 0.060(5) 0.061(5) 0.162(8) -0.042(5) -0.003(5) -0.024(4) F8 0.105(8) 0.069(6) 0.144(9) 0.036(6) -0.030(7) -0.019(6) F9 0.070(6) 0.074(6) 0.313(16) -0.113(9) -0.003(8) 0.000(5) O1 0.046(5) 0.065(6) 0.095(7) -0.043(5) 0.004(5) -0.027(5) O2 0.032(5) 0.059(5) 0.064(5) -0.021(4) -0.007(4) -0.003(4) O3 0.049(5) 0.077(6) 0.046(5) -0.029(4) 0.010(4) -0.032(5) O4 0.148(9) 0.075(6) 0.009(4) -0.020(4) 0.028(5) -0.040(6) O5 0.064(5) 0.025(4) 0.035(4) -0.007(3) 0.011(4) -0.022(4) O6 0.079(6) 0.023(4) 0.040(4) -0.008(3) -0.009(4) -0.012(4) O7 0.121(9) 0.125(9) 0.066(6) -0.062(6) 0.053(6) -0.071(8) O8 0.072(6) 0.039(5) 0.036(4) -0.014(4) 0.003(4) -0.006(4) O9 0.069(6) 0.040(5) 0.160(10) -0.027(6) 0.000(6) -0.030(5) N1 0.033(5) 0.032(5) 0.016(5) -0.008(4) 0.000(4) -0.011(4) N2 0.045(6) 0.026(5) 0.029(5) -0.010(4) 0.000(4) -0.013(4) N3 0.043(5) 0.025(5) 0.019(5) -0.009(4) -0.005(4) -0.008(4) N4 0.037(6) 0.018(5) 0.020(5) -0.003(4) 0.003(4) -0.011(5) N5 0.039(5) 0.027(5) 0.026(6) -0.007(4) 0.006(5) -0.011(4) N6 0.028(6) 0.021(5) 0.025(5) -0.006(4) -0.002(4) -0.011(4) N7 0.029(5) 0.024(5) 0.019(4) -0.007(4) 0.001(4) -0.007(4) C1 0.036(6) 0.026(7) 0.021(6) -0.009(5) 0.002(5) -0.003(5) C2 0.051(7) 0.024(6) 0.028(7) -0.010(6) 0.003(6) -0.011(5) C3 0.063(8) 0.025(6) 0.026(6) -0.002(5) -0.004(6) -0.016(6) C4 0.077(9) 0.028(6) 0.032(6) -0.006(5) -0.008(6) -0.023(6) C5 0.037(8) 0.024(6) 0.029(6) -0.009(5) 0.002(6) -0.012(5) C6 0.048(9) 0.039(7) 0.042(7) -0.012(6) 0.005(6) -0.015(6) C7 0.061(9) 0.066(9) 0.048(8) 0.003(7) -0.022(8) -0.043(8) C8 0.094(12) 0.077(10) 0.035(8) -0.025(7) 0.010(8) -0.054(9) C9 0.090(12) 0.054(8) 0.044(8) -0.027(6) 0.018(7) -0.039(8) C10 0.055(8) 0.036(7) 0.031(6) -0.013(5) 0.010(6) -0.020(6) C11 0.031(6) 0.029(6) 0.023(7) -0.006(5) 0.012(6) -0.015(5) C12 0.036(7) 0.033(6) 0.021(6) -0.004(5) 0.001(5) -0.011(6) C13 0.037(7) 0.032(6) 0.016(6) -0.004(5) 0.002(5) -0.014(6) C14 0.039(7) 0.029(6) 0.029(7) -0.011(5) 0.003(6) -0.005(5) C15 0.023(7) 0.022(6) 0.025(7) -0.008(5) 0.003(5) -0.006(5) C16 0.043(8) 0.021(6) 0.024(7) -0.009(5) 0.000(6) -0.015(6) C17 0.035(7) 0.031(6) 0.030(7) -0.009(5) 0.003(5) -0.011(6) C18 0.047(8) 0.053(8) 0.036(8) -0.028(6) 0.015(7) -0.027(7) C19 0.075(9) 0.040(7) 0.021(7) -0.013(6) 0.023(7) -0.030(7) C20 0.063(9) 0.031(6) 0.016(7) -0.011(5) 0.020(6) -0.017(6) C21 0.040(7) 0.048(7) 0.025(6) -0.008(5) 0.003(5) -0.006(6) C22 0.124(14) 0.057(9) 0.070(10) 0.033(8) -0.045(9) -0.049(10) C23 0.050(8) 0.115(12) 0.036(7) -0.024(8) -0.008(6) 0.005(8) C24 0.043(8) 0.077(9) 0.034(7) -0.001(6) -0.005(6) -0.002(7) C25 0.042(8) 0.092(10) 0.053(8) -0.053(7) 0.020(7) -0.024(7) C26 0.033(10) 0.62(6) 0.18(2) -0.29(3) -0.024(13) 0.07(2) C27 0.066(11) 0.090(12) 0.185(18) -0.099(13) -0.019(11) 0.014(9) C28 0.18(2) 0.18(2) 0.43(5) -0.20(3) 0.25(3) -0.13(2) C29 0.044(8) 0.035(7) 0.022(6) 0.000(5) -0.012(5) -0.022(6) C30 0.017(6) 0.048(7) 0.043(7) -0.016(6) 0.004(5) -0.005(6) C31 0.036(7) 0.036(7) 0.037(6) -0.018(5) -0.001(5) -0.015(6) C32 0.030(7) 0.031(6) 0.034(6) -0.016(5) -0.004(5) -0.008(6) C33 0.032(7) 0.016(6) 0.016(5) 0.006(4) -0.006(5) -0.008(5) C34 0.029(6) 0.023(6) 0.017(5) -0.006(5) 0.004(5) -0.008(5) C35 0.033(7) 0.021(6) 0.022(5) -0.007(4) -0.002(5) -0.002(5) C36 0.028(6) 0.024(6) 0.028(6) -0.008(5) 0.003(5) -0.006(5) C37 0.032(7) 0.030(7) 0.048(7) -0.013(6) 0.003(6) -0.017(6) C38 0.027(7) 0.033(7) 0.026(6) -0.005(5) 0.011(5) -0.002(5) C39 0.032(7) 0.062(9) 0.077(9) -0.038(7) 0.019(7) -0.022(7) C40 0.072(10) 0.124(14) 0.120(13) -0.080(11) 0.063(10) -0.040(10) C41 0.125(18) 0.101(16) 0.24(3) 0.007(17) 0.09(2) 0.051(14) C42 0.069(16) 0.50(6) 0.56(7) -0.40(6) 0.08(3) -0.08(3) C43 0.030(6) 0.033(7) 0.045(7) -0.017(5) 0.002(5) -0.009(6) C44 0.049(8) 0.054(8) 0.078(9) -0.029(7) 0.015(7) -0.032(7) C45 0.084(10) 0.058(8) 0.044(8) -0.018(6) -0.004(7) -0.041(8) C46 0.052(8) 0.038(7) 0.063(8) -0.017(6) 0.001(6) -0.026(6) C47 0.037(9) 0.082(11) 0.062(10) -0.021(8) 0.009(7) 0.006(9) C48 0.088(13) 0.045(10) 0.127(16) -0.025(9) 0.002(11) -0.015(10) C49 0.055(10) 0.041(9) 0.133(15) -0.029(10) -0.001(10) -0.003(8) C50 0.071(9) 0.058(8) 0.051(8) -0.009(6) -0.006(7) -0.033(7) C51 0.21(2) 0.104(15) 0.148(17) -0.105(14) 0.114(16) -0.083(15) C52 0.106(16) 0.12(3) 0.055(11) 0.023(14) 0.017(11) 0.040(19) _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 Rh N2 1.999(8) . ? Rh N1 2.005(7) . ? Rh N5 2.027(8) . ? Rh N6 2.029(8) . ? Rh N7 2.039(7) . ? Rh N4 2.047(7) . ? Cl1 C50 1.753(11) . ? Cl2 C50 1.767(11) . ? Cl3 C51 1.504(17) . ? Cl4 C51 1.715(19) . ? Cl5 C52 1.42(2) . ? Cl6 C52 1.91(2) . ? S1 O1 1.421(7) . ? S1 O2 1.436(8) . ? S1 O3 1.438(8) . ? S1 C47 1.834(14) . ? S2 O5 1.416(7) . ? S2 O6 1.444(8) . ? S2 O4 1.518(8) . ? S2 C48 1.751(17) . ? S3 O9 1.417(8) . ? S3 O8 1.421(8) . ? S3 O7 1.423(9) . ? S3 C49 1.797(15) . ? F1 C47 1.326(14) . ? F2 C47 1.314(15) . ? F3 C47 1.315(16) . ? F4 C48 1.314(16) . ? F5 C48 1.314(16) . ? F6 C48 1.413(19) . ? F7 C49 1.321(16) . ? F8 C49 1.338(19) . ? F9 C49 1.325(17) . ? N1 C1 1.292(12) . ? N2 C2 1.285(12) . ? N3 C1 1.379(12) . ? N3 C2 1.408(12) . ? N3 C5 1.474(12) . ? N4 C15 1.341(12) . ? N4 C11 1.356(12) . ? N5 C20 1.335(12) . ? N5 C16 1.357(12) . ? N6 C33 1.349(11) . ? N6 C29 1.350(12) . ? N7 C38 1.339(12) . ? N7 C34 1.344(12) . ? C1 C3 1.512(13) . ? C2 C4 1.471(13) . ? C5 C10 1.364(14) . ? C5 C6 1.378(15) . ? C6 C7 1.407(16) . ? C7 C8 1.388(18) . ? C8 C9 1.337(18) . ? C9 C10 1.386(15) . ? C11 C12 1.377(13) . ? C12 C13 1.403(14) . ? C13 C14 1.385(13) . ? C13 C21 1.521(14) . ? C14 C15 1.365(13) . ? C15 C16 1.484(14) . ? C16 C17 1.367(14) . ? C17 C18 1.403(14) . ? C18 C19 1.373(15) . ? C18 C25 1.527(16) . ? C19 C20 1.379(15) . ? C21 C22 1.492(16) . ? C21 C24 1.510(15) . ? C21 C23 1.564(17) . ? C25 C27 1.455(17) . ? C25 C26 1.46(2) . ? C25 C28 1.55(2) . ? C29 C30 1.376(15) . ? C30 C31 1.370(14) . ? C31 C32 1.386(14) . ? C31 C39 1.526(16) . ? C32 C33 1.383(14) . ? C33 C34 1.491(13) . ? C34 C35 1.372(13) . ? C35 C36 1.414(13) . ? C36 C37 1.368(14) . ? C36 C43 1.523(14) . ? C37 C38 1.374(13) . ? C39 C42 1.48(3) . ? C39 C40 1.527(17) . ? C39 C41 1.53(2) . ? C43 C45 1.508(15) . ? C43 C44 1.527(15) . ? C43 C46 1.538(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh N1 87.7(3) . . ? N2 Rh N5 87.6(3) . . ? N1 Rh N5 98.1(3) . . ? N2 Rh N6 97.5(3) . . ? N1 Rh N6 86.5(3) . . ? N5 Rh N6 173.3(3) . . ? N2 Rh N7 177.5(3) . . ? N1 Rh N7 92.4(3) . . ? N5 Rh N7 94.9(3) . . ? N6 Rh N7 80.0(3) . . ? N2 Rh N4 91.9(3) . . ? N1 Rh N4 177.3(3) . . ? N5 Rh N4 79.2(3) . . ? N6 Rh N4 96.2(3) . . ? N7 Rh N4 88.2(3) . . ? O1 S1 O2 116.7(5) . . ? O1 S1 O3 114.0(5) . . ? O2 S1 O3 114.6(4) . . ? O1 S1 C47 104.5(6) . . ? O2 S1 C47 102.0(6) . . ? O3 S1 C47 102.4(6) . . ? O5 S2 O6 116.2(5) . . ? O5 S2 O4 112.4(5) . . ? O6 S2 O4 113.9(5) . . ? O5 S2 C48 107.9(6) . . ? O6 S2 C48 104.8(6) . . ? O4 S2 C48 99.8(8) . . ? O9 S3 O8 114.7(6) . . ? O9 S3 O7 115.3(6) . . ? O8 S3 O7 113.1(5) . . ? O9 S3 C49 104.3(6) . . ? O8 S3 C49 103.5(6) . . ? O7 S3 C49 104.0(8) . . ? C1 N1 Rh 128.8(7) . . ? C2 N2 Rh 130.5(6) . . ? C1 N3 C2 126.6(8) . . ? C1 N3 C5 118.2(7) . . ? C2 N3 C5 115.1(8) . . ? C15 N4 C11 118.8(8) . . ? C15 N4 Rh 115.7(6) . . ? C11 N4 Rh 125.5(7) . . ? C20 N5 C16 119.0(9) . . ? C20 N5 Rh 125.4(7) . . ? C16 N5 Rh 115.7(7) . . ? C33 N6 C29 118.8(9) . . ? C33 N6 Rh 115.3(6) . . ? C29 N6 Rh 125.9(7) . . ? C38 N7 C34 118.0(8) . . ? C38 N7 Rh 127.2(7) . . ? C34 N7 Rh 114.8(6) . . ? N1 C1 N3 123.8(8) . . ? N1 C1 C3 119.7(9) . . ? N3 C1 C3 116.6(8) . . ? N2 C2 N3 121.7(9) . . ? N2 C2 C4 121.6(8) . . ? N3 C2 C4 116.7(9) . . ? C10 C5 C6 121.2(10) . . ? C10 C5 N3 119.0(9) . . ? C6 C5 N3 119.7(10) . . ? C5 C6 C7 118.1(11) . . ? C8 C7 C6 119.6(11) . . ? C9 C8 C7 120.7(12) . . ? C8 C9 C10 120.6(12) . . ? C5 C10 C9 119.8(11) . . ? N4 C11 C12 121.8(9) . . ? C11 C12 C13 120.0(9) . . ? C14 C13 C12 116.2(9) . . ? C14 C13 C21 123.0(9) . . ? C12 C13 C21 120.8(9) . . ? C15 C14 C13 121.8(10) . . ? N4 C15 C14 121.3(9) . . ? N4 C15 C16 114.3(8) . . ? C14 C15 C16 124.3(9) . . ? N5 C16 C17 121.3(9) . . ? N5 C16 C15 114.4(9) . . ? C17 C16 C15 124.2(9) . . ? C16 C17 C18 120.8(10) . . ? C19 C18 C17 116.1(10) . . ? C19 C18 C25 122.1(10) . . ? C17 C18 C25 121.8(10) . . ? C18 C19 C20 121.6(10) . . ? N5 C20 C19 121.2(10) . . ? C22 C21 C24 113.8(11) . . ? C22 C21 C13 108.2(9) . . ? C24 C21 C13 112.4(8) . . ? C22 C21 C23 107.8(11) . . ? C24 C21 C23 105.2(9) . . ? C13 C21 C23 109.2(9) . . ? C27 C25 C26 116.9(18) . . ? C27 C25 C18 111.1(10) . . ? C26 C25 C18 111.4(10) . . ? C27 C25 C28 107.4(14) . . ? C26 C25 C28 100.8(19) . . ? C18 C25 C28 108.5(12) . . ? N6 C29 C30 120.5(9) . . ? C31 C30 C29 122.3(10) . . ? C30 C31 C32 116.3(10) . . ? C30 C31 C39 122.4(10) . . ? C32 C31 C39 121.3(9) . . ? C33 C32 C31 120.7(9) . . ? N6 C33 C32 121.3(9) . . ? N6 C33 C34 114.5(9) . . ? C32 C33 C34 124.2(9) . . ? N7 C34 C35 121.7(9) . . ? N7 C34 C33 114.9(8) . . ? C35 C34 C33 123.3(9) . . ? C34 C35 C36 120.3(9) . . ? C37 C36 C35 116.6(9) . . ? C37 C36 C43 123.5(9) . . ? C35 C36 C43 119.9(9) . . ? C36 C37 C38 120.3(10) . . ? N7 C38 C37 123.0(10) . . ? C42 C39 C31 112.9(13) . . ? C42 C39 C40 108.0(18) . . ? C31 C39 C40 111.7(10) . . ? C42 C39 C41 114(2) . . ? C31 C39 C41 106.4(12) . . ? C40 C39 C41 103.0(13) . . ? C45 C43 C36 109.0(8) . . ? C45 C43 C44 109.9(9) . . ? C36 C43 C44 110.6(9) . . ? C45 C43 C46 109.8(9) . . ? C36 C43 C46 108.4(8) . . ? C44 C43 C46 109.2(9) . . ? F2 C47 F3 108.6(12) . . ? F2 C47 F1 109.0(13) . . ? F3 C47 F1 106.7(11) . . ? F2 C47 S1 110.5(9) . . ? F3 C47 S1 111.0(11) . . ? F1 C47 S1 110.9(9) . . ? F4 C48 F5 109.2(14) . . ? F4 C48 F6 104.8(13) . . ? F5 C48 F6 106.8(12) . . ? F4 C48 S2 112.8(11) . . ? F5 C48 S2 114.2(11) . . ? F6 C48 S2 108.5(12) . . ? F7 C49 F9 107.2(12) . . ? F7 C49 F8 106.9(14) . . ? F9 C49 F8 106.9(13) . . ? F7 C49 S3 112.8(10) . . ? F9 C49 S3 111.3(12) . . ? F8 C49 S3 111.4(11) . . ? Cl1 C50 Cl2 109.9(6) . . ? Cl3 C51 Cl4 122.2(10) . . ? Cl5 C52 Cl6 121.1(11) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.93 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.230 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.111