# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_global data_1 #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H120 F12 N12 O18 Rh4 S4' _chemical_formula_weight 2569.98 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.7946(17) _cell_length_b 14.4951(11) _cell_length_c 17.2969(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.2030(10) _cell_angle_gamma 90.00 _cell_volume 5455.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.80 _exptl_crystal_description sheet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7256 _exptl_absorpt_correction_T_max 0.9209 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.38 _diffrn_reflns_number 39843 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 27.82 _reflns_number_total 12847 _reflns_number_gt 10235 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+14.9130P] 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 12847 _refine_ls_number_parameters 709 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.074 _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 Rh1 Rh 0.264740(14) 0.35547(2) 0.268407(18) 0.02192(9) Uani 1 1 d . . . Rh2 Rh 0.296530(14) 0.68945(2) 0.112429(18) 0.02194(9) Uani 1 1 d . . . N1 N 0.24177(16) 0.5003(2) 0.2779(2) 0.0247(7) Uani 1 1 d . . . N2 N 0.30673(15) 0.4092(2) 0.1675(2) 0.0237(7) Uani 1 1 d . . . N3 N 0.31898(15) 0.5446(2) 0.1035(2) 0.0244(7) Uani 1 1 d . . . N4 N 0.25575(16) 0.6368(2) 0.2158(2) 0.0247(7) Uani 1 1 d . . . N5 N 0.18127(16) 0.3470(2) 0.1970(2) 0.0261(7) Uani 1 1 d . . . N6 N -0.20943(16) 0.3440(2) -0.0556(2) 0.0261(7) Uani 1 1 d . . . O1 O 0.1702(2) -0.0223(3) 0.2547(3) 0.0688(13) Uani 1 1 d . . . O2 O 0.0622(3) -0.0116(5) 0.2651(4) 0.112(3) Uani 1 1 d . . . O3 O 0.1065(3) -0.1119(3) 0.1706(4) 0.094(2) Uani 1 1 d . . . O4 O 0.4353(3) 0.0453(4) 0.2240(3) 0.0803(16) Uani 1 1 d . . . O5 O 0.3813(2) 0.0412(5) 0.1000(3) 0.094(2) Uani 1 1 d . . . O6 O 0.4630(3) -0.0697(4) 0.1298(4) 0.095(2) Uani 1 1 d . . . S1 S 0.10959(7) -0.03129(10) 0.21869(11) 0.0539(4) Uani 1 1 d . . . S2 S 0.43638(8) 0.01863(13) 0.14305(10) 0.0595(4) Uani 1 1 d . . . F1 F 0.1117(3) 0.1419(3) 0.1829(4) 0.1061(19) Uani 1 1 d . . . F2 F 0.1473(3) 0.0607(5) 0.0994(4) 0.141(3) Uani 1 1 d . . . F3 F 0.0496(3) 0.0681(4) 0.1137(3) 0.1098(19) Uani 1 1 d . . . F4 F 0.54601(19) 0.0883(3) 0.1394(3) 0.0871(14) Uani 1 1 d . . . F5 F 0.4962(3) 0.0939(4) 0.0315(3) 0.1001(18) Uani 1 1 d . . . F6 F 0.4756(2) 0.1864(3) 0.1220(3) 0.0842(14) Uani 1 1 d . . . C1 C 0.20559(19) 0.5668(3) 0.3119(2) 0.0258(8) Uani 1 1 d . . . C2 C 0.1632(2) 0.5606(3) 0.3696(3) 0.0339(10) Uani 1 1 d . . . H2 H 0.1570 0.5054 0.3955 0.041 Uiso 1 1 calc R . . C3 C 0.1310(3) 0.6391(4) 0.3867(3) 0.0430(12) Uani 1 1 d . . . H3 H 0.1024 0.6364 0.4245 0.052 Uiso 1 1 calc R . . C4 C 0.1402(2) 0.7221(4) 0.3488(3) 0.0419(12) Uani 1 1 d . . . H4 H 0.1176 0.7735 0.3624 0.050 Uiso 1 1 calc R . . C5 C 0.1817(2) 0.7310(3) 0.2918(3) 0.0334(10) Uani 1 1 d . . . H5 H 0.1877 0.7870 0.2671 0.040 Uiso 1 1 calc R . . C6 C 0.2144(2) 0.6516(3) 0.2728(2) 0.0266(8) Uani 1 1 d . . . C7 C 0.26829(18) 0.5470(3) 0.2231(2) 0.0232(8) Uani 1 1 d . . . C8 C 0.30058(18) 0.5006(3) 0.1654(2) 0.0224(8) Uani 1 1 d . . . C9 C 0.33334(18) 0.3895(3) 0.0986(3) 0.0253(8) Uani 1 1 d . . . C10 C 0.3524(2) 0.3060(3) 0.0670(3) 0.0324(10) Uani 1 1 d . . . H10 H 0.3480 0.2505 0.0931 0.039 Uiso 1 1 calc R . . C11 C 0.3778(2) 0.3091(3) -0.0037(3) 0.0376(11) Uani 1 1 d . . . H11 H 0.3918 0.2547 -0.0253 0.045 Uiso 1 1 calc R . . C12 C 0.3833(2) 0.3918(4) -0.0442(3) 0.0374(11) Uani 1 1 d . . . H12 H 0.3999 0.3907 -0.0926 0.045 Uiso 1 1 calc R . . C13 C 0.3648(2) 0.4747(3) -0.0147(3) 0.0318(9) Uani 1 1 d . . . H13 H 0.3687 0.5293 -0.0422 0.038 Uiso 1 1 calc R . . C14 C 0.33991(18) 0.4740(3) 0.0580(2) 0.0263(8) Uani 1 1 d . . . C15 C 0.0177(2) 0.3490(4) 0.0498(3) 0.0368(11) Uani 1 1 d . . . H15 H 0.0191 0.3145 0.0046 0.044 Uiso 1 1 calc R . . C16 C -0.0349(2) 0.3923(3) 0.0630(3) 0.0330(10) Uani 1 1 d . . . H16 H -0.0346 0.4329 0.1047 0.040 Uiso 1 1 calc R . . C17 C 0.18100(19) 0.3169(3) 0.1237(3) 0.0314(10) Uani 1 1 d . . . H17 H 0.2174 0.2951 0.1050 0.038 Uiso 1 1 calc R . . C18 C 0.1282(2) 0.3171(4) 0.0748(3) 0.0335(10) Uani 1 1 d . . . H18 H 0.1293 0.2942 0.0247 0.040 Uiso 1 1 calc R . . C19 C 0.0734(2) 0.3518(3) 0.1013(3) 0.0299(9) Uani 1 1 d . . . C20 C 0.0746(2) 0.3819(4) 0.1779(3) 0.0358(10) Uani 1 1 d . . . H20 H 0.0391 0.4051 0.1984 0.043 Uiso 1 1 calc R . . C21 C 0.1287(2) 0.3769(4) 0.2231(3) 0.0340(10) Uani 1 1 d . . . H21 H 0.1283 0.3954 0.2746 0.041 Uiso 1 1 calc R . . C22 C -0.2024(2) 0.4046(3) 0.0029(3) 0.0304(9) Uani 1 1 d . . . H22 H -0.2370 0.4345 0.0194 0.036 Uiso 1 1 calc R . . C23 C -0.1459(2) 0.4249(3) 0.0399(3) 0.0348(10) Uani 1 1 d . . . H23 H -0.1432 0.4678 0.0799 0.042 Uiso 1 1 calc R . . C24 C -0.0932(2) 0.3809(3) 0.0170(3) 0.0294(9) Uani 1 1 d . . . C25 C -0.0999(2) 0.3192(4) -0.0457(3) 0.0362(11) Uani 1 1 d . . . H25 H -0.0659 0.2894 -0.0642 0.043 Uiso 1 1 calc R . . C26 C -0.1585(2) 0.3035(4) -0.0795(3) 0.0332(10) Uani 1 1 d . . . H26 H -0.1625 0.2627 -0.1210 0.040 Uiso 1 1 calc R . . C27 C 0.2964(2) 0.2186(3) 0.2942(3) 0.0294(9) Uani 1 1 d . . . C28 C 0.3469(2) 0.2826(3) 0.3094(3) 0.0319(10) Uani 1 1 d . . . C29 C 0.3281(2) 0.3464(3) 0.3662(3) 0.0361(11) Uani 1 1 d . . . C30 C 0.2685(2) 0.3187(3) 0.3887(3) 0.0309(9) Uani 1 1 d . . . C31 C 0.2500(2) 0.2401(3) 0.3458(3) 0.0319(9) Uani 1 1 d . . . C32 C 0.2968(3) 0.1362(4) 0.2424(4) 0.0487(14) Uani 1 1 d . . . H32A H 0.3135 0.0843 0.2709 0.073 Uiso 1 1 calc R . . H32B H 0.3217 0.1488 0.1995 0.073 Uiso 1 1 calc R . . H32C H 0.2556 0.1225 0.2234 0.073 Uiso 1 1 calc R . . C33 C 0.4069(2) 0.2807(4) 0.2735(4) 0.0480(13) Uani 1 1 d . . . H33A H 0.4217 0.3426 0.2680 0.072 Uiso 1 1 calc R . . H33B H 0.4022 0.2522 0.2234 0.072 Uiso 1 1 calc R . . H33C H 0.4359 0.2460 0.3057 0.072 Uiso 1 1 calc R . . C34 C 0.3651(3) 0.4251(4) 0.4002(4) 0.0592(18) Uani 1 1 d . . . H34A H 0.4039 0.4278 0.3767 0.089 Uiso 1 1 calc R . . H34B H 0.3719 0.4161 0.4550 0.089 Uiso 1 1 calc R . . H34C H 0.3432 0.4818 0.3907 0.089 Uiso 1 1 calc R . . C35 C 0.2351(3) 0.3605(4) 0.4553(3) 0.0496(14) Uani 1 1 d . . . H35A H 0.1918 0.3489 0.4476 0.074 Uiso 1 1 calc R . . H35B H 0.2422 0.4259 0.4570 0.074 Uiso 1 1 calc R . . H35C H 0.2502 0.3332 0.5032 0.074 Uiso 1 1 calc R . . C36 C 0.1931(3) 0.1863(4) 0.3550(4) 0.0502(14) Uani 1 1 d . . . H36A H 0.2020 0.1348 0.3887 0.075 Uiso 1 1 calc R . . H36B H 0.1776 0.1643 0.3054 0.075 Uiso 1 1 calc R . . H36C H 0.1628 0.2249 0.3770 0.075 Uiso 1 1 calc R . . C37 C 0.37789(19) 0.7584(3) 0.1558(3) 0.0317(10) Uani 1 1 d . . . C38 C 0.3843(2) 0.7406(3) 0.0750(3) 0.0373(11) Uani 1 1 d . . . C39 C 0.3338(2) 0.7843(4) 0.0329(3) 0.0385(11) Uani 1 1 d . . . C40 C 0.2996(2) 0.8349(3) 0.0865(3) 0.0346(10) Uani 1 1 d . . . C41 C 0.3268(2) 0.8203(3) 0.1620(3) 0.0307(9) Uani 1 1 d . . . C42 C 0.4197(3) 0.7281(4) 0.2213(4) 0.0501(14) Uani 1 1 d . . . H42A H 0.4500 0.7750 0.2327 0.075 Uiso 1 1 calc R . . H42B H 0.4397 0.6719 0.2077 0.075 Uiso 1 1 calc R . . H42C H 0.3964 0.7178 0.2660 0.075 Uiso 1 1 calc R . . C43 C 0.4351(3) 0.6873(4) 0.0428(5) 0.0622(19) Uani 1 1 d . . . H43A H 0.4242 0.6712 -0.0100 0.093 Uiso 1 1 calc R . . H43B H 0.4422 0.6321 0.0727 0.093 Uiso 1 1 calc R . . H43C H 0.4718 0.7241 0.0450 0.093 Uiso 1 1 calc R . . C44 C 0.3244(4) 0.7849(5) -0.0537(3) 0.066(2) Uani 1 1 d . . . H44A H 0.2812 0.7859 -0.0679 0.099 Uiso 1 1 calc R . . H44B H 0.3425 0.7306 -0.0745 0.099 Uiso 1 1 calc R . . H44C H 0.3435 0.8387 -0.0740 0.099 Uiso 1 1 calc R . . C45 C 0.2471(3) 0.8991(4) 0.0682(4) 0.0551(16) Uani 1 1 d . . . H45A H 0.2186 0.8958 0.1085 0.083 Uiso 1 1 calc R . . H45B H 0.2266 0.8817 0.0198 0.083 Uiso 1 1 calc R . . H45C H 0.2622 0.9611 0.0646 0.083 Uiso 1 1 calc R . . C46 C 0.3084(3) 0.8632(4) 0.2360(3) 0.0463(13) Uani 1 1 d . . . H46A H 0.3358 0.9133 0.2498 0.069 Uiso 1 1 calc R . . H46B H 0.3106 0.8178 0.2765 0.069 Uiso 1 1 calc R . . H46C H 0.2672 0.8861 0.2293 0.069 Uiso 1 1 calc R . . C47 C 0.1032(3) 0.0595(5) 0.1459(5) 0.068(2) Uani 1 1 d . . . C48 C 0.4910(3) 0.0998(4) 0.1058(4) 0.0538(15) Uani 1 1 d . . . C49 C 0.9769(4) 0.1826(8) 0.2767(5) 0.091(3) Uani 1 1 d . . . H49A H 0.9570 0.2398 0.2876 0.137 Uiso 1 1 calc R . . H49B H 0.9475 0.1333 0.2770 0.137 Uiso 1 1 calc R . . H49C H 0.9938 0.1860 0.2267 0.137 Uiso 1 1 calc R . . O7 O 1.0238(3) 0.1662(6) 0.3328(4) 0.098(2) Uani 1 1 d D . . H7' H 1.039(6) 0.113(5) 0.319(7) 0.147 Uiso 1 1 d D . . C50 C 0.0373(4) 0.3859(8) 0.4199(7) 0.112(4) Uani 1 1 d D . . H50A H 0.0576 0.4344 0.4493 0.169 Uiso 1 1 calc R . . H50B H 0.0032 0.3635 0.4473 0.169 Uiso 1 1 calc R . . H50C H 0.0227 0.4094 0.3703 0.169 Uiso 1 1 calc R . . O8 O 0.0775(3) 0.3160(5) 0.4099(3) 0.0864(18) Uani 1 1 d D . . H8' H 0.050(2) 0.272(2) 0.379(4) 0.057(19) Uiso 1 1 d D . . C51 C 0.5017(3) 0.9359(5) 0.3753(5) 0.0652(18) Uani 1 1 d . . . H51A H 0.5228 0.9704 0.3376 0.098 Uiso 1 1 calc R . . H51B H 0.5217 0.8774 0.3838 0.098 Uiso 1 1 calc R . . H51C H 0.5023 0.9697 0.4230 0.098 Uiso 1 1 calc R . . O9 O 0.4421(3) 0.9217(4) 0.3488(3) 0.0815(16) Uani 1 1 d D . . H9' H 0.440(3) 0.967(3) 0.299(3) 0.039(15) Uiso 1 1 d 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 0.02141(16) 0.01987(16) 0.02386(17) 0.00069(11) -0.00419(11) -0.00147(11) Rh2 0.02037(16) 0.02070(16) 0.02424(17) 0.00257(12) -0.00342(11) -0.00062(11) N1 0.0261(17) 0.0268(17) 0.0212(16) 0.0001(13) 0.0014(13) 0.0018(14) N2 0.0207(16) 0.0184(15) 0.0320(18) -0.0020(14) 0.0010(14) 0.0006(12) N3 0.0212(16) 0.0258(17) 0.0259(17) 0.0021(14) -0.0007(13) 0.0008(13) N4 0.0280(17) 0.0207(16) 0.0250(17) -0.0007(13) -0.0015(14) 0.0025(13) N5 0.0191(16) 0.0305(18) 0.0280(18) -0.0018(14) -0.0038(13) -0.0014(13) N6 0.0218(16) 0.0296(18) 0.0265(18) 0.0012(14) -0.0036(14) -0.0033(14) O1 0.053(3) 0.062(3) 0.090(4) 0.012(3) -0.007(2) 0.003(2) O2 0.096(4) 0.129(6) 0.117(5) 0.078(4) 0.052(4) 0.049(4) O3 0.117(5) 0.042(3) 0.119(5) -0.003(3) -0.024(4) -0.001(3) O4 0.089(4) 0.097(4) 0.055(3) 0.009(3) 0.007(3) 0.025(3) O5 0.062(3) 0.151(6) 0.068(3) 0.019(4) -0.010(3) -0.025(4) O6 0.120(5) 0.063(3) 0.106(5) -0.013(3) 0.040(4) -0.037(3) S1 0.0507(8) 0.0354(7) 0.0764(11) 0.0180(7) 0.0099(7) 0.0006(6) S2 0.0503(8) 0.0662(10) 0.0625(10) 0.0080(8) 0.0089(7) -0.0052(7) F1 0.116(4) 0.050(3) 0.153(5) 0.031(3) 0.011(4) -0.003(3) F2 0.171(6) 0.128(5) 0.134(5) 0.073(4) 0.097(5) 0.074(4) F3 0.113(4) 0.110(4) 0.101(4) 0.025(3) -0.046(3) 0.017(3) F4 0.054(2) 0.070(3) 0.137(4) -0.016(3) -0.007(3) -0.002(2) F5 0.137(4) 0.100(4) 0.067(3) -0.017(3) 0.038(3) -0.056(3) F6 0.095(3) 0.051(2) 0.108(4) 0.001(2) 0.020(3) 0.018(2) C1 0.025(2) 0.029(2) 0.023(2) -0.0016(16) -0.0009(16) 0.0013(16) C2 0.040(2) 0.036(2) 0.026(2) -0.0006(18) 0.0028(19) 0.001(2) C3 0.044(3) 0.053(3) 0.032(3) -0.011(2) 0.009(2) 0.004(2) C4 0.043(3) 0.041(3) 0.042(3) -0.015(2) 0.005(2) 0.013(2) C5 0.039(2) 0.027(2) 0.034(2) -0.0059(18) -0.0014(19) 0.0045(19) C6 0.032(2) 0.026(2) 0.0217(19) -0.0037(16) -0.0048(16) 0.0019(16) C7 0.0219(18) 0.0235(19) 0.0236(19) 0.0004(15) -0.0039(15) 0.0017(15) C8 0.0205(18) 0.0228(19) 0.0238(19) 0.0022(15) 0.0010(15) 0.0027(14) C9 0.0200(18) 0.026(2) 0.029(2) -0.0042(16) -0.0023(16) 0.0000(15) C10 0.027(2) 0.027(2) 0.042(3) -0.0097(19) -0.0054(19) 0.0014(17) C11 0.032(2) 0.037(3) 0.043(3) -0.017(2) -0.001(2) 0.0026(19) C12 0.032(2) 0.049(3) 0.031(2) -0.012(2) 0.0019(19) -0.002(2) C13 0.028(2) 0.038(2) 0.030(2) -0.0038(19) 0.0034(17) -0.0023(18) C14 0.0217(19) 0.029(2) 0.028(2) -0.0052(17) -0.0011(16) 0.0006(16) C15 0.028(2) 0.054(3) 0.028(2) -0.003(2) -0.0044(18) 0.002(2) C16 0.026(2) 0.037(2) 0.035(2) 0.0003(19) -0.0055(18) -0.0017(18) C17 0.0188(19) 0.043(3) 0.032(2) -0.0073(19) -0.0031(17) 0.0015(17) C18 0.023(2) 0.051(3) 0.026(2) -0.007(2) -0.0045(17) -0.0004(19) C19 0.022(2) 0.040(2) 0.027(2) -0.0022(18) -0.0017(16) -0.0016(17) C20 0.022(2) 0.053(3) 0.033(2) -0.007(2) -0.0003(18) 0.0022(19) C21 0.026(2) 0.050(3) 0.025(2) -0.009(2) -0.0014(17) 0.0017(19) C22 0.0226(19) 0.034(2) 0.034(2) -0.0070(19) -0.0031(17) 0.0044(17) C23 0.034(2) 0.032(2) 0.037(2) -0.0067(19) -0.0103(19) 0.0033(19) C24 0.024(2) 0.035(2) 0.028(2) 0.0046(18) -0.0043(17) -0.0035(17) C25 0.021(2) 0.055(3) 0.031(2) -0.003(2) 0.0001(18) 0.0038(19) C26 0.026(2) 0.047(3) 0.025(2) -0.0075(19) -0.0033(17) 0.0051(19) C27 0.029(2) 0.0211(19) 0.038(2) 0.0045(17) -0.0054(18) 0.0018(16) C28 0.026(2) 0.030(2) 0.038(2) 0.0121(19) -0.0087(18) 0.0022(17) C29 0.045(3) 0.029(2) 0.032(2) 0.0064(18) -0.021(2) -0.0048(19) C30 0.042(2) 0.024(2) 0.026(2) 0.0053(17) -0.0092(18) 0.0043(18) C31 0.038(2) 0.024(2) 0.033(2) 0.0055(18) -0.0023(19) -0.0022(18) C32 0.066(4) 0.028(2) 0.053(3) -0.009(2) 0.001(3) 0.004(2) C33 0.028(2) 0.054(3) 0.061(4) 0.015(3) -0.004(2) 0.006(2) C34 0.070(4) 0.038(3) 0.065(4) 0.005(3) -0.038(3) -0.016(3) C35 0.076(4) 0.048(3) 0.024(2) 0.003(2) -0.001(2) 0.015(3) C36 0.050(3) 0.041(3) 0.061(4) 0.001(3) 0.012(3) -0.012(2) C37 0.0218(19) 0.027(2) 0.046(3) 0.0016(19) -0.0059(18) -0.0051(16) C38 0.027(2) 0.031(2) 0.054(3) -0.003(2) 0.004(2) -0.0090(18) C39 0.038(3) 0.037(2) 0.040(3) 0.012(2) -0.004(2) -0.014(2) C40 0.029(2) 0.024(2) 0.050(3) 0.012(2) -0.006(2) -0.0042(17) C41 0.028(2) 0.0203(19) 0.043(3) 0.0023(18) -0.0038(19) -0.0040(16) C42 0.039(3) 0.049(3) 0.059(4) 0.002(3) -0.023(3) 0.002(2) C43 0.034(3) 0.054(4) 0.102(6) -0.018(3) 0.025(3) -0.009(3) C44 0.086(5) 0.075(4) 0.036(3) 0.015(3) 0.002(3) -0.035(4) C45 0.040(3) 0.040(3) 0.083(5) 0.026(3) -0.014(3) 0.005(2) C46 0.053(3) 0.034(3) 0.052(3) -0.016(2) 0.000(3) -0.008(2) C47 0.065(4) 0.063(4) 0.077(5) 0.027(4) 0.026(4) 0.028(3) C48 0.043(3) 0.051(3) 0.069(4) -0.007(3) 0.008(3) 0.002(3) C49 0.061(5) 0.147(9) 0.066(5) 0.010(5) 0.003(4) 0.031(5) O7 0.069(4) 0.153(6) 0.072(4) -0.006(4) 0.002(3) 0.026(4) C50 0.067(5) 0.128(9) 0.139(10) -0.003(7) -0.015(6) 0.026(6) O8 0.068(3) 0.122(5) 0.069(4) 0.003(3) 0.000(3) 0.022(3) C51 0.050(4) 0.069(4) 0.076(5) 0.014(4) -0.005(3) 0.002(3) O9 0.091(4) 0.093(4) 0.059(3) -0.002(3) -0.010(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C29 2.127(4) . ? Rh1 C27 2.140(4) . ? Rh1 N5 2.144(3) . ? Rh1 C30 2.146(4) . ? Rh1 N2 2.161(4) . ? Rh1 C28 2.164(4) . ? Rh1 N1 2.166(3) . ? Rh1 C31 2.178(4) . ? Rh2 C37 2.135(4) . ? Rh2 C39 2.138(5) . ? Rh2 N6 2.144(3) 3_565 ? Rh2 C40 2.158(4) . ? Rh2 N3 2.164(3) . ? Rh2 C41 2.169(4) . ? Rh2 N4 2.179(4) . ? Rh2 C38 2.183(5) . ? N1 C7 1.325(5) . ? N1 C1 1.396(5) . ? N2 C8 1.332(5) . ? N2 C9 1.384(6) . ? N3 C8 1.327(5) . ? N3 C14 1.383(5) . ? N4 C7 1.334(5) . ? N4 C6 1.389(6) . ? N5 C21 1.328(6) . ? N5 C17 1.341(6) . ? N6 C26 1.341(6) . ? N6 C22 1.342(6) . ? N6 Rh2 2.144(3) 3_565 ? O1 S1 1.434(5) . ? O2 S1 1.372(6) . ? O3 S1 1.434(6) . ? O4 S2 1.455(6) . ? O5 S2 1.416(6) . ? O6 S2 1.429(7) . ? S1 C47 1.821(7) . ? S2 C48 1.818(7) . ? F1 C47 1.363(10) . ? F2 C47 1.287(8) . ? F3 C47 1.272(9) . ? F4 C48 1.312(7) . ? F5 C48 1.299(8) . ? F6 C48 1.334(7) . ? C1 C2 1.400(6) . ? C1 C6 1.421(6) . ? C2 C3 1.376(7) . ? C3 C4 1.391(8) . ? C4 C5 1.381(7) . ? C5 C6 1.402(6) . ? C7 C8 1.422(6) . ? C9 C10 1.401(6) . ? C9 C14 1.422(6) . ? C10 C11 1.372(7) . ? C11 C12 1.396(8) . ? C12 C13 1.375(7) . ? C13 C14 1.397(6) . ? C15 C16 1.339(7) . ? C15 C19 1.465(6) . ? C16 C24 1.470(6) . ? C17 C18 1.391(6) . ? C18 C19 1.396(6) . ? C19 C20 1.394(6) . ? C20 C21 1.380(6) . ? C22 C23 1.387(6) . ? C23 C24 1.390(7) . ? C24 C25 1.407(7) . ? C25 C26 1.392(6) . ? C27 C31 1.421(7) . ? C27 C28 1.452(6) . ? C27 C32 1.493(7) . ? C28 C29 1.427(7) . ? C28 C33 1.481(7) . ? C29 C30 1.433(7) . ? C29 C34 1.499(7) . ? C30 C31 1.407(6) . ? C30 C35 1.522(7) . ? C31 C36 1.481(7) . ? C37 C38 1.436(7) . ? C37 C41 1.437(6) . ? C37 C42 1.480(7) . ? C38 C39 1.433(7) . ? C38 C43 1.483(7) . ? C39 C40 1.425(8) . ? C39 C44 1.499(8) . ? C40 C41 1.420(7) . ? C40 C45 1.496(7) . ? C41 C46 1.499(7) . ? C49 O7 1.391(10) . ? C50 O8 1.358(11) . ? C51 O9 1.368(8) . ? 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 C29 Rh1 C27 65.78(17) . . ? C29 Rh1 N5 161.16(18) . . ? C27 Rh1 N5 108.68(15) . . ? C29 Rh1 C30 39.2(2) . . ? C27 Rh1 C30 64.72(17) . . ? N5 Rh1 C30 121.98(17) . . ? C29 Rh1 N2 112.31(17) . . ? C27 Rh1 N2 110.87(16) . . ? N5 Rh1 N2 86.53(13) . . ? C30 Rh1 N2 151.41(16) . . ? C29 Rh1 C28 38.8(2) . . ? C27 Rh1 C28 39.43(17) . . ? N5 Rh1 C28 145.14(16) . . ? C30 Rh1 C28 64.82(18) . . ? N2 Rh1 C28 93.48(15) . . ? C29 Rh1 N1 98.15(16) . . ? C27 Rh1 N1 162.94(15) . . ? N5 Rh1 N1 84.65(13) . . ? C30 Rh1 N1 99.41(15) . . ? N2 Rh1 N1 79.77(13) . . ? C28 Rh1 N1 129.70(16) . . ? C29 Rh1 C31 64.85(18) . . ? C27 Rh1 C31 38.41(18) . . ? N5 Rh1 C31 99.24(16) . . ? C30 Rh1 C31 37.97(17) . . ? N2 Rh1 C31 149.00(16) . . ? C28 Rh1 C31 64.60(18) . . ? N1 Rh1 C31 130.91(16) . . ? C37 Rh2 C39 65.59(18) . . ? C37 Rh2 N6 164.54(16) . 3_565 ? C39 Rh2 N6 102.10(16) . 3_565 ? C37 Rh2 C40 65.18(17) . . ? C39 Rh2 C40 38.7(2) . . ? N6 Rh2 C40 99.39(16) 3_565 . ? C37 Rh2 N3 107.04(15) . . ? C39 Rh2 N3 118.87(18) . . ? N6 Rh2 N3 86.89(13) 3_565 . ? C40 Rh2 N3 157.50(17) . . ? C37 Rh2 C41 39.00(17) . . ? C39 Rh2 C41 64.8(2) . . ? N6 Rh2 C41 128.42(15) 3_565 . ? C40 Rh2 C41 38.31(18) . . ? N3 Rh2 C41 144.26(15) . . ? C37 Rh2 N4 104.14(16) . . ? C39 Rh2 N4 160.18(18) . . ? N6 Rh2 N4 84.58(13) 3_565 . ? C40 Rh2 N4 122.14(17) . . ? N3 Rh2 N4 79.78(13) . . ? C41 Rh2 N4 96.38(16) . . ? C37 Rh2 C38 38.82(19) . . ? C39 Rh2 C38 38.71(19) . . ? N6 Rh2 C38 135.18(17) 3_565 . ? C40 Rh2 C38 64.42(18) . . ? N3 Rh2 C38 95.93(16) . . ? C41 Rh2 C38 64.37(18) . . ? N4 Rh2 C38 140.04(17) . . ? C7 N1 C1 103.2(3) . . ? C7 N1 Rh1 109.2(3) . . ? C1 N1 Rh1 147.1(3) . . ? C8 N2 C9 103.2(3) . . ? C8 N2 Rh1 109.5(3) . . ? C9 N2 Rh1 146.9(3) . . ? C8 N3 C14 103.2(3) . . ? C8 N3 Rh2 109.2(3) . . ? C14 N3 Rh2 147.2(3) . . ? C7 N4 C6 102.8(3) . . ? C7 N4 Rh2 109.1(3) . . ? C6 N4 Rh2 147.0(3) . . ? C21 N5 C17 118.0(4) . . ? C21 N5 Rh1 120.4(3) . . ? C17 N5 Rh1 121.4(3) . . ? C26 N6 C22 117.1(4) . . ? C26 N6 Rh2 119.1(3) . 3_565 ? C22 N6 Rh2 123.7(3) . 3_565 ? O2 S1 O1 115.5(4) . . ? O2 S1 O3 119.8(5) . . ? O1 S1 O3 109.8(3) . . ? O2 S1 C47 102.9(3) . . ? O1 S1 C47 105.5(3) . . ? O3 S1 C47 100.8(4) . . ? O5 S2 O6 117.6(4) . . ? O5 S2 O4 112.7(4) . . ? O6 S2 O4 114.9(4) . . ? O5 S2 C48 102.6(3) . . ? O6 S2 C48 104.0(3) . . ? O4 S2 C48 102.5(3) . . ? N1 C1 C2 131.8(4) . . ? N1 C1 C6 107.6(4) . . ? C2 C1 C6 120.5(4) . . ? C3 C2 C1 117.7(5) . . ? C2 C3 C4 121.7(5) . . ? C5 C4 C3 122.3(5) . . ? C4 C5 C6 116.9(5) . . ? N4 C6 C5 130.7(4) . . ? N4 C6 C1 108.3(4) . . ? C5 C6 C1 120.9(4) . . ? N1 C7 N4 118.1(4) . . ? N1 C7 C8 120.9(4) . . ? N4 C7 C8 120.2(4) . . ? N3 C8 N2 117.7(4) . . ? N3 C8 C7 121.5(4) . . ? N2 C8 C7 120.3(4) . . ? N2 C9 C10 131.4(4) . . ? N2 C9 C14 107.8(4) . . ? C10 C9 C14 120.8(4) . . ? C11 C10 C9 117.5(5) . . ? C10 C11 C12 121.7(4) . . ? C13 C12 C11 121.9(5) . . ? C12 C13 C14 117.7(5) . . ? N3 C14 C13 131.6(4) . . ? N3 C14 C9 108.1(4) . . ? C13 C14 C9 120.3(4) . . ? C16 C15 C19 124.9(5) . . ? C15 C16 C24 125.3(5) . . ? N5 C17 C18 122.3(4) . . ? C17 C18 C19 119.6(4) . . ? C20 C19 C18 117.1(4) . . ? C20 C19 C15 123.8(4) . . ? C18 C19 C15 118.9(4) . . ? C21 C20 C19 119.4(4) . . ? N5 C21 C20 123.5(4) . . ? N6 C22 C23 123.2(4) . . ? C22 C23 C24 119.9(4) . . ? C23 C24 C25 117.3(4) . . ? C23 C24 C16 119.8(4) . . ? C25 C24 C16 122.6(4) . . ? C26 C25 C24 118.8(4) . . ? N6 C26 C25 123.7(4) . . ? C31 C27 C28 107.7(4) . . ? C31 C27 C32 125.5(4) . . ? C28 C27 C32 126.1(5) . . ? C31 C27 Rh1 72.2(2) . . ? C28 C27 Rh1 71.2(2) . . ? C32 C27 Rh1 129.0(4) . . ? C29 C28 C27 107.2(4) . . ? C29 C28 C33 126.6(5) . . ? C27 C28 C33 126.2(5) . . ? C29 C28 Rh1 69.2(2) . . ? C27 C28 Rh1 69.4(2) . . ? C33 C28 Rh1 127.3(3) . . ? C28 C29 C30 107.7(4) . . ? C28 C29 C34 126.5(5) . . ? C30 C29 C34 125.7(5) . . ? C28 C29 Rh1 72.0(2) . . ? C30 C29 Rh1 71.1(2) . . ? C34 C29 Rh1 125.2(3) . . ? C31 C30 C29 108.8(4) . . ? C31 C30 C35 125.9(5) . . ? C29 C30 C35 124.9(5) . . ? C31 C30 Rh1 72.3(3) . . ? C29 C30 Rh1 69.7(3) . . ? C35 C30 Rh1 129.8(3) . . ? C30 C31 C27 108.4(4) . . ? C30 C31 C36 125.9(5) . . ? C27 C31 C36 125.6(4) . . ? C30 C31 Rh1 69.8(3) . . ? C27 C31 Rh1 69.3(2) . . ? C36 C31 Rh1 128.6(4) . . ? C38 C37 C41 107.6(4) . . ? C38 C37 C42 127.0(5) . . ? C41 C37 C42 125.0(5) . . ? C38 C37 Rh2 72.4(2) . . ? C41 C37 Rh2 71.8(2) . . ? C42 C37 Rh2 126.4(4) . . ? C39 C38 C37 107.6(4) . . ? C39 C38 C43 127.4(6) . . ? C37 C38 C43 125.1(5) . . ? C39 C38 Rh2 68.9(3) . . ? C37 C38 Rh2 68.8(3) . . ? C43 C38 Rh2 128.2(4) . . ? C40 C39 C38 108.1(4) . . ? C40 C39 C44 126.8(5) . . ? C38 C39 C44 124.7(6) . . ? C40 C39 Rh2 71.4(3) . . ? C38 C39 Rh2 72.4(3) . . ? C44 C39 Rh2 127.7(4) . . ? C41 C40 C39 108.3(4) . . ? C41 C40 C45 124.3(5) . . ? C39 C40 C45 127.2(5) . . ? C41 C40 Rh2 71.3(2) . . ? C39 C40 Rh2 69.9(3) . . ? C45 C40 Rh2 128.3(3) . . ? C40 C41 C37 108.1(4) . . ? C40 C41 C46 127.3(4) . . ? C37 C41 C46 124.6(5) . . ? C40 C41 Rh2 70.4(3) . . ? C37 C41 Rh2 69.2(2) . . ? C46 C41 Rh2 127.6(3) . . ? F3 C47 F2 115.1(8) . . ? F3 C47 F1 102.5(6) . . ? F2 C47 F1 101.3(7) . . ? F3 C47 S1 114.0(6) . . ? F2 C47 S1 114.3(5) . . ? F1 C47 S1 107.8(6) . . ? F5 C48 F4 107.6(6) . . ? F5 C48 F6 107.8(6) . . ? F4 C48 F6 105.2(5) . . ? F5 C48 S2 113.7(5) . . ? F4 C48 S2 111.2(5) . . ? F6 C48 S2 110.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7' O2 0.88(5) 2.11(6) 2.971(10) 167(12) 1_655 O8 H8' O7 1.02(4) 1.80(3) 2.772(11) 159(4) 1_455 O9 H9' O4 1.08(4) 1.73(4) 2.802(8) 176(5) 1_565 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.386 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 927803' ####################################################################### # # 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_global # Attachment '2.cif' data_2 #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C117 H126 F12 N12 O19 Rh4 S4' _chemical_formula_weight 2772.18 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.3744(15) _cell_length_b 20.4476(16) _cell_length_c 16.1066(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.5370(10) _cell_angle_gamma 90.00 _cell_volume 6378.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6570 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.40 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8797 _exptl_absorpt_correction_T_max 0.9252 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.14 _diffrn_reflns_number 46766 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.56 _reflns_number_total 14646 _reflns_number_gt 9341 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In asymmetric unit of this data, one methanol and one water molecules were strongly disordered and could not be restrained properly so that they were omitted by SQUEEZE algorithm. 9 ISOR and 4 DFIX instructions were used to restrain the anion and guest molecules and there were 58 restraints used. ; _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^)+(0.1044P)^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 14646 _refine_ls_number_parameters 762 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.959 _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 0.163086(17) 0.352410(17) 0.05090(2) 0.02442(10) Uani 1 1 d . . . Rh2 Rh 0.208595(17) 0.559720(18) 0.27233(2) 0.02758(11) Uani 1 1 d . . . N1 N 0.21014(19) 0.37182(19) 0.1724(2) 0.0297(8) Uani 1 1 d . . . N2 N 0.16752(18) 0.45824(18) 0.0496(2) 0.0269(8) Uani 1 1 d . . . N3 N 0.18153(19) 0.54315(18) 0.1406(2) 0.0274(8) Uani 1 1 d . . . N4 N 0.2294(2) 0.45732(19) 0.2617(2) 0.0303(9) Uani 1 1 d . . . N5 N 0.26256(18) 0.34924(19) 0.0012(2) 0.0284(8) Uani 1 1 d . . . N6 N 0.69010(19) 0.4191(2) -0.2372(2) 0.0313(9) Uani 1 1 d . . . S1 S 0.06979(7) 0.69752(7) 0.52676(8) 0.0410(3) Uani 1 1 d . . . S2 S 0.31690(12) 0.40575(11) 0.63485(12) 0.0788(6) Uani 1 1 d . . . O1 O 0.14307(19) 0.6935(2) 0.5206(3) 0.0543(10) Uani 1 1 d D . . O2 O 0.0310(2) 0.6794(3) 0.4542(3) 0.0803(16) Uani 1 1 d . . . O3 O 0.0445(2) 0.75271(19) 0.5701(2) 0.0510(10) Uani 1 1 d . . . O4 O 0.3267(5) 0.4432(3) 0.5648(4) 0.134(3) Uani 1 1 d . . . O5 O 0.3659(5) 0.4131(6) 0.6976(4) 0.189(5) Uani 1 1 d . . . O6 O 0.2917(4) 0.3430(4) 0.6187(6) 0.147(3) Uani 1 1 d . . . F1 F 0.0690(4) 0.5745(2) 0.5690(4) 0.137(2) Uani 1 1 d . . . F2 F 0.0881(3) 0.6398(3) 0.6714(3) 0.1014(16) Uani 1 1 d . . . F3 F -0.0138(3) 0.6306(3) 0.6181(4) 0.122(2) Uani 1 1 d . . . F4 F 0.2185(4) 0.4196(4) 0.7471(4) 0.159(3) Uani 1 1 d . . . F5 F 0.2552(6) 0.5074(5) 0.6963(7) 0.238(5) Uani 1 1 d U . . F6 F 0.1898(4) 0.4479(4) 0.6276(5) 0.169(3) Uani 1 1 d . . . C1 C 0.2482(2) 0.3476(2) 0.2397(3) 0.0330(11) Uani 1 1 d . . . C2 C 0.2758(3) 0.2876(3) 0.2558(3) 0.0381(12) Uani 1 1 d . . . H2 H 0.2681 0.2521 0.2187 0.046 Uiso 1 1 calc R . . C3 C 0.3160(3) 0.2796(3) 0.3289(3) 0.0484(14) Uani 1 1 d . . . H3 H 0.3360 0.2382 0.3415 0.058 Uiso 1 1 calc R . . C4 C 0.3269(3) 0.3321(3) 0.3833(3) 0.0485(14) Uani 1 1 d . . . H4 H 0.3549 0.3257 0.4320 0.058 Uiso 1 1 calc R . . C5 C 0.2990(3) 0.3918(3) 0.3689(3) 0.0379(12) Uani 1 1 d . . . H5 H 0.3059 0.4266 0.4073 0.045 Uiso 1 1 calc R . . C6 C 0.2600(2) 0.4007(2) 0.2962(3) 0.0293(10) Uani 1 1 d . . . C7 C 0.2024(2) 0.4346(2) 0.1900(3) 0.0280(10) Uani 1 1 d . . . C8 C 0.1799(2) 0.4797(2) 0.1268(3) 0.0267(9) Uani 1 1 d . . . C9 C 0.1609(2) 0.5161(2) 0.0050(3) 0.0264(9) Uani 1 1 d . . . C10 C 0.1501(2) 0.5264(3) -0.0797(3) 0.0321(10) Uani 1 1 d . . . H10 H 0.1442 0.4907 -0.1170 0.039 Uiso 1 1 calc R . . C11 C 0.1484(3) 0.5899(3) -0.1075(3) 0.0395(12) Uani 1 1 d . . . H11 H 0.1413 0.5985 -0.1651 0.047 Uiso 1 1 calc R . . C12 C 0.1570(3) 0.6422(3) -0.0517(3) 0.0399(12) Uani 1 1 d . . . H12 H 0.1557 0.6856 -0.0727 0.048 Uiso 1 1 calc R . . C13 C 0.1672(2) 0.6329(2) 0.0316(3) 0.0321(10) Uani 1 1 d . . . H13 H 0.1724 0.6688 0.0687 0.039 Uiso 1 1 calc R . . C14 C 0.1696(2) 0.5685(2) 0.0603(3) 0.0309(10) Uani 1 1 d . . . C15 C 0.4665(2) 0.3532(3) -0.0934(3) 0.0390(12) Uani 1 1 d . . . H15 H 0.5018 0.3319 -0.0615 0.047 Uiso 1 1 calc R . . C16 C 0.4847(2) 0.3819(3) -0.1620(3) 0.0472(14) Uani 1 1 d . . . H16 H 0.4487 0.3988 -0.1970 0.057 Uiso 1 1 calc R . . C17 C 0.2783(2) 0.3868(2) -0.0645(3) 0.0300(10) Uani 1 1 d . . . H17 H 0.2430 0.4129 -0.0896 0.036 Uiso 1 1 calc R . . C18 C 0.3427(2) 0.3890(2) -0.0963(3) 0.0333(11) Uani 1 1 d . . . H18 H 0.3513 0.4165 -0.1424 0.040 Uiso 1 1 calc R . . C19 C 0.3964(2) 0.3509(2) -0.0615(3) 0.0320(10) Uani 1 1 d . . . C20 C 0.3796(2) 0.3114(3) 0.0044(3) 0.0376(11) Uani 1 1 d . . . H20 H 0.4138 0.2843 0.0299 0.045 Uiso 1 1 calc R . . C21 C 0.3130(2) 0.3111(2) 0.0338(3) 0.0356(11) Uani 1 1 d . . . H21 H 0.3026 0.2829 0.0786 0.043 Uiso 1 1 calc R . . C22 C 0.6779(2) 0.3749(3) -0.1776(3) 0.0356(11) Uani 1 1 d . . . H22 H 0.7161 0.3534 -0.1514 0.043 Uiso 1 1 calc R . . C23 C 0.6125(3) 0.3597(3) -0.1530(3) 0.0417(12) Uani 1 1 d . . . H23 H 0.6062 0.3279 -0.1108 0.050 Uiso 1 1 calc R . . C24 C 0.5554(2) 0.3905(3) -0.1896(3) 0.0417(13) Uani 1 1 d . . . C25 C 0.5680(3) 0.4327(3) -0.2542(4) 0.0477(14) Uani 1 1 d . . . H25 H 0.5305 0.4524 -0.2841 0.057 Uiso 1 1 calc R . . C26 C 0.6347(3) 0.4462(3) -0.2753(3) 0.0443(13) Uani 1 1 d . . . H26 H 0.6419 0.4762 -0.3192 0.053 Uiso 1 1 calc R . . C27 C 0.0977(2) 0.3146(3) -0.0460(3) 0.0332(11) Uani 1 1 d . . . C28 C 0.1269(2) 0.2602(2) -0.0009(3) 0.0349(11) Uani 1 1 d . . . C29 C 0.1056(2) 0.2665(3) 0.0826(3) 0.0363(11) Uani 1 1 d . . . C30 C 0.0631(2) 0.3236(3) 0.0886(3) 0.0341(11) Uani 1 1 d . . . C31 C 0.0563(2) 0.3517(2) 0.0082(3) 0.0316(10) Uani 1 1 d . . . C32 C 0.1029(3) 0.3243(3) -0.1374(3) 0.0496(15) Uani 1 1 d . . . H32A H 0.0668 0.2988 -0.1664 0.074 Uiso 1 1 calc R . . H32B H 0.1483 0.3096 -0.1552 0.074 Uiso 1 1 calc R . . H32C H 0.0970 0.3708 -0.1507 0.074 Uiso 1 1 calc R . . C33 C 0.1676(3) 0.2073(3) -0.0372(5) 0.0663(19) Uani 1 1 d . . . H33A H 0.1973 0.1874 0.0061 0.099 Uiso 1 1 calc R . . H33B H 0.1963 0.2252 -0.0810 0.099 Uiso 1 1 calc R . . H33C H 0.1365 0.1740 -0.0609 0.099 Uiso 1 1 calc R . . C34 C 0.1212(3) 0.2201(3) 0.1510(4) 0.066(2) Uani 1 1 d . . . H34A H 0.0850 0.1867 0.1526 0.098 Uiso 1 1 calc R . . H34B H 0.1233 0.2438 0.2039 0.098 Uiso 1 1 calc R . . H34C H 0.1659 0.1991 0.1419 0.098 Uiso 1 1 calc R . . C35 C 0.0274(3) 0.3451(4) 0.1651(4) 0.0596(17) Uani 1 1 d . . . H35A H 0.0107 0.3900 0.1576 0.089 Uiso 1 1 calc R . . H35B H 0.0598 0.3433 0.2128 0.089 Uiso 1 1 calc R . . H35C H -0.0118 0.3161 0.1749 0.089 Uiso 1 1 calc R . . C36 C 0.0145(3) 0.4097(3) -0.0148(4) 0.0493(14) Uani 1 1 d . . . H36A H 0.0379 0.4346 -0.0578 0.074 Uiso 1 1 calc R . . H36B H 0.0088 0.4373 0.0342 0.074 Uiso 1 1 calc R . . H36C H -0.0309 0.3956 -0.0362 0.074 Uiso 1 1 calc R . . C37 C 0.1093(3) 0.5750(3) 0.3225(4) 0.0500(15) Uani 1 1 d . . . C38 C 0.1491(3) 0.5455(3) 0.3818(4) 0.0475(14) Uani 1 1 d . . . C39 C 0.2067(3) 0.5860(3) 0.4002(3) 0.0386(12) Uani 1 1 d . . . C40 C 0.2011(3) 0.6435(2) 0.3524(3) 0.0407(12) Uani 1 1 d . . . C41 C 0.1386(3) 0.6370(3) 0.3001(3) 0.0517(16) Uani 1 1 d . . . C42 C 0.0404(4) 0.5467(5) 0.2865(6) 0.104(3) Uani 1 1 d . . . H42A H 0.0503 0.5143 0.2435 0.156 Uiso 1 1 calc R . . H42B H 0.0125 0.5821 0.2621 0.156 Uiso 1 1 calc R . . H42C H 0.0150 0.5257 0.3310 0.156 Uiso 1 1 calc R . . C43 C 0.1354(4) 0.4811(4) 0.4234(4) 0.074(2) Uani 1 1 d . . . H43A H 0.1019 0.4875 0.4672 0.112 Uiso 1 1 calc R . . H43B H 0.1786 0.4640 0.4478 0.112 Uiso 1 1 calc R . . H43C H 0.1168 0.4500 0.3823 0.112 Uiso 1 1 calc R . . C44 C 0.2609(4) 0.5756(4) 0.4657(4) 0.0650(19) Uani 1 1 d . . . H44A H 0.3052 0.5917 0.4462 0.098 Uiso 1 1 calc R . . H44B H 0.2646 0.5288 0.4782 0.098 Uiso 1 1 calc R . . H44C H 0.2485 0.5994 0.5160 0.098 Uiso 1 1 calc R . . C45 C 0.2489(4) 0.6999(3) 0.3542(5) 0.077(2) Uani 1 1 d . . . H45A H 0.2325 0.7327 0.3935 0.116 Uiso 1 1 calc R . . H45B H 0.2506 0.7192 0.2987 0.116 Uiso 1 1 calc R . . H45C H 0.2951 0.6851 0.3717 0.116 Uiso 1 1 calc R . . C46 C 0.1084(4) 0.6860(4) 0.2430(5) 0.083(2) Uani 1 1 d . . . H46A H 0.0936 0.6646 0.1911 0.124 Uiso 1 1 calc R . . H46B H 0.1430 0.7194 0.2312 0.124 Uiso 1 1 calc R . . H46C H 0.0685 0.7065 0.2686 0.124 Uiso 1 1 calc R . . C47 C 0.0511(4) 0.6320(3) 0.6003(6) 0.079(2) Uani 1 1 d . . . C48 C 0.2450(7) 0.4452(5) 0.6789(6) 0.103(3) Uani 1 1 d . . . C49 C 0.4652(8) 0.4159(7) 0.1422(10) 0.150(5) Uani 1 1 d U . . C50 C 0.4008(8) 0.4257(7) 0.1503(10) 0.136(5) Uani 1 1 d . A . H50 H 0.3748 0.4052 0.1922 0.164 Uiso 1 1 calc R . . C51 C 0.3727(8) 0.4676(7) 0.0946(9) 0.138(5) Uani 1 1 d U . . H51 H 0.3245 0.4755 0.0985 0.165 Uiso 1 1 calc R A . C52 C 0.4066(5) 0.5007(7) 0.0317(9) 0.118(4) Uani 1 1 d U A . C53 C 0.4809(7) 0.4842(6) 0.0291(8) 0.129(4) Uani 1 1 d U . . C54 C 0.5117(6) 0.4387(5) 0.0904(7) 0.107(4) Uani 1 1 d . . . C55 C 0.3770(8) 0.5491(7) -0.0315(10) 0.142(5) Uani 1 1 d . . . H55 H 0.3290 0.5583 -0.0294 0.170 Uiso 1 1 calc R A . C56 C 0.4125(9) 0.5799(8) -0.0895(11) 0.189(7) Uani 1 1 d U . . H56 H 0.3921 0.6106 -0.1269 0.227 Uiso 1 1 calc R . . C57 C 0.5021(15) 0.3576(14) 0.2101(18) 0.169(11) Uani 0.25 1 d PDU A 1 H57 H 0.4809 0.3160 0.2152 0.202 Uiso 0.25 1 calc PR A 1 O7 O 0.5565(13) 0.3702(15) 0.2522(18) 0.116(9) Uani 0.25 1 d PDU A 1 C57' C 0.5021(15) 0.3576(14) 0.2101(18) 0.169(11) Uani 0.25 1 d PD A 2 H57' H 0.5148 0.3630 0.2671 0.202 Uiso 0.25 1 calc PR A 2 O7' O 0.5078(11) 0.3083(9) 0.1671(14) 0.078(6) Uani 0.25 1 d PDU A 2 C58 C 0.2810(7) 0.6790(7) 0.6712(9) 0.166(6) Uani 1 1 d . . . H58A H 0.3244 0.6935 0.6979 0.249 Uiso 1 1 calc R . . H58B H 0.2907 0.6456 0.6295 0.249 Uiso 1 1 calc R . . H58C H 0.2508 0.6606 0.7131 0.249 Uiso 1 1 calc R . . O8 O 0.2483(4) 0.7321(3) 0.6327(5) 0.125(3) Uani 1 1 d D . . H8 H 0.208(3) 0.718(6) 0.618(6) 0.188 Uiso 1 1 d 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 0.02363(17) 0.03050(19) 0.01924(18) -0.00042(14) 0.00274(12) -0.00139(14) Rh2 0.02347(18) 0.0379(2) 0.02153(19) -0.00563(15) 0.00339(13) 0.00024(15) N1 0.032(2) 0.034(2) 0.023(2) 0.0018(16) -0.0034(16) -0.0014(17) N2 0.0277(19) 0.032(2) 0.0205(19) -0.0002(15) -0.0015(15) 0.0007(16) N3 0.0294(19) 0.033(2) 0.0201(19) -0.0001(15) -0.0008(15) 0.0001(16) N4 0.033(2) 0.037(2) 0.021(2) 0.0008(16) 0.0004(15) 0.0029(17) N5 0.0235(18) 0.034(2) 0.027(2) 0.0008(17) 0.0016(15) -0.0011(16) N6 0.0246(19) 0.044(2) 0.026(2) -0.0009(17) 0.0004(15) 0.0002(17) S1 0.0379(7) 0.0469(8) 0.0380(7) -0.0070(6) 0.0004(5) 0.0057(6) S2 0.1044(16) 0.0806(14) 0.0501(11) 0.0199(10) -0.0249(10) -0.0217(12) O1 0.041(2) 0.072(3) 0.050(2) -0.001(2) 0.0137(18) 0.003(2) O2 0.066(3) 0.122(4) 0.052(3) -0.032(3) -0.017(2) 0.023(3) O3 0.053(2) 0.048(2) 0.052(2) -0.0113(19) -0.0004(18) 0.0158(19) O4 0.223(9) 0.122(6) 0.056(4) 0.025(4) 0.000(4) 0.048(5) O5 0.178(8) 0.329(14) 0.056(4) -0.002(6) -0.044(5) 0.031(9) O6 0.132(6) 0.087(5) 0.223(10) -0.010(5) 0.013(6) -0.021(4) F1 0.228(7) 0.046(3) 0.140(5) -0.003(3) 0.069(5) -0.001(3) F2 0.143(5) 0.105(4) 0.057(3) 0.029(3) 0.012(3) 0.005(3) F3 0.100(4) 0.119(4) 0.152(5) -0.011(4) 0.059(4) -0.052(3) F4 0.201(7) 0.202(7) 0.074(4) 0.047(4) 0.000(4) -0.056(6) F5 0.296(11) 0.148(7) 0.274(10) -0.104(7) 0.112(8) -0.039(7) F6 0.178(8) 0.194(8) 0.134(6) 0.042(5) -0.021(5) 0.054(6) C1 0.032(2) 0.044(3) 0.024(2) 0.007(2) 0.0038(18) -0.002(2) C2 0.043(3) 0.039(3) 0.033(3) 0.004(2) -0.002(2) 0.001(2) C3 0.058(3) 0.050(3) 0.037(3) 0.012(3) -0.007(3) 0.016(3) C4 0.056(3) 0.055(4) 0.034(3) 0.012(3) -0.008(3) -0.006(3) C5 0.040(3) 0.048(3) 0.025(3) 0.002(2) -0.004(2) -0.002(2) C6 0.032(2) 0.036(3) 0.020(2) 0.0041(19) 0.0041(18) 0.000(2) C7 0.031(2) 0.034(3) 0.019(2) 0.0009(18) 0.0007(17) 0.0017(19) C8 0.022(2) 0.034(3) 0.024(2) 0.0000(19) 0.0035(17) 0.0006(18) C9 0.023(2) 0.033(2) 0.024(2) 0.0056(18) 0.0033(17) -0.0016(18) C10 0.030(2) 0.045(3) 0.021(2) 0.003(2) 0.0000(18) -0.002(2) C11 0.044(3) 0.047(3) 0.028(3) 0.009(2) 0.000(2) 0.004(2) C12 0.047(3) 0.035(3) 0.038(3) 0.010(2) 0.005(2) -0.004(2) C13 0.037(3) 0.031(3) 0.029(3) 0.0000(19) 0.005(2) 0.000(2) C14 0.021(2) 0.044(3) 0.028(2) 0.000(2) 0.0026(18) 0.0011(19) C15 0.025(2) 0.056(3) 0.036(3) -0.005(2) 0.003(2) -0.006(2) C16 0.022(2) 0.080(4) 0.040(3) -0.004(3) 0.000(2) -0.012(3) C17 0.025(2) 0.038(3) 0.027(2) 0.001(2) 0.0032(18) -0.0003(19) C18 0.034(3) 0.038(3) 0.029(3) 0.000(2) 0.0051(19) -0.005(2) C19 0.027(2) 0.043(3) 0.026(2) -0.007(2) 0.0024(18) -0.004(2) C20 0.031(2) 0.045(3) 0.037(3) 0.001(2) -0.004(2) 0.003(2) C21 0.033(2) 0.038(3) 0.037(3) 0.006(2) 0.001(2) 0.001(2) C22 0.025(2) 0.042(3) 0.039(3) 0.001(2) 0.001(2) -0.001(2) C23 0.035(3) 0.052(3) 0.038(3) 0.003(2) 0.004(2) -0.003(2) C24 0.023(2) 0.066(4) 0.037(3) -0.009(3) 0.003(2) -0.005(2) C25 0.033(3) 0.070(4) 0.040(3) 0.003(3) -0.001(2) -0.003(3) C26 0.036(3) 0.068(4) 0.029(3) 0.004(3) 0.003(2) -0.004(3) C27 0.023(2) 0.049(3) 0.027(2) -0.005(2) 0.0011(18) -0.010(2) C28 0.031(2) 0.034(3) 0.040(3) -0.006(2) 0.006(2) -0.009(2) C29 0.032(2) 0.039(3) 0.038(3) 0.010(2) 0.001(2) -0.010(2) C30 0.027(2) 0.049(3) 0.027(3) -0.005(2) 0.0071(19) -0.011(2) C31 0.020(2) 0.039(3) 0.036(3) -0.002(2) -0.0017(18) -0.0065(19) C32 0.043(3) 0.076(4) 0.029(3) -0.004(3) 0.002(2) -0.017(3) C33 0.058(4) 0.044(4) 0.097(6) -0.028(3) 0.006(4) 0.003(3) C34 0.052(4) 0.075(5) 0.069(5) 0.040(4) -0.009(3) -0.013(3) C35 0.043(3) 0.091(5) 0.045(4) -0.013(3) 0.017(3) -0.006(3) C36 0.034(3) 0.045(3) 0.069(4) 0.007(3) -0.005(3) 0.005(2) C37 0.033(3) 0.072(4) 0.046(3) -0.013(3) 0.020(2) 0.005(3) C38 0.054(3) 0.050(3) 0.040(3) -0.012(3) 0.028(3) -0.009(3) C39 0.049(3) 0.045(3) 0.022(2) -0.008(2) 0.010(2) 0.004(2) C40 0.048(3) 0.034(3) 0.040(3) -0.008(2) 0.018(2) 0.002(2) C41 0.056(3) 0.069(4) 0.031(3) -0.002(3) 0.008(2) 0.038(3) C42 0.032(4) 0.172(10) 0.108(7) -0.039(6) 0.010(4) -0.006(5) C43 0.102(6) 0.063(4) 0.061(5) -0.007(3) 0.046(4) -0.014(4) C44 0.081(5) 0.078(5) 0.036(3) -0.012(3) -0.010(3) 0.026(4) C45 0.083(5) 0.048(4) 0.102(6) -0.025(4) 0.034(4) -0.017(4) C46 0.101(6) 0.086(6) 0.061(5) 0.009(4) 0.019(4) 0.051(5) C47 0.076(5) 0.044(4) 0.120(8) -0.015(4) 0.042(5) -0.014(4) C48 0.163(11) 0.081(6) 0.066(6) 0.002(5) -0.009(6) -0.023(6) C49 0.115(9) 0.164(11) 0.173(11) -0.083(9) 0.050(9) -0.043(8) C50 0.122(11) 0.135(12) 0.154(13) -0.056(10) 0.045(9) -0.034(9) C51 0.155(10) 0.135(10) 0.125(10) -0.090(8) 0.043(9) -0.065(9) C52 0.083(6) 0.129(9) 0.145(10) -0.101(8) 0.035(6) -0.042(6) C53 0.138(8) 0.123(7) 0.128(8) -0.083(6) 0.041(6) -0.054(6) C54 0.116(9) 0.096(7) 0.110(8) -0.061(6) 0.038(7) -0.046(6) C55 0.150(12) 0.124(11) 0.154(13) -0.078(9) 0.060(10) -0.059(9) C56 0.171(12) 0.195(13) 0.204(13) -0.107(11) 0.059(10) -0.087(10) C57 0.203(19) 0.165(18) 0.137(16) -0.036(15) -0.024(15) -0.002(15) O7 0.083(13) 0.147(17) 0.115(15) 0.013(14) -0.037(12) 0.004(13) C57' 0.203(19) 0.165(18) 0.137(16) -0.036(15) -0.024(15) -0.002(15) O7' 0.104(10) 0.048(8) 0.083(9) -0.010(7) 0.000(8) -0.002(7) C58 0.172(12) 0.147(11) 0.175(13) -0.079(10) -0.059(10) 0.074(10) O8 0.121(5) 0.074(4) 0.176(7) -0.023(4) -0.072(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N5 2.108(4) . ? Rh1 C30 2.128(4) . ? Rh1 C27 2.130(4) . ? Rh1 C29 2.149(5) . ? Rh1 C31 2.162(4) . ? Rh1 N2 2.166(4) . ? Rh1 C28 2.171(5) . ? Rh1 N1 2.173(4) . ? Rh2 N6 2.102(4) 3_665 ? Rh2 C37 2.129(5) . ? Rh2 C39 2.130(5) . ? Rh2 C41 2.138(5) . ? Rh2 N4 2.140(4) . ? Rh2 C38 2.151(5) . ? Rh2 C40 2.152(5) . ? Rh2 N3 2.198(4) . ? N1 C7 1.324(6) . ? N1 C1 1.386(6) . ? N2 C8 1.334(5) . ? N2 C9 1.389(6) . ? N3 C8 1.317(6) . ? N3 C14 1.407(6) . ? N4 C7 1.338(6) . ? N4 C6 1.409(6) . ? N5 C21 1.346(6) . ? N5 C17 1.348(6) . ? N6 C26 1.342(6) . ? N6 C22 1.344(6) . ? N6 Rh2 2.102(4) 3_665 ? S1 O3 1.422(4) . ? S1 O2 1.422(4) . ? S1 O1 1.428(4) . ? S1 C47 1.830(9) . ? S2 O5 1.376(7) . ? S2 O4 1.381(6) . ? S2 O6 1.395(7) . ? S2 C48 1.774(13) . ? F1 C47 1.329(8) . ? F2 C47 1.345(10) . ? F3 C47 1.296(9) . ? F4 C48 1.332(11) . ? F5 C48 1.316(11) . ? F6 C48 1.335(12) . ? C1 C2 1.360(7) . ? C1 C6 1.431(7) . ? C2 C3 1.403(7) . ? C3 C4 1.399(8) . ? C4 C5 1.352(8) . ? C5 C6 1.389(6) . ? C7 C8 1.432(6) . ? C9 C10 1.389(6) . ? C9 C14 1.401(7) . ? C10 C11 1.375(7) . ? C11 C12 1.404(7) . ? C12 C13 1.365(7) . ? C13 C14 1.395(7) . ? C15 C16 1.308(8) . ? C15 C19 1.466(6) . ? C16 C24 1.462(7) . ? C17 C18 1.362(6) . ? C18 C19 1.404(7) . ? C19 C20 1.380(7) . ? C20 C21 1.385(7) . ? C22 C23 1.374(7) . ? C23 C24 1.390(7) . ? C24 C25 1.378(8) . ? C25 C26 1.373(7) . ? C27 C31 1.420(7) . ? C27 C28 1.437(7) . ? C27 C32 1.492(7) . ? C28 C29 1.422(7) . ? C28 C33 1.471(7) . ? C29 C30 1.432(7) . ? C29 C34 1.480(7) . ? C30 C31 1.420(7) . ? C30 C35 1.496(7) . ? C31 C36 1.477(7) . ? C37 C38 1.353(9) . ? C37 C41 1.440(9) . ? C37 C42 1.553(9) . ? C38 C39 1.415(8) . ? C38 C43 1.503(9) . ? C39 C40 1.408(7) . ? C39 C44 1.483(8) . ? C40 C41 1.462(8) . ? C40 C45 1.478(8) . ? C41 C46 1.470(9) . ? C49 C50 1.273(16) . ? C49 C54 1.328(16) . ? C49 C57 1.76(3) . ? C50 C51 1.344(18) . ? C51 C52 1.397(17) . ? C52 C53 1.480(16) . ? C52 C55 1.522(19) . ? C53 C53 1.37(2) 3_665 ? C53 C54 1.471(18) . ? C54 C56 1.519(19) 3_665 ? C55 C56 1.331(19) . ? C56 C54 1.519(19) 3_665 ? C57 O7 1.265(18) . ? C58 O8 1.394(13) . ? 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 N5 Rh1 C30 161.46(18) . . ? N5 Rh1 C27 104.05(16) . . ? C30 Rh1 C27 65.17(18) . . ? N5 Rh1 C29 123.39(18) . . ? C30 Rh1 C29 39.1(2) . . ? C27 Rh1 C29 64.84(19) . . ? N5 Rh1 C31 139.06(17) . . ? C30 Rh1 C31 38.65(18) . . ? C27 Rh1 C31 38.62(18) . . ? C29 Rh1 C31 64.68(18) . . ? N5 Rh1 N2 89.44(14) . . ? C30 Rh1 N2 108.43(18) . . ? C27 Rh1 N2 112.26(17) . . ? C29 Rh1 N2 147.13(17) . . ? C31 Rh1 N2 92.37(16) . . ? N5 Rh1 C28 96.72(16) . . ? C30 Rh1 C28 65.25(19) . . ? C27 Rh1 C28 39.03(19) . . ? C29 Rh1 C28 38.43(19) . . ? C31 Rh1 C28 64.87(18) . . ? N2 Rh1 C28 151.26(16) . . ? N5 Rh1 N1 88.97(14) . . ? C30 Rh1 N1 99.02(16) . . ? C27 Rh1 N1 162.45(17) . . ? C29 Rh1 N1 98.24(17) . . ? C31 Rh1 N1 131.49(17) . . ? N2 Rh1 N1 79.06(14) . . ? C28 Rh1 N1 128.91(17) . . ? N6 Rh2 C37 158.7(2) 3_665 . ? N6 Rh2 C39 104.38(18) 3_665 . ? C37 Rh2 C39 63.7(2) . . ? N6 Rh2 C41 120.4(2) 3_665 . ? C37 Rh2 C41 39.4(2) . . ? C39 Rh2 C41 65.4(2) . . ? N6 Rh2 N4 90.02(16) 3_665 . ? C37 Rh2 N4 110.4(2) . . ? C39 Rh2 N4 109.43(18) . . ? C41 Rh2 N4 149.6(2) . . ? N6 Rh2 C38 140.6(2) 3_665 . ? C37 Rh2 C38 36.9(2) . . ? C39 Rh2 C38 38.6(2) . . ? C41 Rh2 C38 64.7(2) . . ? N4 Rh2 C38 92.26(19) . . ? N6 Rh2 C40 94.38(18) 3_665 . ? C37 Rh2 C40 65.1(2) . . ? C39 Rh2 C40 38.4(2) . . ? C41 Rh2 C40 39.8(2) . . ? N4 Rh2 C40 147.46(18) . . ? C38 Rh2 C40 64.5(2) . . ? N6 Rh2 N3 88.42(14) 3_665 . ? C37 Rh2 N3 101.21(19) . . ? C39 Rh2 N3 164.26(18) . . ? C41 Rh2 N3 100.35(18) . . ? N4 Rh2 N3 79.17(14) . . ? C38 Rh2 N3 130.60(19) . . ? C40 Rh2 N3 133.09(18) . . ? C7 N1 C1 103.9(4) . . ? C7 N1 Rh1 108.8(3) . . ? C1 N1 Rh1 147.2(3) . . ? C8 N2 C9 102.4(4) . . ? C8 N2 Rh1 109.0(3) . . ? C9 N2 Rh1 148.5(3) . . ? C8 N3 C14 101.9(4) . . ? C8 N3 Rh2 108.6(3) . . ? C14 N3 Rh2 149.3(3) . . ? C7 N4 C6 101.9(4) . . ? C7 N4 Rh2 109.8(3) . . ? C6 N4 Rh2 148.3(3) . . ? C21 N5 C17 117.3(4) . . ? C21 N5 Rh1 122.1(3) . . ? C17 N5 Rh1 120.6(3) . . ? C26 N6 C22 116.7(4) . . ? C26 N6 Rh2 122.3(3) . 3_665 ? C22 N6 Rh2 120.9(3) . 3_665 ? O3 S1 O2 115.4(3) . . ? O3 S1 O1 115.9(3) . . ? O2 S1 O1 115.6(3) . . ? O3 S1 C47 100.7(3) . . ? O2 S1 C47 103.4(4) . . ? O1 S1 C47 102.6(3) . . ? O5 S2 O4 115.6(6) . . ? O5 S2 O6 117.9(6) . . ? O4 S2 O6 114.4(5) . . ? O5 S2 C48 101.0(6) . . ? O4 S2 C48 101.6(5) . . ? O6 S2 C48 102.5(5) . . ? C2 C1 N1 132.1(5) . . ? C2 C1 C6 120.5(4) . . ? N1 C1 C6 107.3(4) . . ? C1 C2 C3 118.2(5) . . ? C4 C3 C2 120.4(5) . . ? C5 C4 C3 122.2(5) . . ? C4 C5 C6 117.9(5) . . ? C5 C6 N4 130.8(4) . . ? C5 C6 C1 120.7(4) . . ? N4 C6 C1 108.3(4) . . ? N1 C7 N4 118.5(4) . . ? N1 C7 C8 120.4(4) . . ? N4 C7 C8 119.7(4) . . ? N3 C8 N2 118.9(4) . . ? N3 C8 C7 120.6(4) . . ? N2 C8 C7 119.7(4) . . ? N2 C9 C10 130.3(4) . . ? N2 C9 C14 108.3(4) . . ? C10 C9 C14 121.4(4) . . ? C11 C10 C9 117.7(5) . . ? C10 C11 C12 120.6(5) . . ? C13 C12 C11 122.3(5) . . ? C12 C13 C14 117.4(5) . . ? C13 C14 C9 120.6(4) . . ? C13 C14 N3 130.9(4) . . ? C9 C14 N3 108.5(4) . . ? C16 C15 C19 125.7(5) . . ? C15 C16 C24 125.9(5) . . ? N5 C17 C18 122.8(4) . . ? C17 C18 C19 120.5(5) . . ? C20 C19 C18 116.3(4) . . ? C20 C19 C15 121.9(5) . . ? C18 C19 C15 121.8(5) . . ? C19 C20 C21 120.5(5) . . ? N5 C21 C20 122.5(5) . . ? N6 C22 C23 122.7(5) . . ? C22 C23 C24 120.3(5) . . ? C25 C24 C23 116.7(5) . . ? C25 C24 C16 119.4(5) . . ? C23 C24 C16 123.9(5) . . ? C26 C25 C24 120.0(5) . . ? N6 C26 C25 123.5(5) . . ? C31 C27 C28 108.9(4) . . ? C31 C27 C32 126.2(5) . . ? C28 C27 C32 124.5(5) . . ? C31 C27 Rh1 71.9(3) . . ? C28 C27 Rh1 72.0(3) . . ? C32 C27 Rh1 128.3(3) . . ? C29 C28 C27 106.7(4) . . ? C29 C28 C33 128.0(5) . . ? C27 C28 C33 125.2(5) . . ? C29 C28 Rh1 70.0(3) . . ? C27 C28 Rh1 68.9(3) . . ? C33 C28 Rh1 128.3(4) . . ? C28 C29 C30 108.6(4) . . ? C28 C29 C34 125.9(5) . . ? C30 C29 C34 125.3(5) . . ? C28 C29 Rh1 71.6(3) . . ? C30 C29 Rh1 69.7(3) . . ? C34 C29 Rh1 127.1(4) . . ? C31 C30 C29 107.9(4) . . ? C31 C30 C35 126.7(5) . . ? C29 C30 C35 125.1(5) . . ? C31 C30 Rh1 72.0(3) . . ? C29 C30 Rh1 71.2(3) . . ? C35 C30 Rh1 126.8(4) . . ? C27 C31 C30 107.7(4) . . ? C27 C31 C36 126.1(5) . . ? C30 C31 C36 126.2(5) . . ? C27 C31 Rh1 69.5(2) . . ? C30 C31 Rh1 69.4(2) . . ? C36 C31 Rh1 126.0(3) . . ? C38 C37 C41 110.4(5) . . ? C38 C37 C42 124.4(7) . . ? C41 C37 C42 125.1(7) . . ? C38 C37 Rh2 72.5(3) . . ? C41 C37 Rh2 70.6(3) . . ? C42 C37 Rh2 125.4(5) . . ? C37 C38 C39 108.5(5) . . ? C37 C38 C43 126.9(6) . . ? C39 C38 C43 124.5(6) . . ? C37 C38 Rh2 70.7(3) . . ? C39 C38 Rh2 69.9(3) . . ? C43 C38 Rh2 126.1(4) . . ? C40 C39 C38 109.0(5) . . ? C40 C39 C44 123.5(5) . . ? C38 C39 C44 127.2(6) . . ? C40 C39 Rh2 71.7(3) . . ? C38 C39 Rh2 71.5(3) . . ? C44 C39 Rh2 128.5(4) . . ? C39 C40 C41 106.9(5) . . ? C39 C40 C45 126.9(6) . . ? C41 C40 C45 126.2(6) . . ? C39 C40 Rh2 70.0(3) . . ? C41 C40 Rh2 69.6(3) . . ? C45 C40 Rh2 125.4(4) . . ? C37 C41 C40 105.1(5) . . ? C37 C41 C46 127.1(7) . . ? C40 C41 C46 127.5(7) . . ? C37 C41 Rh2 70.0(3) . . ? C40 C41 Rh2 70.6(3) . . ? C46 C41 Rh2 128.1(4) . . ? F3 C47 F1 109.2(6) . . ? F3 C47 F2 108.2(8) . . ? F1 C47 F2 106.8(8) . . ? F3 C47 S1 111.7(7) . . ? F1 C47 S1 110.1(6) . . ? F2 C47 S1 110.7(5) . . ? F5 C48 F4 105.3(9) . . ? F5 C48 F6 101.8(10) . . ? F4 C48 F6 102.0(10) . . ? F5 C48 S2 114.1(9) . . ? F4 C48 S2 118.4(8) . . ? F6 C48 S2 113.3(7) . . ? C50 C49 C54 133.8(19) . . ? C50 C49 C57 115.3(18) . . ? C54 C49 C57 110.9(17) . . ? C49 C50 C51 114.4(17) . . ? C50 C51 C52 127.0(16) . . ? C51 C52 C53 112.8(15) . . ? C51 C52 C55 128.6(13) . . ? C53 C52 C55 118.6(13) . . ? C53 C53 C54 122.8(19) 3_665 . ? C53 C53 C52 117(2) 3_665 . ? C54 C53 C52 120.1(12) . . ? C49 C54 C53 112.0(13) . . ? C49 C54 C56 126.3(16) . 3_665 ? C53 C54 C56 121.7(13) . 3_665 ? C56 C55 C52 125.8(17) . . ? C55 C56 C54 114.0(19) . 3_665 ? O7 C57 C49 121(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O1 0.86(2) 2.05(6) 2.801(7) 145(10) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 1.000 0.000 461.1 84.4 2 0.043 0.059 0.060 10.1 -2.2 3 0.104 0.984 0.238 9.2 -0.2 4 0.896 0.484 0.262 9.2 -0.9 5 0.500 0.500 0.500 461.1 83.9 6 0.957 0.559 0.440 10.1 -1.9 7 0.043 0.441 0.560 10.1 -2.2 8 0.104 0.516 0.738 9.1 -0.5 9 0.896 0.016 0.762 9.2 -0.3 10 0.957 0.941 0.940 10.1 -2.0 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.559 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.132 _database_code_depnum_ccdc_archive 'CCDC 927804' ####################################################################### # # 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_global # Attachment '3.cif' data_3 #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H116 F12 N12 O14 Rh4 S4' _chemical_formula_weight 2525.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9496(2) _cell_length_b 23.8189(4) _cell_length_c 18.5603(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.9010(10) _cell_angle_gamma 90.00 _cell_volume 5670.49(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6785 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 68.14 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 6.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4859 _exptl_absorpt_correction_T_max 0.5570 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.17 _diffrn_reflns_number 25377 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 60.49 _reflns_number_total 8029 _reflns_number_gt 6435 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In this data, there is one disordered diethyl ether molecule in asymmetric unit which could not be restrained properly and it was omitted by SQUEEZE algorithm. On of two pentamethylcyclopentadienyl ligands and triflate anions in the asymmetric unit were disordered and they were refined to two idealized positions (78:22 in Cp* ligand and 60:40 in triflate anion). 19 ISOR instructions and 12 DFIX instructions were used to restrain the disordered Cp* ligand and the triflate anion so that there were 126 restraints in this data. ; _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^)+(0.1643P)^2^+5.4718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8029 _refine_ls_number_parameters 736 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2246 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.005 _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 0.99165(4) 0.10342(2) 0.67420(3) 0.0381(2) Uani 1 1 d . . . Rh2 Rh 0.66674(5) 0.25862(2) 0.66762(3) 0.0427(2) Uani 1 1 d . . . N1 N 0.9346(5) 0.1787(2) 0.6178(3) 0.0410(14) Uani 1 1 d . A . N2 N 0.8733(5) 0.1291(2) 0.7407(3) 0.0386(13) Uani 1 1 d . . . N3 N 0.7382(5) 0.1907(3) 0.7350(3) 0.0419(14) Uani 1 1 d . A . N4 N 0.7996(5) 0.2397(2) 0.6118(3) 0.0390(14) Uani 1 1 d . A . N5 N 0.8642(5) 0.0628(3) 0.6106(3) 0.0394(13) Uani 1 1 d . . . N6 N 0.5887(5) 0.1937(2) 0.6036(3) 0.0422(14) Uani 1 1 d . A . S2 S 0.2626(4) 0.1742(3) 0.3690(2) 0.142(2) Uani 1 1 d . . . O4 O 0.2610(13) 0.2185(7) 0.3168(10) 0.192(7) Uani 1 1 d . . . O5 O 0.3427(10) 0.1368(4) 0.3711(8) 0.133(4) Uani 1 1 d . . . O6 O 0.1701(10) 0.1514(8) 0.3876(10) 0.179(6) Uani 1 1 d . . . F4 F 0.2429(13) 0.2673(7) 0.4561(9) 0.217(7) Uani 1 1 d . . . F5 F 0.3205(13) 0.1991(10) 0.5112(7) 0.246(9) Uani 1 1 d . . . F6 F 0.4023(12) 0.2560(7) 0.4419(9) 0.194(6) Uani 1 1 d . . . C1 C 0.9332(6) 0.2097(3) 0.5540(4) 0.0425(17) Uani 1 1 d . A . C2 C 0.9954(7) 0.2088(4) 0.4993(5) 0.0527(19) Uani 1 1 d . . . H2 H 1.0526 0.1836 0.5016 0.063 Uiso 1 1 calc R . . C3 C 0.9730(8) 0.2453(4) 0.4405(6) 0.068(3) Uani 1 1 d . . . H3 H 1.0146 0.2448 0.4022 0.082 Uiso 1 1 calc R . . C4 C 0.8911(8) 0.2817(4) 0.4381(5) 0.070(3) Uani 1 1 d . . . H4 H 0.8776 0.3062 0.3975 0.084 Uiso 1 1 calc R . . C5 C 0.8274(7) 0.2849(4) 0.4913(5) 0.053(2) Uani 1 1 d . A . H5 H 0.7713 0.3109 0.4879 0.063 Uiso 1 1 calc R . . C6 C 0.8482(6) 0.2483(3) 0.5509(5) 0.0445(18) Uani 1 1 d . . . C7 C 0.8560(6) 0.1995(3) 0.6467(4) 0.0390(16) Uani 1 1 d . . . C8 C 0.8247(6) 0.1733(3) 0.7127(4) 0.0406(16) Uani 1 1 d . A . C9 C 0.8102(6) 0.1128(3) 0.7919(4) 0.0424(17) Uani 1 1 d . A . C10 C 0.8183(8) 0.0678(4) 0.8409(4) 0.056(2) Uani 1 1 d . . . H10 H 0.8746 0.0419 0.8438 0.068 Uiso 1 1 calc R . . C11 C 0.7427(9) 0.0627(5) 0.8837(5) 0.072(3) Uani 1 1 d . . . H11 H 0.7465 0.0322 0.9170 0.086 Uiso 1 1 calc R . . C12 C 0.6603(9) 0.0993(4) 0.8817(5) 0.066(3) Uani 1 1 d . . . H12 H 0.6096 0.0936 0.9134 0.079 Uiso 1 1 calc R . . C13 C 0.6502(7) 0.1446(4) 0.8340(4) 0.056(2) Uani 1 1 d . A . H13 H 0.5937 0.1702 0.8327 0.067 Uiso 1 1 calc R . . C14 C 0.7267(7) 0.1512(3) 0.7877(4) 0.0453(18) Uani 1 1 d . . . C15 C 0.5812(6) 0.0003(3) 0.4872(4) 0.0441(17) Uani 1 1 d . . . H15 H 0.5940 -0.0109 0.4373 0.053 Uiso 1 1 calc R . . C16 C 0.4871(6) 0.0447(3) 0.4817(4) 0.0440(17) Uani 1 1 d . . . H16 H 0.4600 0.0532 0.4297 0.053 Uiso 1 1 calc R . . C17 C 0.8068(6) 0.0256(3) 0.6395(4) 0.0481(18) Uani 1 1 d . . . H17 H 0.8282 0.0145 0.6885 0.058 Uiso 1 1 calc R . . C18 C 0.7170(6) 0.0017(3) 0.6028(4) 0.0454(17) Uani 1 1 d . . . H18 H 0.6792 -0.0253 0.6263 0.055 Uiso 1 1 calc R . . C19 C 0.6829(6) 0.0175(3) 0.5320(4) 0.0416(17) Uani 1 1 d . . . C20 C 0.7462(6) 0.0542(3) 0.5000(4) 0.0458(18) Uani 1 1 d . . . H20 H 0.7286 0.0642 0.4503 0.055 Uiso 1 1 calc R . . C21 C 0.8341(6) 0.0761(3) 0.5398(4) 0.0462(18) Uani 1 1 d . . . H21 H 0.8755 0.1017 0.5169 0.055 Uiso 1 1 calc R . . C22 C 0.5426(7) 0.1517(3) 0.6347(4) 0.0472(18) Uani 1 1 d . . . H22 H 0.5348 0.1550 0.6847 0.057 Uiso 1 1 calc R A . C23 C 0.5055(6) 0.1035(3) 0.5978(4) 0.0430(17) Uani 1 1 d . A . H23 H 0.4757 0.0742 0.6229 0.052 Uiso 1 1 calc R . . C24 C 0.5122(6) 0.0983(3) 0.5243(4) 0.0404(16) Uani 1 1 d . . . C25 C 0.5534(8) 0.1435(4) 0.4914(4) 0.061(2) Uani 1 1 d . A . H25 H 0.5557 0.1429 0.4405 0.073 Uiso 1 1 calc R . . C26 C 0.5914(7) 0.1899(3) 0.5322(4) 0.053(2) Uani 1 1 d . . . H26 H 0.6205 0.2201 0.5082 0.064 Uiso 1 1 calc R A . C27 C 1.1351(6) 0.0814(3) 0.6363(5) 0.0505(19) Uani 1 1 d . . . C28 C 1.1543(6) 0.1249(4) 0.6874(5) 0.056(2) Uani 1 1 d . . . C29 C 1.1256(7) 0.1081(4) 0.7551(5) 0.060(2) Uani 1 1 d . . . C30 C 1.0919(7) 0.0513(4) 0.7481(5) 0.055(2) Uani 1 1 d . . . C31 C 1.0984(7) 0.0341(3) 0.6761(5) 0.053(2) Uani 1 1 d . . . C32 C 1.1590(8) 0.0795(5) 0.5593(6) 0.073(3) Uani 1 1 d . . . H32A H 1.1556 0.1176 0.5390 0.110 Uiso 1 1 calc R . . H32B H 1.1079 0.0556 0.5300 0.110 Uiso 1 1 calc R . . H32C H 1.2291 0.0642 0.5587 0.110 Uiso 1 1 calc R . . C33 C 1.2025(9) 0.1815(5) 0.6714(7) 0.086(3) Uani 1 1 d . . . H33A H 1.2772 0.1767 0.6697 0.128 Uiso 1 1 calc R . . H33B H 1.1923 0.2083 0.7099 0.128 Uiso 1 1 calc R . . H33C H 1.1687 0.1958 0.6245 0.128 Uiso 1 1 calc R . . C34 C 1.1346(10) 0.1434(6) 0.8225(6) 0.089(4) Uani 1 1 d . . . H34A H 1.0739 0.1370 0.8476 0.134 Uiso 1 1 calc R . . H34B H 1.1377 0.1831 0.8091 0.134 Uiso 1 1 calc R . . H34C H 1.1982 0.1332 0.8547 0.134 Uiso 1 1 calc R . . C35 C 1.0680(9) 0.0150(6) 0.8090(7) 0.090(4) Uani 1 1 d . . . H35A H 1.1316 -0.0044 0.8306 0.135 Uiso 1 1 calc R . . H35B H 1.0151 -0.0127 0.7905 0.135 Uiso 1 1 calc R . . H35C H 1.0417 0.0382 0.8461 0.135 Uiso 1 1 calc R . . C36 C 1.0712(9) -0.0231(4) 0.6442(7) 0.079(3) Uani 1 1 d . . . H36A H 1.1169 -0.0514 0.6704 0.119 Uiso 1 1 calc R . . H36B H 1.0804 -0.0233 0.5927 0.119 Uiso 1 1 calc R . . H36C H 0.9984 -0.0318 0.6489 0.119 Uiso 1 1 calc R . . C48 C 0.304(2) 0.2234(13) 0.4437(11) 0.173(11) Uani 1 1 d . . . C37 C 0.5302(5) 0.3122(3) 0.6695(4) 0.052(3) Uani 0.783(14) 1 d PGU A 1 C38 C 0.5800(6) 0.3042(3) 0.7414(3) 0.056(3) Uani 0.783(14) 1 d PGU A 1 C39 C 0.6825(6) 0.3255(3) 0.7458(4) 0.069(4) Uani 0.783(14) 1 d PGU A 1 C40 C 0.6961(5) 0.3465(3) 0.6766(4) 0.074(5) Uani 0.783(14) 1 d PGU A 1 C41 C 0.6020(5) 0.3383(3) 0.6294(4) 0.060(4) Uani 0.783(14) 1 d PGU A 1 C42 C 0.4203(6) 0.2957(4) 0.6408(6) 0.103(6) Uani 0.783(14) 1 d PGU A 1 H42A H 0.3736 0.3274 0.6455 0.154 Uiso 0.783(14) 1 calc PR A 1 H42B H 0.3994 0.2637 0.6687 0.154 Uiso 0.783(14) 1 calc PR A 1 H42C H 0.4163 0.2852 0.5894 0.154 Uiso 0.783(14) 1 calc PR A 1 C43 C 0.5323(10) 0.2779(4) 0.8025(5) 0.111(7) Uani 0.783(14) 1 d PGU A 1 H43A H 0.5830 0.2782 0.8469 0.167 Uiso 0.783(14) 1 calc PR A 1 H43B H 0.5125 0.2390 0.7897 0.167 Uiso 0.783(14) 1 calc PR A 1 H43C H 0.4702 0.2991 0.8108 0.167 Uiso 0.783(14) 1 calc PR A 1 C44 C 0.7629(9) 0.3256(5) 0.8123(6) 0.119(7) Uani 0.783(14) 1 d PGU A 1 H44A H 0.7468 0.3555 0.8453 0.179 Uiso 0.783(14) 1 calc PR A 1 H44B H 0.8320 0.3322 0.7980 0.179 Uiso 0.783(14) 1 calc PR A 1 H44C H 0.7624 0.2893 0.8370 0.179 Uiso 0.783(14) 1 calc PR A 1 C45 C 0.7935(8) 0.3730(4) 0.6566(7) 0.104(6) Uani 0.783(14) 1 d PGU A 1 H45A H 0.8205 0.3502 0.6194 0.156 Uiso 0.783(14) 1 calc PR A 1 H45B H 0.8460 0.3753 0.6998 0.156 Uiso 0.783(14) 1 calc PR A 1 H45C H 0.7775 0.4108 0.6374 0.156 Uiso 0.783(14) 1 calc PR A 1 C46 C 0.5818(9) 0.3545(4) 0.5506(5) 0.108(6) Uani 0.783(14) 1 d PGU A 1 H46A H 0.5584 0.3215 0.5213 0.162 Uiso 0.783(14) 1 calc PR A 1 H46B H 0.6461 0.3691 0.5352 0.162 Uiso 0.783(14) 1 calc PR A 1 H46C H 0.5277 0.3835 0.5437 0.162 Uiso 0.783(14) 1 calc PR A 1 C47 C 0.496(5) 0.4789(14) 0.7379(18) 0.063(6) Uani 0.598(16) 1 d PD B 1 F1 F 0.424(3) 0.4989(19) 0.773(2) 0.078(5) Uani 0.598(16) 1 d PD B 1 F2 F 0.4697(13) 0.4783(11) 0.6639(10) 0.113(7) Uani 0.598(16) 1 d PD B 1 F3 F 0.4977(15) 0.4239(6) 0.7558(15) 0.140(8) Uani 0.598(16) 1 d PD B 1 O1 O 0.6554(17) 0.4958(17) 0.8294(12) 0.148(15) Uani 0.598(16) 1 d PD B 1 O2 O 0.685(2) 0.4773(14) 0.7069(10) 0.078(6) Uani 0.598(16) 1 d PD B 1 O3 O 0.6081(14) 0.5654(6) 0.7408(11) 0.109(6) Uani 0.598(16) 1 d PD B 1 S1 S 0.6291(4) 0.5063(4) 0.7562(4) 0.0607(19) Uani 0.598(16) 1 d PD B 1 C37' C 0.549(2) 0.3068(12) 0.7010(16) 0.064(16) Uani 0.217(14) 1 d PGU A 2 C38' C 0.639(2) 0.3097(10) 0.7563(13) 0.044(11) Uani 0.217(14) 1 d PGU A 2 C39' C 0.7234(17) 0.3352(9) 0.7242(12) 0.035(9) Uani 0.217(14) 1 d PGU A 2 C40' C 0.6853(19) 0.3480(10) 0.6492(13) 0.049(11) Uani 0.217(14) 1 d PGU A 2 C41' C 0.578(2) 0.3304(12) 0.6348(14) 0.08(2) Uani 0.217(14) 1 d PGU A 2 C42' C 0.442(3) 0.2828(19) 0.711(3) 0.15(3) Uani 0.217(14) 1 d PGU A 2 H42D H 0.3984 0.3126 0.7272 0.221 Uiso 0.217(14) 1 calc PR A 2 H42E H 0.4506 0.2527 0.7473 0.221 Uiso 0.217(14) 1 calc PR A 2 H42F H 0.4082 0.2676 0.6645 0.221 Uiso 0.217(14) 1 calc PR A 2 C43' C 0.644(3) 0.2893(17) 0.835(2) 0.12(2) Uani 0.217(14) 1 d PGU A 2 H43D H 0.5878 0.2626 0.8388 0.181 Uiso 0.217(14) 1 calc PR A 2 H43E H 0.6375 0.3214 0.8671 0.181 Uiso 0.217(14) 1 calc PR A 2 H43F H 0.7116 0.2708 0.8501 0.181 Uiso 0.217(14) 1 calc PR A 2 C44' C 0.834(3) 0.3466(17) 0.763(2) 0.14(3) Uani 0.217(14) 1 d PGU A 2 H44D H 0.8369 0.3844 0.7842 0.210 Uiso 0.217(14) 1 calc PR A 2 H44E H 0.8838 0.3438 0.7282 0.210 Uiso 0.217(14) 1 calc PR A 2 H44F H 0.8514 0.3189 0.8020 0.210 Uiso 0.217(14) 1 calc PR A 2 C45' C 0.748(3) 0.3754(17) 0.594(2) 0.108(6) Uani 0.217(14) 1 d PG A 2 H45D H 0.7440 0.4164 0.5982 0.162 Uiso 0.217(14) 1 calc PR A 2 H45E H 0.7198 0.3638 0.5449 0.162 Uiso 0.217(14) 1 calc PR A 2 H45F H 0.8214 0.3637 0.6048 0.162 Uiso 0.217(14) 1 calc PR A 2 C46' C 0.506(3) 0.336(2) 0.562(2) 0.097(18) Uani 0.217(14) 1 d PGU A 2 H46D H 0.4673 0.3714 0.5612 0.145 Uiso 0.217(14) 1 calc PR A 2 H46E H 0.4570 0.3045 0.5563 0.145 Uiso 0.217(14) 1 calc PR A 2 H46F H 0.5483 0.3357 0.5221 0.145 Uiso 0.217(14) 1 calc PR A 2 C47' C 0.505(8) 0.473(2) 0.725(3) 0.063(6) Uani 0.402(16) 1 d PD B 2 F1' F 0.440(5) 0.503(3) 0.755(3) 0.078(5) Uani 0.402(16) 1 d PD B 2 F2' F 0.490(3) 0.5149(18) 0.672(2) 0.172(16) Uani 0.402(16) 1 d PD B 2 F3' F 0.478(2) 0.4338(14) 0.6959(18) 0.132(12) Uani 0.402(16) 1 d PD B 2 O1' O 0.644(3) 0.5332(13) 0.8093(18) 0.106(14) Uani 0.402(16) 1 d PD B 2 O2' O 0.700(3) 0.465(2) 0.7325(16) 0.078(6) Uani 0.402(16) 1 d PD B 2 O3' O 0.619(2) 0.4328(10) 0.8281(11) 0.100(8) Uani 0.402(16) 1 d PD B 2 S1' S 0.6284(6) 0.4779(5) 0.7795(6) 0.060(3) Uani 0.402(16) 1 d PD B 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 0.0387(4) 0.0332(4) 0.0415(3) -0.0001(2) 0.0024(2) 0.0018(2) Rh2 0.0509(4) 0.0281(3) 0.0486(4) -0.0087(2) 0.0050(3) 0.0035(2) N1 0.044(4) 0.032(3) 0.047(3) -0.002(3) 0.007(3) 0.001(3) N2 0.044(3) 0.032(3) 0.038(3) 0.001(3) 0.002(3) 0.003(3) N3 0.050(4) 0.038(3) 0.037(3) -0.008(3) 0.004(3) 0.001(3) N4 0.044(4) 0.028(3) 0.046(3) -0.003(3) 0.011(3) 0.004(3) N5 0.040(3) 0.039(3) 0.039(3) -0.001(3) 0.004(2) 0.000(3) N6 0.055(4) 0.032(3) 0.039(3) -0.004(3) 0.006(3) 0.003(3) S2 0.147(4) 0.180(5) 0.106(3) 0.055(3) 0.045(3) 0.089(4) O4 0.168(14) 0.164(13) 0.228(16) 0.073(13) -0.024(12) 0.047(11) O5 0.137(10) 0.085(6) 0.190(11) 0.022(7) 0.071(8) 0.032(6) O6 0.078(8) 0.225(17) 0.228(16) -0.026(13) 0.000(9) 0.000(9) F4 0.199(15) 0.221(15) 0.231(15) -0.018(12) 0.024(12) 0.116(12) F5 0.192(15) 0.41(3) 0.129(10) 0.056(13) 0.016(9) -0.001(17) F6 0.143(11) 0.252(17) 0.192(13) -0.038(11) 0.040(10) 0.020(11) C1 0.042(4) 0.040(4) 0.045(4) 0.006(3) 0.003(3) -0.002(3) C2 0.052(5) 0.051(5) 0.057(5) 0.014(4) 0.014(4) 0.008(4) C3 0.061(6) 0.080(7) 0.065(6) 0.022(5) 0.018(5) 0.008(5) C4 0.073(7) 0.071(6) 0.066(6) 0.027(5) 0.010(5) -0.003(5) C5 0.055(5) 0.048(5) 0.056(5) 0.014(4) 0.008(4) 0.004(4) C6 0.039(4) 0.041(4) 0.052(5) 0.000(3) 0.002(3) -0.004(3) C7 0.046(4) 0.030(4) 0.041(4) 0.000(3) 0.007(3) 0.000(3) C8 0.036(4) 0.031(4) 0.054(4) -0.011(3) 0.004(3) 0.000(3) C9 0.052(5) 0.043(4) 0.031(3) -0.005(3) 0.005(3) -0.001(3) C10 0.066(6) 0.058(5) 0.045(4) 0.004(4) 0.009(4) 0.002(4) C11 0.085(7) 0.081(7) 0.051(5) 0.014(5) 0.018(5) -0.006(6) C12 0.090(7) 0.059(6) 0.056(5) -0.006(4) 0.032(5) -0.012(5) C13 0.066(6) 0.060(5) 0.044(4) -0.007(4) 0.013(4) 0.001(4) C14 0.056(5) 0.044(4) 0.038(4) -0.010(3) 0.012(3) -0.005(3) C15 0.049(4) 0.047(4) 0.037(4) -0.009(3) 0.009(3) -0.009(3) C16 0.061(5) 0.041(4) 0.030(3) -0.001(3) 0.005(3) -0.012(3) C17 0.047(5) 0.047(5) 0.048(4) 0.013(4) -0.002(3) -0.005(3) C18 0.049(5) 0.043(4) 0.046(4) -0.003(3) 0.012(3) -0.007(3) C19 0.050(4) 0.039(4) 0.039(4) -0.019(3) 0.015(3) -0.011(3) C20 0.047(4) 0.052(5) 0.037(4) -0.005(3) 0.003(3) -0.012(3) C21 0.051(5) 0.047(4) 0.043(4) -0.004(3) 0.011(3) -0.009(3) C22 0.055(5) 0.044(4) 0.044(4) -0.011(3) 0.011(3) -0.003(3) C23 0.044(4) 0.039(4) 0.046(4) -0.003(3) 0.006(3) -0.007(3) C24 0.041(4) 0.043(4) 0.036(4) -0.001(3) 0.001(3) -0.010(3) C25 0.085(7) 0.063(6) 0.032(4) 0.001(4) 0.001(4) -0.021(5) C26 0.077(6) 0.041(4) 0.040(4) 0.003(3) 0.000(4) -0.012(4) C27 0.046(5) 0.044(5) 0.063(5) 0.006(4) 0.010(4) 0.006(4) C28 0.037(4) 0.051(5) 0.076(6) 0.000(5) -0.008(4) -0.002(4) C29 0.051(5) 0.059(6) 0.063(5) -0.003(4) -0.014(4) 0.004(4) C30 0.044(5) 0.065(6) 0.053(5) 0.007(4) 0.001(4) 0.014(4) C31 0.047(5) 0.040(4) 0.071(5) 0.006(4) 0.006(4) 0.015(3) C32 0.063(6) 0.083(7) 0.078(6) 0.014(6) 0.025(5) 0.023(5) C33 0.071(7) 0.069(7) 0.113(9) 0.014(6) 0.001(6) -0.023(6) C34 0.075(8) 0.107(10) 0.079(7) -0.014(7) -0.013(6) 0.005(6) C35 0.070(7) 0.114(10) 0.090(8) 0.051(7) 0.026(6) 0.041(7) C36 0.077(7) 0.046(5) 0.117(9) -0.017(6) 0.021(6) 0.012(5) C48 0.16(2) 0.26(3) 0.106(13) 0.037(16) 0.040(13) 0.10(2) C37 0.047(6) 0.052(7) 0.058(8) -0.014(5) 0.005(5) 0.024(5) C38 0.075(9) 0.048(6) 0.045(6) -0.015(5) 0.008(6) 0.027(6) C39 0.064(9) 0.051(8) 0.090(9) -0.034(7) 0.008(8) -0.001(7) C40 0.078(9) 0.037(7) 0.112(13) -0.022(7) 0.027(9) -0.005(6) C41 0.072(8) 0.033(6) 0.083(9) 0.010(6) 0.034(7) 0.020(6) C42 0.068(9) 0.103(11) 0.139(13) -0.038(10) 0.019(8) 0.034(8) C43 0.141(14) 0.099(11) 0.108(11) -0.017(9) 0.070(11) 0.035(10) C44 0.130(13) 0.090(11) 0.122(12) -0.057(10) -0.041(10) 0.016(10) C45 0.100(11) 0.046(7) 0.170(15) -0.023(9) 0.034(10) -0.004(7) C46 0.125(13) 0.094(10) 0.110(11) 0.027(9) 0.033(10) 0.052(10) C47 0.072(14) 0.068(10) 0.055(14) -0.020(9) 0.026(13) 0.028(8) F1 0.061(13) 0.103(8) 0.080(18) -0.023(12) 0.044(7) -0.001(8) F2 0.091(10) 0.150(19) 0.094(10) -0.059(13) -0.006(7) 0.021(12) F3 0.127(14) 0.056(8) 0.24(2) 0.023(12) 0.045(15) 0.009(8) O1 0.062(11) 0.31(5) 0.063(12) 0.010(19) -0.008(8) 0.00(2) O2 0.065(9) 0.110(16) 0.061(13) -0.019(12) 0.017(10) 0.006(7) O3 0.114(13) 0.083(10) 0.132(15) -0.011(10) 0.021(11) -0.008(9) S1 0.064(3) 0.077(4) 0.044(3) -0.009(3) 0.0161(19) 0.005(2) C37' 0.06(2) 0.06(2) 0.07(2) -0.033(17) -0.002(17) 0.015(15) C38' 0.042(19) 0.035(16) 0.059(18) 0.018(14) 0.020(15) 0.019(14) C39' 0.038(12) 0.029(12) 0.038(12) -0.016(9) 0.003(9) 0.004(9) C40' 0.07(2) 0.039(18) 0.037(16) -0.003(12) 0.019(14) 0.019(15) C41' 0.09(3) 0.06(2) 0.09(3) 0.002(18) -0.007(18) 0.004(18) C42' 0.14(4) 0.15(4) 0.16(4) -0.01(2) 0.04(2) 0.01(2) C43' 0.13(3) 0.12(3) 0.11(3) -0.006(19) 0.025(19) -0.019(19) C44' 0.13(3) 0.15(4) 0.14(3) 0.00(2) 0.03(2) 0.00(2) C45' 0.125(13) 0.094(10) 0.110(11) 0.027(9) 0.033(10) 0.052(10) C46' 0.10(2) 0.09(2) 0.10(2) 0.004(18) 0.003(18) 0.031(18) C47' 0.072(14) 0.068(10) 0.055(14) -0.020(9) 0.026(13) 0.028(8) F1' 0.061(13) 0.103(8) 0.080(18) -0.023(12) 0.044(7) -0.001(8) F2' 0.20(4) 0.15(3) 0.15(3) 0.00(2) -0.04(2) 0.05(3) F3' 0.135(19) 0.11(2) 0.127(19) -0.071(18) -0.050(16) 0.071(17) O1' 0.10(2) 0.14(2) 0.09(2) -0.07(2) 0.06(2) -0.05(2) O2' 0.065(9) 0.110(16) 0.061(13) -0.019(12) 0.017(10) 0.006(7) O3' 0.12(2) 0.087(15) 0.082(13) -0.002(12) -0.007(12) -0.017(13) S1' 0.064(4) 0.072(6) 0.044(5) -0.003(4) 0.011(3) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N5 2.126(6) . ? Rh1 C29 2.136(9) . ? Rh1 C27 2.140(8) . ? Rh1 C30 2.148(8) . ? Rh1 C28 2.149(8) . ? Rh1 C31 2.151(8) . ? Rh1 N1 2.155(6) . ? Rh1 N2 2.184(6) . ? Rh2 C37' 2.07(3) . ? Rh2 C41' 2.11(3) . ? Rh2 C38' 2.12(2) . ? Rh2 N6 2.119(6) . ? Rh2 C40 2.131(6) . ? Rh2 C39 2.145(6) . ? Rh2 C41 2.155(6) . ? Rh2 N3 2.173(6) . ? Rh2 N4 2.173(6) . ? Rh2 C40' 2.17(2) . ? Rh2 C38 2.178(5) . ? Rh2 C39' 2.18(2) . ? N1 C7 1.311(10) . ? N1 C1 1.393(10) . ? N2 C8 1.298(10) . ? N2 C9 1.390(10) . ? N3 C8 1.313(10) . ? N3 C14 1.380(10) . ? N4 C7 1.321(10) . ? N4 C6 1.383(11) . ? N5 C17 1.316(10) . ? N5 C21 1.357(10) . ? N6 C26 1.335(10) . ? N6 C22 1.336(10) . ? S2 O5 1.365(11) . ? S2 O6 1.401(16) . ? S2 O4 1.430(16) . ? S2 C48 1.84(3) . ? F4 C48 1.35(2) . ? F5 C48 1.37(2) . ? F6 C48 1.49(3) . ? C1 C2 1.380(12) . ? C1 C6 1.430(11) . ? C2 C3 1.394(13) . ? C3 C4 1.366(15) . ? C4 C5 1.372(14) . ? C5 C6 1.405(12) . ? C7 C8 1.480(11) . ? C9 C10 1.401(12) . ? C9 C14 1.410(12) . ? C10 C11 1.349(14) . ? C11 C12 1.373(16) . ? C12 C13 1.391(14) . ? C13 C14 1.406(12) . ? C15 C19 1.515(11) . ? C15 C16 1.551(10) 3_656 ? C15 C16 1.607(11) . ? C16 C24 1.513(11) . ? C16 C15 1.551(10) 3_656 ? C17 C18 1.386(11) . ? C18 C19 1.381(11) . ? C19 C20 1.386(11) . ? C20 C21 1.373(11) . ? C22 C23 1.388(11) . ? C23 C24 1.385(11) . ? C24 C25 1.380(12) . ? C25 C26 1.391(12) . ? C27 C28 1.403(13) . ? C27 C31 1.463(12) . ? C27 C32 1.504(13) . ? C28 C29 1.418(14) . ? C28 C33 1.532(13) . ? C29 C30 1.420(13) . ? C29 C34 1.498(15) . ? C30 C31 1.412(13) . ? C30 C35 1.489(14) . ? C31 C36 1.507(13) . ? C37 C38 1.412(4) . ? C37 C41 1.413(4) . ? C37 C42 1.502(4) . ? C38 C39 1.413(4) . ? C38 C43 1.502(4) . ? C39 C40 1.412(4) . ? C39 C44 1.502(4) . ? C40 C41 1.413(4) . ? C40 C45 1.502(4) . ? C41 C46 1.502(4) . ? C47 F1 1.29(3) . ? C47 F3 1.35(3) . ? C47 F2 1.37(4) . ? C47 S1 1.83(6) . ? O1 S1 1.38(2) . ? O2 S1 1.42(2) . ? O3 S1 1.453(18) . ? C37' C41' 1.445(15) . ? C37' C38' 1.445(15) . ? C37' C42' 1.536(16) . ? C38' C39' 1.445(15) . ? C38' C43' 1.536(16) . ? C39' C40' 1.445(15) . ? C39' C44' 1.536(16) . ? C40' C41' 1.445(15) . ? C40' C45' 1.536(16) . ? C41' C46' 1.536(16) . ? C47' F3' 1.12(8) . ? C47' F1' 1.28(4) . ? C47' F2' 1.39(4) . ? C47' S1' 1.77(10) . ? O1' S1' 1.43(3) . ? O2' S1' 1.39(3) . ? O3' S1' 1.42(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Rh1 C29 155.2(3) . . ? N5 Rh1 C27 110.4(3) . . ? C29 Rh1 C27 65.6(4) . . ? N5 Rh1 C30 116.5(3) . . ? C29 Rh1 C30 38.7(4) . . ? C27 Rh1 C30 66.0(3) . . ? N5 Rh1 C28 147.8(3) . . ? C29 Rh1 C28 38.7(4) . . ? C27 Rh1 C28 38.2(4) . . ? C30 Rh1 C28 64.4(4) . . ? N5 Rh1 C31 96.2(3) . . ? C29 Rh1 C31 64.5(4) . . ? C27 Rh1 C31 39.9(3) . . ? C30 Rh1 C31 38.3(3) . . ? C28 Rh1 C31 64.1(3) . . ? N5 Rh1 N1 85.5(2) . . ? C29 Rh1 N1 119.3(3) . . ? C27 Rh1 N1 107.4(3) . . ? C30 Rh1 N1 158.0(3) . . ? C28 Rh1 N1 97.0(3) . . ? C31 Rh1 N1 145.4(3) . . ? N5 Rh1 N2 83.7(2) . . ? C29 Rh1 N2 98.8(3) . . ? C27 Rh1 N2 164.4(3) . . ? C30 Rh1 N2 102.1(3) . . ? C28 Rh1 N2 128.5(3) . . ? C31 Rh1 N2 134.9(3) . . ? N1 Rh1 N2 79.7(2) . . ? C37' Rh2 C41' 40.5(5) . . ? C37' Rh2 C38' 40.4(5) . . ? C41' Rh2 C38' 67.2(8) . . ? C37' Rh2 N6 105.0(8) . . ? C41' Rh2 N6 103.3(7) . . ? C38' Rh2 N6 137.5(7) . . ? C37' Rh2 C40 64.1(7) . . ? C41' Rh2 C40 46.3(8) . . ? C38' Rh2 C40 54.7(6) . . ? N6 Rh2 C40 145.8(3) . . ? C37' Rh2 C39 52.5(7) . . ? C41' Rh2 C39 65.8(7) . . ? C38' Rh2 C39 19.6(6) . . ? N6 Rh2 C39 156.1(3) . . ? C40 Rh2 C39 38.58(13) . . ? C37' Rh2 C41 48.8(8) . . ? C41' Rh2 C41 10.5(8) . . ? C38' Rh2 C41 69.5(6) . . ? N6 Rh2 C41 108.9(3) . . ? C40 Rh2 C41 38.49(13) . . ? C39 Rh2 C41 64.2(2) . . ? C37' Rh2 N3 120.9(8) . . ? C41' Rh2 N3 160.8(7) . . ? C38' Rh2 N3 94.9(7) . . ? N6 Rh2 N3 84.9(2) . . ? C40 Rh2 N3 129.0(3) . . ? C39 Rh2 N3 99.8(2) . . ? C41 Rh2 N3 163.9(2) . . ? C37' Rh2 N4 157.1(8) . . ? C41' Rh2 N4 117.9(8) . . ? C38' Rh2 N4 136.0(7) . . ? N6 Rh2 N4 86.0(2) . . ? C40 Rh2 N4 95.5(2) . . ? C39 Rh2 N4 117.9(3) . . ? C41 Rh2 N4 108.8(2) . . ? N3 Rh2 N4 79.5(2) . . ? C37' Rh2 C40' 66.8(8) . . ? C41' Rh2 C40' 39.4(5) . . ? C38' Rh2 C40' 66.0(7) . . ? N6 Rh2 C40' 132.9(7) . . ? C40 Rh2 C40' 13.5(6) . . ? C39 Rh2 C40' 51.5(6) . . ? C41 Rh2 C40' 29.8(7) . . ? N3 Rh2 C40' 140.5(7) . . ? N4 Rh2 C40' 90.9(6) . . ? C37' Rh2 C38 21.6(7) . . ? C41' Rh2 C38 57.8(7) . . ? C38' Rh2 C38 21.1(6) . . ? N6 Rh2 C38 118.0(3) . . ? C40 Rh2 C38 64.1(2) . . ? C39 Rh2 C38 38.14(12) . . ? C41 Rh2 C38 63.67(19) . . ? N3 Rh2 C38 103.0(2) . . ? N4 Rh2 C38 156.0(3) . . ? C40' Rh2 C38 71.8(6) . . ? C37' Rh2 C39' 66.7(7) . . ? C41' Rh2 C39' 66.1(8) . . ? C38' Rh2 C39' 39.3(5) . . ? N6 Rh2 C39' 169.4(6) . . ? C40 Rh2 C39' 25.3(6) . . ? C39 Rh2 C39' 19.7(5) . . ? C41 Rh2 C39' 60.8(6) . . ? N3 Rh2 C39' 104.9(6) . . ? N4 Rh2 C39' 99.6(6) . . ? C40' Rh2 C39' 38.7(5) . . ? C38 Rh2 C39' 56.5(5) . . ? C7 N1 C1 103.2(6) . . ? C7 N1 Rh1 110.4(5) . . ? C1 N1 Rh1 144.8(5) . . ? C8 N2 C9 101.7(6) . . ? C8 N2 Rh1 109.9(5) . . ? C9 N2 Rh1 146.3(5) . . ? C8 N3 C14 100.9(6) . . ? C8 N3 Rh2 111.6(5) . . ? C14 N3 Rh2 146.8(5) . . ? C7 N4 C6 103.0(6) . . ? C7 N4 Rh2 109.7(5) . . ? C6 N4 Rh2 147.0(5) . . ? C17 N5 C21 116.7(7) . . ? C17 N5 Rh1 121.3(5) . . ? C21 N5 Rh1 121.9(5) . . ? C26 N6 C22 116.9(7) . . ? C26 N6 Rh2 122.1(5) . . ? C22 N6 Rh2 120.8(5) . . ? O5 S2 O6 114.3(10) . . ? O5 S2 O4 116.2(10) . . ? O6 S2 O4 121.3(11) . . ? O5 S2 C48 104.5(10) . . ? O6 S2 C48 103.6(11) . . ? O4 S2 C48 91.0(12) . . ? C2 C1 N1 132.6(7) . . ? C2 C1 C6 120.2(7) . . ? N1 C1 C6 107.2(7) . . ? C1 C2 C3 119.1(8) . . ? C4 C3 C2 119.9(9) . . ? C3 C4 C5 123.5(9) . . ? C4 C5 C6 117.6(8) . . ? N4 C6 C5 132.5(8) . . ? N4 C6 C1 107.8(7) . . ? C5 C6 C1 119.6(8) . . ? N1 C7 N4 118.8(6) . . ? N1 C7 C8 119.8(6) . . ? N4 C7 C8 121.1(7) . . ? N2 C8 N3 121.1(7) . . ? N2 C8 C7 120.0(7) . . ? N3 C8 C7 118.1(7) . . ? N2 C9 C10 131.2(8) . . ? N2 C9 C14 107.5(6) . . ? C10 C9 C14 121.3(8) . . ? C11 C10 C9 117.1(9) . . ? C10 C11 C12 123.5(9) . . ? C11 C12 C13 120.9(9) . . ? C12 C13 C14 117.5(9) . . ? N3 C14 C13 131.5(8) . . ? N3 C14 C9 108.9(7) . . ? C13 C14 C9 119.6(7) . . ? C19 C15 C16 118.7(6) . 3_656 ? C19 C15 C16 116.8(6) . . ? C16 C15 C16 90.8(6) 3_656 . ? C24 C16 C15 118.7(6) . 3_656 ? C24 C16 C15 114.5(6) . . ? C15 C16 C15 89.2(6) 3_656 . ? N5 C17 C18 123.9(7) . . ? C19 C18 C17 119.6(7) . . ? C18 C19 C20 116.7(7) . . ? C18 C19 C15 126.1(7) . . ? C20 C19 C15 117.2(7) . . ? C21 C20 C19 120.4(7) . . ? N5 C21 C20 122.6(7) . . ? N6 C22 C23 123.5(7) . . ? C24 C23 C22 119.7(7) . . ? C25 C24 C23 116.5(7) . . ? C25 C24 C16 119.7(7) . . ? C23 C24 C16 123.5(7) . . ? C24 C25 C26 120.6(7) . . ? N6 C26 C25 122.6(8) . . ? C28 C27 C31 105.5(8) . . ? C28 C27 C32 128.6(9) . . ? C31 C27 C32 125.5(8) . . ? C28 C27 Rh1 71.3(5) . . ? C31 C27 Rh1 70.5(5) . . ? C32 C27 Rh1 128.4(6) . . ? C27 C28 C29 110.3(8) . . ? C27 C28 C33 124.0(10) . . ? C29 C28 C33 125.7(9) . . ? C27 C28 Rh1 70.5(5) . . ? C29 C28 Rh1 70.2(5) . . ? C33 C28 Rh1 127.3(7) . . ? C28 C29 C30 107.6(8) . . ? C28 C29 C34 125.5(10) . . ? C30 C29 C34 126.8(10) . . ? C28 C29 Rh1 71.2(5) . . ? C30 C29 Rh1 71.1(5) . . ? C34 C29 Rh1 125.3(7) . . ? C31 C30 C29 107.8(8) . . ? C31 C30 C35 126.5(10) . . ? C29 C30 C35 125.2(9) . . ? C31 C30 Rh1 70.9(5) . . ? C29 C30 Rh1 70.2(5) . . ? C35 C30 Rh1 130.5(7) . . ? C30 C31 C27 108.7(8) . . ? C30 C31 C36 126.4(9) . . ? C27 C31 C36 124.9(9) . . ? C30 C31 Rh1 70.7(5) . . ? C27 C31 Rh1 69.6(4) . . ? C36 C31 Rh1 124.9(7) . . ? F4 C48 F5 101.0(18) . . ? F4 C48 F6 97(2) . . ? F5 C48 F6 103(2) . . ? F4 C48 S2 120.0(18) . . ? F5 C48 S2 114(2) . . ? F6 C48 S2 118.6(14) . . ? C38 C37 C41 108.0 . . ? C38 C37 C42 126.0 . . ? C41 C37 C42 126.0 . . ? C38 C37 Rh2 70.9(2) . . ? C41 C37 Rh2 69.9(2) . . ? C42 C37 Rh2 124.84(19) . . ? C37 C38 C39 108.0 . . ? C37 C38 C43 126.0 . . ? C39 C38 C43 126.0 . . ? C37 C38 Rh2 71.34(19) . . ? C39 C38 Rh2 69.66(19) . . ? C43 C38 Rh2 124.6(2) . . ? C40 C39 C38 108.0 . . ? C40 C39 C44 126.0 . . ? C38 C39 C44 126.0 . . ? C40 C39 Rh2 70.2(2) . . ? C38 C39 Rh2 72.20(19) . . ? C44 C39 Rh2 123.28(19) . . ? C39 C40 C41 108.0 . . ? C39 C40 C45 126.0 . . ? C41 C40 C45 126.0 . . ? C39 C40 Rh2 71.3(2) . . ? C41 C40 Rh2 71.7(2) . . ? C45 C40 Rh2 122.73(19) . . ? C37 C41 C40 108.0 . . ? C37 C41 C46 126.0 . . ? C40 C41 C46 126.0 . . ? C37 C41 Rh2 72.10(19) . . ? C40 C41 Rh2 69.81(19) . . ? C46 C41 Rh2 123.7(2) . . ? F1 C47 F3 103(4) . . ? F1 C47 F2 114(4) . . ? F3 C47 F2 103(3) . . ? F1 C47 S1 120(3) . . ? F3 C47 S1 108(3) . . ? F2 C47 S1 107(3) . . ? O1 S1 O2 117.8(16) . . ? O1 S1 O3 112.6(19) . . ? O2 S1 O3 116.3(14) . . ? O1 S1 C47 102.6(17) . . ? O2 S1 C47 104.9(16) . . ? O3 S1 C47 99.4(13) . . ? C41' C37' C38' 108.0 . . ? C41' C37' C42' 126.0 . . ? C38' C37' C42' 126.0 . . ? C41' C37' Rh2 71.1(9) . . ? C38' C37' Rh2 71.6(8) . . ? C42' C37' Rh2 123.0(8) . . ? C37' C38' C39' 108.0 . . ? C37' C38' C43' 126.0 . . ? C39' C38' C43' 126.0 . . ? C37' C38' Rh2 68.1(9) . . ? C39' C38' Rh2 72.8(9) . . ? C43' C38' Rh2 124.7(8) . . ? C40' C39' C38' 108.0 . . ? C40' C39' C44' 126.0 . . ? C38' C39' C44' 126.0 . . ? C40' C39' Rh2 70.4(8) . . ? C38' C39' Rh2 68.0(9) . . ? C44' C39' Rh2 127.2(8) . . ? C39' C40' C41' 108.0 . . ? C39' C40' C45' 126.0 . . ? C41' C40' C45' 126.0 . . ? C39' C40' Rh2 70.8(8) . . ? C41' C40' Rh2 67.7(9) . . ? C45' C40' Rh2 127.0(8) . . ? C37' C41' C40' 108.0 . . ? C37' C41' C46' 126.0 . . ? C40' C41' C46' 126.0 . . ? C37' C41' Rh2 68.4(9) . . ? C40' C41' Rh2 72.8(9) . . ? C46' C41' Rh2 124.4(8) . . ? F3' C47' F1' 119(10) . . ? F3' C47' F2' 105(5) . . ? F1' C47' F2' 84(4) . . ? F3' C47' S1' 122(5) . . ? F1' C47' S1' 108(6) . . ? F2' C47' S1' 113(6) . . ? O2' S1' O3' 111(2) . . ? O2' S1' O1' 112(3) . . ? O3' S1' O1' 118.1(19) . . ? O2' S1' C47' 105(3) . . ? O3' S1' C47' 100(2) . . ? O1' S1' C47' 110(3) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.002 0.000 0.000 667.6 116.0 2 -0.016 0.500 0.500 667.7 116.9 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 60.49 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 3.750 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.161 _database_code_depnum_ccdc_archive 'CCDC 927805' ####################################################################### # # 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_global # Attachment '4.cif' data_4 #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H124 F12 N12 O14 Rh4 S4' _chemical_formula_weight 2846.29 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.4313(10) _cell_length_b 20.8183(11) _cell_length_c 16.1878(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.1880(10) _cell_angle_gamma 90.00 _cell_volume 6547.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.39 _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9044 _exptl_absorpt_correction_T_max 0.9100 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.46 _diffrn_reflns_number 47795 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.52 _reflns_number_total 14985 _reflns_number_gt 10868 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^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 14985 _refine_ls_number_parameters 912 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.006 _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 0.208515(15) 0.440981(15) 0.274595(18) 0.02125(9) Uani 1 1 d . . . Rh2 Rh 0.163604(14) 0.643555(15) 0.052714(17) 0.01943(9) Uani 1 1 d . . . N1 N 0.23118(17) 0.54207(17) 0.2622(2) 0.0244(7) Uani 1 1 d . . . N2 N 0.18399(17) 0.45524(16) 0.1423(2) 0.0235(7) Uani 1 1 d . . . N3 N 0.17024(17) 0.53936(17) 0.05124(19) 0.0233(7) Uani 1 1 d . . . N4 N 0.21253(16) 0.62531(16) 0.17263(19) 0.0224(7) Uani 1 1 d . . . N5 N 0.31115(16) 0.41961(17) 0.2424(2) 0.0247(7) Uani 1 1 d . . . N6 N 0.73735(16) 0.35284(16) -0.0002(2) 0.0216(7) Uani 1 1 d . . . S1 S 0.93363(6) 0.69874(6) 0.47407(7) 0.0358(3) Uani 1 1 d . . . S2 S 0.28981(18) 0.58924(12) 0.64515(15) 0.1160(11) Uani 1 1 d DU . . F1 F 1.0190(2) 0.6334(3) 0.3845(3) 0.1109(18) Uani 1 1 d . . . F2 F 0.9380(4) 0.5764(2) 0.4352(4) 0.150(3) Uani 1 1 d . . . F3 F 0.9171(3) 0.6400(3) 0.3318(3) 0.0960(15) Uani 1 1 d . . . F4 F 0.1574(4) 0.5616(3) 0.6319(4) 0.147(3) Uani 1 1 d . . . F5 F 0.2194(5) 0.4872(4) 0.6751(6) 0.215(4) Uani 1 1 d U . . F6 F 0.1983(4) 0.5688(5) 0.7518(4) 0.188(3) Uani 1 1 d U . . O1 O 0.85982(17) 0.6940(2) 0.4801(2) 0.0489(9) Uani 1 1 d . . . O2 O 0.9707(2) 0.6825(3) 0.5481(3) 0.0798(16) Uani 1 1 d . . . O3 O 0.95797(19) 0.75320(18) 0.4301(2) 0.0512(9) Uani 1 1 d . . . O4 O 0.3404(5) 0.5683(5) 0.7022(4) 0.166(4) Uani 1 1 d U . . O5 O 0.2982(5) 0.5659(4) 0.5670(3) 0.147(3) Uani 1 1 d . . . O6 O 0.2724(4) 0.6541(4) 0.6467(7) 0.175(4) Uani 1 1 d U . . C1 C 0.2582(2) 0.5977(2) 0.2986(2) 0.0245(8) Uani 1 1 d . . . C2 C 0.2942(2) 0.6074(2) 0.3729(2) 0.0294(9) Uani 1 1 d . . . H2 H 0.3019 0.5732 0.4110 0.035 Uiso 1 1 calc R . . C3 C 0.3184(2) 0.6687(2) 0.3888(3) 0.0357(10) Uani 1 1 d . . . H3 H 0.3440 0.6765 0.4385 0.043 Uiso 1 1 calc R . . C4 C 0.3065(2) 0.7191(2) 0.3343(3) 0.0354(10) Uani 1 1 d . . . H4 H 0.3236 0.7606 0.3482 0.042 Uiso 1 1 calc R . . C5 C 0.2705(2) 0.7109(2) 0.2607(3) 0.0310(9) Uani 1 1 d . . . H5 H 0.2626 0.7458 0.2239 0.037 Uiso 1 1 calc R . . C6 C 0.2465(2) 0.6498(2) 0.2427(2) 0.0235(8) Uani 1 1 d . . . C7 C 0.2071(2) 0.56290(19) 0.1896(2) 0.0233(8) Uani 1 1 d . . . C8 C 0.18352(19) 0.5187(2) 0.1282(2) 0.0228(8) Uani 1 1 d . . . C9 C 0.16978(19) 0.4301(2) 0.0638(2) 0.0232(8) Uani 1 1 d . . . C10 C 0.1651(2) 0.3673(2) 0.0365(3) 0.0296(9) Uani 1 1 d . . . H10 H 0.1707 0.3324 0.0737 0.036 Uiso 1 1 calc R . . C11 C 0.1517(2) 0.3569(2) -0.0477(3) 0.0336(10) Uani 1 1 d . . . H11 H 0.1472 0.3142 -0.0678 0.040 Uiso 1 1 calc R . . C12 C 0.1450(2) 0.4084(2) -0.1026(3) 0.0314(10) Uani 1 1 d . . . H12 H 0.1374 0.3996 -0.1596 0.038 Uiso 1 1 calc R . . C13 C 0.1489(2) 0.4713(2) -0.0771(2) 0.0270(9) Uani 1 1 d . . . H13 H 0.1438 0.5058 -0.1151 0.032 Uiso 1 1 calc R . . C14 C 0.1609(2) 0.4825(2) 0.0076(2) 0.0239(8) Uani 1 1 d . . . C15 C 0.5174(2) 0.3867(2) 0.1697(3) 0.0323(10) Uani 1 1 d . . . H15 H 0.5527 0.4060 0.2027 0.039 Uiso 1 1 calc R . . C16 C 0.5363(2) 0.3555(2) 0.1019(3) 0.0285(9) Uani 1 1 d . . . H16 H 0.5016 0.3322 0.0725 0.034 Uiso 1 1 calc R . . C17 C 0.3250(2) 0.3731(2) 0.1873(3) 0.0307(9) Uani 1 1 d . . . H17 H 0.2880 0.3490 0.1639 0.037 Uiso 1 1 calc R . . C18 C 0.3911(2) 0.3595(2) 0.1639(3) 0.0306(9) Uani 1 1 d . . . H18 H 0.3987 0.3265 0.1246 0.037 Uiso 1 1 calc R . . C19 C 0.4468(2) 0.3934(2) 0.1971(3) 0.0300(9) Uani 1 1 d . . . C20 C 0.4321(2) 0.4388(2) 0.2581(3) 0.0330(10) Uani 1 1 d . . . H20 H 0.4684 0.4613 0.2856 0.040 Uiso 1 1 calc R . . C21 C 0.3650(2) 0.4506(2) 0.2779(3) 0.0330(10) Uani 1 1 d . . . H21 H 0.3561 0.4822 0.3186 0.040 Uiso 1 1 calc R . . C22 C 0.7237(2) 0.3885(2) 0.0667(2) 0.0256(8) Uani 1 1 d . . . H22 H 0.7599 0.4136 0.0903 0.031 Uiso 1 1 calc R . . C23 C 0.6602(2) 0.3909(2) 0.1032(3) 0.0268(9) Uani 1 1 d . . . H23 H 0.6532 0.4168 0.1506 0.032 Uiso 1 1 calc R . . C24 C 0.6058(2) 0.3540(2) 0.0688(2) 0.0243(8) Uani 1 1 d . . . C25 C 0.6206(2) 0.3169(2) 0.0005(2) 0.0280(9) Uani 1 1 d . . . H25 H 0.5855 0.2912 -0.0244 0.034 Uiso 1 1 calc R . . C26 C 0.6861(2) 0.3167(2) -0.0322(3) 0.0268(9) Uani 1 1 d . . . H26 H 0.6950 0.2902 -0.0785 0.032 Uiso 1 1 calc R . . C27 C 0.1073(2) 0.4272(3) 0.3224(3) 0.0370(11) Uani 1 1 d . . . C28 C 0.1361(2) 0.3654(2) 0.3014(3) 0.0331(10) Uani 1 1 d . . . C29 C 0.1964(2) 0.3566(2) 0.3507(3) 0.0300(9) Uani 1 1 d . . . C30 C 0.2066(2) 0.4131(2) 0.4014(2) 0.0295(9) Uani 1 1 d . . . C31 C 0.1489(2) 0.4547(2) 0.3850(3) 0.0319(10) Uani 1 1 d . . . C32 C 0.0410(3) 0.4539(4) 0.2889(4) 0.0623(18) Uani 1 1 d . . . H32A H 0.0026 0.4364 0.3203 0.093 Uiso 1 1 calc R . . H32B H 0.0353 0.4420 0.2306 0.093 Uiso 1 1 calc R . . H32C H 0.0415 0.5008 0.2939 0.093 Uiso 1 1 calc R . . C33 C 0.1045(3) 0.3184(3) 0.2443(3) 0.0539(15) Uani 1 1 d . . . H33A H 0.1404 0.2907 0.2218 0.081 Uiso 1 1 calc R . . H33B H 0.0807 0.3411 0.1990 0.081 Uiso 1 1 calc R . . H33C H 0.0714 0.2920 0.2740 0.081 Uiso 1 1 calc R . . C34 C 0.2427(3) 0.3000(2) 0.3517(3) 0.0481(13) Uani 1 1 d . . . H34A H 0.2299 0.2710 0.3965 0.072 Uiso 1 1 calc R . . H34B H 0.2904 0.3142 0.3604 0.072 Uiso 1 1 calc R . . H34C H 0.2385 0.2773 0.2987 0.072 Uiso 1 1 calc R . . C35 C 0.2611(3) 0.4219(3) 0.4661(3) 0.0448(12) Uani 1 1 d . . . H35A H 0.2666 0.4678 0.4781 0.067 Uiso 1 1 calc R . . H35B H 0.3047 0.4045 0.4464 0.067 Uiso 1 1 calc R . . H35C H 0.2480 0.3992 0.5165 0.067 Uiso 1 1 calc R . . C36 C 0.1376(3) 0.5191(3) 0.4259(3) 0.0488(13) Uani 1 1 d . . . H36A H 0.1214 0.5502 0.3844 0.073 Uiso 1 1 calc R . . H36B H 0.1810 0.5342 0.4509 0.073 Uiso 1 1 calc R . . H36C H 0.1030 0.5146 0.4688 0.073 Uiso 1 1 calc R . . C37 C 0.0620(2) 0.6674(2) 0.0903(2) 0.0280(9) Uani 1 1 d . . . C38 C 0.1026(2) 0.7255(2) 0.0892(3) 0.0304(9) Uani 1 1 d . . . C39 C 0.1252(2) 0.7356(2) 0.0088(3) 0.0325(10) Uani 1 1 d . . . C40 C 0.0993(2) 0.6844(2) -0.0420(2) 0.0278(9) Uani 1 1 d . . . C41 C 0.0579(2) 0.6439(2) 0.0078(3) 0.0267(9) Uani 1 1 d . . . C42 C 0.0266(3) 0.6407(3) 0.1639(3) 0.0547(16) Uani 1 1 d . . . H42A H -0.0127 0.6680 0.1773 0.082 Uiso 1 1 calc R . . H42B H 0.0590 0.6395 0.2111 0.082 Uiso 1 1 calc R . . H42C H 0.0104 0.5971 0.1516 0.082 Uiso 1 1 calc R . . C43 C 0.1142(3) 0.7679(3) 0.1618(4) 0.0590(17) Uani 1 1 d . . . H43A H 0.1538 0.7959 0.1521 0.088 Uiso 1 1 calc R . . H43B H 0.1232 0.7416 0.2110 0.088 Uiso 1 1 calc R . . H43C H 0.0731 0.7943 0.1703 0.088 Uiso 1 1 calc R . . C44 C 0.1645(3) 0.7923(3) -0.0221(5) 0.0659(19) Uani 1 1 d . . . H44A H 0.1329 0.8284 -0.0317 0.099 Uiso 1 1 calc R . . H44B H 0.1866 0.7810 -0.0740 0.099 Uiso 1 1 calc R . . H44C H 0.1998 0.8047 0.0190 0.099 Uiso 1 1 calc R . . C45 C 0.1054(3) 0.6790(3) -0.1338(3) 0.0500(15) Uani 1 1 d . . . H45A H 0.1099 0.6337 -0.1491 0.075 Uiso 1 1 calc R . . H45B H 0.1462 0.7027 -0.1515 0.075 Uiso 1 1 calc R . . H45C H 0.0642 0.6971 -0.1608 0.075 Uiso 1 1 calc R . . C46 C 0.0179(2) 0.5867(2) -0.0199(4) 0.0434(12) Uani 1 1 d . . . H46A H -0.0276 0.6003 -0.0403 0.065 Uiso 1 1 calc R . . H46B H 0.0127 0.5571 0.0266 0.065 Uiso 1 1 calc R . . H46C H 0.0423 0.5650 -0.0644 0.065 Uiso 1 1 calc R . . C47 C 0.9527(4) 0.6329(3) 0.4018(5) 0.072(2) Uani 1 1 d . . . C48 C 0.2212(7) 0.5555(5) 0.6788(5) 0.130(5) Uani 1 1 d DU . . C49 C 0.4984(6) 0.2281(6) 0.8748(7) 0.127(8) Uani 0.50 1 d PGU A 1 C50 C 0.5077(7) 0.1781(6) 0.9260(9) 0.085(4) Uani 0.50 1 d PGU A 1 H50 H 0.5446 0.1491 0.9179 0.102 Uiso 0.50 1 calc PR A 1 C51 C 0.4647(8) 0.1691(6) 0.9886(8) 0.143(9) Uani 0.50 1 d PGU A 1 H51 H 0.4712 0.1336 1.0249 0.171 Uiso 0.50 1 calc PR A 1 C52 C 0.4125(7) 0.2100(8) 1.0001(7) 0.093(6) Uani 0.50 1 d PG A 1 H52 H 0.3821 0.2035 1.0445 0.112 Uiso 0.50 1 calc PR A 1 C53 C 0.4033(5) 0.2599(7) 0.9489(8) 0.101(7) Uani 0.50 1 d PG A 1 C63 C 0.4463(6) 0.2690(5) 0.8863(7) 0.064(4) Uani 0.50 1 d PG A 1 C54 C 0.3507(8) 0.2905(9) 0.9746(9) 0.086(5) Uani 0.50 1 d PU A 1 H54 H 0.3241 0.2788 1.0209 0.103 Uiso 0.50 1 calc PR A 1 C55 C 0.3394(11) 0.3401(12) 0.9274(14) 0.102(6) Uani 0.50 1 d PU A 1 H55 H 0.3010 0.3654 0.9427 0.123 Uiso 0.50 1 calc PR A 1 C56 C 0.3739(6) 0.3632(6) 0.8576(8) 0.099(5) Uani 0.50 1 d PG A 1 C57 C 0.3617(7) 0.4183(6) 0.8069(9) 0.105(6) Uani 0.50 1 d PGU A 1 H57 H 0.3242 0.4460 0.8178 0.126 Uiso 0.50 1 calc PR A 1 C58 C 0.4059(7) 0.4316(6) 0.7398(8) 0.109(6) Uani 0.50 1 d PGU A 1 H58 H 0.3978 0.4683 0.7061 0.130 Uiso 0.50 1 calc PR A 1 C59 C 0.4623(7) 0.3900(7) 0.7234(8) 0.103(6) Uani 0.50 1 d PG A 1 H59 H 0.4917 0.3989 0.6787 0.123 Uiso 0.50 1 calc PR A 1 C60 C 0.4744(6) 0.3349(6) 0.7741(9) 0.087(9) Uani 0.50 1 d PG A 1 C64 C 0.4302(6) 0.3216(6) 0.8412(8) 0.060(4) Uani 0.50 1 d PG A 1 C61 C 0.5320(8) 0.2959(9) 0.7533(10) 0.066(4) Uani 0.50 1 d P A 1 H61 H 0.5605 0.3050 0.7077 0.079 Uiso 0.50 1 calc PR A 1 C62 C 0.5435(8) 0.2410(11) 0.8080(11) 0.097(6) Uani 0.50 1 d PU A 1 H62 H 0.5815 0.2133 0.7990 0.117 Uiso 0.50 1 calc PR A 1 C65 C 0.4340(7) 0.3782(10) 0.8585(10) 0.081(5) Uani 0.50 1 d P B 2 C66 C 0.445(2) 0.340(2) 0.7897(19) 0.183(18) Uani 0.50 1 d P B 2 C67 C 0.5211(16) 0.3367(19) 0.7680(15) 0.139(11) Uani 0.50 1 d P B 2 C68 C 0.5701(10) 0.3890(12) 0.8075(15) 0.115(7) Uani 0.50 1 d PU B 2 C69 C 0.5484(7) 0.4241(9) 0.8715(11) 0.079(5) Uani 0.50 1 d P . 2 C70 C 0.5957(5) 0.4676(6) 0.9123(7) 0.113(4) Uani 1 1 d . . 2 C71 C 0.5688(13) 0.5100(12) 0.9846(17) 0.116(7) Uani 0.50 1 d PU . 2 C72 C 0.5000 0.5000 1.0000 0.092(5) Uani 1 2 d S . 2 C73 C 0.4665(11) 0.5433(7) 1.0730(10) 0.076(5) Uani 0.50 1 d PU . 2 C75 C 0.3580(9) 0.4964(8) 1.0492(9) 0.081(5) Uani 0.50 1 d P . 2 C76 C 0.3849(7) 0.4570(6) 0.9837(7) 0.053(3) Uani 0.50 1 d P . 2 C77 C 0.3412(6) 0.4146(8) 0.9399(10) 0.076(4) Uani 0.50 1 d P B 2 C78 C 0.3585(14) 0.3742(12) 0.8890(14) 0.099(5) Uani 0.50 1 d P B 2 C79 C 0.4785(6) 0.4200(8) 0.8947(8) 0.066(4) Uani 0.50 1 d P . 2 C80 C 0.4551(7) 0.4612(7) 0.9601(7) 0.055(3) Uani 0.50 1 d PU . 2 C81 C 0.7300(4) 0.6822(4) 0.3247(5) 0.088(3) Uani 1 1 d . . . H81A H 0.6991 0.6588 0.3611 0.131 Uiso 1 1 calc R . . H81B H 0.7668 0.6536 0.3068 0.131 Uiso 1 1 calc R . . H81C H 0.7039 0.6978 0.2762 0.131 Uiso 1 1 calc R . . O7 O 0.7586(3) 0.7342(2) 0.3672(3) 0.0689(12) Uani 1 1 d D . . H7 H 0.743(4) 0.736(5) 0.416(2) 0.12(4) Uiso 1 1 d 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 0.02052(16) 0.02412(17) 0.01919(16) 0.00147(12) 0.00287(11) 0.00091(12) Rh2 0.01821(15) 0.02313(17) 0.01697(15) -0.00020(11) 0.00106(10) -0.00102(11) N1 0.0254(17) 0.0270(18) 0.0207(16) -0.0024(14) -0.0016(13) 0.0000(14) N2 0.0231(17) 0.0238(18) 0.0236(17) 0.0002(13) 0.0000(13) 0.0002(13) N3 0.0266(17) 0.0244(18) 0.0189(16) -0.0007(13) -0.0011(13) -0.0007(13) N4 0.0247(17) 0.0248(17) 0.0176(15) -0.0002(13) -0.0007(12) -0.0010(13) N5 0.0184(16) 0.0307(19) 0.0251(17) 0.0001(14) 0.0022(13) 0.0020(14) N6 0.0180(15) 0.0251(17) 0.0218(16) 0.0012(13) 0.0017(12) -0.0011(13) S1 0.0290(6) 0.0434(7) 0.0350(6) 0.0060(5) 0.0013(4) -0.0029(5) S2 0.198(3) 0.0723(14) 0.0739(14) -0.0369(12) -0.0774(17) 0.0634(17) F1 0.091(3) 0.112(4) 0.133(4) 0.009(3) 0.056(3) 0.052(3) F2 0.228(7) 0.042(3) 0.184(6) 0.009(3) 0.089(5) 0.016(3) F3 0.112(4) 0.118(4) 0.058(3) -0.035(3) 0.018(2) -0.013(3) F4 0.201(7) 0.129(6) 0.110(5) -0.022(4) -0.009(5) -0.039(5) F5 0.272(8) 0.149(6) 0.229(7) 0.058(6) 0.097(6) 0.033(6) F6 0.209(6) 0.265(8) 0.090(4) -0.050(5) 0.005(4) 0.061(6) O1 0.0298(17) 0.067(3) 0.050(2) 0.0028(19) 0.0053(15) -0.0040(17) O2 0.058(3) 0.130(5) 0.050(2) 0.033(3) -0.015(2) -0.010(3) O3 0.047(2) 0.044(2) 0.063(2) 0.0120(18) -0.0016(18) -0.0126(17) O4 0.211(8) 0.218(9) 0.068(4) -0.027(5) -0.037(5) 0.130(7) O5 0.254(9) 0.134(6) 0.051(3) 0.010(3) -0.049(4) -0.083(6) O6 0.147(6) 0.097(5) 0.277(8) -0.064(5) -0.072(6) 0.034(4) C1 0.024(2) 0.027(2) 0.0227(19) -0.0051(16) 0.0017(15) 0.0004(16) C2 0.033(2) 0.035(2) 0.0200(19) -0.0018(17) -0.0042(16) 0.0063(18) C3 0.035(2) 0.043(3) 0.029(2) -0.010(2) -0.0064(18) 0.003(2) C4 0.039(2) 0.032(2) 0.036(2) -0.014(2) -0.0055(19) -0.0028(19) C5 0.034(2) 0.028(2) 0.031(2) -0.0047(18) -0.0018(18) -0.0019(18) C6 0.0226(19) 0.029(2) 0.0193(18) -0.0035(16) 0.0001(14) -0.0009(16) C7 0.027(2) 0.023(2) 0.0194(18) -0.0011(15) 0.0015(15) -0.0005(16) C8 0.0206(18) 0.025(2) 0.0227(19) -0.0012(16) -0.0009(14) -0.0016(15) C9 0.0185(18) 0.028(2) 0.0230(19) -0.0015(16) 0.0003(14) -0.0020(15) C10 0.024(2) 0.031(2) 0.034(2) -0.0032(18) 0.0017(17) 0.0013(17) C11 0.032(2) 0.030(2) 0.038(2) -0.014(2) 0.0034(19) 0.0004(18) C12 0.031(2) 0.040(3) 0.023(2) -0.0093(18) -0.0018(16) -0.0010(19) C13 0.026(2) 0.032(2) 0.0224(19) -0.0006(17) -0.0009(15) -0.0031(17) C14 0.0214(19) 0.023(2) 0.027(2) -0.0057(16) 0.0001(15) -0.0011(15) C15 0.021(2) 0.041(3) 0.035(2) 0.004(2) 0.0001(17) -0.0013(18) C16 0.0196(19) 0.036(2) 0.030(2) 0.0049(18) -0.0009(16) -0.0001(17) C17 0.025(2) 0.035(2) 0.032(2) -0.0032(19) 0.0031(17) -0.0006(18) C18 0.026(2) 0.034(2) 0.032(2) -0.0070(19) 0.0052(17) 0.0004(17) C19 0.026(2) 0.037(3) 0.027(2) 0.0031(18) 0.0052(16) 0.0012(18) C20 0.023(2) 0.046(3) 0.030(2) -0.008(2) 0.0013(17) -0.0045(19) C21 0.032(2) 0.039(3) 0.028(2) -0.0068(19) -0.0005(17) 0.0007(19) C22 0.023(2) 0.029(2) 0.025(2) -0.0018(17) 0.0019(15) -0.0008(16) C23 0.026(2) 0.030(2) 0.024(2) -0.0003(17) 0.0028(16) -0.0001(17) C24 0.0223(19) 0.026(2) 0.025(2) 0.0047(16) 0.0024(15) 0.0011(16) C25 0.024(2) 0.035(2) 0.026(2) 0.0006(18) -0.0018(16) -0.0061(17) C26 0.024(2) 0.032(2) 0.025(2) -0.0027(17) 0.0002(15) -0.0017(17) C27 0.024(2) 0.054(3) 0.034(2) 0.011(2) 0.0114(18) 0.000(2) C28 0.031(2) 0.038(3) 0.031(2) 0.0029(19) 0.0098(18) -0.0121(19) C29 0.034(2) 0.029(2) 0.028(2) 0.0049(18) 0.0114(17) -0.0018(18) C30 0.035(2) 0.033(2) 0.0211(19) 0.0093(17) 0.0102(16) -0.0006(18) C31 0.035(2) 0.034(2) 0.027(2) 0.0039(18) 0.0168(18) 0.0024(19) C32 0.023(3) 0.093(5) 0.071(4) 0.014(4) 0.002(2) 0.007(3) C33 0.051(3) 0.064(4) 0.047(3) -0.008(3) 0.010(2) -0.029(3) C34 0.063(3) 0.028(3) 0.054(3) 0.010(2) 0.020(3) 0.008(2) C35 0.053(3) 0.052(3) 0.029(2) 0.012(2) -0.006(2) -0.005(2) C36 0.060(3) 0.043(3) 0.045(3) 0.001(2) 0.027(3) 0.011(3) C37 0.0155(18) 0.046(3) 0.0228(19) 0.0010(18) 0.0034(15) 0.0061(17) C38 0.026(2) 0.034(2) 0.031(2) -0.0079(19) -0.0024(16) 0.0099(18) C39 0.022(2) 0.029(2) 0.047(3) 0.007(2) 0.0036(18) 0.0053(17) C40 0.026(2) 0.036(2) 0.0215(19) 0.0061(17) 0.0020(16) 0.0080(17) C41 0.0219(19) 0.029(2) 0.029(2) 0.0024(17) -0.0019(16) 0.0020(16) C42 0.036(3) 0.095(5) 0.034(3) 0.014(3) 0.016(2) -0.005(3) C43 0.045(3) 0.067(4) 0.065(4) -0.041(3) -0.011(3) 0.018(3) C44 0.052(3) 0.032(3) 0.114(6) 0.022(3) 0.011(3) -0.002(3) C45 0.047(3) 0.085(4) 0.019(2) 0.010(2) 0.0055(19) 0.023(3) C46 0.026(2) 0.040(3) 0.064(3) -0.012(3) -0.009(2) -0.001(2) C47 0.075(5) 0.048(4) 0.094(6) 0.008(4) 0.042(4) 0.013(3) C48 0.233(12) 0.125(8) 0.033(4) 0.006(4) 0.019(6) 0.126(8) C49 0.124(13) 0.114(14) 0.142(14) -0.023(12) -0.055(12) -0.061(11) C50 0.117(9) 0.056(7) 0.082(8) -0.005(6) -0.034(7) -0.030(7) C51 0.159(16) 0.146(16) 0.121(15) 0.012(13) -0.036(13) -0.068(14) C52 0.094(13) 0.118(15) 0.068(10) -0.009(10) 0.000(9) -0.073(12) C53 0.061(10) 0.16(2) 0.083(12) -0.055(13) -0.010(9) -0.040(11) C63 0.054(7) 0.068(9) 0.069(8) -0.026(7) -0.015(6) -0.012(7) C54 0.077(9) 0.122(12) 0.058(7) -0.026(8) 0.011(7) -0.073(9) C55 0.100(9) 0.110(10) 0.096(9) -0.037(8) -0.008(8) -0.044(8) C56 0.121(13) 0.094(10) 0.082(13) -0.059(9) -0.031(10) -0.001(8) C57 0.114(12) 0.065(9) 0.133(13) -0.007(10) -0.079(11) -0.006(9) C58 0.095(11) 0.095(12) 0.135(14) -0.021(11) -0.042(11) 0.028(10) C59 0.091(13) 0.126(18) 0.091(13) -0.033(12) -0.004(10) -0.036(12) C60 0.054(11) 0.077(12) 0.13(3) -0.029(13) -0.033(13) 0.007(10) C64 0.045(7) 0.068(9) 0.067(9) -0.018(8) -0.027(7) 0.002(6) C61 0.057(8) 0.082(11) 0.059(9) -0.037(8) 0.002(6) 0.000(7) C62 0.072(9) 0.132(13) 0.088(10) -0.064(10) 0.010(8) -0.048(9) C65 0.046(8) 0.126(15) 0.070(10) -0.019(10) -0.013(7) 0.022(9) C66 0.20(4) 0.28(5) 0.065(16) -0.03(2) -0.06(2) 0.04(3) C67 0.14(2) 0.19(3) 0.084(16) -0.033(18) 0.051(17) 0.04(3) C68 0.088(11) 0.136(14) 0.123(13) 0.066(11) 0.062(10) 0.058(10) C69 0.042(7) 0.114(14) 0.080(11) 0.058(10) 0.013(7) 0.017(8) C70 0.085(6) 0.120(9) 0.131(9) 0.098(8) -0.032(6) -0.019(6) C71 0.128(15) 0.102(13) 0.118(14) 0.068(11) -0.050(12) -0.020(12) C72 0.090(8) 0.077(8) 0.107(9) 0.063(7) -0.064(7) -0.040(6) C73 0.132(13) 0.038(7) 0.055(8) 0.018(6) -0.049(8) 0.000(8) C75 0.101(12) 0.075(10) 0.065(9) 0.042(8) -0.014(8) 0.003(9) C76 0.061(7) 0.059(8) 0.038(6) 0.001(5) -0.003(5) -0.005(6) C77 0.037(7) 0.091(11) 0.103(12) -0.005(9) 0.023(7) 0.002(7) C78 0.121(13) 0.094(10) 0.082(13) -0.059(9) -0.031(10) -0.001(8) C79 0.040(6) 0.105(11) 0.053(7) 0.039(7) -0.004(5) 0.007(7) C80 0.066(8) 0.066(8) 0.033(6) 0.029(5) -0.013(5) -0.007(6) C81 0.110(6) 0.086(6) 0.065(4) 0.022(4) -0.036(4) -0.047(5) O7 0.070(3) 0.055(3) 0.081(4) 0.000(3) -0.020(3) -0.004(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 Rh1 N5 2.119(3) . ? Rh1 C30 2.134(4) . ? Rh1 C27 2.148(4) . ? Rh1 N1 2.160(4) . ? Rh1 C28 2.161(4) . ? Rh1 C29 2.162(4) . ? Rh1 C31 2.169(4) . ? Rh1 N2 2.204(3) . ? Rh2 N6 2.122(3) 3_665 ? Rh2 C40 2.134(4) . ? Rh2 C37 2.136(4) . ? Rh2 C41 2.165(4) . ? Rh2 C38 2.166(4) . ? Rh2 C39 2.171(4) . ? Rh2 N3 2.173(3) . ? Rh2 N4 2.177(3) . ? N1 C7 1.329(5) . ? N1 C1 1.397(5) . ? N2 C8 1.341(5) . ? N2 C9 1.397(5) . ? N3 C8 1.338(5) . ? N3 C14 1.389(5) . ? N4 C7 1.333(5) . ? N4 C6 1.397(5) . ? N5 C17 1.347(5) . ? N5 C21 1.348(5) . ? N6 C26 1.343(5) . ? N6 C22 1.344(5) . ? N6 Rh2 2.122(3) 3_665 ? S1 O3 1.425(4) . ? S1 O2 1.427(4) . ? S1 O1 1.443(3) . ? S1 C47 1.844(7) . ? S2 O5 1.368(7) . ? S2 O6 1.392(8) . ? S2 O4 1.405(7) . ? S2 C48 1.612(13) . ? F1 C47 1.324(8) . ? F2 C47 1.328(8) . ? F3 C47 1.323(9) . ? F4 C48 1.446(12) . ? F5 C48 1.424(13) . ? F6 C48 1.302(9) . ? C1 C2 1.395(5) . ? C1 C6 1.428(6) . ? C2 C3 1.383(7) . ? C3 C4 1.388(7) . ? C4 C5 1.380(6) . ? C5 C6 1.384(6) . ? C7 C8 1.423(5) . ? C9 C10 1.382(6) . ? C9 C14 1.428(6) . ? C10 C11 1.399(6) . ? C11 C12 1.396(7) . ? C12 C13 1.376(6) . ? C13 C14 1.405(5) . ? C15 C16 1.333(6) . ? C15 C19 1.458(6) . ? C16 C24 1.464(5) . ? C17 C18 1.375(6) . ? C18 C19 1.391(6) . ? C19 C20 1.400(6) . ? C20 C21 1.370(6) . ? C22 C23 1.379(5) . ? C23 C24 1.411(6) . ? C24 C25 1.384(6) . ? C25 C26 1.388(6) . ? C27 C31 1.406(7) . ? C27 C28 1.447(7) . ? C27 C32 1.494(7) . ? C28 C29 1.415(6) . ? C28 C33 1.472(7) . ? C29 C30 1.445(6) . ? C29 C34 1.483(6) . ? C30 C31 1.437(6) . ? C30 C35 1.486(6) . ? C31 C36 1.513(7) . ? C37 C41 1.423(6) . ? C37 C38 1.444(7) . ? C37 C42 1.496(6) . ? C38 C39 1.398(6) . ? C38 C43 1.483(6) . ? C39 C40 1.431(6) . ? C39 C44 1.498(7) . ? C40 C41 1.428(6) . ? C40 C45 1.498(6) . ? C41 C46 1.486(6) . ? C49 C63 1.340(7) . ? C49 C50 1.340(7) . ? C49 C62 1.431(19) . ? C50 C51 1.340(7) . ? C51 C52 1.340(7) . ? C52 C53 1.340(7) . ? C53 C54 1.28(2) . ? C53 C63 1.340(7) . ? C63 C64 1.348(16) . ? C54 C55 1.30(3) . ? C55 C56 1.41(3) . ? C56 C64 1.426(8) . ? C56 C57 1.426(8) . ? C57 C58 1.426(8) . ? C58 C59 1.426(8) . ? C59 C60 1.426(8) . ? C60 C64 1.426(8) . ? C60 C61 1.429(19) . ? C61 C62 1.46(3) . ? C65 C79 1.35(2) . ? C65 C66 1.39(4) . ? C65 C78 1.56(3) . ? C66 C67 1.52(5) . ? C67 C68 1.57(4) . ? C68 C69 1.34(3) . ? C69 C73 1.17(2) 3_667 ? C69 C79 1.420(17) . ? C69 C70 1.44(2) . ? C70 C73 1.26(2) 3_667 ? C70 C75 1.32(2) 3_667 ? C70 C71 1.57(3) . ? C71 C80 1.18(3) 3_667 ? C71 C76 1.23(2) 3_667 ? C71 C72 1.38(3) . ? C71 C75 1.54(3) 3_667 ? C71 C73 1.60(3) 3_667 ? C72 C80 1.344(13) . ? C72 C80 1.344(13) 3_667 ? C72 C71 1.38(3) 3_667 ? C72 C73 1.63(2) 3_667 ? C72 C73 1.63(2) . ? C73 C69 1.17(2) 3_667 ? C73 C70 1.26(2) 3_667 ? C73 C79 1.41(2) 3_667 ? C73 C71 1.60(3) 3_667 ? C73 C80 1.63(3) 3_667 ? C75 C70 1.32(2) 3_667 ? C75 C76 1.45(2) . ? C75 C71 1.54(3) 3_667 ? C76 C71 1.23(3) 3_667 ? C76 C77 1.41(2) . ? C76 C80 1.426(19) . ? C77 C78 1.23(2) . ? C79 C73 1.41(2) 3_667 ? C79 C80 1.44(2) . ? C80 C71 1.18(3) 3_667 ? C80 C73 1.63(3) 3_667 ? C81 O7 1.392(8) . ? 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 N5 Rh1 C30 102.41(15) . . ? N5 Rh1 C27 159.11(17) . . ? C30 Rh1 C27 65.35(17) . . ? N5 Rh1 N1 89.25(13) . . ? C30 Rh1 N1 111.26(15) . . ? C27 Rh1 N1 110.70(17) . . ? N5 Rh1 C28 121.09(16) . . ? C30 Rh1 C28 65.41(17) . . ? C27 Rh1 C28 39.25(19) . . ? N1 Rh1 C28 149.66(16) . . ? N5 Rh1 C29 94.81(15) . . ? C30 Rh1 C29 39.31(17) . . ? C27 Rh1 C29 64.84(18) . . ? N1 Rh1 C29 150.44(15) . . ? C28 Rh1 C29 38.21(17) . . ? N5 Rh1 C31 138.74(16) . . ? C30 Rh1 C31 39.00(17) . . ? C27 Rh1 C31 38.01(18) . . ? N1 Rh1 C31 93.56(15) . . ? C28 Rh1 C31 64.48(17) . . ? C29 Rh1 C31 64.58(16) . . ? N5 Rh1 N2 88.57(12) . . ? C30 Rh1 N2 164.40(15) . . ? C27 Rh1 N2 100.74(15) . . ? N1 Rh1 N2 79.55(12) . . ? C28 Rh1 N2 99.48(15) . . ? C29 Rh1 N2 129.73(15) . . ? C31 Rh1 N2 132.42(15) . . ? N6 Rh2 C40 102.72(14) 3_665 . ? N6 Rh2 C37 163.19(15) 3_665 . ? C40 Rh2 C37 65.23(15) . . ? N6 Rh2 C41 136.69(14) 3_665 . ? C40 Rh2 C41 38.78(15) . . ? C37 Rh2 C41 38.62(15) . . ? N6 Rh2 C38 125.98(15) 3_665 . ? C40 Rh2 C38 64.30(16) . . ? C37 Rh2 C38 39.22(17) . . ? C41 Rh2 C38 64.43(16) . . ? N6 Rh2 C39 98.40(14) 3_665 . ? C40 Rh2 C39 38.81(17) . . ? C37 Rh2 C39 64.82(16) . . ? C41 Rh2 C39 64.54(16) . . ? C38 Rh2 C39 37.60(17) . . ? N6 Rh2 N3 88.65(12) 3_665 . ? C40 Rh2 N3 115.10(15) . . ? C37 Rh2 N3 106.89(16) . . ? C41 Rh2 N3 93.17(14) . . ? C38 Rh2 N3 145.28(15) . . ? C39 Rh2 N3 153.85(15) . . ? N6 Rh2 N4 88.89(12) 3_665 . ? C40 Rh2 N4 161.48(14) . . ? C37 Rh2 N4 100.13(14) . . ? C41 Rh2 N4 133.93(14) . . ? C38 Rh2 N4 97.22(14) . . ? C39 Rh2 N4 125.92(16) . . ? N3 Rh2 N4 79.09(12) . . ? C7 N1 C1 103.0(3) . . ? C7 N1 Rh1 109.4(3) . . ? C1 N1 Rh1 147.6(3) . . ? C8 N2 C9 102.3(3) . . ? C8 N2 Rh1 107.4(2) . . ? C9 N2 Rh1 150.3(3) . . ? C8 N3 C14 102.7(3) . . ? C8 N3 Rh2 108.7(3) . . ? C14 N3 Rh2 148.2(3) . . ? C7 N4 C6 103.2(3) . . ? C7 N4 Rh2 108.6(3) . . ? C6 N4 Rh2 148.2(3) . . ? C17 N5 C21 117.5(4) . . ? C17 N5 Rh1 121.1(3) . . ? C21 N5 Rh1 121.4(3) . . ? C26 N6 C22 117.6(3) . . ? C26 N6 Rh2 122.5(3) . 3_665 ? C22 N6 Rh2 120.0(3) . 3_665 ? O3 S1 O2 116.2(3) . . ? O3 S1 O1 115.4(2) . . ? O2 S1 O1 114.4(3) . . ? O3 S1 C47 101.6(3) . . ? O2 S1 C47 104.6(4) . . ? O1 S1 C47 101.8(3) . . ? O5 S2 O6 113.2(6) . . ? O5 S2 O4 113.8(5) . . ? O6 S2 O4 117.1(5) . . ? O5 S2 C48 105.8(5) . . ? O6 S2 C48 102.3(6) . . ? O4 S2 C48 102.5(6) . . ? C2 C1 N1 131.3(4) . . ? C2 C1 C6 120.5(4) . . ? N1 C1 C6 108.1(3) . . ? C3 C2 C1 117.1(4) . . ? C2 C3 C4 121.9(4) . . ? C5 C4 C3 122.0(4) . . ? C4 C5 C6 117.3(4) . . ? C5 C6 N4 131.2(4) . . ? C5 C6 C1 121.1(4) . . ? N4 C6 C1 107.6(3) . . ? N1 C7 N4 118.2(4) . . ? N1 C7 C8 120.6(4) . . ? N4 C7 C8 120.8(4) . . ? N3 C8 N2 118.5(4) . . ? N3 C8 C7 119.7(4) . . ? N2 C8 C7 121.1(4) . . ? C10 C9 N2 131.0(4) . . ? C10 C9 C14 120.8(4) . . ? N2 C9 C14 108.2(3) . . ? C9 C10 C11 117.9(4) . . ? C12 C11 C10 121.0(4) . . ? C13 C12 C11 122.4(4) . . ? C12 C13 C14 117.2(4) . . ? N3 C14 C13 130.8(4) . . ? N3 C14 C9 108.3(3) . . ? C13 C14 C9 120.7(4) . . ? C16 C15 C19 125.0(4) . . ? C15 C16 C24 125.7(4) . . ? N5 C17 C18 122.1(4) . . ? C17 C18 C19 120.8(4) . . ? C18 C19 C20 116.5(4) . . ? C18 C19 C15 124.3(4) . . ? C20 C19 C15 119.1(4) . . ? C21 C20 C19 119.7(4) . . ? N5 C21 C20 123.3(4) . . ? N6 C22 C23 123.9(4) . . ? C22 C23 C24 118.7(4) . . ? C25 C24 C23 116.9(4) . . ? C25 C24 C16 120.9(4) . . ? C23 C24 C16 122.2(4) . . ? C24 C25 C26 120.8(4) . . ? N6 C26 C25 122.0(4) . . ? C31 C27 C28 108.1(4) . . ? C31 C27 C32 126.1(5) . . ? C28 C27 C32 125.5(5) . . ? C31 C27 Rh1 71.8(2) . . ? C28 C27 Rh1 70.9(2) . . ? C32 C27 Rh1 127.5(4) . . ? C29 C28 C27 107.6(4) . . ? C29 C28 C33 126.7(5) . . ? C27 C28 C33 125.5(5) . . ? C29 C28 Rh1 70.9(2) . . ? C27 C28 Rh1 69.9(2) . . ? C33 C28 Rh1 128.5(3) . . ? C28 C29 C30 108.4(4) . . ? C28 C29 C34 127.2(5) . . ? C30 C29 C34 124.4(4) . . ? C28 C29 Rh1 70.9(2) . . ? C30 C29 Rh1 69.3(2) . . ? C34 C29 Rh1 125.3(3) . . ? C31 C30 C29 106.8(4) . . ? C31 C30 C35 126.7(4) . . ? C29 C30 C35 126.0(4) . . ? C31 C30 Rh1 71.8(2) . . ? C29 C30 Rh1 71.4(2) . . ? C35 C30 Rh1 128.1(3) . . ? C27 C31 C30 108.8(4) . . ? C27 C31 C36 126.1(5) . . ? C30 C31 C36 125.1(5) . . ? C27 C31 Rh1 70.2(2) . . ? C30 C31 Rh1 69.2(2) . . ? C36 C31 Rh1 124.2(3) . . ? C41 C37 C38 107.3(4) . . ? C41 C37 C42 127.0(4) . . ? C38 C37 C42 125.5(4) . . ? C41 C37 Rh2 71.8(2) . . ? C38 C37 Rh2 71.5(2) . . ? C42 C37 Rh2 125.7(3) . . ? C39 C38 C37 108.6(4) . . ? C39 C38 C43 127.1(5) . . ? C37 C38 C43 124.2(5) . . ? C39 C38 Rh2 71.4(2) . . ? C37 C38 Rh2 69.3(2) . . ? C43 C38 Rh2 127.6(3) . . ? C38 C39 C40 108.0(4) . . ? C38 C39 C44 127.0(5) . . ? C40 C39 C44 124.8(5) . . ? C38 C39 Rh2 71.0(3) . . ? C40 C39 Rh2 69.2(2) . . ? C44 C39 Rh2 129.1(3) . . ? C41 C40 C39 108.2(4) . . ? C41 C40 C45 124.9(4) . . ? C39 C40 C45 126.3(4) . . ? C41 C40 Rh2 71.8(2) . . ? C39 C40 Rh2 72.0(2) . . ? C45 C40 Rh2 128.7(3) . . ? C37 C41 C40 107.7(4) . . ? C37 C41 C46 125.3(4) . . ? C40 C41 C46 127.0(4) . . ? C37 C41 Rh2 69.6(2) . . ? C40 C41 Rh2 69.4(2) . . ? C46 C41 Rh2 125.8(3) . . ? F3 C47 F1 108.2(6) . . ? F3 C47 F2 109.5(8) . . ? F1 C47 F2 108.1(6) . . ? F3 C47 S1 110.6(5) . . ? F1 C47 S1 109.8(6) . . ? F2 C47 S1 110.6(5) . . ? F6 C48 F5 104.0(9) . . ? F6 C48 F4 98.7(9) . . ? F5 C48 F4 92.7(10) . . ? F6 C48 S2 121.0(11) . . ? F5 C48 S2 116.1(7) . . ? F4 C48 S2 119.4(6) . . ? C63 C49 C50 120.0 . . ? C63 C49 C62 117.5(14) . . ? C50 C49 C62 122.5(14) . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 106.4(14) . . ? C54 C53 C63 133.6(14) . . ? C52 C53 C63 120.0 . . ? C49 C63 C53 120.0 . . ? C49 C63 C64 127.5(11) . . ? C53 C63 C64 112.5(11) . . ? C53 C54 C55 109.3(17) . . ? C54 C55 C56 132(2) . . ? C55 C56 C64 108.8(14) . . ? C55 C56 C57 131.2(14) . . ? C64 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C59 C58 C57 120.0 . . ? C58 C59 C60 120.0 . . ? C64 C60 C59 120.0 . . ? C64 C60 C61 123.7(12) . . ? C59 C60 C61 116.3(12) . . ? C63 C64 C56 124.2(10) . . ? C63 C64 C60 115.8(10) . . ? C56 C64 C60 120.0 . . ? C60 C61 C62 114.4(15) . . ? C49 C62 C61 121.1(17) . . ? C79 C65 C66 127(3) . . ? C79 C65 C78 119.6(14) . . ? C66 C65 C78 113(3) . . ? C65 C66 C67 112(3) . . ? C66 C67 C68 117(3) . . ? C69 C68 C67 119.6(16) . . ? C73 C69 C68 176(2) 3_667 . ? C73 C69 C79 64.9(13) 3_667 . ? C68 C69 C79 119.2(19) . . ? C73 C69 C70 56.5(15) 3_667 . ? C68 C69 C70 119.3(16) . . ? C79 C69 C70 121.4(17) . . ? C73 C70 C75 131.4(18) 3_667 3_667 ? C73 C70 C69 50.8(10) 3_667 . ? C75 C70 C69 175.6(13) 3_667 . ? C73 C70 C71 67.8(13) 3_667 . ? C75 C70 C71 63.9(13) 3_667 . ? C69 C70 C71 118.5(14) . . ? C80 C71 C76 72(2) 3_667 3_667 ? C80 C71 C72 62.7(17) 3_667 . ? C76 C71 C72 135(3) 3_667 . ? C80 C71 C75 134(2) 3_667 3_667 ? C76 C71 C75 61.7(14) 3_667 3_667 ? C72 C71 C75 163(3) . 3_667 ? C80 C71 C70 175(2) 3_667 . ? C76 C71 C70 112(2) 3_667 . ? C72 C71 C70 112.9(18) . . ? C75 C71 C70 50.2(14) 3_667 . ? C80 C71 C73 129(2) 3_667 3_667 ? C76 C71 C73 159(3) 3_667 3_667 ? C72 C71 C73 66.0(14) . 3_667 ? C75 C71 C73 97(2) 3_667 3_667 ? C70 C71 C73 46.9(13) . 3_667 ? C80 C72 C80 179.996(4) . 3_667 ? C80 C72 C71 128.7(13) . . ? C80 C72 C71 51.3(13) 3_667 . ? C80 C72 C71 51.3(13) . 3_667 ? C80 C72 C71 128.7(13) 3_667 3_667 ? C71 C72 C71 179.997(4) . 3_667 ? C80 C72 C73 65.5(9) . 3_667 ? C80 C72 C73 114.5(9) 3_667 3_667 ? C71 C72 C73 63.3(14) . 3_667 ? C71 C72 C73 116.7(14) 3_667 3_667 ? C80 C72 C73 114.5(9) . . ? C80 C72 C73 65.5(9) 3_667 . ? C71 C72 C73 116.7(14) . . ? C71 C72 C73 63.3(14) 3_667 . ? C73 C72 C73 179.999(7) 3_667 . ? C69 C73 C70 72.7(18) 3_667 3_667 ? C69 C73 C79 66.2(12) 3_667 3_667 ? C70 C73 C79 139(2) 3_667 3_667 ? C69 C73 C71 138(2) 3_667 3_667 ? C70 C73 C71 65.3(14) 3_667 3_667 ? C79 C73 C71 156(2) 3_667 3_667 ? C69 C73 C80 122.4(15) 3_667 3_667 ? C70 C73 C80 164.1(16) 3_667 3_667 ? C79 C73 C80 56.3(11) 3_667 3_667 ? C71 C73 C80 99.3(17) 3_667 3_667 ? C69 C73 C72 170.9(18) 3_667 . ? C70 C73 C72 115.9(12) 3_667 . ? C79 C73 C72 105.0(16) 3_667 . ? C71 C73 C72 50.6(13) 3_667 . ? C80 C73 C72 48.7(8) 3_667 . ? C70 C75 C76 114.6(15) 3_667 . ? C70 C75 C71 66.0(14) 3_667 3_667 ? C76 C75 C71 48.7(13) . 3_667 ? C71 C76 C77 170(2) 3_667 . ? C71 C76 C80 52.0(16) 3_667 . ? C77 C76 C80 118.3(12) . . ? C71 C76 C75 69.6(18) 3_667 . ? C77 C76 C75 120.1(13) . . ? C80 C76 C75 121.5(13) . . ? C78 C77 C76 126.7(16) . . ? C77 C78 C65 116.6(19) . . ? C65 C79 C73 170.4(17) . 3_667 ? C65 C79 C69 122.1(16) . . ? C73 C79 C69 48.9(12) 3_667 . ? C65 C79 C80 119.5(12) . . ? C73 C79 C80 69.6(13) 3_667 . ? C69 C79 C80 118.4(15) . . ? C71 C80 C72 66.0(14) 3_667 . ? C71 C80 C76 55.6(14) 3_667 . ? C72 C80 C76 121.5(13) . . ? C71 C80 C79 173.1(18) 3_667 . ? C72 C80 C79 119.9(11) . . ? C76 C80 C79 118.5(12) . . ? C71 C80 C73 131.7(17) 3_667 3_667 ? C72 C80 C73 65.8(8) . 3_667 ? C76 C80 C73 172.2(14) . 3_667 ? C79 C80 C73 54.1(9) . 3_667 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.000 115.9 23.1 2 0.089 0.023 0.250 8.8 -0.8 3 0.911 0.523 0.250 8.8 -0.9 4 0.500 0.500 0.500 115.9 23.2 5 0.089 0.477 0.750 8.8 -0.7 6 0.911 0.977 0.750 8.8 -0.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.487 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.125 _database_code_depnum_ccdc_archive 'CCDC 927806'