# Electronic Supplementary Material (ESI) for Chemical Science # 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_d:\xray\yong005\yong005 #TrackingRef 'compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H46 B2 F12 N10 O Rh2' _chemical_formula_weight 1162.33 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.042(2) _cell_length_b 32.589(7) _cell_length_c 14.243(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.66(3) _cell_angle_gamma 90.00 _cell_volume 5036.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9294 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53723 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.81 _reflns_number_total 10690 _reflns_number_gt 7850 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+18.7840P] 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 10690 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.004 _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 0.93484(4) 0.153046(13) 0.69841(3) 0.03235(12) Uani 1 1 d . . . Rh2 Rh 1.08536(4) 0.147648(12) 0.85889(3) 0.03090(11) Uani 1 1 d . . . N9 N 0.7990(4) 0.15599(14) 0.5597(3) 0.0376(10) Uani 1 1 d . . . N1 N 1.0164(4) 0.10022(14) 0.6654(3) 0.0356(10) Uani 1 1 d . . . N2 N 1.1839(4) 0.10809(13) 0.7905(3) 0.0336(10) Uani 1 1 d . . . N3 N 0.8172(4) 0.11899(13) 0.7631(3) 0.0345(10) Uani 1 1 d . . . C20 C 1.1272(5) 0.08966(16) 0.7115(3) 0.0328(11) Uani 1 1 d . . . H20 H 1.1684 0.0677 0.6866 0.039 Uiso 1 1 calc R . . N4 N 0.9781(4) 0.10031(13) 0.8858(3) 0.0327(9) Uani 1 1 d . . . F10 F 1.6495(3) 0.05378(11) 0.9693(2) 0.0533(9) Uani 1 1 d . . . C7 C 0.8621(5) 0.09733(16) 0.8399(4) 0.0338(11) Uani 1 1 d . . . H7 H 0.8089 0.0786 0.8635 0.041 Uiso 1 1 calc R . . C5 C 0.6123(5) 0.1464(2) 0.6976(4) 0.0493(15) Uani 1 1 d . . . H5 H 0.6425 0.1733 0.7141 0.059 Uiso 1 1 calc R . . C21 C 1.3031(5) 0.09349(16) 0.8348(3) 0.0326(11) Uani 1 1 d . . . C28 C 1.3466(7) 0.1443(2) 1.1671(5) 0.0650(19) Uani 1 1 d . . . H28A H 1.3947 0.1188 1.1775 0.098 Uiso 1 1 calc R . . H28B H 1.2951 0.1468 1.2160 0.098 Uiso 1 1 calc R . . H28C H 1.4026 0.1678 1.1714 0.098 Uiso 1 1 calc R . . C24 C 1.5353(5) 0.06709(19) 0.9252(4) 0.0401(13) Uani 1 1 d . . . C13 C 1.1015(5) 0.04556(17) 0.9745(4) 0.0453(14) Uani 1 1 d . . . H13 H 1.1321 0.0388 0.9183 0.054 Uiso 1 1 calc R . . C27 C 1.2682(5) 0.14331(17) 1.0725(4) 0.0427(13) Uani 1 1 d . . . C4 C 0.6911(5) 0.11305(18) 0.7191(4) 0.0382(12) Uani 1 1 d . . . C26 C 1.3949(5) 0.12172(17) 0.8759(4) 0.0371(12) Uani 1 1 d . . . H26 H 1.3772 0.1503 0.8726 0.045 Uiso 1 1 calc R . . C22 C 1.3322(5) 0.05182(17) 0.8404(4) 0.0378(12) Uani 1 1 d . . . H22 H 1.2719 0.0323 0.8134 0.045 Uiso 1 1 calc R . . C25 C 1.5101(5) 0.10843(18) 0.9208(4) 0.0410(13) Uani 1 1 d . . . H25 H 1.5711 0.1277 0.9483 0.049 Uiso 1 1 calc R . . C8 C 1.0150(5) 0.07640(16) 0.9715(4) 0.0348(11) Uani 1 1 d . . . C30 C 0.7133(6) 0.15526(17) 0.5000(4) 0.0440(14) Uani 1 1 d . . . C29 C 0.6023(7) 0.1531(2) 0.4256(5) 0.0627(18) Uani 1 1 d . . . H29A H 0.6077 0.1292 0.3847 0.094 Uiso 1 1 calc R . . H29B H 0.5955 0.1781 0.3869 0.094 Uiso 1 1 calc R . . H29C H 0.5296 0.1505 0.4555 0.094 Uiso 1 1 calc R . . F6 F 0.4108(4) 0.21860(14) 0.0098(3) 0.0800(13) Uani 1 1 d . . . F5 F 0.5999(4) 0.19912(14) 0.0831(4) 0.0890(14) Uani 1 1 d . . . F7 F 0.5790(4) 0.25460(18) -0.0120(4) 0.117(2) Uani 1 1 d . . . F8 F 0.5153(5) 0.2561(2) 0.1282(5) 0.128(2) Uani 1 1 d . . . B2 B 0.5248(7) 0.2322(2) 0.0515(6) 0.0523(18) Uani 1 1 d . . . N5 N 1.0552(4) 0.18398(15) 0.6324(3) 0.0403(11) Uani 1 1 d . . . N6 N 0.8617(4) 0.20664(14) 0.7367(3) 0.0406(11) Uani 1 1 d . . . N8 N 0.9830(4) 0.18381(14) 0.9306(3) 0.0356(10) Uani 1 1 d . . . N7 N 1.1873(4) 0.19686(14) 0.8303(3) 0.0368(10) Uani 1 1 d . . . C37 C 0.9339(5) 0.20144(19) 0.9811(4) 0.0433(14) Uani 1 1 d . . . C33 C 0.8171(5) 0.23566(18) 0.7615(4) 0.0423(13) Uani 1 1 d . . . C17 C 0.9664(5) 0.07765(16) 0.5801(3) 0.0348(12) Uani 1 1 d . . . C16 C 0.8993(6) 0.0427(2) 0.5847(5) 0.0614(18) Uani 1 1 d . . . H16 H 0.8869 0.0329 0.6450 0.074 Uiso 1 1 calc R . . C12 C 1.1439(6) 0.02441(19) 1.0579(5) 0.0545(17) Uani 1 1 d . . . H12 H 1.2053 0.0038 1.0598 0.065 Uiso 1 1 calc R . . C3 C 0.6453(6) 0.0743(2) 0.6959(4) 0.0500(15) Uani 1 1 d . . . H3 H 0.6975 0.0511 0.7099 0.060 Uiso 1 1 calc R . . C23 C 1.4492(5) 0.03833(19) 0.8852(4) 0.0436(14) Uani 1 1 d . . . H23 H 1.4689 0.0099 0.8881 0.052 Uiso 1 1 calc R . . C35 C 1.2495(5) 0.22317(17) 0.8188(4) 0.0393(12) Uani 1 1 d . . . C34 C 0.7588(7) 0.2718(2) 0.7953(5) 0.0598(18) Uani 1 1 d . . . H34A H 0.7080 0.2857 0.7408 0.090 Uiso 1 1 calc R . . H34B H 0.8225 0.2906 0.8271 0.090 Uiso 1 1 calc R . . H34C H 0.7067 0.2632 0.8405 0.090 Uiso 1 1 calc R . . C2 C 0.5197(6) 0.0690(2) 0.6511(5) 0.0587(18) Uani 1 1 d . . . H2 H 0.4865 0.0424 0.6359 0.070 Uiso 1 1 calc R . . C1 C 0.4493(6) 0.1030(3) 0.6310(4) 0.0592(19) Uani 1 1 d . . . C6 C 0.4910(6) 0.1414(2) 0.6529(5) 0.0577(18) Uani 1 1 d . . . H6 H 0.4383 0.1645 0.6379 0.069 Uiso 1 1 calc R . . C36 C 1.3327(6) 0.2566(2) 0.8021(5) 0.0603(18) Uani 1 1 d . . . H36A H 1.4087 0.2553 0.8501 0.090 Uiso 1 1 calc R . . H36B H 1.2921 0.2831 0.8070 0.090 Uiso 1 1 calc R . . H36C H 1.3526 0.2538 0.7382 0.090 Uiso 1 1 calc R . . N10 N 1.2084(4) 0.14215(13) 0.9982(3) 0.0373(10) Uani 1 1 d . . . F12 F 0.3284(3) 0.09716(17) 0.5846(3) 0.0861(15) Uani 1 1 d . . . F11 F 1.1414(6) 0.01173(16) 1.2190(3) 0.1115(19) Uani 1 1 d . . . C31 C 1.1180(6) 0.2012(2) 0.5923(4) 0.0530(16) Uani 1 1 d . . . C9 C 0.9699(9) 0.0850(2) 1.0530(5) 0.082(3) Uani 1 1 d . . . H9 H 0.9086 0.1055 1.0523 0.098 Uiso 1 1 calc R . . C32 C 1.2011(7) 0.2240(3) 0.5403(5) 0.091(3) Uani 1 1 d . . . H32A H 1.1767 0.2189 0.4716 0.137 Uiso 1 1 calc R . . H32B H 1.2861 0.2147 0.5620 0.137 Uiso 1 1 calc R . . H32C H 1.1955 0.2534 0.5528 0.137 Uiso 1 1 calc R . . C11 C 1.0981(8) 0.0331(2) 1.1356(5) 0.073(2) Uani 1 1 d . . . C15 C 0.8485(7) 0.0213(3) 0.5010(8) 0.090(3) Uani 1 1 d . . . H15 H 0.7999 -0.0025 0.5040 0.108 Uiso 1 1 calc R . . O1 O 0.5513(5) 0.07764(14) 0.2734(3) 0.0685(13) Uani 1 1 d . . . F1 F 0.1630(5) 0.15480(16) 0.3317(4) 0.1105(19) Uani 1 1 d . . . F3 F -0.0394(5) 0.15226(17) 0.2530(6) 0.130(2) Uani 1 1 d . . . F9 F 0.8216(6) 0.01375(18) 0.3358(4) 0.143(3) Uani 1 1 d . . . F2 F 0.0379(5) 0.20673(19) 0.3369(5) 0.140(3) Uani 1 1 d . . . F4 F 0.0925(5) 0.1942(2) 0.2042(5) 0.145(3) Uani 1 1 d . . . C41 C 0.6105(7) 0.0730(2) 0.1930(5) 0.0659(19) Uani 1 1 d . . . H41A H 0.5477 0.0703 0.1340 0.079 Uiso 1 1 calc R . . H41B H 0.6616 0.0479 0.2005 0.079 Uiso 1 1 calc R . . C38 C 0.8710(7) 0.2238(3) 1.0472(5) 0.075(2) Uani 1 1 d . . . H38A H 0.7884 0.2124 1.0444 0.112 Uiso 1 1 calc R . . H38B H 0.8644 0.2529 1.0291 0.112 Uiso 1 1 calc R . . H38C H 0.9182 0.2212 1.1123 0.112 Uiso 1 1 calc R . . C42 C 0.6902(7) 0.1098(3) 0.1856(6) 0.082(2) Uani 1 1 d . . . H42A H 0.6390 0.1346 0.1772 0.123 Uiso 1 1 calc R . . H42B H 0.7314 0.1066 0.1307 0.123 Uiso 1 1 calc R . . H42C H 0.7523 0.1123 0.2442 0.123 Uiso 1 1 calc R . . C14 C 0.8700(9) 0.0353(3) 0.4161(6) 0.088(3) Uani 1 1 d . . . C19 C 0.9834(9) 0.0913(2) 0.4922(5) 0.084(3) Uani 1 1 d . . . H19 H 1.0301 0.1154 0.4871 0.100 Uiso 1 1 calc R . . C39 C 0.4733(10) 0.0438(3) 0.2831(6) 0.097(3) Uani 1 1 d . . . H39A H 0.5214 0.0180 0.2894 0.116 Uiso 1 1 calc R . . H39B H 0.4071 0.0416 0.2261 0.116 Uiso 1 1 calc R . . B1 B 0.0602(9) 0.1750(3) 0.2853(8) 0.073(3) Uani 1 1 d . . . C40 C 0.4169(13) 0.0507(3) 0.3731(7) 0.132(5) Uani 1 1 d . . . H40A H 0.4824 0.0576 0.4271 0.198 Uiso 1 1 calc R . . H40B H 0.3750 0.0257 0.3878 0.198 Uiso 1 1 calc R . . H40C H 0.3574 0.0733 0.3617 0.198 Uiso 1 1 calc R . . C10 C 1.0146(11) 0.0633(3) 1.1373(5) 0.111(4) Uani 1 1 d . . . H10 H 0.9866 0.0697 1.1948 0.134 Uiso 1 1 calc R . . C18 C 0.9313(12) 0.0693(3) 0.4101(5) 0.116(4) Uani 1 1 d . . . H18 H 0.9406 0.0791 0.3491 0.139 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0345(2) 0.0400(2) 0.0249(2) 0.00340(16) 0.01173(16) 0.00347(18) Rh2 0.0328(2) 0.0380(2) 0.0244(2) 0.00055(16) 0.01176(15) 0.00221(17) N9 0.040(3) 0.043(3) 0.032(2) 0.0041(19) 0.014(2) 0.005(2) N1 0.037(3) 0.048(3) 0.023(2) -0.0007(18) 0.0075(18) 0.001(2) N2 0.030(2) 0.047(3) 0.026(2) 0.0005(19) 0.0095(17) 0.0047(19) N3 0.032(2) 0.043(3) 0.030(2) 0.0039(18) 0.0107(18) 0.0041(19) C20 0.039(3) 0.037(3) 0.026(2) 0.002(2) 0.016(2) 0.003(2) N4 0.036(2) 0.038(2) 0.025(2) 0.0032(17) 0.0098(18) 0.0048(19) F10 0.0343(18) 0.074(2) 0.051(2) 0.0053(18) 0.0076(15) 0.0128(17) C7 0.035(3) 0.038(3) 0.031(3) 0.000(2) 0.012(2) 0.001(2) C5 0.038(3) 0.067(4) 0.045(3) 0.014(3) 0.013(3) 0.009(3) C21 0.033(3) 0.040(3) 0.028(3) 0.003(2) 0.013(2) 0.008(2) C28 0.070(5) 0.068(5) 0.051(4) -0.004(3) -0.006(3) 0.007(4) C24 0.027(3) 0.061(4) 0.035(3) 0.003(3) 0.013(2) 0.010(3) C13 0.048(3) 0.037(3) 0.056(4) 0.012(3) 0.025(3) 0.005(3) C27 0.045(3) 0.043(3) 0.040(3) -0.002(2) 0.008(3) 0.005(3) C4 0.038(3) 0.052(3) 0.028(3) 0.005(2) 0.014(2) -0.001(3) C26 0.038(3) 0.039(3) 0.037(3) -0.001(2) 0.013(2) -0.002(2) C22 0.040(3) 0.045(3) 0.030(3) -0.004(2) 0.011(2) 0.000(2) C25 0.032(3) 0.054(4) 0.038(3) 0.001(3) 0.009(2) 0.001(3) C8 0.040(3) 0.034(3) 0.031(3) 0.006(2) 0.010(2) 0.002(2) C30 0.057(4) 0.039(3) 0.037(3) 0.005(2) 0.011(3) -0.004(3) C29 0.067(5) 0.068(5) 0.048(4) 0.001(3) -0.004(3) -0.012(4) F6 0.051(2) 0.089(3) 0.096(3) 0.001(3) 0.002(2) -0.014(2) F5 0.076(3) 0.073(3) 0.113(4) 0.016(3) 0.007(3) 0.010(2) F7 0.063(3) 0.138(5) 0.149(5) 0.074(4) 0.013(3) -0.007(3) F8 0.102(4) 0.138(5) 0.140(5) -0.073(4) 0.010(4) 0.002(4) B2 0.037(4) 0.053(4) 0.066(5) 0.004(4) 0.008(3) 0.004(3) N5 0.039(3) 0.049(3) 0.034(2) 0.007(2) 0.008(2) 0.000(2) N6 0.045(3) 0.046(3) 0.032(2) 0.006(2) 0.009(2) 0.009(2) N8 0.038(3) 0.043(3) 0.027(2) -0.0016(19) 0.0093(19) 0.001(2) N7 0.041(3) 0.041(3) 0.028(2) -0.0010(19) 0.0069(19) 0.004(2) C37 0.037(3) 0.062(4) 0.029(3) -0.006(3) 0.004(2) 0.008(3) C33 0.050(4) 0.042(3) 0.036(3) 0.007(2) 0.014(3) 0.008(3) C17 0.037(3) 0.043(3) 0.024(2) -0.001(2) 0.005(2) 0.009(2) C16 0.065(4) 0.058(4) 0.070(5) -0.024(3) 0.033(4) -0.016(3) C12 0.039(3) 0.047(4) 0.078(5) 0.018(3) 0.010(3) 0.006(3) C3 0.041(3) 0.063(4) 0.047(4) 0.005(3) 0.012(3) 0.001(3) C23 0.047(3) 0.052(3) 0.036(3) 0.001(3) 0.017(3) 0.014(3) C35 0.043(3) 0.039(3) 0.037(3) 0.001(2) 0.011(2) 0.002(3) C34 0.074(5) 0.051(4) 0.056(4) 0.000(3) 0.019(4) 0.021(3) C2 0.049(4) 0.082(5) 0.046(4) 0.008(3) 0.011(3) -0.015(4) C1 0.033(3) 0.113(6) 0.035(3) 0.017(4) 0.014(3) -0.002(4) C6 0.041(4) 0.089(5) 0.046(4) 0.020(3) 0.016(3) 0.015(4) C36 0.064(4) 0.047(4) 0.074(5) 0.011(3) 0.022(4) -0.011(3) N10 0.044(3) 0.040(3) 0.031(2) -0.0005(19) 0.014(2) 0.000(2) F12 0.033(2) 0.168(5) 0.058(2) 0.017(3) 0.0087(18) -0.010(2) F11 0.176(5) 0.094(4) 0.054(3) 0.038(3) -0.005(3) 0.041(4) C31 0.043(4) 0.080(5) 0.036(3) 0.018(3) 0.009(3) -0.004(3) C9 0.137(7) 0.077(5) 0.044(4) 0.026(3) 0.048(4) 0.064(5) C32 0.067(5) 0.149(8) 0.058(5) 0.042(5) 0.011(4) -0.036(5) C11 0.107(6) 0.053(4) 0.051(4) 0.018(3) -0.004(4) 0.020(4) C15 0.054(5) 0.093(6) 0.125(8) -0.065(6) 0.023(5) -0.020(4) O1 0.092(4) 0.055(3) 0.058(3) -0.001(2) 0.013(3) -0.003(3) F1 0.108(4) 0.106(4) 0.119(4) 0.052(3) 0.026(3) 0.041(3) F3 0.097(4) 0.087(4) 0.209(7) -0.046(4) 0.037(4) -0.037(3) F9 0.168(6) 0.126(5) 0.096(4) -0.073(3) -0.078(4) 0.075(4) F2 0.082(4) 0.116(5) 0.199(7) -0.068(5) -0.032(4) 0.019(3) F4 0.092(4) 0.194(7) 0.133(5) 0.078(5) -0.022(4) -0.003(4) C41 0.076(5) 0.064(5) 0.057(4) -0.005(3) 0.012(4) 0.007(4) C38 0.065(5) 0.113(6) 0.046(4) -0.029(4) 0.009(3) 0.036(4) C42 0.062(5) 0.086(6) 0.099(6) -0.008(5) 0.014(4) -0.012(4) C14 0.093(6) 0.093(7) 0.061(5) -0.044(5) -0.032(5) 0.038(5) C19 0.168(9) 0.056(4) 0.033(3) -0.004(3) 0.034(4) -0.010(5) C39 0.163(10) 0.061(5) 0.078(6) -0.004(4) 0.051(6) -0.024(6) B1 0.066(6) 0.054(5) 0.096(7) 0.007(5) 0.006(5) 0.001(4) C40 0.256(15) 0.082(7) 0.077(6) -0.028(5) 0.077(8) -0.060(8) C10 0.216(12) 0.095(6) 0.033(4) 0.023(4) 0.051(5) 0.080(7) C18 0.240(14) 0.076(6) 0.026(4) -0.010(4) 0.012(6) 0.034(8) _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 2.032(5) . ? Rh1 N1 2.038(4) . ? Rh1 N6 2.040(5) . ? Rh1 N3 2.052(4) . ? Rh1 N9 2.251(5) . ? Rh1 Rh2 2.5714(10) . ? Rh2 N4 2.025(4) . ? Rh2 N8 2.033(4) . ? Rh2 N7 2.043(5) . ? Rh2 N2 2.046(4) . ? Rh2 N10 2.195(5) . ? N9 C30 1.150(7) . ? N1 C20 1.322(7) . ? N1 C17 1.440(6) . ? N2 C20 1.326(6) . ? N2 C21 1.432(6) . ? N3 C7 1.319(6) . ? N3 C4 1.431(7) . ? N4 C7 1.329(7) . ? N4 C8 1.442(6) . ? F10 C24 1.371(6) . ? C5 C6 1.382(9) . ? C5 C4 1.391(8) . ? C21 C22 1.395(7) . ? C21 C26 1.413(7) . ? C28 C27 1.461(9) . ? C24 C25 1.375(8) . ? C24 C23 1.381(8) . ? C13 C12 1.378(8) . ? C13 C8 1.381(7) . ? C27 N10 1.140(7) . ? C4 C3 1.377(8) . ? C26 C25 1.383(8) . ? C22 C23 1.402(8) . ? C8 C9 1.374(8) . ? C30 C29 1.466(9) . ? F6 B2 1.363(8) . ? F5 B2 1.383(8) . ? F7 B2 1.382(9) . ? F8 B2 1.363(9) . ? N5 C31 1.127(7) . ? N6 C33 1.151(7) . ? N8 C37 1.135(7) . ? N7 C35 1.130(7) . ? C37 C38 1.463(8) . ? C33 C34 1.466(8) . ? C17 C16 1.366(8) . ? C17 C19 1.373(8) . ? C16 C15 1.406(10) . ? C12 C11 1.330(10) . ? C3 C2 1.426(9) . ? C35 C36 1.473(8) . ? C2 C1 1.354(10) . ? C1 C6 1.352(10) . ? C1 F12 1.388(7) . ? F11 C11 1.383(7) . ? C31 C32 1.481(9) . ? C9 C10 1.402(9) . ? C11 C10 1.351(11) . ? C15 C14 1.353(13) . ? O1 C39 1.423(9) . ? O1 C41 1.427(8) . ? F1 B1 1.372(10) . ? F3 B1 1.336(11) . ? F9 C14 1.364(8) . ? F2 B1 1.317(11) . ? F4 B1 1.416(11) . ? C41 C42 1.503(10) . ? C14 C18 1.309(14) . ? C19 C18 1.402(11) . ? C39 C40 1.542(11) . ? 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 N1 87.57(18) . . ? N5 Rh1 N6 91.37(19) . . ? N1 Rh1 N6 176.88(18) . . ? N5 Rh1 N3 177.00(18) . . ? N1 Rh1 N3 89.42(17) . . ? N6 Rh1 N3 91.63(18) . . ? N5 Rh1 N9 87.66(17) . . ? N1 Rh1 N9 94.86(16) . . ? N6 Rh1 N9 88.03(17) . . ? N3 Rh1 N9 92.45(16) . . ? N5 Rh1 Rh2 94.31(13) . . ? N1 Rh1 Rh2 84.64(12) . . ? N6 Rh1 Rh2 92.51(13) . . ? N3 Rh1 Rh2 85.56(12) . . ? N9 Rh1 Rh2 177.95(12) . . ? N4 Rh2 N8 86.98(17) . . ? N4 Rh2 N7 177.65(17) . . ? N8 Rh2 N7 91.31(18) . . ? N4 Rh2 N2 89.51(17) . . ? N8 Rh2 N2 176.36(17) . . ? N7 Rh2 N2 92.22(17) . . ? N4 Rh2 N10 93.00(16) . . ? N8 Rh2 N10 84.36(16) . . ? N7 Rh2 N10 88.44(17) . . ? N2 Rh2 N10 94.85(16) . . ? N4 Rh2 Rh1 85.18(12) . . ? N8 Rh2 Rh1 94.53(12) . . ? N7 Rh2 Rh1 93.34(12) . . ? N2 Rh2 Rh1 86.15(12) . . ? N10 Rh2 Rh1 177.93(12) . . ? C30 N9 Rh1 166.5(4) . . ? C20 N1 C17 117.4(4) . . ? C20 N1 Rh1 120.9(3) . . ? C17 N1 Rh1 120.6(3) . . ? C20 N2 C21 118.3(4) . . ? C20 N2 Rh2 118.7(3) . . ? C21 N2 Rh2 121.7(3) . . ? C7 N3 C4 118.5(4) . . ? C7 N3 Rh1 119.3(4) . . ? C4 N3 Rh1 121.5(3) . . ? N1 C20 N2 123.4(5) . . ? C7 N4 C8 118.3(4) . . ? C7 N4 Rh2 120.4(3) . . ? C8 N4 Rh2 119.2(3) . . ? N3 C7 N4 123.3(5) . . ? C6 C5 C4 121.5(7) . . ? C22 C21 C26 118.0(5) . . ? C22 C21 N2 122.2(5) . . ? C26 C21 N2 119.8(5) . . ? F10 C24 C25 119.5(5) . . ? F10 C24 C23 118.6(5) . . ? C25 C24 C23 121.9(5) . . ? C12 C13 C8 120.9(6) . . ? N10 C27 C28 178.8(7) . . ? C3 C4 C5 118.5(6) . . ? C3 C4 N3 120.9(5) . . ? C5 C4 N3 120.6(5) . . ? C25 C26 C21 121.0(5) . . ? C21 C22 C23 121.0(5) . . ? C24 C25 C26 119.3(5) . . ? C9 C8 C13 118.6(5) . . ? C9 C8 N4 121.0(5) . . ? C13 C8 N4 120.3(5) . . ? N9 C30 C29 177.9(6) . . ? F8 B2 F6 109.5(6) . . ? F8 B2 F7 109.3(7) . . ? F6 B2 F7 111.3(6) . . ? F8 B2 F5 108.4(7) . . ? F6 B2 F5 109.8(6) . . ? F7 B2 F5 108.6(6) . . ? C31 N5 Rh1 177.0(5) . . ? C33 N6 Rh1 176.3(5) . . ? C37 N8 Rh2 170.9(4) . . ? C35 N7 Rh2 175.6(5) . . ? N8 C37 C38 179.3(7) . . ? N6 C33 C34 178.1(6) . . ? C16 C17 C19 118.7(6) . . ? C16 C17 N1 120.7(5) . . ? C19 C17 N1 120.6(6) . . ? C17 C16 C15 120.5(7) . . ? C11 C12 C13 119.3(6) . . ? C4 C3 C2 120.2(6) . . ? C24 C23 C22 118.8(5) . . ? N7 C35 C36 178.2(6) . . ? C1 C2 C3 117.9(7) . . ? C6 C1 C2 123.5(6) . . ? C6 C1 F12 119.5(7) . . ? C2 C1 F12 116.9(7) . . ? C1 C6 C5 118.4(6) . . ? C27 N10 Rh2 172.8(4) . . ? N5 C31 C32 179.6(9) . . ? C8 C9 C10 119.7(6) . . ? C12 C11 C10 122.4(6) . . ? C12 C11 F11 118.9(7) . . ? C10 C11 F11 118.6(7) . . ? C14 C15 C16 118.9(8) . . ? C39 O1 C41 111.8(6) . . ? O1 C41 C42 109.5(6) . . ? C18 C14 C15 121.5(7) . . ? C18 C14 F9 120.4(10) . . ? C15 C14 F9 118.1(10) . . ? C17 C19 C18 119.4(8) . . ? O1 C39 C40 108.1(7) . . ? F2 B1 F3 113.6(8) . . ? F2 B1 F1 109.4(8) . . ? F3 B1 F1 117.0(8) . . ? F2 B1 F4 102.1(8) . . ? F3 B1 F4 106.2(9) . . ? F1 B1 F4 107.1(8) . . ? C11 C10 C9 119.0(7) . . ? C14 C18 C19 121.0(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.915 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 932776' ####################################################################### # # 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_d:\xray\yong039\work_1\work\1 #TrackingRef 'compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 B2 F8 N12 Rh2' _chemical_formula_weight 1074.33 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.135(3) _cell_length_b 21.331(4) _cell_length_c 31.170(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9399(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9057 _exptl_absorpt_correction_T_max 0.9404 _exptl_absorpt_process_details 'SADABS, v 2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 71887 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 23.02 _reflns_number_total 6557 _reflns_number_gt 5210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+50.7082P] 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 6557 _refine_ls_number_parameters 587 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _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 Rh2 Rh 0.10570(4) 0.13980(3) 0.649695(19) 0.0353(2) Uani 1 1 d . . . Rh1 Rh -0.04025(4) 0.07271(3) 0.645974(19) 0.0357(2) Uani 1 1 d . . . N4 N 0.0419(4) 0.0126(3) 0.61230(19) 0.0301(14) Uani 1 1 d . . . N11 N -0.1745(5) 0.0191(3) 0.6394(2) 0.0387(16) Uani 1 1 d . . . N2 N -0.0345(4) 0.1797(3) 0.5853(2) 0.0343(15) Uani 1 1 d . . . N12 N 0.2289(5) 0.2030(3) 0.65061(19) 0.0382(15) Uani 1 1 d . . . N3 N 0.0345(4) 0.1971(3) 0.6096(2) 0.0336(15) Uani 1 1 d . . . N5 N 0.1123(4) 0.0335(3) 0.58932(19) 0.0311(14) Uani 1 1 d . . . N1 N -0.0635(4) 0.1220(3) 0.5915(2) 0.0339(15) Uani 1 1 d . . . N6 N 0.1454(4) 0.0884(3) 0.59870(19) 0.0293(14) Uani 1 1 d . . . C18 C 0.0446(6) -0.0769(3) 0.5621(2) 0.0379(19) Uani 1 1 d . . . H18 H 0.0830 -0.0535 0.5429 0.046 Uiso 1 1 calc R . . C19 C 0.0166(5) -0.0504(3) 0.6006(2) 0.0314(17) Uani 1 1 d . . . C22 C 0.2112(5) 0.1101(3) 0.5674(2) 0.0296(17) Uani 1 1 d . . . C21 C -0.0671(6) -0.1459(3) 0.6170(3) 0.043(2) Uani 1 1 d . . . H21 H -0.1058 -0.1694 0.6361 0.051 Uiso 1 1 calc R . . C8 C 0.0641(5) 0.2611(3) 0.6035(2) 0.0329(18) Uani 1 1 d . . . C17 C 0.0169(6) -0.1377(4) 0.5512(3) 0.044(2) Uani 1 1 d . . . H17 H 0.0376 -0.1555 0.5249 0.053 Uiso 1 1 calc R . . C9 C 0.0278(6) 0.3070(4) 0.6305(3) 0.042(2) Uani 1 1 d . . . H9 H -0.0206 0.2970 0.6505 0.051 Uiso 1 1 calc R . . C20 C -0.0383(5) -0.0859(3) 0.6286(3) 0.0355(18) Uani 1 1 d . . . H20 H -0.0562 -0.0691 0.6556 0.043 Uiso 1 1 calc R . . C16 C -0.0403(5) -0.1720(4) 0.5783(3) 0.0389(19) Uani 1 1 d . . . C24 C 0.3675(6) 0.1397(4) 0.5469(3) 0.050(2) Uani 1 1 d . . . H24 H 0.4320 0.1462 0.5541 0.060 Uiso 1 1 calc R . . C5 C -0.1464(5) 0.1065(3) 0.5669(3) 0.0370(19) Uani 1 1 d . . . C23 C 0.3062(5) 0.1187(3) 0.5783(3) 0.0357(18) Uani 1 1 d . . . H23 H 0.3280 0.1104 0.6065 0.043 Uiso 1 1 calc R . . C6 C -0.1454(6) 0.0525(3) 0.5426(2) 0.0347(18) Uani 1 1 d . . . H6 H -0.0882 0.0298 0.5390 0.042 Uiso 1 1 calc R . . C7 C -0.2279(6) 0.0313(4) 0.5237(3) 0.041(2) Uani 1 1 d . . . H7 H -0.2266 -0.0060 0.5070 0.049 Uiso 1 1 calc R . . C10 C 0.0629(7) 0.3672(4) 0.6279(3) 0.052(2) Uani 1 1 d . . . H10 H 0.0371 0.3986 0.6461 0.062 Uiso 1 1 calc R . . N7 N -0.1221(6) 0.1348(3) 0.6770(3) 0.056(2) Uani 1 1 d . . . C39 C 0.2828(6) 0.2422(4) 0.6501(2) 0.0386(19) Uani 1 1 d . . . N10 N 0.1763(5) 0.0812(3) 0.6880(2) 0.0493(18) Uani 1 1 d . . . N8 N -0.0164(6) 0.0263(3) 0.7008(2) 0.054(2) Uani 1 1 d . . . N9 N 0.0614(5) 0.1904(3) 0.7008(2) 0.0448(17) Uani 1 1 d . . . C2 C -0.3103(6) 0.0627(4) 0.5284(3) 0.050(2) Uani 1 1 d . . . C37 C -0.2452(7) -0.0044(4) 0.6340(3) 0.045(2) Uani 1 1 d . . . C13 C 0.1319(5) 0.2764(3) 0.5737(2) 0.0359(18) Uani 1 1 d . . . H13 H 0.1554 0.2453 0.5547 0.043 Uiso 1 1 calc R . . C25 C 0.3385(6) 0.1515(3) 0.5055(3) 0.044(2) Uani 1 1 d . . . C26 C 0.2437(6) 0.1421(3) 0.4953(3) 0.043(2) Uani 1 1 d . . . H26 H 0.2218 0.1501 0.4670 0.051 Uiso 1 1 calc R . . C33 C 0.0392(7) 0.2220(4) 0.7283(3) 0.053(2) Uani 1 1 d . . . C40 C 0.3527(7) 0.2917(5) 0.6481(3) 0.061(3) Uani 1 1 d . . . H40A H 0.4162 0.2734 0.6499 0.092 Uiso 1 1 calc R . . H40B H 0.3432 0.3207 0.6721 0.092 Uiso 1 1 calc R . . H40C H 0.3461 0.3145 0.6210 0.092 Uiso 1 1 calc R . . C11 C 0.1345(6) 0.3831(4) 0.5997(3) 0.048(2) Uani 1 1 d . . . C12 C 0.1660(6) 0.3373(4) 0.5715(3) 0.045(2) Uani 1 1 d . . . H12 H 0.2117 0.3478 0.5504 0.054 Uiso 1 1 calc R . . C29 C -0.1760(8) 0.1629(5) 0.6940(4) 0.085(4) Uani 1 1 d . . . C27 C 0.1811(6) 0.1209(3) 0.5264(2) 0.0358(18) Uani 1 1 d . . . H27 H 0.1167 0.1139 0.5191 0.043 Uiso 1 1 calc R . . C1 C -0.4013(6) 0.0371(4) 0.5105(4) 0.063(3) Uani 1 1 d . . . H1A H -0.3910 -0.0058 0.5002 0.095 Uiso 1 1 calc R . . H1B H -0.4223 0.0635 0.4866 0.095 Uiso 1 1 calc R . . H1C H -0.4498 0.0369 0.5329 0.095 Uiso 1 1 calc R . . C28 C 0.4068(8) 0.1755(5) 0.4718(3) 0.070(3) Uani 1 1 d . . . H28A H 0.4716 0.1650 0.4802 0.105 Uiso 1 1 calc R . . H28B H 0.4005 0.2211 0.4693 0.105 Uiso 1 1 calc R . . H28C H 0.3923 0.1559 0.4442 0.105 Uiso 1 1 calc R . . C4 C -0.2278(6) 0.1399(4) 0.5705(4) 0.067(3) Uani 1 1 d . . . H4 H -0.2285 0.1781 0.5860 0.080 Uiso 1 1 calc R . . C3 C -0.3091(7) 0.1182(4) 0.5515(4) 0.079(4) Uani 1 1 d . . . H3 H -0.3659 0.1417 0.5544 0.094 Uiso 1 1 calc R . . C38 C -0.3341(7) -0.0361(5) 0.6262(4) 0.074(3) Uani 1 1 d . . . H38A H -0.3391 -0.0468 0.5958 0.110 Uiso 1 1 calc R . . H38B H -0.3866 -0.0085 0.6343 0.110 Uiso 1 1 calc R . . H38C H -0.3369 -0.0745 0.6434 0.110 Uiso 1 1 calc R . . C14 C 0.1773(8) 0.4483(4) 0.5996(4) 0.073(3) Uani 1 1 d . . . H14A H 0.2187 0.4531 0.6246 0.109 Uiso 1 1 calc R . . H14B H 0.1267 0.4796 0.6008 0.109 Uiso 1 1 calc R . . H14C H 0.2143 0.4542 0.5733 0.109 Uiso 1 1 calc R . . C31 C -0.0057(9) -0.0009(5) 0.7313(3) 0.071(3) Uani 1 1 d . . . F1 F 0.0827(6) 0.0962(4) 0.8056(3) 0.125(3) Uani 1 1 d . . . C15 C -0.0718(7) -0.2375(4) 0.5661(3) 0.056(2) Uani 1 1 d . . . H15A H -0.1399 -0.2418 0.5713 0.084 Uiso 1 1 calc R . . H15B H -0.0375 -0.2683 0.5836 0.084 Uiso 1 1 calc R . . H15C H -0.0584 -0.2449 0.5357 0.084 Uiso 1 1 calc R . . F4 F -0.0634(8) 0.1212(5) 0.7965(4) 0.151(4) Uani 1 1 d . . . C35 C 0.2203(7) 0.0509(5) 0.7099(3) 0.066(3) Uani 1 1 d . . . F8 F -0.3255(9) -0.1617(6) 0.7021(4) 0.200(6) Uani 1 1 d . . . F5 F -0.1987(8) -0.1105(7) 0.7159(4) 0.199(6) Uani 1 1 d . . . C34 C 0.0119(10) 0.2639(6) 0.7639(4) 0.092(4) Uani 1 1 d . . . H34A H 0.0461 0.3037 0.7614 0.138 Uiso 1 1 calc R . . H34B H 0.0277 0.2440 0.7913 0.138 Uiso 1 1 calc R . . H34C H -0.0564 0.2718 0.7627 0.138 Uiso 1 1 calc R . . B1 B 0.0068(17) 0.1125(7) 0.8279(6) 0.104(6) Uani 1 1 d . . . B2 B -0.2709(16) -0.1410(10) 0.7293(7) 0.112(6) Uani 1 1 d U . . C32 C -0.0045(14) -0.0402(7) 0.7708(4) 0.134(7) Uani 1 1 d . . . H32A H -0.0370 -0.0179 0.7941 0.201 Uiso 1 1 calc R . . H32B H 0.0611 -0.0485 0.7792 0.201 Uiso 1 1 calc R . . H32C H -0.0369 -0.0799 0.7652 0.201 Uiso 1 1 calc R . . C30 C -0.2520(12) 0.1937(8) 0.7175(9) 0.228(14) Uani 1 1 d . . . H30A H -0.2375 0.1933 0.7482 0.342 Uiso 1 1 calc R . . H30B H -0.3116 0.1713 0.7124 0.342 Uiso 1 1 calc R . . H30C H -0.2581 0.2371 0.7076 0.342 Uiso 1 1 calc R . . C36 C 0.2716(15) 0.0242(10) 0.7452(8) 0.248(15) Uani 1 1 d . . . H36A H 0.3088 0.0569 0.7593 0.372 Uiso 1 1 calc R . . H36B H 0.3140 -0.0087 0.7346 0.372 Uiso 1 1 calc R . . H36C H 0.2269 0.0060 0.7658 0.372 Uiso 1 1 calc R . . F3 F -0.0222(8) 0.0644(4) 0.8525(3) 0.178(6) Uani 1 1 d . . . F2 F 0.0117(8) 0.1658(4) 0.8489(3) 0.142(4) Uani 1 1 d . . . F7 F -0.2375(11) -0.1853(6) 0.7578(3) 0.209(6) Uani 1 1 d . . . F6 F -0.3148(10) -0.1085(7) 0.7649(5) 0.230(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh2 0.0449(4) 0.0283(4) 0.0327(4) -0.0014(3) 0.0033(3) -0.0079(3) Rh1 0.0435(4) 0.0266(4) 0.0371(4) 0.0000(3) 0.0088(3) -0.0075(3) N4 0.032(3) 0.024(3) 0.035(3) 0.004(3) 0.002(3) -0.008(3) N11 0.049(4) 0.027(3) 0.040(4) -0.002(3) 0.016(3) -0.004(3) N2 0.034(4) 0.026(4) 0.043(4) -0.003(3) 0.006(3) -0.003(3) N12 0.047(4) 0.035(4) 0.033(4) -0.006(3) -0.003(3) 0.001(3) N3 0.039(4) 0.023(3) 0.039(4) -0.001(3) 0.005(3) -0.001(3) N5 0.033(3) 0.021(3) 0.039(4) 0.005(3) -0.005(3) 0.000(3) N1 0.031(3) 0.022(3) 0.050(4) 0.000(3) 0.004(3) -0.007(3) N6 0.030(3) 0.024(3) 0.034(3) 0.002(3) 0.000(3) 0.002(3) C18 0.052(5) 0.028(4) 0.034(4) -0.002(3) -0.001(4) -0.010(4) C19 0.032(4) 0.022(4) 0.040(4) 0.002(3) -0.006(3) -0.001(3) C22 0.040(4) 0.017(4) 0.032(4) -0.001(3) 0.004(3) -0.001(3) C21 0.043(5) 0.024(4) 0.061(6) 0.013(4) -0.004(4) -0.004(4) C8 0.039(4) 0.019(4) 0.041(5) 0.000(3) -0.005(4) 0.002(3) C17 0.053(5) 0.035(5) 0.045(5) -0.007(4) -0.012(4) 0.002(4) C9 0.050(5) 0.034(5) 0.043(5) 0.000(4) 0.007(4) 0.000(4) C20 0.045(5) 0.017(4) 0.044(5) 0.002(3) 0.006(4) 0.001(3) C16 0.033(4) 0.030(4) 0.054(5) 0.005(4) -0.012(4) 0.000(4) C24 0.043(5) 0.035(5) 0.071(7) -0.012(4) 0.014(5) -0.013(4) C5 0.031(4) 0.022(4) 0.058(5) 0.003(4) 0.002(4) -0.005(3) C23 0.038(5) 0.025(4) 0.044(5) -0.004(3) 0.000(4) -0.004(3) C6 0.037(4) 0.032(4) 0.036(4) 0.001(3) 0.007(4) 0.005(4) C7 0.046(5) 0.025(4) 0.050(5) -0.002(4) -0.002(4) 0.000(4) C10 0.073(6) 0.032(5) 0.051(5) -0.014(4) -0.001(5) 0.000(4) N7 0.052(5) 0.045(4) 0.070(5) -0.015(4) 0.025(4) -0.013(4) C39 0.039(5) 0.040(5) 0.037(5) -0.001(4) -0.002(4) -0.002(4) N10 0.061(5) 0.043(4) 0.044(4) 0.005(4) -0.008(4) -0.008(4) N8 0.077(6) 0.045(4) 0.041(4) 0.001(4) 0.008(4) -0.015(4) N9 0.051(4) 0.040(4) 0.044(4) 0.000(3) 0.007(3) -0.008(3) C2 0.037(5) 0.032(5) 0.081(7) -0.004(4) -0.008(5) 0.000(4) C37 0.056(6) 0.029(4) 0.049(5) -0.002(4) 0.010(4) -0.006(4) C13 0.039(4) 0.027(4) 0.043(5) 0.000(3) 0.002(4) 0.000(3) C25 0.054(6) 0.022(4) 0.057(6) 0.000(4) 0.022(5) -0.001(4) C26 0.059(6) 0.030(4) 0.039(5) 0.002(4) 0.010(4) 0.010(4) C33 0.064(6) 0.048(6) 0.045(5) -0.004(5) 0.011(5) 0.007(5) C40 0.052(6) 0.067(6) 0.065(6) 0.006(5) -0.003(5) -0.023(5) C11 0.055(5) 0.026(4) 0.065(6) 0.000(4) 0.000(5) -0.013(4) C12 0.040(5) 0.030(4) 0.065(6) 0.006(4) 0.011(4) -0.002(4) C29 0.053(6) 0.073(7) 0.128(11) -0.044(7) 0.043(7) -0.006(6) C27 0.037(4) 0.027(4) 0.044(5) -0.001(3) 0.005(4) 0.001(3) C1 0.040(5) 0.036(5) 0.114(9) -0.013(5) -0.017(5) -0.001(4) C28 0.085(8) 0.050(6) 0.076(7) -0.001(5) 0.042(6) -0.017(5) C4 0.044(6) 0.028(5) 0.128(9) -0.029(5) -0.013(6) 0.005(4) C3 0.039(5) 0.030(5) 0.167(12) -0.035(6) -0.025(6) 0.012(4) C38 0.063(7) 0.066(7) 0.092(8) 0.001(6) 0.015(6) -0.036(6) C14 0.078(7) 0.032(5) 0.109(9) -0.006(5) 0.004(6) -0.030(5) C31 0.130(10) 0.040(5) 0.042(6) 0.005(5) -0.005(6) -0.006(6) F1 0.129(7) 0.110(6) 0.137(7) -0.021(5) 0.069(6) -0.030(5) C15 0.059(6) 0.026(4) 0.081(7) -0.003(4) -0.014(5) -0.008(4) F4 0.141(8) 0.139(8) 0.175(10) -0.042(7) -0.004(8) -0.022(7) C35 0.053(6) 0.073(7) 0.072(7) 0.048(6) -0.031(5) -0.015(5) F8 0.200(12) 0.170(10) 0.229(13) 0.061(10) -0.107(11) -0.049(9) F5 0.177(10) 0.271(14) 0.148(9) -0.027(9) 0.062(8) -0.113(10) C34 0.118(10) 0.086(8) 0.071(8) -0.029(6) 0.016(7) 0.015(8) B1 0.168(19) 0.057(9) 0.086(11) -0.005(8) 0.040(13) -0.025(11) B2 0.112(6) 0.112(6) 0.112(6) -0.0001(10) 0.0001(10) 0.0003(10) C32 0.25(2) 0.088(10) 0.067(8) 0.028(7) -0.010(10) -0.050(12) C30 0.113(13) 0.116(13) 0.46(4) -0.132(19) 0.147(19) -0.015(11) C36 0.20(2) 0.22(2) 0.32(3) 0.19(2) -0.17(2) -0.080(18) F3 0.239(12) 0.085(6) 0.211(11) 0.040(6) 0.166(10) 0.034(7) F2 0.243(11) 0.071(5) 0.111(6) -0.029(4) -0.033(7) 0.028(6) F7 0.310(16) 0.209(12) 0.109(7) 0.005(8) 0.002(9) 0.087(13) F6 0.201(13) 0.233(14) 0.255(16) 0.053(13) 0.076(12) 0.030(12) _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 Rh2 N10 1.996(7) . ? Rh2 N6 2.010(6) . ? Rh2 N3 2.018(6) . ? Rh2 N9 2.025(7) . ? Rh2 N12 2.202(7) . ? Rh2 Rh1 2.5134(9) . ? Rh1 N8 2.003(8) . ? Rh1 N7 2.006(8) . ? Rh1 N4 2.024(6) . ? Rh1 N1 2.025(6) . ? Rh1 N11 2.225(7) . ? N4 N5 1.304(8) . ? N4 C19 1.437(9) . ? N11 C37 1.130(10) . ? N2 N3 1.291(8) . ? N2 N1 1.312(8) . ? N12 C39 1.132(10) . ? N3 C8 1.440(9) . ? N5 N6 1.295(8) . ? N1 C5 1.438(10) . ? N6 C22 1.426(9) . ? C18 C19 1.384(11) . ? C18 C17 1.397(11) . ? C19 C20 1.392(10) . ? C22 C27 1.367(10) . ? C22 C23 1.397(10) . ? C21 C16 1.381(12) . ? C21 C20 1.390(10) . ? C8 C13 1.372(10) . ? C8 C9 1.389(11) . ? C17 C16 1.380(11) . ? C9 C10 1.378(11) . ? C16 C15 1.516(11) . ? C24 C25 1.375(13) . ? C24 C23 1.381(11) . ? C5 C4 1.358(11) . ? C5 C6 1.378(10) . ? C6 C7 1.383(11) . ? C7 C2 1.353(11) . ? C10 C11 1.382(13) . ? N7 C29 1.106(11) . ? C39 C40 1.447(12) . ? N10 C35 1.127(10) . ? N8 C31 1.124(11) . ? N9 C33 1.133(10) . ? C2 C3 1.385(12) . ? C2 C1 1.505(12) . ? C37 C38 1.448(13) . ? C13 C12 1.388(11) . ? C25 C26 1.392(12) . ? C25 C28 1.516(11) . ? C26 C27 1.386(11) . ? C33 C34 1.477(13) . ? C11 C12 1.389(12) . ? C11 C14 1.516(11) . ? C29 C30 1.456(16) . ? C4 C3 1.373(13) . ? C31 C32 1.490(14) . ? F1 B1 1.32(2) . ? F4 B1 1.40(2) . ? C35 C36 1.436(17) . ? F8 B2 1.23(2) . ? F5 B2 1.28(2) . ? B1 F2 1.314(17) . ? B1 F3 1.345(16) . ? B2 F7 1.38(2) . ? B2 F6 1.45(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 N10 Rh2 N6 89.5(3) . . ? N10 Rh2 N3 178.3(3) . . ? N6 Rh2 N3 88.8(2) . . ? N10 Rh2 N9 91.0(3) . . ? N6 Rh2 N9 178.1(3) . . ? N3 Rh2 N9 90.6(3) . . ? N10 Rh2 N12 88.9(3) . . ? N6 Rh2 N12 97.1(2) . . ? N3 Rh2 N12 91.8(2) . . ? N9 Rh2 N12 84.7(2) . . ? N10 Rh2 Rh1 94.7(2) . . ? N6 Rh2 Rh1 83.23(17) . . ? N3 Rh2 Rh1 84.69(18) . . ? N9 Rh2 Rh1 94.93(19) . . ? N12 Rh2 Rh1 176.45(17) . . ? N8 Rh1 N7 90.7(3) . . ? N8 Rh1 N4 91.9(3) . . ? N7 Rh1 N4 177.4(3) . . ? N8 Rh1 N1 178.3(3) . . ? N7 Rh1 N1 88.2(3) . . ? N4 Rh1 N1 89.3(2) . . ? N8 Rh1 N11 88.2(3) . . ? N7 Rh1 N11 83.8(3) . . ? N4 Rh1 N11 96.7(2) . . ? N1 Rh1 N11 92.9(2) . . ? N8 Rh1 Rh2 95.9(2) . . ? N7 Rh1 Rh2 94.3(2) . . ? N4 Rh1 Rh2 85.04(16) . . ? N1 Rh1 Rh2 82.91(17) . . ? N11 Rh1 Rh2 175.47(17) . . ? N5 N4 C19 111.7(6) . . ? N5 N4 Rh1 120.4(4) . . ? C19 N4 Rh1 125.5(5) . . ? C37 N11 Rh1 174.6(7) . . ? N3 N2 N1 114.9(6) . . ? C39 N12 Rh2 170.0(6) . . ? N2 N3 C8 114.5(6) . . ? N2 N3 Rh2 124.5(5) . . ? C8 N3 Rh2 120.8(5) . . ? N6 N5 N4 117.4(6) . . ? N2 N1 C5 113.0(6) . . ? N2 N1 Rh1 124.0(5) . . ? C5 N1 Rh1 117.4(4) . . ? N5 N6 C22 111.9(6) . . ? N5 N6 Rh2 124.8(5) . . ? C22 N6 Rh2 123.2(4) . . ? C19 C18 C17 120.7(7) . . ? C18 C19 C20 118.7(7) . . ? C18 C19 N4 122.0(7) . . ? C20 C19 N4 119.3(7) . . ? C27 C22 C23 120.2(7) . . ? C27 C22 N6 119.5(7) . . ? C23 C22 N6 120.2(7) . . ? C16 C21 C20 121.1(8) . . ? C13 C8 C9 120.0(7) . . ? C13 C8 N3 121.1(6) . . ? C9 C8 N3 118.7(7) . . ? C16 C17 C18 120.5(8) . . ? C10 C9 C8 119.3(8) . . ? C21 C20 C19 120.1(7) . . ? C17 C16 C21 118.8(7) . . ? C17 C16 C15 120.5(8) . . ? C21 C16 C15 120.7(8) . . ? C25 C24 C23 122.4(8) . . ? C4 C5 C6 119.4(8) . . ? C4 C5 N1 121.7(7) . . ? C6 C5 N1 118.4(7) . . ? C24 C23 C22 118.3(8) . . ? C5 C6 C7 120.0(7) . . ? C2 C7 C6 121.1(7) . . ? C9 C10 C11 121.9(8) . . ? C29 N7 Rh1 170.7(8) . . ? N12 C39 C40 178.1(9) . . ? C35 N10 Rh2 175.7(7) . . ? C31 N8 Rh1 177.6(9) . . ? C33 N9 Rh2 175.6(7) . . ? C7 C2 C3 118.0(8) . . ? C7 C2 C1 121.0(8) . . ? C3 C2 C1 120.9(8) . . ? N11 C37 C38 178.1(10) . . ? C8 C13 C12 119.8(7) . . ? C24 C25 C26 118.3(8) . . ? C24 C25 C28 121.4(9) . . ? C26 C25 C28 120.2(9) . . ? C27 C26 C25 120.1(8) . . ? N9 C33 C34 178.9(11) . . ? C10 C11 C12 117.7(7) . . ? C10 C11 C14 121.3(8) . . ? C12 C11 C14 121.0(8) . . ? C13 C12 C11 121.1(8) . . ? N7 C29 C30 173.9(14) . . ? C22 C27 C26 120.6(8) . . ? C5 C4 C3 119.9(8) . . ? C4 C3 C2 121.4(8) . . ? N8 C31 C32 172.5(14) . . ? N10 C35 C36 166.0(17) . . ? F2 B1 F1 116.4(17) . . ? F2 B1 F3 113.0(14) . . ? F1 B1 F3 110.2(15) . . ? F2 B1 F4 105.7(16) . . ? F1 B1 F4 104.1(13) . . ? F3 B1 F4 106.4(17) . . ? F8 B2 F5 117(2) . . ? F8 B2 F7 114.4(19) . . ? F5 B2 F7 106.6(19) . . ? F8 B2 F6 116(2) . . ? F5 B2 F6 110.4(18) . . ? F7 B2 F6 88.9(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.944 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.173 _database_code_depnum_ccdc_archive 'CCDC 932777' ####################################################################### # # 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_d:\xray\yong003\yong003 #TrackingRef 'compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 B2 F8 N10 Rh2' _chemical_formula_weight 1072.34 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.338(3) _cell_length_b 21.619(4) _cell_length_c 31.136(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9651(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8336 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 105468 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.62 _reflns_number_total 11808 _reflns_number_gt 9811 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+13.1764P] 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 11808 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.538564(10) 0.433188(6) 0.149138(5) 0.01506(4) Uani 1 1 d . . . F1 F 0.82359(15) 0.10878(9) 0.22580(8) 0.0836(7) Uani 1 1 d . . . N1 N 0.45519(11) 0.49293(7) 0.11273(5) 0.0174(3) Uani 1 1 d . . . C1 C 0.38367(13) 0.46789(9) 0.09272(6) 0.0184(4) Uani 1 1 d . . . H1 H 0.3548 0.4913 0.0706 0.022 Uiso 1 1 calc R . . B1 B 0.7528(3) 0.14344(14) 0.24383(14) 0.0563(9) Uani 1 1 d . . . Rh2 Rh 0.393354(10) 0.359333(6) 0.152737(5) 0.01525(4) Uani 1 1 d . . . F2 F 0.78819(18) 0.19530(8) 0.26365(7) 0.0859(8) Uani 1 1 d . . . N2 N 0.34937(11) 0.41284(7) 0.10111(5) 0.0180(3) Uani 1 1 d . . . C2 C 0.53601(14) 0.32606(9) 0.08812(6) 0.0200(4) Uani 1 1 d . . . H2 H 0.5649 0.3005 0.0672 0.024 Uiso 1 1 calc R . . B2 B 0.4805(3) 0.39207(16) 0.32825(12) 0.0488(8) Uani 1 1 d . . . F3 F 0.70600(16) 0.10866(9) 0.27481(7) 0.0749(6) Uani 1 1 d . . . N3 N 0.56799(11) 0.38285(7) 0.09330(5) 0.0193(3) Uani 1 1 d . . . C3 C 0.48187(13) 0.55430(9) 0.10109(6) 0.0197(4) Uani 1 1 d . . . F4 F 0.68967(15) 0.16019(9) 0.21224(7) 0.0719(6) Uani 1 1 d . . . N4 N 0.46679(11) 0.30324(7) 0.11024(5) 0.0183(3) Uani 1 1 d . . . C4 C 0.52546(14) 0.59221(9) 0.13127(7) 0.0224(4) Uani 1 1 d . . . H4 H 0.5333 0.5779 0.1599 0.027 Uiso 1 1 calc R . . F5 F 0.55494(18) 0.38619(12) 0.30127(9) 0.0962(8) Uani 1 1 d . . . N5 N 0.66905(14) 0.34408(9) 0.19677(8) 0.0388(5) Uani 1 1 d . . . C5 C 0.55762(15) 0.65071(9) 0.11999(8) 0.0269(4) Uani 1 1 d . . . H5 H 0.5888 0.6751 0.1409 0.032 Uiso 1 1 calc R . . F6 F 0.46664(17) 0.33687(9) 0.34956(7) 0.0757(6) Uani 1 1 d . . . N6 N 0.46689(13) 0.28154(9) 0.22871(6) 0.0285(4) Uani 1 1 d . . . C6 C 0.54537(16) 0.67436(10) 0.07888(8) 0.0293(5) Uani 1 1 d . . . F7 F 0.49664(17) 0.43926(10) 0.35679(7) 0.0797(7) Uani 1 1 d . . . N7 N 0.49164(13) 0.50489(8) 0.23209(6) 0.0247(4) Uani 1 1 d . . . C7 C 0.49932(16) 0.63733(10) 0.04946(8) 0.0299(5) Uani 1 1 d . . . H7 H 0.4881 0.6529 0.0214 0.036 Uiso 1 1 calc R . . F8 F 0.40351(16) 0.40695(11) 0.30445(8) 0.0888(8) Uani 1 1 d . . . N8 N 0.27837(13) 0.44254(9) 0.21278(6) 0.0294(4) Uani 1 1 d . . . C8 C 0.46892(15) 0.57795(10) 0.05973(7) 0.0252(4) Uani 1 1 d . . . H8 H 0.4392 0.5533 0.0385 0.030 Uiso 1 1 calc R . . C39 C 0.65871(14) 0.48750(9) 0.14140(6) 0.0200(4) Uani 1 1 d . . . C9 C 0.5803(2) 0.73808(11) 0.06716(9) 0.0428(6) Uani 1 1 d . . . H9A H 0.5757 0.7439 0.0360 0.064 Uiso 1 1 calc R . . H9B H 0.6455 0.7423 0.0761 0.064 Uiso 1 1 calc R . . H9C H 0.5424 0.7694 0.0818 0.064 Uiso 1 1 calc R . . C41 C 0.28076(14) 0.29876(9) 0.15014(6) 0.0203(4) Uani 1 1 d . . . C10 C 0.28055(14) 0.39124(9) 0.07151(6) 0.0191(4) Uani 1 1 d . . . C11 C 0.30668(17) 0.37659(10) 0.02984(7) 0.0283(5) Uani 1 1 d . . . H11 H 0.3700 0.3806 0.0213 0.034 Uiso 1 1 calc R . . C12 C 0.2407(2) 0.35609(11) 0.00051(8) 0.0390(6) Uani 1 1 d . . . H12 H 0.2593 0.3462 -0.0280 0.047 Uiso 1 1 calc R . . C13 C 0.1480(2) 0.34987(11) 0.01225(9) 0.0418(7) Uani 1 1 d . . . C14 C 0.12274(17) 0.36504(10) 0.05395(9) 0.0367(6) Uani 1 1 d . . . H14 H 0.0593 0.3614 0.0623 0.044 Uiso 1 1 calc R . . C15 C 0.18765(15) 0.38543(9) 0.08374(7) 0.0257(4) Uani 1 1 d . . . H15 H 0.1689 0.3953 0.1122 0.031 Uiso 1 1 calc R . . C16 C 0.0761(3) 0.32732(15) -0.01972(12) 0.0724(12) Uani 1 1 d . . . H16A H 0.0988 0.3347 -0.0490 0.109 Uiso 1 1 calc R . . H16B H 0.0175 0.3498 -0.0154 0.109 Uiso 1 1 calc R . . H16C H 0.0655 0.2829 -0.0155 0.109 Uiso 1 1 calc R . . C17 C 0.64956(14) 0.39972(9) 0.07002(7) 0.0215(4) Uani 1 1 d . . . C18 C 0.73286(16) 0.36835(10) 0.07635(9) 0.0373(6) Uani 1 1 d . . . H18 H 0.7338 0.3316 0.0931 0.045 Uiso 1 1 calc R . . C19 C 0.81465(17) 0.39052(11) 0.05826(10) 0.0441(7) Uani 1 1 d . . . H19 H 0.8714 0.3689 0.0629 0.053 Uiso 1 1 calc R . . C20 C 0.81485(16) 0.44399(10) 0.03337(8) 0.0315(5) Uani 1 1 d . . . C21 C 0.73102(15) 0.47395(10) 0.02638(7) 0.0254(4) Uani 1 1 d . . . H21 H 0.7296 0.5098 0.0088 0.031 Uiso 1 1 calc R . . C22 C 0.64896(14) 0.45251(9) 0.04461(6) 0.0220(4) Uani 1 1 d . . . H22 H 0.5921 0.4740 0.0397 0.026 Uiso 1 1 calc R . . C23 C 0.90506(18) 0.46960(12) 0.01608(10) 0.0458(7) Uani 1 1 d . . . H23A H 0.9292 0.4420 -0.0063 0.069 Uiso 1 1 calc R . . H23B H 0.9507 0.4727 0.0394 0.069 Uiso 1 1 calc R . . H23C H 0.8940 0.5107 0.0039 0.069 Uiso 1 1 calc R . . C24 C 0.44097(14) 0.23966(9) 0.10431(6) 0.0202(4) Uani 1 1 d . . . C25 C 0.47949(17) 0.19428(10) 0.13013(7) 0.0290(5) Uani 1 1 d . . . H25 H 0.5274 0.2047 0.1499 0.035 Uiso 1 1 calc R . . C26 C 0.44853(19) 0.13360(10) 0.12723(8) 0.0357(6) Uani 1 1 d . . . H26 H 0.4759 0.1029 0.1451 0.043 Uiso 1 1 calc R . . C27 C 0.37854(18) 0.11690(10) 0.09890(8) 0.0350(5) Uani 1 1 d . . . C28 C 0.34292(16) 0.16217(11) 0.07180(8) 0.0330(5) Uani 1 1 d . . . H28 H 0.2970 0.1513 0.0511 0.040 Uiso 1 1 calc R . . C29 C 0.37361(15) 0.22321(10) 0.07445(7) 0.0254(4) Uani 1 1 d . . . H29 H 0.3483 0.2536 0.0558 0.030 Uiso 1 1 calc R . . C30 C 0.3409(3) 0.05130(13) 0.09824(11) 0.0596(9) Uani 1 1 d . . . H30A H 0.3923 0.0220 0.1023 0.089 Uiso 1 1 calc R . . H30B H 0.3106 0.0433 0.0706 0.089 Uiso 1 1 calc R . . H30C H 0.2953 0.0461 0.1214 0.089 Uiso 1 1 calc R . . C31 C 0.61597(14) 0.37470(9) 0.17981(7) 0.0240(4) Uani 1 1 d . . . C32 C 0.7390(2) 0.30790(14) 0.21836(14) 0.0767(13) Uani 1 1 d . . . H32A H 0.8000 0.3277 0.2149 0.115 Uiso 1 1 calc R . . H32B H 0.7409 0.2663 0.2059 0.115 Uiso 1 1 calc R . . H32C H 0.7237 0.3050 0.2490 0.115 Uiso 1 1 calc R . . C33 C 0.44184(14) 0.31227(9) 0.20120(6) 0.0216(4) Uani 1 1 d . . . C34 C 0.4988(2) 0.24196(14) 0.26288(9) 0.0504(8) Uani 1 1 d . . . H34A H 0.4526 0.2093 0.2680 0.076 Uiso 1 1 calc R . . H34B H 0.5069 0.2664 0.2891 0.076 Uiso 1 1 calc R . . H34C H 0.5584 0.2232 0.2548 0.076 Uiso 1 1 calc R . . C35 C 0.50571(14) 0.47652(9) 0.20192(6) 0.0199(4) Uani 1 1 d . . . C36 C 0.4786(2) 0.54263(12) 0.26955(8) 0.0414(6) Uani 1 1 d . . . H36A H 0.5282 0.5738 0.2710 0.062 Uiso 1 1 calc R . . H36B H 0.4808 0.5166 0.2953 0.062 Uiso 1 1 calc R . . H36C H 0.4179 0.5633 0.2679 0.062 Uiso 1 1 calc R . . C37 C 0.32472(14) 0.41388(9) 0.19074(6) 0.0209(4) Uani 1 1 d . . . C38 C 0.2169(2) 0.47455(13) 0.24109(11) 0.0591(9) Uani 1 1 d . . . H38A H 0.1554 0.4548 0.2405 0.089 Uiso 1 1 calc R . . H38B H 0.2111 0.5177 0.2318 0.089 Uiso 1 1 calc R . . H38C H 0.2420 0.4732 0.2704 0.089 Uiso 1 1 calc R . . N9 N 0.72785(12) 0.51278(8) 0.13782(6) 0.0250(4) Uani 1 1 d . . . C40 C 0.81338(17) 0.54583(12) 0.13089(9) 0.0395(6) Uani 1 1 d . . . H40A H 0.8155 0.5608 0.1012 0.059 Uiso 1 1 calc R . . H40B H 0.8663 0.5182 0.1361 0.059 Uiso 1 1 calc R . . H40C H 0.8166 0.5811 0.1506 0.059 Uiso 1 1 calc R . . N10 N 0.22262(13) 0.26308(9) 0.14894(6) 0.0267(4) Uani 1 1 d . . . C42 C 0.15079(18) 0.21740(12) 0.14426(9) 0.0405(6) Uani 1 1 d . . . H42A H 0.0896 0.2376 0.1448 0.061 Uiso 1 1 calc R . . H42B H 0.1548 0.1876 0.1679 0.061 Uiso 1 1 calc R . . H42C H 0.1588 0.1957 0.1169 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01394(7) 0.01366(7) 0.01760(7) -0.00071(5) -0.00126(5) -0.00005(5) F1 0.0761(14) 0.0583(12) 0.1163(18) 0.0382(12) 0.0429(13) 0.0180(11) N1 0.0166(8) 0.0156(7) 0.0202(8) 0.0014(6) -0.0019(6) 0.0001(6) C1 0.0180(9) 0.0195(9) 0.0177(9) 0.0001(7) -0.0003(7) 0.0027(7) B1 0.059(2) 0.0232(14) 0.086(3) 0.0036(16) -0.014(2) 0.0001(14) Rh2 0.01413(7) 0.01567(7) 0.01594(7) -0.00044(5) 0.00155(5) -0.00058(5) F2 0.1208(19) 0.0393(10) 0.0975(16) 0.0122(10) -0.0590(15) -0.0153(11) N2 0.0161(8) 0.0190(8) 0.0190(8) 0.0001(6) -0.0026(6) -0.0006(6) C2 0.0187(9) 0.0181(9) 0.0234(9) -0.0033(7) 0.0039(8) 0.0003(7) B2 0.054(2) 0.0440(18) 0.0487(19) 0.0077(14) -0.0081(16) -0.0086(15) F3 0.0831(15) 0.0559(12) 0.0859(15) -0.0061(10) 0.0269(12) 0.0006(11) N3 0.0167(8) 0.0174(8) 0.0240(8) -0.0030(6) 0.0051(7) -0.0023(6) C3 0.0166(9) 0.0172(9) 0.0253(10) 0.0011(7) 0.0018(7) 0.0023(7) F4 0.0737(14) 0.0539(11) 0.0881(15) -0.0148(10) -0.0254(12) -0.0035(10) N4 0.0187(8) 0.0152(7) 0.0209(8) -0.0034(6) 0.0033(6) -0.0022(6) C4 0.0229(10) 0.0163(9) 0.0281(10) -0.0002(8) -0.0002(8) 0.0018(8) F5 0.0905(17) 0.0951(18) 0.1029(19) 0.0106(15) 0.0405(15) -0.0189(14) N5 0.0281(10) 0.0234(9) 0.0648(15) 0.0134(9) -0.0160(10) -0.0048(8) C5 0.0257(11) 0.0171(9) 0.0381(12) -0.0042(9) 0.0033(9) -0.0005(8) F6 0.1087(18) 0.0492(11) 0.0691(13) 0.0225(9) 0.0202(12) 0.0056(11) N6 0.0314(10) 0.0292(10) 0.0249(9) 0.0053(8) 0.0023(8) 0.0046(8) C6 0.0275(11) 0.0178(10) 0.0426(13) 0.0035(9) 0.0107(10) 0.0022(8) F7 0.0929(16) 0.0602(12) 0.0860(15) -0.0174(11) -0.0401(13) 0.0048(11) N7 0.0281(9) 0.0246(9) 0.0214(9) -0.0020(7) -0.0012(7) 0.0003(7) C7 0.0320(12) 0.0257(11) 0.0319(11) 0.0085(9) 0.0061(9) 0.0040(9) F8 0.0839(16) 0.0812(15) 0.1012(17) 0.0298(13) -0.0517(14) -0.0317(13) N8 0.0265(10) 0.0262(9) 0.0354(10) -0.0083(8) 0.0109(8) -0.0037(8) C8 0.0244(10) 0.0245(10) 0.0268(11) 0.0032(8) -0.0001(8) -0.0008(8) C39 0.0218(10) 0.0177(9) 0.0206(9) 0.0006(7) -0.0029(7) 0.0022(8) C9 0.0523(16) 0.0200(11) 0.0561(17) 0.0058(11) 0.0149(13) -0.0035(11) C41 0.0203(9) 0.0218(9) 0.0189(9) -0.0011(7) 0.0016(7) 0.0014(8) C10 0.0211(9) 0.0147(8) 0.0216(9) 0.0000(7) -0.0060(8) 0.0001(7) C11 0.0330(12) 0.0271(11) 0.0249(11) 0.0001(8) -0.0047(9) 0.0063(9) C12 0.0614(17) 0.0286(12) 0.0271(11) -0.0074(9) -0.0180(12) 0.0103(12) C13 0.0524(16) 0.0216(11) 0.0515(16) -0.0045(10) -0.0329(13) 0.0002(11) C14 0.0255(12) 0.0258(11) 0.0587(16) 0.0033(11) -0.0178(11) -0.0050(9) C15 0.0217(10) 0.0215(10) 0.0339(12) 0.0006(8) -0.0046(9) -0.0002(8) C16 0.083(3) 0.0507(18) 0.083(3) -0.0174(17) -0.062(2) 0.0013(18) C17 0.0198(10) 0.0175(9) 0.0272(10) -0.0045(8) 0.0067(8) -0.0041(7) C18 0.0275(12) 0.0198(10) 0.0646(17) 0.0141(11) 0.0173(11) 0.0038(9) C19 0.0240(12) 0.0282(12) 0.080(2) 0.0164(13) 0.0190(13) 0.0075(10) C20 0.0240(11) 0.0257(11) 0.0448(14) 0.0013(10) 0.0130(10) -0.0046(9) C21 0.0286(11) 0.0235(10) 0.0242(10) 0.0030(8) 0.0035(8) -0.0043(8) C22 0.0218(10) 0.0250(10) 0.0191(9) -0.0008(8) 0.0005(8) -0.0002(8) C23 0.0284(13) 0.0369(14) 0.072(2) 0.0108(13) 0.0188(13) -0.0050(11) C24 0.0200(9) 0.0176(9) 0.0229(10) -0.0034(7) 0.0068(8) -0.0019(7) C25 0.0368(13) 0.0242(11) 0.0258(11) -0.0014(8) -0.0021(9) -0.0023(9) C26 0.0556(16) 0.0202(10) 0.0311(12) 0.0040(9) 0.0015(11) -0.0026(10) C27 0.0415(14) 0.0224(11) 0.0410(13) -0.0036(10) 0.0112(11) -0.0117(10) C28 0.0272(12) 0.0288(11) 0.0429(14) -0.0112(10) -0.0003(10) -0.0063(9) C29 0.0250(11) 0.0225(10) 0.0288(11) -0.0043(8) -0.0012(8) -0.0004(8) C30 0.076(2) 0.0281(13) 0.075(2) -0.0016(14) 0.0055(18) -0.0241(14) C31 0.0218(10) 0.0179(9) 0.0323(11) 0.0026(8) -0.0036(9) -0.0041(8) C32 0.0503(19) 0.0397(16) 0.140(4) 0.037(2) -0.049(2) -0.0013(14) C33 0.0213(10) 0.0207(9) 0.0227(10) -0.0020(8) 0.0040(8) -0.0005(8) C34 0.0628(19) 0.0531(17) 0.0353(14) 0.0210(12) 0.0007(13) 0.0240(15) C35 0.0195(9) 0.0184(9) 0.0217(10) 0.0023(7) -0.0037(7) -0.0007(7) C36 0.0609(18) 0.0363(13) 0.0269(12) -0.0130(10) 0.0030(12) 0.0044(12) C37 0.0202(10) 0.0211(9) 0.0213(9) -0.0002(8) 0.0008(8) -0.0047(8) C38 0.0562(19) 0.0418(15) 0.079(2) -0.0284(15) 0.0406(17) -0.0055(14) N9 0.0239(9) 0.0225(9) 0.0288(9) -0.0003(7) -0.0045(7) -0.0036(7) C40 0.0291(12) 0.0408(14) 0.0486(15) -0.0011(12) -0.0010(11) -0.0172(11) N10 0.0228(9) 0.0290(9) 0.0283(9) -0.0028(7) 0.0045(7) -0.0054(7) C42 0.0318(13) 0.0446(14) 0.0451(15) -0.0115(12) 0.0089(11) -0.0216(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C31 1.935(2) . ? Rh1 C35 1.949(2) . ? Rh1 N1 2.0933(16) . ? Rh1 N3 2.0942(17) . ? Rh1 C39 2.099(2) . ? Rh1 Rh2 2.6261(4) . ? F1 B1 1.381(4) . ? N1 C1 1.316(2) . ? N1 C3 1.428(2) . ? C1 N2 1.314(2) . ? B1 F2 1.377(4) . ? B1 F4 1.384(4) . ? B1 F3 1.395(4) . ? Rh2 C37 1.939(2) . ? Rh2 C33 1.948(2) . ? Rh2 N2 2.0784(16) . ? Rh2 C41 2.080(2) . ? Rh2 N4 2.0810(16) . ? N2 C10 1.429(2) . ? C2 N4 1.305(2) . ? C2 N3 1.320(2) . ? B2 F5 1.364(4) . ? B2 F8 1.368(4) . ? B2 F7 1.372(4) . ? B2 F6 1.380(4) . ? N3 C17 1.423(2) . ? C3 C4 1.395(3) . ? C3 C8 1.398(3) . ? N4 C24 1.435(2) . ? C4 C5 1.391(3) . ? N5 C31 1.139(3) . ? N5 C32 1.438(3) . ? C5 C6 1.390(3) . ? N6 C33 1.142(3) . ? N6 C34 1.440(3) . ? C6 C7 1.384(3) . ? C6 C9 1.510(3) . ? N7 C35 1.140(3) . ? N7 C36 1.435(3) . ? C7 C8 1.393(3) . ? N8 C37 1.139(3) . ? N8 C38 1.426(3) . ? C39 N9 1.137(3) . ? C41 N10 1.136(3) . ? C10 C11 1.387(3) . ? C10 C15 1.391(3) . ? C11 C12 1.388(3) . ? C12 C13 1.385(4) . ? C13 C14 1.387(4) . ? C13 C16 1.513(3) . ? C14 C15 1.386(3) . ? C17 C18 1.387(3) . ? C17 C22 1.389(3) . ? C18 C19 1.386(3) . ? C19 C20 1.392(3) . ? C20 C21 1.383(3) . ? C20 C23 1.506(3) . ? C21 C22 1.386(3) . ? C24 C25 1.383(3) . ? C24 C29 1.387(3) . ? C25 C26 1.388(3) . ? C26 C27 1.384(4) . ? C27 C28 1.390(4) . ? C27 C30 1.518(3) . ? C28 C29 1.393(3) . ? N9 C40 1.436(3) . ? N10 C42 1.434(3) . ? 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 C31 Rh1 C35 92.09(9) . . ? C31 Rh1 N1 176.54(8) . . ? C35 Rh1 N1 91.26(7) . . ? C31 Rh1 N3 87.40(8) . . ? C35 Rh1 N3 176.70(7) . . ? N1 Rh1 N3 89.20(7) . . ? C31 Rh1 C39 87.22(8) . . ? C35 Rh1 C39 91.50(8) . . ? N1 Rh1 C39 93.52(7) . . ? N3 Rh1 C39 91.73(7) . . ? C31 Rh1 Rh2 92.08(6) . . ? C35 Rh1 Rh2 93.71(6) . . ? N1 Rh1 Rh2 86.88(5) . . ? N3 Rh1 Rh2 83.06(5) . . ? C39 Rh1 Rh2 174.77(5) . . ? C1 N1 C3 118.08(16) . . ? C1 N1 Rh1 116.58(13) . . ? C3 N1 Rh1 123.91(12) . . ? N2 C1 N1 124.74(18) . . ? F2 B1 F1 110.6(3) . . ? F2 B1 F4 110.3(2) . . ? F1 B1 F4 109.5(3) . . ? F2 B1 F3 107.8(3) . . ? F1 B1 F3 110.0(2) . . ? F4 B1 F3 108.6(3) . . ? C37 Rh2 C33 91.49(8) . . ? C37 Rh2 N2 88.82(8) . . ? C33 Rh2 N2 176.36(7) . . ? C37 Rh2 C41 90.73(8) . . ? C33 Rh2 C41 88.75(8) . . ? N2 Rh2 C41 94.87(7) . . ? C37 Rh2 N4 177.93(7) . . ? C33 Rh2 N4 90.44(8) . . ? N2 Rh2 N4 89.20(7) . . ? C41 Rh2 N4 90.06(7) . . ? C37 Rh2 Rh1 93.36(6) . . ? C33 Rh2 Rh1 93.88(6) . . ? N2 Rh2 Rh1 82.48(5) . . ? C41 Rh2 Rh1 175.07(5) . . ? N4 Rh2 Rh1 85.76(5) . . ? C1 N2 C10 115.23(16) . . ? C1 N2 Rh2 122.98(13) . . ? C10 N2 Rh2 121.77(12) . . ? N4 C2 N3 123.46(18) . . ? F5 B2 F8 108.6(3) . . ? F5 B2 F7 109.7(3) . . ? F8 B2 F7 108.2(3) . . ? F5 B2 F6 109.2(3) . . ? F8 B2 F6 110.3(3) . . ? F7 B2 F6 110.8(3) . . ? C2 N3 C17 117.48(16) . . ? C2 N3 Rh1 120.97(13) . . ? C17 N3 Rh1 117.07(12) . . ? C4 C3 C8 117.73(18) . . ? C4 C3 N1 119.68(18) . . ? C8 C3 N1 122.56(18) . . ? C2 N4 C24 119.37(16) . . ? C2 N4 Rh2 120.00(13) . . ? C24 N4 Rh2 120.62(12) . . ? C5 C4 C3 120.8(2) . . ? C31 N5 C32 177.3(2) . . ? C6 C5 C4 121.7(2) . . ? C33 N6 C34 179.0(2) . . ? C7 C6 C5 117.2(2) . . ? C7 C6 C9 121.7(2) . . ? C5 C6 C9 121.1(2) . . ? C35 N7 C36 176.8(2) . . ? C6 C7 C8 122.0(2) . . ? C37 N8 C38 176.0(2) . . ? C7 C8 C3 120.5(2) . . ? N9 C39 Rh1 174.52(17) . . ? N10 C41 Rh2 176.25(18) . . ? C11 C10 C15 119.61(19) . . ? C11 C10 N2 119.44(19) . . ? C15 C10 N2 120.94(18) . . ? C10 C11 C12 120.3(2) . . ? C13 C12 C11 120.8(2) . . ? C12 C13 C14 118.3(2) . . ? C12 C13 C16 120.7(3) . . ? C14 C13 C16 121.0(3) . . ? C15 C14 C13 121.8(2) . . ? C14 C15 C10 119.2(2) . . ? C18 C17 C22 119.20(19) . . ? C18 C17 N3 120.65(19) . . ? C22 C17 N3 119.70(18) . . ? C19 C18 C17 120.1(2) . . ? C18 C19 C20 121.0(2) . . ? C21 C20 C19 118.4(2) . . ? C21 C20 C23 121.2(2) . . ? C19 C20 C23 120.4(2) . . ? C20 C21 C22 121.1(2) . . ? C21 C22 C17 120.19(19) . . ? C25 C24 C29 119.06(19) . . ? C25 C24 N4 120.09(19) . . ? C29 C24 N4 120.75(18) . . ? C24 C25 C26 120.3(2) . . ? C27 C26 C25 121.3(2) . . ? C26 C27 C28 118.0(2) . . ? C26 C27 C30 120.7(3) . . ? C28 C27 C30 121.3(3) . . ? C27 C28 C29 121.0(2) . . ? C24 C29 C28 120.2(2) . . ? N5 C31 Rh1 172.95(19) . . ? N6 C33 Rh2 175.59(19) . . ? N7 C35 Rh1 174.92(19) . . ? N8 C37 Rh2 174.28(18) . . ? C39 N9 C40 176.7(2) . . ? C41 N10 C42 175.9(2) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.827 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.069 _database_code_depnum_ccdc_archive 'CCDC 932778' ####################################################################### # # 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_d:\xray\yong004\yong004 #TrackingRef 'compound6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H46 B2 F12 N10 O Rh2' _chemical_formula_weight 1162.33 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 11.110(2) _cell_length_b 31.777(6) _cell_length_c 14.195(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.13(3) _cell_angle_gamma 90.00 _cell_volume 4917.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9210 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44350 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8664 _reflns_number_gt 7232 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+9.8789P] 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 8664 _refine_ls_number_parameters 630 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.91509(2) 0.151201(8) 0.637042(19) 0.02486(9) Uani 1 1 d . . . F9 F 1.6714(2) 0.09818(14) 0.9117(2) 0.0971(13) Uani 1 1 d . . . O1 O 0.4633(4) 0.07696(12) 0.2211(3) 0.0771(11) Uani 1 1 d . . . N1 N 1.1854(3) 0.12062(9) 0.7345(2) 0.0296(7) Uani 1 1 d . . . C1 C 1.3892(4) 0.14839(16) 0.7989(3) 0.0489(11) Uani 1 1 d . . . H1 H 1.3584 0.1759 0.7824 0.059 Uiso 1 1 calc R . . Rh2 Rh 1.06818(3) 0.157052(9) 0.800974(19) 0.02657(9) Uani 1 1 d . . . F10 F 0.8725(4) 0.00800(9) 0.2821(2) 0.0844(11) Uani 1 1 d . . . N2 N 1.0249(3) 0.10084(9) 0.6127(2) 0.0266(6) Uani 1 1 d . . . C2 C 1.5098(4) 0.1437(2) 0.8431(4) 0.0609(14) Uani 1 1 d . . . H2 H 1.5622 0.1675 0.8570 0.073 Uiso 1 1 calc R . . F11 F 1.1562(3) 0.01860(9) 1.17374(19) 0.0771(10) Uani 1 1 d . . . N3 N 0.9810(3) 0.10254(9) 0.8334(2) 0.0285(7) Uani 1 1 d . . . C3 C 1.5514(4) 0.1048(2) 0.8659(3) 0.0631(16) Uani 1 1 d . . . F12 F 0.3539(2) 0.05340(8) 0.52861(18) 0.0510(6) Uani 1 1 d . . . N4 N 0.8146(3) 0.11014(9) 0.7076(2) 0.0278(6) Uani 1 1 d . . . C4 C 1.4810(5) 0.0698(2) 0.8465(4) 0.0646(15) Uani 1 1 d . . . H4 H 1.5148 0.0427 0.8626 0.077 Uiso 1 1 calc R . . F7 F 1.0523(3) 0.34628(9) 0.7582(3) 0.0808(10) Uani 1 1 d . . . N5 N 0.8885(3) 0.20618(10) 0.9005(2) 0.0367(8) Uani 1 1 d . . . C5 C 1.3569(4) 0.07440(16) 0.8020(3) 0.0502(11) Uani 1 1 d . . . H5 H 1.3055 0.0504 0.7889 0.060 Uiso 1 1 calc R . . F6 F 0.9108(3) 0.30316(10) 0.8009(2) 0.0794(9) Uani 1 1 d . . . N6 N 0.7556(3) 0.22649(10) 0.6769(2) 0.0342(7) Uani 1 1 d . . . C6 C 1.3106(3) 0.11408(13) 0.7775(3) 0.0369(9) Uani 1 1 d . . . F8 F 0.8515(4) 0.35204(13) 0.6855(3) 0.1135(15) Uani 1 1 d . . . N7 N 1.1832(3) 0.23864(11) 0.7387(2) 0.0391(8) Uani 1 1 d . . . C7 C 1.1390(3) 0.09793(11) 0.6588(2) 0.0288(8) Uani 1 1 d . . . H7 H 1.1912 0.0783 0.6360 0.035 Uiso 1 1 calc R . . F5 F 0.9603(3) 0.29711(12) 0.6562(2) 0.0857(10) Uani 1 1 d . . . N8 N 1.0758(3) 0.20211(10) 0.5240(2) 0.0320(7) Uani 1 1 d . . . C8 C 0.9898(3) 0.07619(11) 0.5276(3) 0.0290(8) Uani 1 1 d . . . F2 F 0.5936(2) 0.21863(9) 0.4851(2) 0.0661(8) Uani 1 1 d . . . N9 N 1.2789(4) 0.15474(11) 0.9939(3) 0.0470(9) Uani 1 1 d . . . C9 C 0.8973(4) 0.04693(12) 0.5225(3) 0.0374(9) Uani 1 1 d . . . H9 H 0.8608 0.0422 0.5768 0.045 Uiso 1 1 calc R . . F4 F 0.4262(3) 0.25750(12) 0.4947(3) 0.1094(14) Uani 1 1 d . . . N10 N 0.7398(3) 0.14245(11) 0.4307(3) 0.0400(8) Uani 1 1 d . . . C10 C 0.8567(4) 0.02425(12) 0.4389(3) 0.0432(10) Uani 1 1 d . . . H10 H 0.7916 0.0045 0.4346 0.052 Uiso 1 1 calc R . . B2 B 0.9451(6) 0.3253(2) 0.7255(5) 0.0639(16) Uani 1 1 d . . . F3 F 0.4929(3) 0.25142(14) 0.3549(3) 0.1134(15) Uani 1 1 d . . . C11 C 0.9125(5) 0.03103(14) 0.3637(3) 0.0532(12) Uani 1 1 d . . . F1 F 0.4067(3) 0.19630(9) 0.4137(2) 0.0720(8) Uani 1 1 d . . . C12 C 1.0046(6) 0.05914(16) 0.3662(3) 0.0736(18) Uani 1 1 d . . . H12 H 1.0419 0.0629 0.3120 0.088 Uiso 1 1 calc R . . C13 C 1.0434(5) 0.08227(14) 0.4490(3) 0.0539(13) Uani 1 1 d . . . H13 H 1.1073 0.1024 0.4517 0.065 Uiso 1 1 calc R . . C14 C 0.9927(6) 0.09284(15) 1.0053(3) 0.0626(15) Uani 1 1 d . . . H14 H 0.9383 0.1160 1.0046 0.075 Uiso 1 1 calc R . . C15 C 1.0364(6) 0.07241(16) 1.0904(3) 0.0764(19) Uani 1 1 d . . . H15 H 1.0129 0.0811 1.1483 0.092 Uiso 1 1 calc R . . C16 C 1.1135(5) 0.03972(14) 1.0896(3) 0.0497(11) Uani 1 1 d . . . C17 C 1.1484(5) 0.02613(15) 1.0093(4) 0.0606(14) Uani 1 1 d . . . H17 H 1.2030 0.0030 1.0113 0.073 Uiso 1 1 calc R . . C18 C 1.1028(4) 0.04674(14) 0.9230(3) 0.0493(11) Uani 1 1 d . . . H18 H 1.1251 0.0373 0.8653 0.059 Uiso 1 1 calc R . . C19 C 1.0262(3) 0.08040(11) 0.9212(2) 0.0285(8) Uani 1 1 d . . . C20 C 0.8717(3) 0.09192(11) 0.7870(2) 0.0294(8) Uani 1 1 d . . . H20 H 0.8309 0.0696 0.8123 0.035 Uiso 1 1 calc R . . C21 C 0.6961(3) 0.09467(11) 0.6641(2) 0.0288(8) Uani 1 1 d . . . C22 C 0.6683(4) 0.05208(12) 0.6597(3) 0.0341(9) Uani 1 1 d . . . H22 H 0.7284 0.0322 0.6880 0.041 Uiso 1 1 calc R . . C23 C 0.5527(4) 0.03838(13) 0.6138(3) 0.0395(9) Uani 1 1 d . . . H23 H 0.5334 0.0092 0.6107 0.047 Uiso 1 1 calc R . . C24 C 0.4678(3) 0.06723(14) 0.5738(3) 0.0389(9) Uani 1 1 d . . . C25 C 0.4915(3) 0.10956(13) 0.5764(3) 0.0371(9) Uani 1 1 d . . . H25 H 0.4305 0.1291 0.5477 0.045 Uiso 1 1 calc R . . C26 C 0.6059(3) 0.12314(12) 0.6217(3) 0.0338(8) Uani 1 1 d . . . H26 H 0.6238 0.1524 0.6242 0.041 Uiso 1 1 calc R . . C27 C 1.1387(4) 0.20878(12) 0.7612(3) 0.0334(8) Uani 1 1 d . . . C28 C 1.2399(4) 0.27459(14) 0.7038(3) 0.0512(12) Uani 1 1 d . . . H28A H 1.3099 0.2653 0.6763 0.077 Uiso 1 1 calc R . . H28B H 1.2683 0.2941 0.7570 0.077 Uiso 1 1 calc R . . H28C H 1.1801 0.2889 0.6543 0.077 Uiso 1 1 calc R . . C29 C 1.0184(3) 0.18510(11) 0.5704(2) 0.0275(8) Uani 1 1 d . . . C30 C 1.1473(4) 0.22134(16) 0.4612(3) 0.0548(13) Uani 1 1 d . . . H30A H 1.2337 0.2135 0.4818 0.082 Uiso 1 1 calc R . . H30B H 1.1392 0.2520 0.4638 0.082 Uiso 1 1 calc R . . H30C H 1.1177 0.2116 0.3953 0.082 Uiso 1 1 calc R . . C31 C 0.9527(4) 0.18823(12) 0.8602(3) 0.0316(8) Uani 1 1 d . . . C32 C 0.8083(4) 0.23024(15) 0.9482(3) 0.0492(11) Uani 1 1 d . . . H32A H 0.8145 0.2601 0.9328 0.074 Uiso 1 1 calc R . . H32B H 0.8323 0.2262 1.0178 0.074 Uiso 1 1 calc R . . H32C H 0.7236 0.2207 0.9266 0.074 Uiso 1 1 calc R . . C33 C 0.8184(3) 0.19935(12) 0.6648(3) 0.0300(8) Uani 1 1 d . . . C34 C 0.6718(4) 0.25949(14) 0.6891(4) 0.0512(12) Uani 1 1 d . . . H34A H 0.5976 0.2572 0.6393 0.077 Uiso 1 1 calc R . . H34B H 0.7106 0.2869 0.6838 0.077 Uiso 1 1 calc R . . H34C H 0.6499 0.2570 0.7525 0.077 Uiso 1 1 calc R . . C35 C 1.1992(3) 0.15612(11) 0.9324(3) 0.0289(8) Uani 1 1 d . . . C36 C 1.3908(5) 0.15157(17) 1.0684(4) 0.0649(15) Uani 1 1 d . . . H36A H 1.4628 0.1505 1.0379 0.097 Uiso 1 1 calc R . . H36B H 1.3874 0.1259 1.1062 0.097 Uiso 1 1 calc R . . H36C H 1.3968 0.1762 1.1106 0.097 Uiso 1 1 calc R . . C37 C 0.7994(3) 0.14335(11) 0.5049(3) 0.0273(8) Uani 1 1 d . . . C38 C 0.6603(5) 0.14109(18) 0.3374(3) 0.0650(14) Uani 1 1 d . . . H38A H 0.6110 0.1153 0.3318 0.098 Uiso 1 1 calc R . . H38B H 0.7100 0.1414 0.2874 0.098 Uiso 1 1 calc R . . H38C H 0.6060 0.1657 0.3297 0.098 Uiso 1 1 calc R . . C39 C 0.6111(10) 0.0541(3) 0.1277(5) 0.152(4) Uani 1 1 d . . . H39A H 0.5558 0.0464 0.0678 0.228 Uiso 1 1 calc R . . H39B H 0.6864 0.0374 0.1348 0.228 Uiso 1 1 calc R . . H39C H 0.6314 0.0841 0.1262 0.228 Uiso 1 1 calc R . . C40 C 0.5472(9) 0.0454(2) 0.2139(6) 0.130(3) Uani 1 1 d . . . H40A H 0.5046 0.0179 0.2048 0.156 Uiso 1 1 calc R . . H40B H 0.6095 0.0441 0.2739 0.156 Uiso 1 1 calc R . . C41 C 0.3990(6) 0.07144(18) 0.2973(5) 0.0744(16) Uani 1 1 d . . . H41A H 0.4586 0.0694 0.3587 0.089 Uiso 1 1 calc R . . H41B H 0.3520 0.0448 0.2878 0.089 Uiso 1 1 calc R . . C42 C 0.3139(6) 0.1069(2) 0.3024(5) 0.093(2) Uani 1 1 d . . . H42A H 0.3612 0.1325 0.3219 0.140 Uiso 1 1 calc R . . H42B H 0.2627 0.1003 0.3495 0.140 Uiso 1 1 calc R . . H42C H 0.2615 0.1112 0.2392 0.140 Uiso 1 1 calc R . . B1 B 0.4794(4) 0.23163(17) 0.4384(4) 0.0502(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02635(16) 0.02773(15) 0.02193(15) 0.00165(11) 0.00821(11) -0.00083(11) F9 0.0283(14) 0.198(4) 0.0625(19) -0.022(2) 0.0018(13) 0.0216(19) O1 0.096(3) 0.065(2) 0.063(2) 0.0009(19) -0.004(2) 0.015(2) N1 0.0255(16) 0.0374(17) 0.0273(16) -0.0026(13) 0.0082(13) -0.0002(13) C1 0.031(2) 0.073(3) 0.044(3) -0.015(2) 0.0121(19) -0.009(2) Rh2 0.02885(16) 0.03045(16) 0.02190(15) -0.00060(11) 0.00858(12) -0.00179(12) F10 0.136(3) 0.0652(19) 0.0419(16) -0.0195(14) -0.0081(17) -0.0238(19) N2 0.0283(16) 0.0279(15) 0.0242(15) 0.0001(12) 0.0064(12) -0.0003(12) C2 0.038(3) 0.097(4) 0.050(3) -0.025(3) 0.015(2) -0.012(3) F11 0.109(3) 0.0661(19) 0.0434(16) 0.0245(14) -0.0184(16) -0.0088(17) N3 0.0311(17) 0.0313(16) 0.0249(15) 0.0036(13) 0.0096(13) -0.0002(13) C3 0.028(2) 0.122(5) 0.041(3) -0.025(3) 0.009(2) -0.002(3) F12 0.0320(13) 0.0660(16) 0.0545(15) -0.0059(13) 0.0071(11) -0.0153(12) N4 0.0282(16) 0.0307(16) 0.0253(16) 0.0031(13) 0.0074(13) -0.0030(13) C4 0.056(3) 0.091(4) 0.046(3) 0.004(3) 0.009(2) 0.030(3) F7 0.079(2) 0.0597(19) 0.108(3) -0.0200(17) 0.030(2) -0.0239(16) N5 0.0390(19) 0.0440(19) 0.0283(17) -0.0045(15) 0.0100(15) 0.0012(15) C5 0.038(2) 0.069(3) 0.043(3) 0.002(2) 0.005(2) 0.012(2) F6 0.072(2) 0.087(2) 0.074(2) 0.0308(18) -0.0003(17) -0.0140(17) N6 0.0318(17) 0.0335(18) 0.0369(18) -0.0029(14) 0.0054(14) 0.0006(14) C6 0.028(2) 0.057(3) 0.028(2) -0.0063(18) 0.0100(16) 0.0035(18) F8 0.087(3) 0.111(3) 0.148(4) 0.075(3) 0.036(3) 0.036(2) N7 0.046(2) 0.0405(19) 0.0305(18) -0.0013(15) 0.0068(15) -0.0123(16) C7 0.033(2) 0.0286(19) 0.0275(19) 0.0003(15) 0.0120(16) -0.0002(15) F5 0.069(2) 0.104(3) 0.078(2) -0.017(2) -0.0004(17) -0.0151(19) N8 0.0297(17) 0.0392(18) 0.0277(16) 0.0070(14) 0.0071(14) -0.0031(14) C8 0.033(2) 0.0244(18) 0.0285(19) 0.0012(15) 0.0025(16) 0.0029(15) F2 0.0436(16) 0.0731(19) 0.079(2) 0.0057(16) 0.0045(14) 0.0043(14) N9 0.065(3) 0.041(2) 0.039(2) -0.0039(16) 0.020(2) 0.0062(18) C9 0.035(2) 0.032(2) 0.048(2) -0.0037(18) 0.0161(19) 0.0014(17) F4 0.059(2) 0.097(3) 0.174(4) -0.056(3) 0.027(2) 0.0030(19) N10 0.0385(19) 0.0403(19) 0.042(2) 0.0012(16) 0.0114(17) 0.0000(15) C10 0.036(2) 0.028(2) 0.063(3) -0.0110(19) 0.001(2) -0.0016(17) B2 0.058(4) 0.052(3) 0.082(5) 0.013(3) 0.014(3) 0.002(3) F3 0.077(2) 0.139(3) 0.119(3) 0.069(3) 0.004(2) -0.010(2) C11 0.082(4) 0.037(2) 0.033(2) -0.0052(19) -0.006(2) -0.005(2) F1 0.0573(18) 0.0682(19) 0.089(2) -0.0056(16) 0.0108(16) -0.0078(15) C12 0.134(5) 0.063(3) 0.029(2) -0.008(2) 0.027(3) -0.037(3) C13 0.084(4) 0.049(3) 0.034(2) -0.006(2) 0.024(2) -0.032(2) C14 0.113(4) 0.048(3) 0.033(2) 0.009(2) 0.030(3) 0.025(3) C15 0.155(6) 0.052(3) 0.025(2) 0.007(2) 0.023(3) 0.020(3) C16 0.064(3) 0.049(3) 0.030(2) 0.0110(19) -0.005(2) -0.009(2) C17 0.055(3) 0.054(3) 0.075(4) 0.028(3) 0.017(3) 0.021(2) C18 0.061(3) 0.051(3) 0.041(2) 0.009(2) 0.023(2) 0.018(2) C19 0.031(2) 0.0290(18) 0.0258(19) 0.0017(15) 0.0066(15) -0.0020(15) C20 0.032(2) 0.0318(19) 0.0272(19) -0.0017(15) 0.0133(16) -0.0021(16) C21 0.032(2) 0.035(2) 0.0227(18) -0.0002(15) 0.0128(15) -0.0039(16) C22 0.034(2) 0.041(2) 0.029(2) 0.0031(16) 0.0125(16) -0.0044(17) C23 0.044(2) 0.041(2) 0.036(2) -0.0003(18) 0.0149(19) -0.0131(19) C24 0.027(2) 0.058(3) 0.034(2) -0.0028(19) 0.0112(17) -0.0100(19) C25 0.029(2) 0.049(2) 0.035(2) -0.0008(18) 0.0121(17) -0.0010(18) C26 0.033(2) 0.038(2) 0.033(2) -0.0011(17) 0.0134(17) -0.0024(17) C27 0.036(2) 0.039(2) 0.0255(19) -0.0045(16) 0.0066(16) -0.0059(18) C28 0.061(3) 0.047(3) 0.047(3) 0.004(2) 0.012(2) -0.022(2) C29 0.0270(19) 0.0297(19) 0.0245(18) 0.0015(15) 0.0021(15) 0.0021(15) C30 0.051(3) 0.077(3) 0.040(2) 0.010(2) 0.017(2) -0.023(2) C31 0.038(2) 0.033(2) 0.0231(19) -0.0023(15) 0.0040(17) -0.0039(17) C32 0.047(3) 0.062(3) 0.041(2) -0.015(2) 0.016(2) 0.008(2) C33 0.030(2) 0.037(2) 0.0237(18) 0.0026(16) 0.0053(15) -0.0051(17) C34 0.046(3) 0.044(3) 0.064(3) -0.012(2) 0.012(2) 0.013(2) C35 0.030(2) 0.033(2) 0.0249(19) -0.0009(15) 0.0078(17) -0.0004(16) C36 0.070(3) 0.075(4) 0.041(3) -0.006(2) -0.010(2) 0.021(3) C37 0.0289(19) 0.0285(19) 0.027(2) 0.0026(15) 0.0112(16) -0.0018(15) C38 0.059(3) 0.086(4) 0.042(3) -0.005(3) -0.009(2) -0.008(3) C39 0.285(13) 0.115(6) 0.058(4) 0.012(4) 0.041(6) 0.102(7) C40 0.207(10) 0.080(5) 0.101(6) -0.011(4) 0.024(6) 0.059(6) C41 0.074(4) 0.066(4) 0.082(4) 0.012(3) 0.012(3) -0.014(3) C42 0.062(4) 0.110(5) 0.108(5) 0.023(4) 0.016(4) 0.008(4) B1 0.029(3) 0.051(3) 0.068(4) 0.009(3) 0.006(2) 0.005(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 C29 1.947(4) . ? Rh1 C33 1.953(4) . ? Rh1 C37 2.074(4) . ? Rh1 N2 2.081(3) . ? Rh1 N4 2.094(3) . ? Rh1 Rh2 2.6104(10) . ? F9 C3 1.382(5) . ? O1 C40 1.386(8) . ? O1 C41 1.417(7) . ? N1 C7 1.315(5) . ? N1 C6 1.422(5) . ? N1 Rh2 2.098(3) . ? C1 C2 1.374(7) . ? C1 C6 1.393(6) . ? Rh2 C31 1.936(4) . ? Rh2 C27 1.950(4) . ? Rh2 N3 2.079(3) . ? Rh2 C35 2.133(4) . ? F10 C11 1.369(5) . ? N2 C7 1.313(5) . ? N2 C8 1.429(4) . ? C2 C3 1.339(8) . ? F11 C16 1.372(5) . ? N3 C20 1.309(5) . ? N3 C19 1.435(4) . ? C3 C4 1.356(8) . ? F12 C24 1.376(4) . ? N4 C20 1.316(5) . ? N4 C21 1.429(5) . ? C4 C5 1.409(6) . ? F7 B2 1.365(7) . ? N5 C31 1.148(5) . ? N5 C32 1.439(5) . ? C5 C6 1.381(6) . ? F6 B2 1.395(7) . ? N6 C33 1.142(5) . ? N6 C34 1.435(5) . ? F8 B2 1.377(7) . ? N7 C27 1.144(5) . ? N7 C28 1.438(5) . ? F5 B2 1.366(7) . ? N8 C29 1.138(4) . ? N8 C30 1.440(5) . ? C8 C13 1.377(6) . ? C8 C9 1.377(5) . ? F2 B1 1.377(6) . ? N9 C35 1.118(5) . ? N9 C36 1.472(6) . ? C9 C10 1.387(6) . ? F4 B1 1.359(7) . ? N10 C37 1.130(5) . ? N10 C38 1.444(6) . ? C10 C11 1.352(7) . ? F3 B1 1.374(7) . ? C11 C12 1.354(7) . ? F1 B1 1.388(6) . ? C12 C13 1.383(6) . ? C14 C15 1.375(6) . ? C14 C19 1.376(6) . ? C15 C16 1.348(7) . ? C16 C17 1.345(7) . ? C17 C18 1.395(6) . ? C18 C19 1.364(5) . ? C21 C22 1.387(5) . ? C21 C26 1.397(5) . ? C22 C23 1.393(5) . ? C23 C24 1.358(6) . ? C24 C25 1.370(6) . ? C25 C26 1.379(5) . ? C39 C40 1.553(11) . ? C41 C42 1.481(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 C33 93.65(15) . . ? C29 Rh1 C37 87.00(14) . . ? C33 Rh1 C37 90.43(14) . . ? C29 Rh1 N2 85.72(13) . . ? C33 Rh1 N2 177.25(13) . . ? C37 Rh1 N2 92.20(13) . . ? C29 Rh1 N4 174.79(13) . . ? C33 Rh1 N4 91.52(13) . . ? C37 Rh1 N4 93.61(12) . . ? N2 Rh1 N4 89.09(12) . . ? C29 Rh1 Rh2 92.87(10) . . ? C33 Rh1 Rh2 93.07(10) . . ? C37 Rh1 Rh2 176.50(10) . . ? N2 Rh1 Rh2 84.30(8) . . ? N4 Rh1 Rh2 86.21(8) . . ? C40 O1 C41 114.3(5) . . ? C7 N1 C6 117.9(3) . . ? C7 N1 Rh2 119.4(2) . . ? C6 N1 Rh2 121.9(2) . . ? C2 C1 C6 122.0(5) . . ? C31 Rh2 C27 91.79(16) . . ? C31 Rh2 N3 87.36(14) . . ? C27 Rh2 N3 175.16(14) . . ? C31 Rh2 N1 176.69(14) . . ? C27 Rh2 N1 90.92(14) . . ? N3 Rh2 N1 89.78(12) . . ? C31 Rh2 C35 91.42(14) . . ? C27 Rh2 C35 91.17(15) . . ? N3 Rh2 C35 93.62(13) . . ? N1 Rh2 C35 90.43(13) . . ? C31 Rh2 Rh1 92.94(11) . . ? C27 Rh2 Rh1 91.78(11) . . ? N3 Rh2 Rh1 83.50(8) . . ? N1 Rh2 Rh1 85.08(8) . . ? C35 Rh2 Rh1 174.66(10) . . ? C7 N2 C8 117.5(3) . . ? C7 N2 Rh1 120.8(2) . . ? C8 N2 Rh1 119.2(2) . . ? C3 C2 C1 118.1(5) . . ? C20 N3 C19 116.5(3) . . ? C20 N3 Rh2 122.0(2) . . ? C19 N3 Rh2 120.0(2) . . ? C2 C3 C4 123.4(5) . . ? C2 C3 F9 120.7(5) . . ? C4 C3 F9 115.9(6) . . ? C20 N4 C21 118.1(3) . . ? C20 N4 Rh1 118.0(2) . . ? C21 N4 Rh1 122.6(2) . . ? C3 C4 C5 118.8(5) . . ? C31 N5 C32 177.5(4) . . ? C6 C5 C4 119.5(5) . . ? C33 N6 C34 177.1(4) . . ? C5 C6 C1 118.2(4) . . ? C5 C6 N1 121.8(4) . . ? C1 C6 N1 119.9(4) . . ? C27 N7 C28 175.7(4) . . ? N2 C7 N1 123.8(3) . . ? C29 N8 C30 176.3(4) . . ? C13 C8 C9 119.2(4) . . ? C13 C8 N2 121.2(3) . . ? C9 C8 N2 119.6(3) . . ? C35 N9 C36 174.6(4) . . ? C8 C9 C10 120.8(4) . . ? C37 N10 C38 178.1(4) . . ? C11 C10 C9 118.0(4) . . ? F7 B2 F5 110.2(5) . . ? F7 B2 F8 112.3(5) . . ? F5 B2 F8 107.2(6) . . ? F7 B2 F6 109.6(5) . . ? F5 B2 F6 108.2(5) . . ? F8 B2 F6 109.3(5) . . ? C10 C11 C12 123.0(4) . . ? C10 C11 F10 117.4(4) . . ? C12 C11 F10 119.7(5) . . ? C11 C12 C13 118.9(5) . . ? C8 C13 C12 120.1(4) . . ? C15 C14 C19 121.2(5) . . ? C16 C15 C14 118.3(5) . . ? C17 C16 C15 122.8(4) . . ? C17 C16 F11 118.2(4) . . ? C15 C16 F11 118.9(4) . . ? C16 C17 C18 118.6(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C14 118.8(4) . . ? C18 C19 N3 120.9(3) . . ? C14 C19 N3 120.3(3) . . ? N3 C20 N4 124.4(3) . . ? C22 C21 C26 118.6(3) . . ? C22 C21 N4 122.2(3) . . ? C26 C21 N4 119.2(3) . . ? C21 C22 C23 120.2(4) . . ? C24 C23 C22 119.2(4) . . ? C23 C24 C25 122.5(4) . . ? C23 C24 F12 118.8(4) . . ? C25 C24 F12 118.7(4) . . ? C24 C25 C26 118.3(4) . . ? C25 C26 C21 121.2(4) . . ? N7 C27 Rh2 178.1(4) . . ? N8 C29 Rh1 173.1(3) . . ? N5 C31 Rh2 176.0(3) . . ? N6 C33 Rh1 175.6(3) . . ? N9 C35 Rh2 170.8(3) . . ? N10 C37 Rh1 173.9(3) . . ? O1 C40 C39 110.2(6) . . ? O1 C41 C42 111.3(5) . . ? F4 B1 F3 111.2(5) . . ? F4 B1 F2 111.3(5) . . ? F3 B1 F2 108.0(4) . . ? F4 B1 F1 109.9(4) . . ? F3 B1 F1 107.9(5) . . ? F2 B1 F1 108.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.081 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 932779' ####################################################################### # # 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_g:\xray\frames\yong01~1\work1\yong015 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 B2 F8 N12 Rh2' _chemical_formula_weight 1074.33 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.126(3) _cell_length_b 21.399(4) _cell_length_c 31.434(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9502(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 83459 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 24.73 _reflns_number_total 8110 _reflns_number_gt 6030 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+35.3455P] 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 8110 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.60344(3) 0.142172(16) 0.651480(11) 0.02001(11) Uani 1 1 d . . . Rh2 Rh 0.45591(2) 0.070848(16) 0.647584(12) 0.02083(11) Uani 1 1 d . . . N5 N 0.6123(3) 0.03366(17) 0.58964(12) 0.0227(9) Uani 1 1 d . . . N4 N 0.5431(3) 0.01161(17) 0.61222(12) 0.0231(9) Uani 1 1 d . . . N2 N 0.4602(3) 0.18037(17) 0.58598(12) 0.0238(9) Uani 1 1 d . . . N3 N 0.5283(3) 0.19893(17) 0.61029(12) 0.0222(9) Uani 1 1 d . . . N6 N 0.6429(3) 0.08874(17) 0.59926(12) 0.0226(9) Uani 1 1 d . . . N1 N 0.4319(3) 0.12343(17) 0.59255(13) 0.0237(9) Uani 1 1 d . . . C37 C 0.7195(4) 0.2032(2) 0.64949(15) 0.0267(11) Uani 1 1 d . . . C27 C 0.5463(4) -0.0759(2) 0.56103(16) 0.0296(12) Uani 1 1 d . . . H27 H 0.5824 -0.0513 0.5418 0.036 Uiso 1 1 calc R . . C39 C 0.3327(4) 0.0182(2) 0.63813(16) 0.0288(12) Uani 1 1 d . . . C26 C 0.5199(4) -0.1366(2) 0.55003(17) 0.0329(12) Uani 1 1 d . . . H26 H 0.5404 -0.1534 0.5236 0.040 Uiso 1 1 calc R . . C35 C 0.5557(4) 0.1889(2) 0.70020(16) 0.0287(12) Uani 1 1 d . . . C6 C 0.5245(4) 0.3090(2) 0.63076(16) 0.0304(12) Uani 1 1 d . . . H6 H 0.4764 0.2996 0.6509 0.037 Uiso 1 1 calc R . . C15 C 0.7102(3) 0.1104(2) 0.56793(15) 0.0230(11) Uani 1 1 d . . . C25 C 0.4644(4) -0.1730(2) 0.57683(18) 0.0321(12) Uani 1 1 d . . . C24 C 0.4394(4) -0.1480(2) 0.61583(18) 0.0324(12) Uani 1 1 d . . . H24 H 0.4027 -0.1726 0.6349 0.039 Uiso 1 1 calc R . . C31 C 0.4858(4) 0.0254(2) 0.69960(17) 0.0277(11) Uani 1 1 d . . . C9 C 0.3547(4) 0.0525(2) 0.54335(15) 0.0285(11) Uani 1 1 d . . . H9 H 0.4124 0.0301 0.5404 0.034 Uiso 1 1 calc R . . C22 C 0.5196(3) -0.0514(2) 0.60023(16) 0.0231(11) Uani 1 1 d . . . C16 C 0.8044(4) 0.1187(2) 0.57829(18) 0.0302(12) Uani 1 1 d . . . H16 H 0.8260 0.1108 0.6064 0.036 Uiso 1 1 calc R . . C5 C 0.5576(3) 0.2631(2) 0.60366(15) 0.0243(11) Uani 1 1 d . . . C19 C 0.7429(4) 0.1421(2) 0.49649(17) 0.0372(13) Uani 1 1 d . . . H19 H 0.7212 0.1498 0.4684 0.045 Uiso 1 1 calc R . . C8 C 0.3514(3) 0.1069(2) 0.56713(16) 0.0274(11) Uani 1 1 d . . . C18 C 0.8377(4) 0.1514(2) 0.50621(19) 0.0383(14) Uani 1 1 d . . . C29 C 0.6723(4) 0.0857(2) 0.68848(17) 0.0313(12) Uani 1 1 d . . . C23 C 0.4664(3) -0.0883(2) 0.62796(17) 0.0281(11) Uani 1 1 d . . . H23 H 0.4486 -0.0725 0.6551 0.034 Uiso 1 1 calc R . . C33 C 0.3755(4) 0.1293(2) 0.67828(18) 0.0339(13) Uani 1 1 d . . . C11 C 0.1885(4) 0.0620(2) 0.5274(2) 0.0414(14) Uani 1 1 d . . . C4 C 0.6255(4) 0.2777(2) 0.57371(16) 0.0303(12) Uani 1 1 d . . . H4 H 0.6471 0.2466 0.5545 0.036 Uiso 1 1 calc R . . C20 C 0.6792(4) 0.1218(2) 0.52710(15) 0.0291(12) Uani 1 1 d . . . H20 H 0.6145 0.1158 0.5200 0.035 Uiso 1 1 calc R . . C10 C 0.2728(4) 0.0310(2) 0.52380(16) 0.0319(12) Uani 1 1 d . . . H10 H 0.2754 -0.0063 0.5074 0.038 Uiso 1 1 calc R . . C17 C 0.8670(4) 0.1386(2) 0.54725(19) 0.0386(14) Uani 1 1 d . . . H17 H 0.9320 0.1436 0.5543 0.046 Uiso 1 1 calc R . . C13 C 0.2685(4) 0.1398(3) 0.5700(2) 0.058(2) Uani 1 1 d . . . H13 H 0.2669 0.1781 0.5852 0.070 Uiso 1 1 calc R . . N11 N 0.7776(3) 0.23928(19) 0.64921(13) 0.0289(9) Uani 1 1 d . . . N9 N 0.5003(3) -0.0041(2) 0.72909(14) 0.0338(10) Uani 1 1 d . . . N8 N 0.5303(3) 0.2195(2) 0.72792(14) 0.0345(11) Uani 1 1 d . . . N12 N 0.2610(3) -0.0061(2) 0.63387(14) 0.0345(10) Uani 1 1 d . . . F1 F 1.0154(4) 0.1621(2) 0.65100(14) 0.0988(17) Uani 1 1 d . . . F3 F 0.9799(4) 0.0584(2) 0.64911(18) 0.119(2) Uani 1 1 d . . . C38 C 0.8505(4) 0.2858(3) 0.64613(19) 0.0443(15) Uani 1 1 d . . . H38A H 0.9126 0.2656 0.6481 0.066 Uiso 1 1 calc R . . H38B H 0.8435 0.3159 0.6694 0.066 Uiso 1 1 calc R . . H38C H 0.8451 0.3076 0.6188 0.066 Uiso 1 1 calc R . . C7 C 0.5616(4) 0.3687(2) 0.62854(18) 0.0402(14) Uani 1 1 d . . . H7 H 0.5378 0.4002 0.6470 0.048 Uiso 1 1 calc R . . C2 C 0.6330(4) 0.3837(2) 0.5999(2) 0.0423(15) Uani 1 1 d . . . N10 N 0.7168(3) 0.0563(2) 0.71074(17) 0.0519(14) Uani 1 1 d . . . N7 N 0.3215(4) 0.1585(2) 0.6961(2) 0.0630(18) Uani 1 1 d . . . C3 C 0.6625(4) 0.3380(2) 0.57166(18) 0.0375(14) Uani 1 1 d . . . H3 H 0.7085 0.3478 0.5507 0.045 Uiso 1 1 calc R . . C14 C 0.0984(4) 0.0357(3) 0.5090(2) 0.060(2) Uani 1 1 d . . . H14A H 0.1114 -0.0051 0.4961 0.090 Uiso 1 1 calc R . . H14B H 0.0738 0.0642 0.4873 0.090 Uiso 1 1 calc R . . H14C H 0.0513 0.0308 0.5317 0.090 Uiso 1 1 calc R . . C28 C 0.4349(4) -0.2382(2) 0.5640(2) 0.0461(16) Uani 1 1 d . . . H28A H 0.4574 -0.2682 0.5853 0.069 Uiso 1 1 calc R . . H28B H 0.4623 -0.2484 0.5362 0.069 Uiso 1 1 calc R . . H28C H 0.3657 -0.2403 0.5622 0.069 Uiso 1 1 calc R . . C40 C 0.1735(4) -0.0383(3) 0.6261(2) 0.0552(18) Uani 1 1 d . . . H40A H 0.1703 -0.0508 0.5962 0.083 Uiso 1 1 calc R . . H40B H 0.1203 -0.0104 0.6327 0.083 Uiso 1 1 calc R . . H40C H 0.1700 -0.0755 0.6442 0.083 Uiso 1 1 calc R . . B1 B 1.0034(7) 0.1083(4) 0.6737(3) 0.060(2) Uani 1 1 d . . . F2 F 1.0841(4) 0.0940(2) 0.69540(17) 0.1011(17) Uani 1 1 d . . . F4 F 0.9330(4) 0.1173(3) 0.7029(2) 0.122(2) Uani 1 1 d . . . C21 C 0.9059(5) 0.1743(3) 0.4727(2) 0.063(2) Uani 1 1 d . . . H21A H 0.8981 0.2194 0.4689 0.095 Uiso 1 1 calc R . . H21B H 0.8929 0.1530 0.4457 0.095 Uiso 1 1 calc R . . H21C H 0.9709 0.1653 0.4817 0.095 Uiso 1 1 calc R . . C12 C 0.1870(5) 0.1175(3) 0.5509(3) 0.076(3) Uani 1 1 d . . . H12 H 0.1295 0.1401 0.5537 0.092 Uiso 1 1 calc R . . F8 F 0.7940(5) 0.3851(4) 0.7308(2) 0.169(3) Uani 1 1 d . . . C1 C 0.6789(5) 0.4476(3) 0.6007(3) 0.069(2) Uani 1 1 d . . . H1A H 0.6298 0.4798 0.6019 0.104 Uiso 1 1 calc R . . H1B H 0.7168 0.4532 0.5748 0.104 Uiso 1 1 calc R . . H1C H 0.7199 0.4510 0.6257 0.104 Uiso 1 1 calc R . . C36 C 0.4953(5) 0.2582(3) 0.76208(19) 0.0605(19) Uani 1 1 d . . . H36A H 0.5440 0.2886 0.7702 0.091 Uiso 1 1 calc R . . H36B H 0.4797 0.2319 0.7866 0.091 Uiso 1 1 calc R . . H36C H 0.4384 0.2804 0.7526 0.091 Uiso 1 1 calc R . . C32 C 0.5150(5) -0.0429(3) 0.76603(19) 0.0586(19) Uani 1 1 d . . . H32A H 0.5076 -0.0177 0.7918 0.088 Uiso 1 1 calc R . . H32B H 0.5790 -0.0606 0.7652 0.088 Uiso 1 1 calc R . . H32C H 0.4685 -0.0769 0.7662 0.088 Uiso 1 1 calc R . . F5 F 0.7057(7) 0.3119(4) 0.7452(4) 0.256(6) Uani 1 1 d . . . C34 C 0.2501(6) 0.1912(4) 0.7198(4) 0.130(5) Uani 1 1 d . . . H34A H 0.1918 0.1664 0.7202 0.195 Uiso 1 1 calc R . . H34B H 0.2376 0.2317 0.7063 0.195 Uiso 1 1 calc R . . H34C H 0.2721 0.1978 0.7490 0.195 Uiso 1 1 calc R . . C30 C 0.7769(6) 0.0233(4) 0.7400(3) 0.116(4) Uani 1 1 d . . . H30A H 0.8299 0.0501 0.7483 0.173 Uiso 1 1 calc R . . H30B H 0.8013 -0.0146 0.7263 0.173 Uiso 1 1 calc R . . H30C H 0.7404 0.0117 0.7653 0.173 Uiso 1 1 calc R . . B2 B 0.7471(9) 0.3568(4) 0.7659(7) 0.132(7) Uani 1 1 d . . . F7 F 0.8140(4) 0.3395(3) 0.7924(2) 0.129(2) Uani 1 1 d . . . F6 F 0.6878(6) 0.3985(3) 0.7816(2) 0.191(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0197(2) 0.01874(19) 0.0216(2) 0.00121(15) -0.00064(16) -0.00095(15) Rh2 0.0193(2) 0.01715(19) 0.0261(2) 0.00153(16) 0.00350(16) -0.00035(15) N5 0.021(2) 0.018(2) 0.029(2) 0.0025(17) 0.0028(18) -0.0004(17) N4 0.022(2) 0.017(2) 0.030(2) 0.0025(17) 0.0031(18) 0.0029(17) N2 0.027(2) 0.017(2) 0.028(2) -0.0017(17) -0.0031(19) 0.0005(17) N3 0.024(2) 0.017(2) 0.025(2) 0.0011(16) -0.0049(18) -0.0028(17) N6 0.023(2) 0.018(2) 0.027(2) 0.0000(16) 0.0013(18) -0.0012(17) N1 0.020(2) 0.018(2) 0.034(2) 0.0010(17) -0.0046(18) -0.0049(17) C37 0.031(3) 0.026(3) 0.023(3) 0.002(2) -0.001(2) 0.007(2) C27 0.029(3) 0.023(3) 0.037(3) 0.000(2) 0.001(2) -0.004(2) C39 0.030(3) 0.025(3) 0.032(3) -0.003(2) 0.008(2) 0.005(2) C26 0.033(3) 0.024(3) 0.042(3) -0.008(2) -0.002(2) 0.002(2) C35 0.024(3) 0.028(3) 0.034(3) 0.000(2) -0.004(2) -0.002(2) C6 0.036(3) 0.027(3) 0.029(3) 0.001(2) 0.002(2) 0.000(2) C15 0.023(3) 0.015(2) 0.031(3) 0.001(2) 0.007(2) 0.000(2) C25 0.031(3) 0.014(2) 0.051(3) 0.001(2) -0.012(3) 0.003(2) C24 0.028(3) 0.020(3) 0.049(3) 0.006(2) 0.001(2) 0.000(2) C31 0.027(3) 0.023(3) 0.033(3) -0.001(2) 0.005(2) -0.005(2) C9 0.024(3) 0.032(3) 0.029(3) -0.007(2) -0.001(2) 0.002(2) C22 0.018(3) 0.015(2) 0.036(3) 0.003(2) -0.003(2) 0.0021(19) C16 0.026(3) 0.023(3) 0.042(3) -0.003(2) 0.002(2) -0.001(2) C5 0.023(3) 0.018(2) 0.033(3) 0.002(2) -0.007(2) -0.003(2) C19 0.054(4) 0.028(3) 0.030(3) 0.005(2) 0.015(3) 0.007(3) C8 0.024(3) 0.019(3) 0.039(3) 0.004(2) -0.004(2) -0.003(2) C18 0.049(4) 0.017(3) 0.049(4) -0.002(2) 0.025(3) -0.007(3) C29 0.023(3) 0.036(3) 0.034(3) 0.003(2) -0.004(2) -0.007(2) C23 0.027(3) 0.017(2) 0.040(3) 0.003(2) 0.004(2) 0.002(2) C33 0.024(3) 0.029(3) 0.048(3) -0.002(3) 0.003(3) -0.006(2) C11 0.031(3) 0.027(3) 0.066(4) -0.005(3) -0.017(3) -0.006(2) C4 0.032(3) 0.023(3) 0.035(3) 0.001(2) 0.002(2) 0.000(2) C20 0.032(3) 0.029(3) 0.026(3) 0.001(2) 0.005(2) 0.005(2) C10 0.033(3) 0.026(3) 0.037(3) -0.004(2) -0.002(2) -0.002(2) C17 0.029(3) 0.030(3) 0.057(4) -0.005(3) 0.018(3) -0.007(2) C13 0.036(4) 0.023(3) 0.117(6) -0.027(3) -0.031(4) 0.011(3) N11 0.028(2) 0.030(2) 0.029(2) 0.0020(19) -0.0027(19) -0.007(2) N9 0.039(3) 0.032(2) 0.030(2) 0.007(2) 0.004(2) -0.003(2) N8 0.037(3) 0.036(3) 0.031(2) -0.006(2) -0.001(2) 0.005(2) N12 0.030(3) 0.030(2) 0.044(3) -0.003(2) 0.009(2) -0.005(2) F1 0.146(5) 0.065(3) 0.085(3) 0.030(2) 0.018(3) 0.022(3) F3 0.144(5) 0.076(3) 0.138(5) -0.033(3) -0.088(4) 0.017(3) C38 0.040(3) 0.044(3) 0.048(4) 0.013(3) -0.011(3) -0.022(3) C7 0.051(4) 0.026(3) 0.043(3) -0.006(3) -0.001(3) 0.000(3) C2 0.049(4) 0.019(3) 0.060(4) -0.001(3) -0.003(3) -0.009(3) N10 0.035(3) 0.055(3) 0.066(4) 0.033(3) -0.019(3) -0.006(2) N7 0.033(3) 0.038(3) 0.118(5) -0.036(3) 0.029(3) -0.005(2) C3 0.033(3) 0.027(3) 0.052(4) 0.011(3) 0.008(3) -0.002(2) C14 0.034(4) 0.040(4) 0.104(6) -0.019(4) -0.022(4) 0.000(3) C28 0.048(4) 0.021(3) 0.070(4) -0.003(3) -0.013(3) -0.004(3) C40 0.035(4) 0.054(4) 0.077(5) -0.010(4) 0.008(3) -0.025(3) B1 0.065(6) 0.051(5) 0.066(6) 0.002(4) -0.018(5) -0.014(4) F2 0.097(4) 0.081(3) 0.126(4) 0.024(3) -0.061(3) -0.024(3) F4 0.107(4) 0.103(4) 0.158(6) 0.011(4) 0.035(4) -0.021(3) C21 0.073(5) 0.047(4) 0.069(5) 0.000(3) 0.045(4) -0.015(4) C12 0.034(4) 0.040(4) 0.156(8) -0.036(4) -0.041(4) 0.021(3) F8 0.109(5) 0.226(9) 0.171(7) -0.106(6) -0.001(5) 0.014(6) C1 0.075(5) 0.027(3) 0.107(6) -0.004(4) 0.005(5) -0.026(3) C36 0.074(5) 0.064(4) 0.044(4) -0.019(3) 0.002(4) 0.024(4) C32 0.079(5) 0.051(4) 0.045(4) 0.028(3) -0.001(4) 0.004(4) F5 0.260(10) 0.124(6) 0.384(14) 0.110(8) -0.207(10) -0.087(7) C34 0.062(6) 0.079(6) 0.248(13) -0.088(8) 0.073(7) -0.011(5) C30 0.074(6) 0.117(8) 0.155(9) 0.088(7) -0.066(6) -0.012(5) B2 0.075(8) 0.025(5) 0.29(2) 0.027(8) -0.031(11) -0.031(5) F7 0.096(4) 0.116(5) 0.175(6) -0.057(4) -0.044(4) 0.016(4) F6 0.230(8) 0.139(6) 0.206(7) 0.111(5) 0.145(6) 0.121(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C29 1.939(5) . ? Rh1 C35 1.949(5) . ? Rh1 N3 2.068(4) . ? Rh1 N6 2.077(4) . ? Rh1 C37 2.097(5) . ? Rh1 Rh2 2.5861(6) . ? Rh2 C33 1.945(6) . ? Rh2 C31 1.948(5) . ? Rh2 N4 2.088(4) . ? Rh2 N1 2.091(4) . ? Rh2 C39 2.095(6) . ? N5 N6 1.291(5) . ? N5 N4 1.297(5) . ? N4 C22 1.439(6) . ? N2 N3 1.292(5) . ? N2 N1 1.299(5) . ? N3 C5 1.450(6) . ? N6 C15 1.445(6) . ? N1 C8 1.434(6) . ? C37 N11 1.127(6) . ? C27 C22 1.391(7) . ? C27 C26 1.395(7) . ? C39 N12 1.146(6) . ? C26 C25 1.391(7) . ? C35 N8 1.147(6) . ? C6 C5 1.381(7) . ? C6 C7 1.383(7) . ? C15 C20 1.378(7) . ? C15 C16 1.381(7) . ? C25 C24 1.383(7) . ? C25 C28 1.511(7) . ? C24 C23 1.388(7) . ? C31 N9 1.141(6) . ? C9 C8 1.385(7) . ? C9 C10 1.388(7) . ? C22 C23 1.395(7) . ? C16 C17 1.385(7) . ? C5 C4 1.380(7) . ? C19 C20 1.387(7) . ? C19 C18 1.388(8) . ? C8 C13 1.369(7) . ? C18 C17 1.382(8) . ? C18 C21 1.509(7) . ? C29 N10 1.131(6) . ? C33 N7 1.136(7) . ? C11 C10 1.368(7) . ? C11 C12 1.398(8) . ? C11 C14 1.507(7) . ? C4 C3 1.393(7) . ? C13 C12 1.383(8) . ? N11 C38 1.435(6) . ? N9 C32 1.442(7) . ? N8 C36 1.444(7) . ? N12 C40 1.436(7) . ? F1 B1 1.365(9) . ? F3 B1 1.361(9) . ? C7 C2 1.389(8) . ? C2 C3 1.385(8) . ? C2 C1 1.513(7) . ? N10 C30 1.437(8) . ? N7 C34 1.435(8) . ? B1 F2 1.363(9) . ? B1 F4 1.366(11) . ? F8 B2 1.423(17) . ? F5 B2 1.300(15) . ? B2 F7 1.313(15) . ? B2 F6 1.319(16) . ? 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 C35 91.3(2) . . ? C29 Rh1 N3 177.37(19) . . ? C35 Rh1 N3 90.74(18) . . ? C29 Rh1 N6 89.79(19) . . ? C35 Rh1 N6 175.06(18) . . ? N3 Rh1 N6 88.06(15) . . ? C29 Rh1 C37 90.77(19) . . ? C35 Rh1 C37 88.5(2) . . ? N3 Rh1 C37 90.97(16) . . ? N6 Rh1 C37 96.28(17) . . ? C29 Rh1 Rh2 93.72(15) . . ? C35 Rh1 Rh2 93.51(15) . . ? N3 Rh1 Rh2 84.46(11) . . ? N6 Rh1 Rh2 81.60(11) . . ? C37 Rh1 Rh2 175.02(13) . . ? C33 Rh2 C31 91.8(2) . . ? C33 Rh2 N4 177.06(19) . . ? C31 Rh2 N4 90.93(18) . . ? C33 Rh2 N1 88.3(2) . . ? C31 Rh2 N1 176.10(18) . . ? N4 Rh2 N1 88.96(15) . . ? C33 Rh2 C39 86.0(2) . . ? C31 Rh2 C39 91.8(2) . . ? N4 Rh2 C39 95.07(17) . . ? N1 Rh2 C39 92.12(17) . . ? C33 Rh2 Rh1 93.88(15) . . ? C31 Rh2 Rh1 94.61(14) . . ? N4 Rh2 Rh1 84.73(11) . . ? N1 Rh2 Rh1 81.50(10) . . ? C39 Rh2 Rh1 173.63(14) . . ? N6 N5 N4 117.1(4) . . ? N5 N4 C22 111.8(4) . . ? N5 N4 Rh2 121.0(3) . . ? C22 N4 Rh2 124.9(3) . . ? N3 N2 N1 115.1(4) . . ? N2 N3 C5 114.7(4) . . ? N2 N3 Rh1 124.9(3) . . ? C5 N3 Rh1 120.0(3) . . ? N5 N6 C15 110.7(4) . . ? N5 N6 Rh1 126.7(3) . . ? C15 N6 Rh1 122.6(3) . . ? N2 N1 C8 112.7(4) . . ? N2 N1 Rh2 125.9(3) . . ? C8 N1 Rh2 117.2(3) . . ? N11 C37 Rh1 175.1(4) . . ? C22 C27 C26 119.8(5) . . ? N12 C39 Rh2 174.2(4) . . ? C25 C26 C27 121.5(5) . . ? N8 C35 Rh1 176.0(5) . . ? C5 C6 C7 119.8(5) . . ? C20 C15 C16 120.2(5) . . ? C20 C15 N6 118.8(4) . . ? C16 C15 N6 121.0(5) . . ? C24 C25 C26 117.7(5) . . ? C24 C25 C28 121.5(5) . . ? C26 C25 C28 120.8(5) . . ? C25 C24 C23 122.0(5) . . ? N9 C31 Rh2 175.9(5) . . ? C8 C9 C10 119.4(5) . . ? C27 C22 C23 119.1(4) . . ? C27 C22 N4 121.5(4) . . ? C23 C22 N4 119.4(4) . . ? C15 C16 C17 119.3(5) . . ? C4 C5 C6 119.7(4) . . ? C4 C5 N3 120.7(4) . . ? C6 C5 N3 119.3(4) . . ? C20 C19 C18 121.2(5) . . ? C13 C8 C9 119.7(5) . . ? C13 C8 N1 121.1(5) . . ? C9 C8 N1 118.8(4) . . ? C17 C18 C19 117.8(5) . . ? C17 C18 C21 121.6(6) . . ? C19 C18 C21 120.6(6) . . ? N10 C29 Rh1 175.0(5) . . ? C24 C23 C22 119.8(5) . . ? N7 C33 Rh2 172.7(5) . . ? C10 C11 C12 118.0(5) . . ? C10 C11 C14 121.5(5) . . ? C12 C11 C14 120.5(5) . . ? C5 C4 C3 120.1(5) . . ? C15 C20 C19 119.7(5) . . ? C11 C10 C9 121.8(5) . . ? C18 C17 C16 121.8(5) . . ? C8 C13 C12 120.4(5) . . ? C37 N11 C38 176.5(5) . . ? C31 N9 C32 177.6(6) . . ? C35 N8 C36 178.0(6) . . ? C39 N12 C40 176.4(5) . . ? C6 C7 C2 121.4(5) . . ? C3 C2 C7 118.1(5) . . ? C3 C2 C1 121.3(6) . . ? C7 C2 C1 120.6(6) . . ? C29 N10 C30 175.6(7) . . ? C33 N7 C34 175.7(7) . . ? C2 C3 C4 120.8(5) . . ? F3 B1 F2 108.1(7) . . ? F3 B1 F1 113.2(7) . . ? F2 B1 F1 110.3(7) . . ? F3 B1 F4 108.3(7) . . ? F2 B1 F4 107.8(7) . . ? F1 B1 F4 108.9(7) . . ? C13 C12 C11 120.7(6) . . ? F5 B2 F7 115.7(9) . . ? F5 B2 F6 113.7(12) . . ? F7 B2 F6 114.3(16) . . ? F5 B2 F8 97.8(16) . . ? F7 B2 F8 106.1(10) . . ? F6 B2 F8 107.3(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.076 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 932780' ####################################################################### # # 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_e:\yong032\1 #TrackingRef 'compound8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H92 B4 F16 N12 P4 Rh4' _chemical_formula_weight 2296.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 ? _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 22.272(4) _cell_length_b 22.161(4) _cell_length_c 22.409(4) _cell_angle_alpha 90.00 _cell_angle_beta 119.43(3) _cell_angle_gamma 90.00 _cell_volume 9633(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8794 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details 'SADABS, v2.03, (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 107654 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.32 _reflns_number_total 21603 _reflns_number_gt 16962 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^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 21603 _refine_ls_number_parameters 1256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.189430(10) 0.374415(9) 0.265239(10) 0.01476(5) Uani 1 1 d . . . Rh2 Rh 0.296895(10) 0.368280(9) 0.236671(10) 0.01565(6) Uani 1 1 d . . . P2 P 0.22186(3) 0.42286(3) 0.14110(3) 0.01742(14) Uani 1 1 d . . . P1 P 0.26200(3) 0.44096(3) 0.34750(3) 0.01866(15) Uani 1 1 d . . . Rh3 Rh 0.300335(10) 0.591123(9) 0.815492(10) 0.01398(5) Uani 1 1 d . . . Rh4 Rh 0.197885(10) 0.591155(9) 0.679580(10) 0.01382(5) Uani 1 1 d . . . P4 P 0.27364(3) 0.65296(3) 0.66590(3) 0.01463(13) Uani 1 1 d . . . P3 P 0.22502(3) 0.65290(3) 0.82973(3) 0.01456(13) Uani 1 1 d . . . C50 C 0.10387(13) 0.70281(12) 0.63171(13) 0.0178(5) Uani 1 1 d . . . H50 H 0.0916 0.6878 0.5874 0.021 Uiso 1 1 calc R . . C49 C 0.15346(13) 0.67110(11) 0.68975(13) 0.0151(5) Uani 1 1 d . . . C84 C 0.33102(13) 0.61624(11) 0.63931(13) 0.0170(5) Uani 1 1 d . . . C69 C 0.42780(14) 0.75323(12) 0.85865(14) 0.0222(6) Uani 1 1 d . . . H69 H 0.4611 0.7728 0.8992 0.027 Uiso 1 1 calc R . . C72 C 0.33100(12) 0.69508(11) 0.74156(13) 0.0157(5) Uani 1 1 d . . . C71 C 0.36464(13) 0.74698(11) 0.73691(13) 0.0184(5) Uani 1 1 d . . . H71 H 0.3545 0.7618 0.6931 0.022 Uiso 1 1 calc R . . C57 C 0.05947(14) 0.60522(13) 0.85499(14) 0.0235(6) Uani 1 1 d . . . H57 H 0.0127 0.6171 0.8368 0.028 Uiso 1 1 calc R . . C70 C 0.41228(13) 0.77670(12) 0.79520(14) 0.0198(6) Uani 1 1 d . . . H70 H 0.4340 0.8125 0.7920 0.024 Uiso 1 1 calc R . . C54 C 0.16729(12) 0.69482(11) 0.75371(13) 0.0154(5) Uani 1 1 d . . . C60 C 0.19507(14) 0.57036(12) 0.90692(14) 0.0211(6) Uani 1 1 d . . . H60 H 0.2414 0.5576 0.9245 0.025 Uiso 1 1 calc R . . C56 C 0.10033(13) 0.63317(12) 0.83199(13) 0.0201(6) Uani 1 1 d . . . H56 H 0.0813 0.6642 0.7985 0.024 Uiso 1 1 calc R . . C79 C 0.40051(14) 0.63153(12) 0.66845(14) 0.0206(6) Uani 1 1 d . . . H79 H 0.4192 0.6614 0.7033 0.025 Uiso 1 1 calc R . . C52 C 0.08766(13) 0.77772(12) 0.70005(14) 0.0206(6) Uani 1 1 d . . . H52 H 0.0664 0.8138 0.7033 0.025 Uiso 1 1 calc R . . C73 C 0.22900(13) 0.70944(12) 0.59905(13) 0.0186(5) Uani 1 1 d . . . C82 C 0.34744(15) 0.54480(13) 0.56654(14) 0.0271(6) Uani 1 1 d . . . H82 H 0.3289 0.5154 0.5312 0.032 Uiso 1 1 calc R . . C55 C 0.16888(13) 0.61612(11) 0.85757(13) 0.0166(5) Uani 1 1 d . . . C67 C 0.34536(12) 0.67109(11) 0.80583(13) 0.0153(5) Uani 1 1 d . . . C58 C 0.08621(15) 0.56048(13) 0.90395(14) 0.0259(6) Uani 1 1 d . . . H58 H 0.0580 0.5415 0.9194 0.031 Uiso 1 1 calc R . . C81 C 0.41659(15) 0.56015(13) 0.59661(15) 0.0257(6) Uani 1 1 d . . . H81 H 0.4457 0.5410 0.5825 0.031 Uiso 1 1 calc R . . C51 C 0.07255(13) 0.75496(12) 0.63700(14) 0.0209(6) Uani 1 1 d . . . H51 H 0.0402 0.7753 0.5966 0.025 Uiso 1 1 calc R . . C53 C 0.13429(13) 0.74719(12) 0.75862(13) 0.0185(5) Uani 1 1 d . . . H53 H 0.1440 0.7617 0.8024 0.022 Uiso 1 1 calc R . . C75 C 0.17811(14) 0.80831(13) 0.56397(16) 0.0284(7) Uani 1 1 d . . . H75 H 0.1697 0.8475 0.5755 0.034 Uiso 1 1 calc R . . C68 C 0.39560(13) 0.70193(12) 0.86357(13) 0.0195(6) Uani 1 1 d . . . H68 H 0.4079 0.6868 0.9078 0.023 Uiso 1 1 calc R . . C80 C 0.44267(14) 0.60377(13) 0.64743(14) 0.0235(6) Uani 1 1 d . . . H80 H 0.4899 0.6147 0.6681 0.028 Uiso 1 1 calc R . . C78 C 0.20208(14) 0.69473(13) 0.52983(14) 0.0234(6) Uani 1 1 d . . . H78 H 0.2101 0.6557 0.5176 0.028 Uiso 1 1 calc R . . C77 C 0.16395(15) 0.73620(14) 0.47909(15) 0.0289(7) Uani 1 1 d . . . H77 H 0.1455 0.7255 0.4323 0.035 Uiso 1 1 calc R . . C74 C 0.21625(13) 0.76698(12) 0.61588(14) 0.0227(6) Uani 1 1 d . . . H74 H 0.2335 0.7779 0.6625 0.027 Uiso 1 1 calc R . . C76 C 0.15261(15) 0.79310(14) 0.49637(16) 0.0308(7) Uani 1 1 d . . . H76 H 0.1271 0.8218 0.4615 0.037 Uiso 1 1 calc R . . F5 F 0.35488(9) 0.36794(8) 0.02205(9) 0.0367(4) Uani 1 1 d . . . F7 F 0.45465(9) 0.42235(8) 0.06729(9) 0.0369(4) Uani 1 1 d . . . F6 F 0.37750(9) 0.42819(9) -0.04677(9) 0.0405(5) Uani 1 1 d . . . F8 F 0.43945(9) 0.34229(8) -0.00235(9) 0.0356(4) Uani 1 1 d . . . B2 B 0.40695(18) 0.38999(16) 0.01041(17) 0.0277(7) Uani 1 1 d . . . F13 F 0.02478(10) 0.36250(8) 0.76862(9) 0.0380(4) Uani 1 1 d . . . F14 F 0.04978(10) 0.35394(9) 0.68230(10) 0.0433(5) Uani 1 1 d . . . F15 F 0.09809(11) 0.29038(9) 0.77220(10) 0.0500(5) Uani 1 1 d . . . F16 F -0.01533(11) 0.28272(10) 0.69554(11) 0.0590(6) Uani 1 1 d . . . B4 B 0.03924(18) 0.32155(15) 0.72979(17) 0.0257(7) Uani 1 1 d . . . F9 F 0.07491(10) 0.34179(9) 0.50466(10) 0.0445(5) Uani 1 1 d . . . F12 F 0.16307(10) 0.36779(9) 0.48717(11) 0.0482(5) Uani 1 1 d . . . F10 F 0.06467(10) 0.42377(8) 0.44064(9) 0.0434(5) Uani 1 1 d . . . F11 F 0.13628(10) 0.42578(10) 0.55464(10) 0.0534(6) Uani 1 1 d . . . B3 B 0.10996(19) 0.38984(16) 0.49722(18) 0.0305(8) Uani 1 1 d . . . F4 F 0.49055(12) 0.73740(11) 0.19286(11) 0.0670(7) Uani 1 1 d . A . F2 F 0.53946(15) 0.66034(14) 0.16604(13) 0.0977(10) Uani 1 1 d . A . B1 B 0.5263(3) 0.6844(2) 0.2145(2) 0.0460(11) Uani 1 1 d . . . N8 N 0.41294(11) 0.52756(10) 0.79156(11) 0.0203(5) Uani 1 1 d . . . N9 N 0.08548(11) 0.52894(10) 0.70477(11) 0.0193(5) Uani 1 1 d . . . N12 N 0.07953(11) 0.57611(10) 0.52550(11) 0.0209(5) Uani 1 1 d . . . C87 C 0.24240(13) 0.51402(12) 0.67281(13) 0.0185(5) Uani 1 1 d . . . N10 N 0.26797(11) 0.47193(10) 0.66586(11) 0.0211(5) Uani 1 1 d . . . C95 C 0.37117(14) 0.58400(12) 0.91660(14) 0.0195(6) Uani 1 1 d . . . N7 N 0.23125(12) 0.47034(10) 0.82632(12) 0.0258(5) Uani 1 1 d . . . C89 C 0.12980(13) 0.54976(11) 0.69971(13) 0.0177(5) Uani 1 1 d . . . C85 C 0.36887(13) 0.54938(11) 0.79620(12) 0.0173(5) Uani 1 1 d . . . C93 C 0.12464(13) 0.58391(11) 0.57889(13) 0.0184(5) Uani 1 1 d . . . N11 N 0.41369(12) 0.57602(10) 0.97155(12) 0.0224(5) Uani 1 1 d . . . C91 C 0.25620(13) 0.51364(12) 0.82088(13) 0.0197(6) Uani 1 1 d . . . C61 C 0.27010(13) 0.70886(11) 0.89771(13) 0.0166(5) Uani 1 1 d . . . N5 N 0.08149(11) 0.35371(10) 0.31581(11) 0.0210(5) Uani 1 1 d . . . N2 N 0.40921(11) 0.30894(10) 0.37345(11) 0.0228(5) Uani 1 1 d . . . N3 N 0.08544(11) 0.30113(10) 0.13430(11) 0.0219(5) Uani 1 1 d . . . C45 C 0.11931(13) 0.36838(12) 0.29757(13) 0.0183(5) Uani 1 1 d . . . C37 C 0.12549(13) 0.32645(11) 0.18196(13) 0.0177(5) Uani 1 1 d . . . N6 N 0.40367(11) 0.33950(10) 0.18567(11) 0.0226(5) Uani 1 1 d . . . C43 C 0.36546(13) 0.33089(12) 0.32627(13) 0.0186(5) Uani 1 1 d . . . N1 N 0.25791(12) 0.26127(10) 0.35886(12) 0.0240(5) Uani 1 1 d . . . C19 C 0.33905(13) 0.45114(12) 0.28285(13) 0.0194(6) Uani 1 1 d . . . C46 C 0.03564(14) 0.32568(13) 0.33549(14) 0.0250(6) Uani 1 1 d . . . H46A H 0.0130 0.2910 0.3056 0.037 Uiso 1 1 calc R . . H46B H 0.0007 0.3549 0.3312 0.037 Uiso 1 1 calc R . . H46C H 0.0620 0.3120 0.3831 0.037 Uiso 1 1 calc R . . C41 C 0.23361(13) 0.30174(12) 0.32338(13) 0.0188(5) Uani 1 1 d . . . C7 C 0.26569(13) 0.48102(12) 0.11891(14) 0.0209(6) Uani 1 1 d . . . C13 C 0.17816(13) 0.37883(12) 0.06153(14) 0.0202(6) Uani 1 1 d . . . C24 C 0.32018(13) 0.48010(12) 0.32622(14) 0.0224(6) Uani 1 1 d . . . C94 C 0.01955(14) 0.56521(15) 0.45937(14) 0.0316(7) Uani 1 1 d . . . H94A H 0.0227 0.5249 0.4432 0.047 Uiso 1 1 calc R . . H94B H 0.0175 0.5955 0.4266 0.047 Uiso 1 1 calc R . . H94C H -0.0222 0.5679 0.4635 0.047 Uiso 1 1 calc R . . C66 C 0.29690(13) 0.69204(12) 0.96602(13) 0.0213(6) Uani 1 1 d . . . H66 H 0.2884 0.6525 0.9766 0.026 Uiso 1 1 calc R . . C86 C 0.46885(14) 0.50059(14) 0.78632(15) 0.0283(7) Uani 1 1 d . . . H86A H 0.5128 0.5155 0.8236 0.042 Uiso 1 1 calc R . . H86B H 0.4651 0.5113 0.7422 0.042 Uiso 1 1 calc R . . H86C H 0.4668 0.4566 0.7896 0.042 Uiso 1 1 calc R . . C47 C 0.36614(13) 0.35451(12) 0.20354(13) 0.0202(6) Uani 1 1 d . . . C20 C 0.39031(13) 0.47952(12) 0.27371(14) 0.0235(6) Uani 1 1 d . . . H20 H 0.4069 0.4598 0.2470 0.028 Uiso 1 1 calc R . . C83 C 0.30513(14) 0.57225(12) 0.58787(14) 0.0227(6) Uani 1 1 d . . . H83 H 0.2580 0.5610 0.5672 0.027 Uiso 1 1 calc R . . N4 N 0.23517(11) 0.23679(10) 0.19223(12) 0.0233(5) Uani 1 1 d . . . C1 C 0.14333(13) 0.44835(11) 0.20196(13) 0.0173(5) Uani 1 1 d . . . C62 C 0.28256(14) 0.76685(12) 0.88327(14) 0.0227(6) Uani 1 1 d . . . H62 H 0.2653 0.7790 0.8370 0.027 Uiso 1 1 calc R . . C88 C 0.30310(16) 0.42339(13) 0.65338(17) 0.0314(7) Uani 1 1 d . . . H88A H 0.2704 0.4013 0.6122 0.047 Uiso 1 1 calc R . . H88B H 0.3227 0.3960 0.6928 0.047 Uiso 1 1 calc R . . H88C H 0.3402 0.4398 0.6466 0.047 Uiso 1 1 calc R . . C31 C 0.19333(13) 0.49095(13) 0.41276(14) 0.0226(6) Uani 1 1 d . . . H31 H 0.2048 0.4545 0.4384 0.027 Uiso 1 1 calc R . . C8 C 0.29449(14) 0.46715(13) 0.07801(14) 0.0248(6) Uani 1 1 d . . . H8 H 0.2884 0.4280 0.0586 0.030 Uiso 1 1 calc R . . C36 C 0.21619(13) 0.50029(12) 0.36602(13) 0.0206(6) Uani 1 1 d . . . C64 C 0.34649(14) 0.79002(13) 1.00362(15) 0.0284(7) Uani 1 1 d . . . H64 H 0.3718 0.8180 1.0395 0.034 Uiso 1 1 calc R . . C25 C 0.31812(14) 0.40871(13) 0.43233(14) 0.0259(7) Uani 1 1 d . . . C17 C 0.08761(16) 0.36552(14) -0.05509(15) 0.0338(7) Uani 1 1 d . . . H17 H 0.0451 0.3785 -0.0925 0.041 Uiso 1 1 calc R . . C39 C 0.25616(13) 0.28518(13) 0.20352(13) 0.0210(6) Uani 1 1 d . . . C6 C 0.15646(13) 0.46485(12) 0.14884(13) 0.0196(6) Uani 1 1 d . . . C90 C 0.02903(14) 0.50413(13) 0.71121(15) 0.0252(6) Uani 1 1 d . . . H90A H 0.0344 0.5151 0.7560 0.038 Uiso 1 1 calc R . . H90B H 0.0290 0.4601 0.7073 0.038 Uiso 1 1 calc R . . H90C H -0.0146 0.5204 0.6748 0.038 Uiso 1 1 calc R . . C2 C 0.09308(13) 0.48289(12) 0.20769(14) 0.0197(6) Uani 1 1 d . . . H2 H 0.0816 0.4726 0.2420 0.024 Uiso 1 1 calc R . . C38 C 0.03635(16) 0.26799(14) 0.07531(15) 0.0351(8) Uani 1 1 d . . . H38A H 0.0603 0.2472 0.0544 0.053 Uiso 1 1 calc R . . H38B H 0.0022 0.2959 0.0420 0.053 Uiso 1 1 calc R . . H38C H 0.0131 0.2382 0.0893 0.053 Uiso 1 1 calc R . . C35 C 0.19782(14) 0.55401(12) 0.32829(15) 0.0263(6) Uani 1 1 d . . . H35 H 0.2126 0.5613 0.2957 0.032 Uiso 1 1 calc R . . C63 C 0.32016(15) 0.80710(13) 0.93599(15) 0.0288(7) Uani 1 1 d . . . H63 H 0.3279 0.8469 0.9255 0.035 Uiso 1 1 calc R . . C18 C 0.11499(14) 0.39606(13) 0.00658(14) 0.0262(6) Uani 1 1 d . . . H18 H 0.0905 0.4290 0.0115 0.031 Uiso 1 1 calc R . . C16 C 0.12112(15) 0.31652(14) -0.06295(15) 0.0303(7) Uani 1 1 d . . . H16 H 0.1023 0.2962 -0.1057 0.036 Uiso 1 1 calc R . . C3 C 0.05991(14) 0.53156(13) 0.16452(14) 0.0247(6) Uani 1 1 d . . . H3 H 0.0272 0.5544 0.1706 0.030 Uiso 1 1 calc R . . C12 C 0.27517(14) 0.53875(13) 0.14765(15) 0.0259(6) Uani 1 1 d . . . H12 H 0.2558 0.5487 0.1759 0.031 Uiso 1 1 calc R . . C5 C 0.12193(14) 0.51346(12) 0.10482(14) 0.0236(6) Uani 1 1 d . . . H5 H 0.1316 0.5234 0.0692 0.028 Uiso 1 1 calc R . . C48 C 0.45099(15) 0.31565(14) 0.16594(15) 0.0306(7) Uani 1 1 d . . . H48A H 0.4790 0.2841 0.1983 0.046 Uiso 1 1 calc R . . H48B H 0.4811 0.3480 0.1662 0.046 Uiso 1 1 calc R . . H48C H 0.4253 0.2985 0.1198 0.046 Uiso 1 1 calc R . . C4 C 0.07417(14) 0.54676(12) 0.11304(14) 0.0249(6) Uani 1 1 d . . . H4 H 0.0513 0.5798 0.0836 0.030 Uiso 1 1 calc R . . C14 C 0.21076(15) 0.32853(13) 0.05313(14) 0.0279(7) Uani 1 1 d . . . H14 H 0.2534 0.3155 0.0903 0.034 Uiso 1 1 calc R . . C59 C 0.15454(15) 0.54336(13) 0.93055(14) 0.0264(6) Uani 1 1 d . . . H59 H 0.1736 0.5131 0.9650 0.032 Uiso 1 1 calc R . . C96 C 0.47055(14) 0.56636(16) 1.03932(14) 0.0338(8) Uani 1 1 d . . . H96A H 0.5137 0.5657 1.0377 0.051 Uiso 1 1 calc R . . H96B H 0.4646 0.5277 1.0570 0.051 Uiso 1 1 calc R . . H96C H 0.4722 0.5991 1.0695 0.051 Uiso 1 1 calc R . . C65 C 0.33564(14) 0.73180(14) 1.01864(14) 0.0274(6) Uani 1 1 d . . . H65 H 0.3547 0.7192 1.0650 0.033 Uiso 1 1 calc R . . C30 C 0.29085(17) 0.37017(13) 0.46246(15) 0.0312(7) Uani 1 1 d . . . H30 H 0.2435 0.3592 0.4378 0.037 Uiso 1 1 calc R . . C9 C 0.33236(14) 0.51032(14) 0.06526(15) 0.0303(7) Uani 1 1 d . . . H9 H 0.3519 0.5007 0.0371 0.036 Uiso 1 1 calc R . . C34 C 0.15796(15) 0.59657(13) 0.33846(16) 0.0309(7) Uani 1 1 d . . . H34 H 0.1457 0.6329 0.3127 0.037 Uiso 1 1 calc R . . C11 C 0.31311(15) 0.58125(14) 0.13460(16) 0.0319(7) Uani 1 1 d . . . H11 H 0.3196 0.6204 0.1541 0.038 Uiso 1 1 calc R . . C10 C 0.34139(15) 0.56740(14) 0.09377(16) 0.0329(7) Uani 1 1 d . . . H10 H 0.3671 0.5969 0.0851 0.039 Uiso 1 1 calc R . . C33 C 0.13604(14) 0.58677(13) 0.38523(16) 0.0302(7) Uani 1 1 d . . . H33 H 0.1087 0.6162 0.3917 0.036 Uiso 1 1 calc R . . C32 C 0.15379(14) 0.53431(13) 0.42260(15) 0.0286(7) Uani 1 1 d . . . H32 H 0.1390 0.5276 0.4553 0.034 Uiso 1 1 calc R . . C15 C 0.18229(15) 0.29720(14) -0.00816(15) 0.0313(7) Uani 1 1 d . . . H15 H 0.2048 0.2624 -0.0125 0.038 Uiso 1 1 calc R . . C21 C 0.41763(14) 0.53523(13) 0.30231(16) 0.0309(7) Uani 1 1 d . . . H21 H 0.4517 0.5533 0.2943 0.037 Uiso 1 1 calc R . . C44 C 0.46686(15) 0.28077(15) 0.43092(16) 0.0372(8) Uani 1 1 d . . . H44A H 0.4986 0.2646 0.4164 0.056 Uiso 1 1 calc R . . H44B H 0.4503 0.2479 0.4483 0.056 Uiso 1 1 calc R . . H44C H 0.4910 0.3107 0.4672 0.056 Uiso 1 1 calc R . . C23 C 0.34840(15) 0.53614(13) 0.35585(16) 0.0332(7) Uani 1 1 d . . . H23 H 0.3349 0.5549 0.3856 0.040 Uiso 1 1 calc R . . C40 C 0.20017(16) 0.18002(13) 0.18202(18) 0.0388(8) Uani 1 1 d . . . H40A H 0.1625 0.1845 0.1924 0.058 Uiso 1 1 calc R . . H40B H 0.2328 0.1496 0.2124 0.058 Uiso 1 1 calc R . . H40C H 0.1814 0.1673 0.1343 0.058 Uiso 1 1 calc R . . C22 C 0.39559(15) 0.56426(14) 0.34212(17) 0.0346(7) Uani 1 1 d . . . H22 H 0.4126 0.6033 0.3600 0.042 Uiso 1 1 calc R . . C26 C 0.38797(16) 0.42249(15) 0.46896(16) 0.0390(8) Uani 1 1 d . . . H26 H 0.4077 0.4481 0.4492 0.047 Uiso 1 1 calc R . . C42 C 0.29424(17) 0.21544(14) 0.40854(16) 0.0395(8) Uani 1 1 d . . . H42A H 0.3144 0.1868 0.3900 0.059 Uiso 1 1 calc R . . H42B H 0.2622 0.1942 0.4194 0.059 Uiso 1 1 calc R . . H42C H 0.3310 0.2340 0.4502 0.059 Uiso 1 1 calc R . . C29 C 0.3324(2) 0.34778(16) 0.52810(16) 0.0461(9) Uani 1 1 d . . . H29 H 0.3131 0.3222 0.5484 0.055 Uiso 1 1 calc R . . C27 C 0.42895(19) 0.39926(19) 0.53389(19) 0.0577(12) Uani 1 1 d . . . H27 H 0.4767 0.4088 0.5581 0.069 Uiso 1 1 calc R . . C92 C 0.19653(19) 0.41928(15) 0.8353(2) 0.0558(11) Uani 1 1 d . . . H92A H 0.2239 0.4036 0.8820 0.084 Uiso 1 1 calc R . . H92B H 0.1910 0.3877 0.8024 0.084 Uiso 1 1 calc R . . H92C H 0.1511 0.4318 0.8277 0.084 Uiso 1 1 calc R . . C28 C 0.4013(2) 0.36247(19) 0.56386(18) 0.0599(13) Uani 1 1 d . . . H28 H 0.4297 0.3474 0.6089 0.072 Uiso 1 1 calc R . . F3 F 0.5950(5) 0.7014(6) 0.2657(8) 0.104(5) Uani 0.423(18) 1 d P A 1 F1 F 0.5126(7) 0.6415(3) 0.2548(6) 0.063(4) Uani 0.423(18) 1 d P A 1 F3' F 0.5720(6) 0.6859(5) 0.2743(3) 0.088(4) Uani 0.577(18) 1 d P A 2 F1' F 0.4724(7) 0.6471(4) 0.2024(10) 0.125(5) Uani 0.577(18) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01346(10) 0.01590(11) 0.01434(10) -0.00097(8) 0.00639(8) -0.00036(8) Rh2 0.01375(10) 0.01697(11) 0.01600(11) 0.00047(8) 0.00712(9) 0.00257(8) P2 0.0166(3) 0.0193(3) 0.0176(3) 0.0021(3) 0.0093(3) 0.0034(3) P1 0.0155(3) 0.0206(4) 0.0192(3) -0.0054(3) 0.0080(3) -0.0012(3) Rh3 0.01403(10) 0.01433(11) 0.01309(10) 0.00025(7) 0.00628(8) 0.00071(7) Rh4 0.01409(10) 0.01437(11) 0.01302(10) -0.00116(7) 0.00668(8) -0.00030(7) P4 0.0149(3) 0.0156(3) 0.0134(3) 0.0002(3) 0.0070(3) 0.0003(3) P3 0.0153(3) 0.0150(3) 0.0136(3) -0.0001(3) 0.0073(3) -0.0001(3) C50 0.0171(13) 0.0221(14) 0.0139(12) 0.0009(10) 0.0074(11) -0.0005(10) C49 0.0170(13) 0.0127(12) 0.0170(13) 0.0012(10) 0.0095(11) -0.0009(10) C84 0.0194(13) 0.0181(13) 0.0156(13) 0.0026(10) 0.0101(11) 0.0035(10) C69 0.0180(14) 0.0252(15) 0.0215(14) -0.0079(12) 0.0082(12) -0.0043(11) C72 0.0141(12) 0.0160(13) 0.0166(13) -0.0024(10) 0.0073(11) 0.0020(10) C71 0.0173(13) 0.0181(13) 0.0206(14) 0.0012(11) 0.0099(11) 0.0003(10) C57 0.0163(13) 0.0325(16) 0.0214(14) -0.0086(12) 0.0091(12) -0.0067(12) C70 0.0159(13) 0.0180(13) 0.0267(15) -0.0033(11) 0.0114(12) -0.0034(10) C54 0.0149(12) 0.0155(13) 0.0155(12) 0.0013(10) 0.0073(10) 0.0013(10) C60 0.0193(14) 0.0218(14) 0.0217(14) 0.0024(11) 0.0097(12) -0.0004(11) C56 0.0201(14) 0.0209(14) 0.0181(13) -0.0027(11) 0.0086(11) -0.0020(11) C79 0.0205(14) 0.0225(14) 0.0184(13) 0.0020(11) 0.0093(12) 0.0007(11) C52 0.0191(14) 0.0163(13) 0.0266(15) 0.0007(11) 0.0114(12) 0.0023(11) C73 0.0146(13) 0.0226(14) 0.0185(13) 0.0016(11) 0.0081(11) -0.0030(10) C82 0.0327(16) 0.0304(16) 0.0223(15) -0.0046(12) 0.0169(13) 0.0017(13) C55 0.0186(13) 0.0182(13) 0.0141(12) -0.0046(10) 0.0088(11) -0.0038(10) C67 0.0125(12) 0.0156(13) 0.0176(13) -0.0010(10) 0.0073(11) 0.0013(10) C58 0.0272(15) 0.0314(16) 0.0228(15) -0.0037(12) 0.0150(13) -0.0091(13) C81 0.0275(15) 0.0276(16) 0.0288(16) 0.0034(13) 0.0191(13) 0.0088(12) C51 0.0178(13) 0.0220(14) 0.0213(14) 0.0056(11) 0.0084(12) 0.0046(11) C53 0.0203(14) 0.0183(13) 0.0181(13) -0.0019(11) 0.0103(11) -0.0006(10) C75 0.0251(15) 0.0206(15) 0.0383(18) 0.0068(13) 0.0147(14) 0.0036(12) C68 0.0185(13) 0.0235(14) 0.0164(13) -0.0020(11) 0.0087(11) -0.0002(11) C80 0.0179(14) 0.0325(16) 0.0207(14) 0.0069(12) 0.0100(12) 0.0066(12) C78 0.0241(15) 0.0253(15) 0.0202(14) 0.0017(12) 0.0104(12) -0.0018(12) C77 0.0261(15) 0.0382(18) 0.0178(14) 0.0083(13) 0.0072(12) -0.0022(13) C74 0.0189(14) 0.0236(15) 0.0241(15) 0.0017(12) 0.0093(12) -0.0012(11) C76 0.0232(15) 0.0309(17) 0.0315(17) 0.0165(14) 0.0081(13) 0.0040(13) F5 0.0342(10) 0.0431(11) 0.0393(11) -0.0137(8) 0.0231(9) -0.0087(8) F7 0.0353(10) 0.0337(10) 0.0332(10) -0.0092(8) 0.0103(9) -0.0085(8) F6 0.0390(11) 0.0458(12) 0.0314(10) 0.0078(9) 0.0132(9) 0.0084(9) F8 0.0318(10) 0.0331(10) 0.0424(11) -0.0086(8) 0.0186(9) 0.0004(8) B2 0.0285(18) 0.0287(18) 0.0252(18) -0.0043(14) 0.0127(15) -0.0017(14) F13 0.0447(11) 0.0368(11) 0.0428(11) -0.0005(8) 0.0293(10) 0.0034(9) F14 0.0568(13) 0.0444(12) 0.0434(11) 0.0136(9) 0.0361(10) 0.0042(10) F15 0.0541(13) 0.0463(12) 0.0436(12) 0.0132(10) 0.0194(10) 0.0232(10) F16 0.0577(14) 0.0689(15) 0.0559(14) -0.0245(12) 0.0321(12) -0.0337(12) B4 0.0288(18) 0.0256(18) 0.0252(17) 0.0021(14) 0.0152(15) -0.0019(14) F9 0.0563(13) 0.0401(11) 0.0430(11) 0.0067(9) 0.0290(10) -0.0067(10) F12 0.0451(12) 0.0507(13) 0.0599(14) 0.0052(10) 0.0343(11) 0.0096(10) F10 0.0523(12) 0.0336(10) 0.0372(11) 0.0102(9) 0.0166(10) 0.0080(9) F11 0.0438(12) 0.0552(13) 0.0438(12) -0.0206(10) 0.0082(10) -0.0032(10) B3 0.036(2) 0.0296(19) 0.0255(18) 0.0004(15) 0.0148(16) 0.0013(15) F4 0.0744(16) 0.0794(17) 0.0422(13) 0.0004(12) 0.0248(12) 0.0357(14) F2 0.109(2) 0.132(3) 0.0650(17) -0.0185(17) 0.0527(17) 0.045(2) B1 0.065(3) 0.039(2) 0.053(3) -0.017(2) 0.043(3) -0.004(2) N8 0.0196(12) 0.0208(12) 0.0199(12) 0.0028(9) 0.0091(10) 0.0035(9) N9 0.0195(12) 0.0194(12) 0.0184(11) -0.0022(9) 0.0088(10) -0.0018(9) N12 0.0206(12) 0.0256(13) 0.0175(12) -0.0013(10) 0.0102(10) 0.0024(10) C87 0.0173(13) 0.0201(14) 0.0175(13) -0.0025(11) 0.0081(11) -0.0035(11) N10 0.0224(12) 0.0195(12) 0.0221(12) -0.0041(10) 0.0114(10) -0.0002(10) C95 0.0190(14) 0.0213(14) 0.0214(14) -0.0006(11) 0.0124(12) -0.0001(11) N7 0.0210(12) 0.0207(13) 0.0314(14) 0.0041(10) 0.0095(11) 0.0009(10) C89 0.0165(13) 0.0178(13) 0.0144(13) -0.0016(10) 0.0042(11) 0.0012(10) C85 0.0209(14) 0.0164(13) 0.0125(12) 0.0002(10) 0.0066(11) -0.0012(11) C93 0.0191(14) 0.0188(14) 0.0181(14) -0.0010(11) 0.0099(12) 0.0005(11) N11 0.0214(12) 0.0247(13) 0.0205(12) 0.0009(10) 0.0097(11) -0.0023(10) C91 0.0187(13) 0.0197(14) 0.0178(13) 0.0007(11) 0.0068(11) 0.0050(11) C61 0.0142(12) 0.0188(13) 0.0166(13) -0.0029(10) 0.0075(11) 0.0001(10) N5 0.0188(12) 0.0234(12) 0.0190(12) -0.0009(10) 0.0079(10) 0.0007(9) N2 0.0190(12) 0.0276(13) 0.0203(12) 0.0038(10) 0.0085(10) 0.0025(10) N3 0.0192(12) 0.0233(12) 0.0203(12) -0.0024(10) 0.0075(10) 0.0011(10) C45 0.0130(13) 0.0215(14) 0.0178(13) -0.0009(11) 0.0057(11) 0.0010(10) C37 0.0169(13) 0.0168(13) 0.0223(14) 0.0025(11) 0.0118(12) 0.0055(10) N6 0.0209(12) 0.0261(13) 0.0217(12) 0.0042(10) 0.0111(10) 0.0047(10) C43 0.0179(13) 0.0195(14) 0.0203(14) 0.0000(11) 0.0110(12) -0.0004(11) N1 0.0240(12) 0.0211(12) 0.0253(13) 0.0003(10) 0.0107(11) -0.0012(10) C19 0.0149(13) 0.0199(14) 0.0207(14) 0.0008(11) 0.0067(11) 0.0002(10) C46 0.0232(15) 0.0301(16) 0.0254(15) 0.0019(12) 0.0148(13) -0.0057(12) C41 0.0161(13) 0.0197(14) 0.0193(13) -0.0022(11) 0.0077(11) -0.0036(11) C7 0.0183(14) 0.0221(14) 0.0241(14) 0.0068(11) 0.0119(12) 0.0028(11) C13 0.0194(14) 0.0223(14) 0.0214(14) 0.0037(11) 0.0120(12) 0.0012(11) C24 0.0139(13) 0.0247(15) 0.0264(15) -0.0059(12) 0.0081(12) -0.0050(11) C94 0.0216(15) 0.050(2) 0.0171(14) -0.0062(14) 0.0047(12) 0.0015(14) C66 0.0239(14) 0.0225(14) 0.0184(13) -0.0009(11) 0.0110(12) -0.0002(11) C86 0.0278(16) 0.0347(17) 0.0273(16) 0.0046(13) 0.0173(14) 0.0121(13) C47 0.0175(13) 0.0211(14) 0.0203(14) 0.0036(11) 0.0079(12) 0.0025(11) C20 0.0155(13) 0.0248(15) 0.0298(16) 0.0004(12) 0.0108(12) 0.0016(11) C83 0.0213(14) 0.0255(15) 0.0207(14) -0.0027(12) 0.0099(12) -0.0022(11) N4 0.0230(12) 0.0200(13) 0.0266(13) -0.0051(10) 0.0120(11) 0.0018(10) C1 0.0171(13) 0.0120(12) 0.0202(13) -0.0024(10) 0.0072(11) -0.0003(10) C62 0.0235(14) 0.0220(14) 0.0224(14) -0.0028(11) 0.0110(12) -0.0027(11) C88 0.0360(18) 0.0224(15) 0.0423(19) -0.0052(13) 0.0241(16) 0.0062(13) C31 0.0183(14) 0.0273(15) 0.0207(14) -0.0046(12) 0.0083(12) 0.0020(11) C8 0.0242(15) 0.0282(16) 0.0232(15) 0.0039(12) 0.0125(13) 0.0035(12) C36 0.0165(13) 0.0208(14) 0.0208(14) -0.0081(11) 0.0063(11) -0.0024(11) C64 0.0222(15) 0.0306(16) 0.0302(16) -0.0134(13) 0.0111(13) -0.0046(12) C25 0.0215(15) 0.0282(16) 0.0190(14) -0.0098(12) 0.0029(12) 0.0085(12) C17 0.0298(17) 0.0337(18) 0.0221(16) -0.0002(13) 0.0007(13) 0.0031(14) C39 0.0157(13) 0.0266(15) 0.0199(14) 0.0006(12) 0.0083(11) 0.0076(11) C6 0.0159(13) 0.0198(14) 0.0238(14) 0.0001(11) 0.0104(12) 0.0011(10) C90 0.0221(15) 0.0302(16) 0.0292(16) -0.0045(13) 0.0171(13) -0.0079(12) C2 0.0173(13) 0.0200(14) 0.0246(14) -0.0010(11) 0.0125(12) -0.0002(11) C38 0.0344(18) 0.0336(18) 0.0225(16) -0.0115(13) 0.0026(14) -0.0078(14) C35 0.0278(15) 0.0238(15) 0.0267(15) -0.0037(12) 0.0131(13) -0.0035(12) C63 0.0271(16) 0.0210(15) 0.0336(17) -0.0060(13) 0.0113(14) -0.0027(12) C18 0.0224(15) 0.0249(15) 0.0258(15) 0.0019(12) 0.0077(13) 0.0053(12) C16 0.0317(17) 0.0341(17) 0.0200(15) -0.0070(13) 0.0088(13) -0.0034(13) C3 0.0195(14) 0.0238(15) 0.0337(16) -0.0015(12) 0.0152(13) 0.0046(11) C12 0.0240(15) 0.0259(15) 0.0275(16) 0.0049(12) 0.0123(13) 0.0038(12) C5 0.0243(15) 0.0253(15) 0.0236(15) 0.0042(12) 0.0136(13) 0.0040(12) C48 0.0289(16) 0.0392(18) 0.0318(17) 0.0001(14) 0.0211(14) 0.0092(14) C4 0.0218(14) 0.0210(15) 0.0305(16) 0.0076(12) 0.0117(13) 0.0071(11) C14 0.0248(15) 0.0303(16) 0.0234(15) 0.0000(12) 0.0078(13) 0.0062(12) C59 0.0297(16) 0.0276(16) 0.0228(15) 0.0032(12) 0.0135(13) -0.0030(12) C96 0.0218(15) 0.056(2) 0.0133(14) 0.0089(14) 0.0007(12) -0.0074(14) C65 0.0253(15) 0.0369(18) 0.0158(14) -0.0055(12) 0.0068(12) 0.0003(13) C30 0.0388(18) 0.0291(17) 0.0206(15) -0.0031(12) 0.0107(14) 0.0139(14) C9 0.0244(16) 0.0388(19) 0.0339(17) 0.0106(14) 0.0191(14) 0.0060(13) C34 0.0292(17) 0.0175(15) 0.0362(18) -0.0002(13) 0.0085(14) 0.0001(12) C11 0.0287(17) 0.0241(16) 0.0383(18) 0.0056(13) 0.0128(15) 0.0017(13) C10 0.0270(16) 0.0301(17) 0.0409(19) 0.0171(14) 0.0162(15) 0.0031(13) C33 0.0208(15) 0.0252(16) 0.0413(19) -0.0114(14) 0.0128(14) 0.0014(12) C32 0.0235(15) 0.0334(17) 0.0311(16) -0.0088(13) 0.0151(13) -0.0017(13) C15 0.0322(17) 0.0320(17) 0.0265(16) -0.0030(13) 0.0119(14) 0.0063(13) C21 0.0181(14) 0.0279(16) 0.048(2) 0.0016(14) 0.0167(14) -0.0035(12) C44 0.0280(17) 0.042(2) 0.0294(17) 0.0131(15) 0.0048(14) 0.0105(14) C23 0.0239(16) 0.0296(17) 0.0443(19) -0.0155(14) 0.0153(15) -0.0075(13) C40 0.0357(18) 0.0205(16) 0.055(2) -0.0066(14) 0.0186(17) -0.0055(13) C22 0.0230(16) 0.0258(16) 0.050(2) -0.0078(15) 0.0136(15) -0.0055(13) C26 0.0250(16) 0.045(2) 0.0340(18) -0.0117(15) 0.0041(14) 0.0107(14) C42 0.045(2) 0.0265(17) 0.0375(19) 0.0112(14) 0.0135(16) 0.0091(15) C29 0.065(3) 0.043(2) 0.0271(18) 0.0022(15) 0.0205(18) 0.0263(19) C27 0.032(2) 0.071(3) 0.038(2) -0.018(2) -0.0074(17) 0.0203(19) C92 0.039(2) 0.0266(18) 0.099(3) 0.016(2) 0.032(2) -0.0067(15) C28 0.064(3) 0.066(3) 0.0194(17) -0.0051(18) -0.0032(18) 0.040(2) F3 0.037(4) 0.049(5) 0.179(12) -0.031(6) 0.017(5) -0.008(3) F1 0.099(8) 0.048(4) 0.078(7) 0.007(4) 0.072(6) 0.014(4) F3' 0.108(7) 0.088(7) 0.029(3) -0.003(3) 0.002(4) 0.051(6) F1' 0.132(8) 0.080(5) 0.207(15) -0.068(7) 0.118(10) -0.056(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C41 2.000(3) . ? Rh1 C37 2.007(3) . ? Rh1 C45 2.023(3) . ? Rh1 C1 2.078(3) . ? Rh1 P1 2.2928(9) . ? Rh1 Rh2 2.7682(6) . ? Rh2 C43 2.009(3) . ? Rh2 C39 2.026(3) . ? Rh2 C47 2.037(3) . ? Rh2 C19 2.090(3) . ? Rh2 P2 2.3076(10) . ? P2 C6 1.807(3) . ? P2 C7 1.827(3) . ? P2 C13 1.837(3) . ? P1 C24 1.807(3) . ? P1 C25 1.831(3) . ? P1 C36 1.832(3) . ? Rh3 C85 2.005(3) . ? Rh3 C91 2.011(3) . ? Rh3 C95 2.033(3) . ? Rh3 C67 2.099(3) . ? Rh3 P3 2.3056(7) . ? Rh3 Rh4 2.7664(12) . ? Rh4 C89 2.004(3) . ? Rh4 C87 2.019(3) . ? Rh4 C93 2.040(3) . ? Rh4 C49 2.096(2) . ? Rh4 P4 2.3075(7) . ? P4 C72 1.803(3) . ? P4 C73 1.826(3) . ? P4 C84 1.844(3) . ? P3 C54 1.807(3) . ? P3 C61 1.834(3) . ? P3 C55 1.839(3) . ? C50 C51 1.385(4) . ? C50 C49 1.412(3) . ? C50 H50 0.9500 . ? C49 C54 1.411(3) . ? C84 C79 1.394(4) . ? C84 C83 1.399(4) . ? C69 C68 1.377(4) . ? C69 C70 1.389(4) . ? C69 H69 0.9500 . ? C72 C71 1.404(3) . ? C72 C67 1.417(3) . ? C71 C70 1.380(4) . ? C71 H71 0.9500 . ? C57 C58 1.378(4) . ? C57 C56 1.392(4) . ? C57 H57 0.9500 . ? C70 H70 0.9500 . ? C54 C53 1.407(3) . ? C60 C59 1.387(4) . ? C60 C55 1.399(4) . ? C60 H60 0.9500 . ? C56 C55 1.394(4) . ? C56 H56 0.9500 . ? C79 C80 1.384(4) . ? C79 H79 0.9500 . ? C52 C51 1.377(4) . ? C52 C53 1.386(4) . ? C52 H52 0.9500 . ? C73 C74 1.398(4) . ? C73 C78 1.399(4) . ? C82 C81 1.386(4) . ? C82 C83 1.389(4) . ? C82 H82 0.9500 . ? C67 C68 1.404(3) . ? C58 C59 1.387(4) . ? C58 H58 0.9500 . ? C81 C80 1.385(4) . ? C81 H81 0.9500 . ? C51 H51 0.9500 . ? C53 H53 0.9500 . ? C75 C76 1.373(4) . ? C75 C74 1.394(4) . ? C75 H75 0.9500 . ? C68 H68 0.9500 . ? C80 H80 0.9500 . ? C78 C77 1.382(4) . ? C78 H78 0.9500 . ? C77 C76 1.378(4) . ? C77 H77 0.9500 . ? C74 H74 0.9500 . ? C76 H76 0.9500 . ? F5 B2 1.396(4) . ? F7 B2 1.392(4) . ? F6 B2 1.401(4) . ? F8 B2 1.388(4) . ? F13 B4 1.400(4) . ? F14 B4 1.396(4) . ? F15 B4 1.369(4) . ? F16 B4 1.375(4) . ? F9 B3 1.378(4) . ? F12 B3 1.396(4) . ? F10 B3 1.391(4) . ? F11 B3 1.376(4) . ? F4 B1 1.366(5) . ? F2 B1 1.367(4) . ? B1 F3' 1.222(8) . ? B1 F1' 1.369(7) . ? B1 F3 1.440(11) . ? B1 F1 1.443(8) . ? N8 C85 1.144(3) . ? N8 C86 1.437(3) . ? N9 C89 1.144(3) . ? N9 C90 1.443(3) . ? N12 C93 1.135(3) . ? N12 C94 1.447(3) . ? C87 N10 1.143(3) . ? N10 C88 1.436(3) . ? C95 N11 1.140(3) . ? N7 C91 1.145(3) . ? N7 C92 1.440(4) . ? N11 C96 1.437(3) . ? C61 C62 1.386(4) . ? C61 C66 1.393(3) . ? N5 C45 1.149(3) . ? N5 C46 1.437(3) . ? N2 C43 1.136(3) . ? N2 C44 1.439(3) . ? N3 C37 1.147(3) . ? N3 C38 1.436(3) . ? N6 C47 1.140(3) . ? N6 C48 1.430(3) . ? N1 C41 1.143(3) . ? N1 C42 1.428(3) . ? C19 C24 1.391(4) . ? C19 C20 1.404(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C7 C8 1.387(4) . ? C7 C12 1.401(4) . ? C13 C18 1.392(4) . ? C13 C14 1.393(4) . ? C24 C23 1.403(4) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C66 C65 1.383(4) . ? C66 H66 0.9500 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C83 H83 0.9500 . ? N4 C39 1.147(3) . ? N4 C40 1.438(3) . ? C1 C6 1.407(4) . ? C1 C2 1.413(3) . ? C62 C63 1.386(4) . ? C62 H62 0.9500 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C31 C36 1.387(4) . ? C31 C32 1.392(4) . ? C31 H31 0.9500 . ? C8 C9 1.395(4) . ? C8 H8 0.9500 . ? C36 C35 1.400(4) . ? C64 C63 1.382(4) . ? C64 C65 1.384(4) . ? C64 H64 0.9500 . ? C25 C26 1.390(4) . ? C25 C30 1.399(4) . ? C17 C16 1.377(4) . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C6 C5 1.407(4) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C2 C3 1.394(4) . ? C2 H2 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C35 C34 1.389(4) . ? C35 H35 0.9500 . ? C63 H63 0.9500 . ? C18 H18 0.9500 . ? C16 C15 1.380(4) . ? C16 H16 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C12 C11 1.389(4) . ? C12 H12 0.9500 . ? C5 C4 1.379(4) . ? C5 H5 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C4 H4 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C59 H59 0.9500 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C65 H65 0.9500 . ? C30 C29 1.389(4) . ? C30 H30 0.9500 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C34 C33 1.373(4) . ? C34 H34 0.9500 . ? C11 C10 1.376(4) . ? C11 H11 0.9500 . ? C10 H10 0.9500 . ? C33 C32 1.373(4) . ? C33 H33 0.9500 . ? C32 H32 0.9500 . ? C15 H15 0.9500 . ? C21 C22 1.372(4) . ? C21 H21 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C23 C22 1.380(4) . ? C23 H23 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C22 H22 0.9500 . ? C26 C27 1.382(5) . ? C26 H26 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C29 C28 1.378(6) . ? C29 H29 0.9500 . ? C27 C28 1.378(6) . ? C27 H27 0.9500 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C28 H28 0.9500 . ? 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 C41 Rh1 C37 94.39(10) . . ? C41 Rh1 C45 86.14(10) . . ? C37 Rh1 C45 88.74(10) . . ? C41 Rh1 C1 178.03(10) . . ? C37 Rh1 C1 84.04(10) . . ? C45 Rh1 C1 94.99(10) . . ? C41 Rh1 P1 93.86(8) . . ? C37 Rh1 P1 170.37(8) . . ? C45 Rh1 P1 96.77(8) . . ? C1 Rh1 P1 87.61(8) . . ? C41 Rh1 Rh2 84.64(7) . . ? C37 Rh1 Rh2 93.32(7) . . ? C45 Rh1 Rh2 170.68(7) . . ? C1 Rh1 Rh2 94.26(7) . . ? P1 Rh1 Rh2 82.50(2) . . ? C43 Rh2 C39 88.57(11) . . ? C43 Rh2 C47 87.86(10) . . ? C39 Rh2 C47 90.75(10) . . ? C43 Rh2 C19 86.08(10) . . ? C39 Rh2 C19 172.46(10) . . ? C47 Rh2 C19 94.35(10) . . ? C43 Rh2 P2 172.67(8) . . ? C39 Rh2 P2 98.43(8) . . ? C47 Rh2 P2 94.19(8) . . ? C19 Rh2 P2 86.75(8) . . ? C43 Rh2 Rh1 96.21(7) . . ? C39 Rh2 Rh1 81.20(7) . . ? C47 Rh2 Rh1 170.86(8) . . ? C19 Rh2 Rh1 94.09(7) . . ? P2 Rh2 Rh1 82.80(3) . . ? C6 P2 C7 103.09(12) . . ? C6 P2 C13 107.40(12) . . ? C7 P2 C13 102.09(12) . . ? C6 P2 Rh2 115.54(9) . . ? C7 P2 Rh2 112.47(9) . . ? C13 P2 Rh2 114.79(9) . . ? C24 P1 C25 104.42(13) . . ? C24 P1 C36 105.46(13) . . ? C25 P1 C36 102.53(12) . . ? C24 P1 Rh1 114.21(9) . . ? C25 P1 Rh1 115.83(10) . . ? C36 P1 Rh1 113.12(9) . . ? C85 Rh3 C91 93.74(10) . . ? C85 Rh3 C95 87.04(10) . . ? C91 Rh3 C95 90.08(10) . . ? C85 Rh3 C67 85.09(10) . . ? C91 Rh3 C67 177.71(10) . . ? C95 Rh3 C67 91.83(10) . . ? C85 Rh3 P3 170.55(7) . . ? C91 Rh3 P3 95.07(8) . . ? C95 Rh3 P3 96.36(8) . . ? C67 Rh3 P3 85.98(7) . . ? C85 Rh3 Rh4 93.80(7) . . ? C91 Rh3 Rh4 84.45(7) . . ? C95 Rh3 Rh4 174.50(7) . . ? C67 Rh3 Rh4 93.65(7) . . ? P3 Rh3 Rh4 83.66(3) . . ? C89 Rh4 C87 94.77(10) . . ? C89 Rh4 C93 86.03(10) . . ? C87 Rh4 C93 90.32(10) . . ? C89 Rh4 C49 84.98(10) . . ? C87 Rh4 C49 178.32(10) . . ? C93 Rh4 C49 91.33(10) . . ? C89 Rh4 P4 170.08(7) . . ? C87 Rh4 P4 94.27(7) . . ? C93 Rh4 P4 98.00(8) . . ? C49 Rh4 P4 85.86(7) . . ? C89 Rh4 Rh3 93.33(7) . . ? C87 Rh4 Rh3 84.99(7) . . ? C93 Rh4 Rh3 175.20(7) . . ? C49 Rh4 Rh3 93.36(7) . . ? P4 Rh4 Rh3 83.40(3) . . ? C72 P4 C73 105.37(12) . . ? C72 P4 C84 104.42(12) . . ? C73 P4 C84 102.81(12) . . ? C72 P4 Rh4 114.14(9) . . ? C73 P4 Rh4 112.14(9) . . ? C84 P4 Rh4 116.69(9) . . ? C54 P3 C61 106.31(12) . . ? C54 P3 C55 105.09(12) . . ? C61 P3 C55 101.76(11) . . ? C54 P3 Rh3 113.81(8) . . ? C61 P3 Rh3 112.20(9) . . ? C55 P3 Rh3 116.48(9) . . ? C51 C50 C49 122.4(2) . . ? C51 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? C54 C49 C50 115.6(2) . . ? C54 C49 Rh4 123.11(18) . . ? C50 C49 Rh4 121.20(18) . . ? C79 C84 C83 117.9(2) . . ? C79 C84 P4 121.9(2) . . ? C83 C84 P4 120.2(2) . . ? C68 C69 C70 120.9(3) . . ? C68 C69 H69 119.5 . . ? C70 C69 H69 119.5 . . ? C71 C72 C67 121.4(2) . . ? C71 C72 P4 120.78(19) . . ? C67 C72 P4 117.61(19) . . ? C70 C71 C72 120.7(2) . . ? C70 C71 H71 119.6 . . ? C72 C71 H71 119.6 . . ? C58 C57 C56 120.6(3) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C71 C70 C69 118.6(2) . . ? C71 C70 H70 120.7 . . ? C69 C70 H70 120.7 . . ? C53 C54 C49 121.7(2) . . ? C53 C54 P3 120.49(19) . . ? C49 C54 P3 117.71(19) . . ? C59 C60 C55 121.2(3) . . ? C59 C60 H60 119.4 . . ? C55 C60 H60 119.4 . . ? C57 C56 C55 120.7(3) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C80 C79 C84 121.0(3) . . ? C80 C79 H79 119.5 . . ? C84 C79 H79 119.5 . . ? C51 C52 C53 119.0(2) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C74 C73 C78 118.6(2) . . ? C74 C73 P4 120.3(2) . . ? C78 C73 P4 120.9(2) . . ? C81 C82 C83 120.3(3) . . ? C81 C82 H82 119.8 . . ? C83 C82 H82 119.8 . . ? C56 C55 C60 117.9(2) . . ? C56 C55 P3 122.0(2) . . ? C60 C55 P3 120.0(2) . . ? C68 C67 C72 115.7(2) . . ? C68 C67 Rh3 121.39(19) . . ? C72 C67 Rh3 122.76(18) . . ? C57 C58 C59 119.5(3) . . ? C57 C58 H58 120.2 . . ? C59 C58 H58 120.2 . . ? C80 C81 C82 119.2(3) . . ? C80 C81 H81 120.4 . . ? C82 C81 H81 120.4 . . ? C52 C51 C50 120.9(2) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C52 C53 C54 120.4(2) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C76 C75 C74 120.8(3) . . ? C76 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? C69 C68 C67 122.6(2) . . ? C69 C68 H68 118.7 . . ? C67 C68 H68 118.7 . . ? C79 C80 C81 120.6(3) . . ? C79 C80 H80 119.7 . . ? C81 C80 H80 119.7 . . ? C77 C78 C73 120.8(3) . . ? C77 C78 H78 119.6 . . ? C73 C78 H78 119.6 . . ? C76 C77 C78 120.0(3) . . ? C76 C77 H77 120.0 . . ? C78 C77 H77 120.0 . . ? C75 C74 C73 119.7(3) . . ? C75 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C75 C76 C77 120.1(3) . . ? C75 C76 H76 120.0 . . ? C77 C76 H76 120.0 . . ? F8 B2 F7 109.9(3) . . ? F8 B2 F5 109.7(3) . . ? F7 B2 F5 109.8(3) . . ? F8 B2 F6 109.2(3) . . ? F7 B2 F6 109.3(3) . . ? F5 B2 F6 108.9(3) . . ? F15 B4 F16 110.7(3) . . ? F15 B4 F14 109.1(3) . . ? F16 B4 F14 109.3(3) . . ? F15 B4 F13 109.3(3) . . ? F16 B4 F13 110.0(3) . . ? F14 B4 F13 108.5(2) . . ? F11 B3 F9 109.9(3) . . ? F11 B3 F10 108.9(3) . . ? F9 B3 F10 109.1(3) . . ? F11 B3 F12 110.4(3) . . ? F9 B3 F12 108.9(3) . . ? F10 B3 F12 109.5(3) . . ? F3' B1 F4 113.1(5) . . ? F3' B1 F2 119.6(6) . . ? F4 B1 F2 111.6(4) . . ? F3' B1 F1' 114.3(7) . . ? F4 B1 F1' 98.5(7) . . ? F2 B1 F1' 96.6(5) . . ? F3' B1 F3 29.9(7) . . ? F4 B1 F3 105.3(6) . . ? F2 B1 F3 100.1(7) . . ? F1' B1 F3 143.2(8) . . ? F3' B1 F1 69.6(5) . . ? F4 B1 F1 121.7(4) . . ? F2 B1 F1 115.6(5) . . ? F1' B1 F1 45.0(5) . . ? F3 B1 F1 98.3(7) . . ? C85 N8 C86 179.4(3) . . ? C89 N9 C90 178.6(3) . . ? C93 N12 C94 176.5(3) . . ? N10 C87 Rh4 175.9(2) . . ? C87 N10 C88 173.5(3) . . ? N11 C95 Rh3 173.7(2) . . ? C91 N7 C92 174.8(3) . . ? N9 C89 Rh4 172.5(2) . . ? N8 C85 Rh3 173.1(2) . . ? N12 C93 Rh4 171.9(2) . . ? C95 N11 C96 176.2(3) . . ? N7 C91 Rh3 177.3(2) . . ? C62 C61 C66 118.5(2) . . ? C62 C61 P3 121.6(2) . . ? C66 C61 P3 119.7(2) . . ? C45 N5 C46 170.7(3) . . ? C43 N2 C44 176.5(3) . . ? C37 N3 C38 178.5(3) . . ? N5 C45 Rh1 167.3(2) . . ? N3 C37 Rh1 175.5(2) . . ? C47 N6 C48 175.0(3) . . ? N2 C43 Rh2 171.7(2) . . ? C41 N1 C42 173.4(3) . . ? C24 C19 C20 116.2(2) . . ? C24 C19 Rh2 122.34(19) . . ? C20 C19 Rh2 121.4(2) . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1 C41 Rh1 176.6(2) . . ? C8 C7 C12 119.5(3) . . ? C8 C7 P2 120.4(2) . . ? C12 C7 P2 119.9(2) . . ? C18 C13 C14 117.9(3) . . ? C18 C13 P2 122.4(2) . . ? C14 C13 P2 119.6(2) . . ? C19 C24 C23 121.4(3) . . ? C19 C24 P1 117.7(2) . . ? C23 C24 P1 120.8(2) . . ? N12 C94 H94A 109.5 . . ? N12 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? N12 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C65 C66 C61 121.2(3) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? N8 C86 H86A 109.5 . . ? N8 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N8 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N6 C47 Rh2 171.7(2) . . ? C21 C20 C19 122.4(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C82 C83 C84 120.9(3) . . ? C82 C83 H83 119.5 . . ? C84 C83 H83 119.5 . . ? C39 N4 C40 169.5(3) . . ? C6 C1 C2 116.1(2) . . ? C6 C1 Rh1 122.96(18) . . ? C2 C1 Rh1 120.86(19) . . ? C63 C62 C61 120.3(3) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? N10 C88 H88A 109.5 . . ? N10 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N10 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C36 C31 C32 120.8(3) . . ? C36 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C31 C36 C35 118.4(3) . . ? C31 C36 P1 121.1(2) . . ? C35 C36 P1 120.2(2) . . ? C63 C64 C65 119.4(3) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C26 C25 C30 118.3(3) . . ? C26 C25 P1 121.5(3) . . ? C30 C25 P1 120.2(2) . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? N4 C39 Rh2 172.3(2) . . ? C1 C6 C5 121.5(2) . . ? C1 C6 P2 117.37(19) . . ? C5 C6 P2 121.1(2) . . ? N9 C90 H90A 109.5 . . ? N9 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N9 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C3 C2 C1 122.0(2) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C35 C36 119.9(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C64 C63 C62 120.8(3) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C17 C16 C15 119.4(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C4 C3 C2 120.5(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C11 C12 C7 119.5(3) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? N6 C48 H48A 109.5 . . ? N6 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N6 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C15 C14 C13 121.4(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C60 C59 C58 120.0(3) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? N11 C96 H96A 109.5 . . ? N11 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? N11 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C66 C65 C64 119.8(3) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C29 C30 C25 120.6(3) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? N2 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C27 C26 C25 120.6(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C28 C29 C30 120.2(4) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N7 C92 H92A 109.5 . . ? N7 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N7 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C29 C28 C27 119.5(3) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C41 Rh1 Rh2 C43 -29.42(10) . . . . ? C37 Rh1 Rh2 C43 -123.52(11) . . . . ? C45 Rh1 Rh2 C43 -20.9(5) . . . . ? C1 Rh1 Rh2 C43 152.21(10) . . . . ? P1 Rh1 Rh2 C43 65.20(8) . . . . ? C41 Rh1 Rh2 C39 58.16(11) . . . . ? C37 Rh1 Rh2 C39 -35.94(10) . . . . ? C45 Rh1 Rh2 C39 66.7(5) . . . . ? C1 Rh1 Rh2 C39 -120.21(10) . . . . ? P1 Rh1 Rh2 C39 152.78(8) . . . . ? C41 Rh1 Rh2 C47 86.6(5) . . . . ? C37 Rh1 Rh2 C47 -7.5(5) . . . . ? C45 Rh1 Rh2 C47 95.2(7) . . . . ? C1 Rh1 Rh2 C47 -91.7(5) . . . . ? P1 Rh1 Rh2 C47 -178.7(5) . . . . ? C41 Rh1 Rh2 C19 -115.92(10) . . . . ? C37 Rh1 Rh2 C19 149.98(10) . . . . ? C45 Rh1 Rh2 C19 -107.4(5) . . . . ? C1 Rh1 Rh2 C19 65.72(11) . . . . ? P1 Rh1 Rh2 C19 -21.30(7) . . . . ? C41 Rh1 Rh2 P2 157.89(7) . . . . ? C37 Rh1 Rh2 P2 63.79(8) . . . . ? C45 Rh1 Rh2 P2 166.4(5) . . . . ? C1 Rh1 Rh2 P2 -20.47(7) . . . . ? P1 Rh1 Rh2 P2 -107.49(4) . . . . ? C43 Rh2 P2 C6 -59.5(6) . . . . ? C39 Rh2 P2 C6 103.16(12) . . . . ? C47 Rh2 P2 C6 -165.46(12) . . . . ? C19 Rh2 P2 C6 -71.33(12) . . . . ? Rh1 Rh2 P2 C6 23.21(10) . . . . ? C43 Rh2 P2 C7 58.5(6) . . . . ? C39 Rh2 P2 C7 -138.85(12) . . . . ? C47 Rh2 P2 C7 -47.47(12) . . . . ? C19 Rh2 P2 C7 46.66(12) . . . . ? Rh1 Rh2 P2 C7 141.20(10) . . . . ? C43 Rh2 P2 C13 174.7(6) . . . . ? C39 Rh2 P2 C13 -22.70(12) . . . . ? C47 Rh2 P2 C13 68.68(12) . . . . ? C19 Rh2 P2 C13 162.81(12) . . . . ? Rh1 Rh2 P2 C13 -102.65(9) . . . . ? C41 Rh1 P1 C24 112.20(12) . . . . ? C37 Rh1 P1 C24 -36.7(4) . . . . ? C45 Rh1 P1 C24 -161.24(12) . . . . ? C1 Rh1 P1 C24 -66.49(12) . . . . ? Rh2 Rh1 P1 C24 28.13(10) . . . . ? C41 Rh1 P1 C25 -9.21(13) . . . . ? C37 Rh1 P1 C25 -158.1(4) . . . . ? C45 Rh1 P1 C25 77.36(13) . . . . ? C1 Rh1 P1 C25 172.11(13) . . . . ? Rh2 Rh1 P1 C25 -93.27(11) . . . . ? C41 Rh1 P1 C36 -127.16(12) . . . . ? C37 Rh1 P1 C36 84.0(4) . . . . ? C45 Rh1 P1 C36 -40.60(12) . . . . ? C1 Rh1 P1 C36 54.15(12) . . . . ? Rh2 Rh1 P1 C36 148.77(10) . . . . ? C85 Rh3 Rh4 C89 125.17(11) . . . . ? C91 Rh3 Rh4 C89 31.77(10) . . . . ? C95 Rh3 Rh4 C89 26.6(8) . . . . ? C67 Rh3 Rh4 C89 -149.52(10) . . . . ? P3 Rh3 Rh4 C89 -63.97(7) . . . . ? C85 Rh3 Rh4 C87 30.66(10) . . . . ? C91 Rh3 Rh4 C87 -62.73(11) . . . . ? C95 Rh3 Rh4 C87 -67.9(8) . . . . ? C67 Rh3 Rh4 C87 115.98(10) . . . . ? P3 Rh3 Rh4 C87 -158.48(7) . . . . ? C85 Rh3 Rh4 C93 43.0(9) . . . . ? C91 Rh3 Rh4 C93 -50.4(9) . . . . ? C95 Rh3 Rh4 C93 -55.6(13) . . . . ? C67 Rh3 Rh4 C93 128.3(9) . . . . ? P3 Rh3 Rh4 C93 -146.1(9) . . . . ? C85 Rh3 Rh4 C49 -149.67(10) . . . . ? C91 Rh3 Rh4 C49 116.93(10) . . . . ? C95 Rh3 Rh4 C49 111.8(8) . . . . ? C67 Rh3 Rh4 C49 -64.35(10) . . . . ? P3 Rh3 Rh4 C49 21.19(7) . . . . ? C85 Rh3 Rh4 P4 -64.23(7) . . . . ? C91 Rh3 Rh4 P4 -157.63(8) . . . . ? C95 Rh3 Rh4 P4 -162.8(8) . . . . ? C67 Rh3 Rh4 P4 21.08(7) . . . . ? P3 Rh3 Rh4 P4 106.62(3) . . . . ? C89 Rh4 P4 C72 44.3(4) . . . . ? C87 Rh4 P4 C72 -111.36(12) . . . . ? C93 Rh4 P4 C72 157.72(11) . . . . ? C49 Rh4 P4 C72 66.96(11) . . . . ? Rh3 Rh4 P4 C72 -26.91(9) . . . . ? C89 Rh4 P4 C73 -75.5(4) . . . . ? C87 Rh4 P4 C73 128.90(12) . . . . ? C93 Rh4 P4 C73 37.98(12) . . . . ? C49 Rh4 P4 C73 -52.78(12) . . . . ? Rh3 Rh4 P4 C73 -146.65(10) . . . . ? C89 Rh4 P4 C84 166.3(4) . . . . ? C87 Rh4 P4 C84 10.70(12) . . . . ? C93 Rh4 P4 C84 -80.22(12) . . . . ? C49 Rh4 P4 C84 -170.98(11) . . . . ? Rh3 Rh4 P4 C84 95.15(9) . . . . ? C85 Rh3 P3 C54 48.3(5) . . . . ? C91 Rh3 P3 C54 -110.39(12) . . . . ? C95 Rh3 P3 C54 158.96(12) . . . . ? C67 Rh3 P3 C54 67.56(11) . . . . ? Rh4 Rh3 P3 C54 -26.57(9) . . . . ? C85 Rh3 P3 C61 -72.5(5) . . . . ? C91 Rh3 P3 C61 128.83(12) . . . . ? C95 Rh3 P3 C61 38.19(12) . . . . ? C67 Rh3 P3 C61 -53.21(11) . . . . ? Rh4 Rh3 P3 C61 -147.34(9) . . . . ? C85 Rh3 P3 C55 170.8(4) . . . . ? C91 Rh3 P3 C55 12.14(12) . . . . ? C95 Rh3 P3 C55 -78.51(12) . . . . ? C67 Rh3 P3 C55 -169.91(11) . . . . ? Rh4 Rh3 P3 C55 95.96(9) . . . . ? C51 C50 C49 C54 2.2(4) . . . . ? C51 C50 C49 Rh4 178.47(19) . . . . ? C89 Rh4 C49 C54 76.2(2) . . . . ? C87 Rh4 C49 C54 -5(3) . . . . ? C93 Rh4 C49 C54 162.1(2) . . . . ? P4 Rh4 C49 C54 -99.9(2) . . . . ? Rh3 Rh4 C49 C54 -16.8(2) . . . . ? C89 Rh4 C49 C50 -99.8(2) . . . . ? C87 Rh4 C49 C50 179(100) . . . . ? C93 Rh4 C49 C50 -13.9(2) . . . . ? P4 Rh4 C49 C50 84.0(2) . . . . ? Rh3 Rh4 C49 C50 167.17(19) . . . . ? C72 P4 C84 C79 -10.6(2) . . . . ? C73 P4 C84 C79 99.2(2) . . . . ? Rh4 P4 C84 C79 -137.65(19) . . . . ? C72 P4 C84 C83 170.3(2) . . . . ? C73 P4 C84 C83 -79.9(2) . . . . ? Rh4 P4 C84 C83 43.3(2) . . . . ? C73 P4 C72 C71 -36.9(2) . . . . ? C84 P4 C72 C71 71.1(2) . . . . ? Rh4 P4 C72 C71 -160.36(17) . . . . ? C73 P4 C72 C67 148.47(19) . . . . ? C84 P4 C72 C67 -103.6(2) . . . . ? Rh4 P4 C72 C67 25.0(2) . . . . ? C67 C72 C71 C70 -0.9(4) . . . . ? P4 C72 C71 C70 -175.32(19) . . . . ? C72 C71 C70 C69 1.9(4) . . . . ? C68 C69 C70 C71 -1.1(4) . . . . ? C50 C49 C54 C53 -0.9(4) . . . . ? Rh4 C49 C54 C53 -177.16(19) . . . . ? C50 C49 C54 P3 175.10(18) . . . . ? Rh4 C49 C54 P3 -1.1(3) . . . . ? C61 P3 C54 C53 -35.7(2) . . . . ? C55 P3 C54 C53 71.7(2) . . . . ? Rh3 P3 C54 C53 -159.73(18) . . . . ? C61 P3 C54 C49 148.20(19) . . . . ? C55 P3 C54 C49 -104.4(2) . . . . ? Rh3 P3 C54 C49 24.2(2) . . . . ? C58 C57 C56 C55 0.5(4) . . . . ? C83 C84 C79 C80 -0.4(4) . . . . ? P4 C84 C79 C80 -179.5(2) . . . . ? C72 P4 C73 C74 -30.7(2) . . . . ? C84 P4 C73 C74 -139.8(2) . . . . ? Rh4 P4 C73 C74 94.1(2) . . . . ? C72 P4 C73 C78 154.5(2) . . . . ? C84 P4 C73 C78 45.4(2) . . . . ? Rh4 P4 C73 C78 -80.7(2) . . . . ? C57 C56 C55 C60 -0.1(4) . . . . ? C57 C56 C55 P3 -178.8(2) . . . . ? C59 C60 C55 C56 -1.0(4) . . . . ? C59 C60 C55 P3 177.7(2) . . . . ? C54 P3 C55 C56 -14.3(2) . . . . ? C61 P3 C55 C56 96.4(2) . . . . ? Rh3 P3 C55 C56 -141.28(19) . . . . ? C54 P3 C55 C60 167.0(2) . . . . ? C61 P3 C55 C60 -82.3(2) . . . . ? Rh3 P3 C55 C60 40.0(2) . . . . ? C71 C72 C67 C68 -0.9(3) . . . . ? P4 C72 C67 C68 173.69(18) . . . . ? C71 C72 C67 Rh3 -176.66(18) . . . . ? P4 C72 C67 Rh3 -2.1(3) . . . . ? C85 Rh3 C67 C68 -98.2(2) . . . . ? C91 Rh3 C67 C68 -158(2) . . . . ? C95 Rh3 C67 C68 -11.3(2) . . . . ? P3 Rh3 C67 C68 84.9(2) . . . . ? Rh4 Rh3 C67 C68 168.29(19) . . . . ? C85 Rh3 C67 C72 77.3(2) . . . . ? C91 Rh3 C67 C72 18(3) . . . . ? C95 Rh3 C67 C72 164.2(2) . . . . ? P3 Rh3 C67 C72 -99.6(2) . . . . ? Rh4 Rh3 C67 C72 -16.2(2) . . . . ? C56 C57 C58 C59 0.1(4) . . . . ? C83 C82 C81 C80 -0.9(4) . . . . ? C53 C52 C51 C50 -0.8(4) . . . . ? C49 C50 C51 C52 -1.3(4) . . . . ? C51 C52 C53 C54 2.0(4) . . . . ? C49 C54 C53 C52 -1.1(4) . . . . ? P3 C54 C53 C52 -177.1(2) . . . . ? C70 C69 C68 C67 -0.8(4) . . . . ? C72 C67 C68 C69 1.7(4) . . . . ? Rh3 C67 C68 C69 177.6(2) . . . . ? C84 C79 C80 C81 0.2(4) . . . . ? C82 C81 C80 C79 0.4(4) . . . . ? C74 C73 C78 C77 0.3(4) . . . . ? P4 C73 C78 C77 175.2(2) . . . . ? C73 C78 C77 C76 0.7(4) . . . . ? C76 C75 C74 C73 0.3(4) . . . . ? C78 C73 C74 C75 -0.8(4) . . . . ? P4 C73 C74 C75 -175.7(2) . . . . ? C74 C75 C76 C77 0.7(4) . . . . ? C78 C77 C76 C75 -1.2(4) . . . . ? C89 Rh4 C87 N10 143(3) . . . . ? C93 Rh4 C87 N10 57(3) . . . . ? C49 Rh4 C87 N10 -136(4) . . . . ? P4 Rh4 C87 N10 -41(3) . . . . ? Rh3 Rh4 C87 N10 -124(3) . . . . ? Rh4 C87 N10 C88 20(5) . . . . ? C85 Rh3 C95 N11 -18(2) . . . . ? C91 Rh3 C95 N11 75(2) . . . . ? C67 Rh3 C95 N11 -103(2) . . . . ? P3 Rh3 C95 N11 170(2) . . . . ? Rh4 Rh3 C95 N11 81(2) . . . . ? C90 N9 C89 Rh4 -61(12) . . . . ? C87 Rh4 C89 N9 -119.1(18) . . . . ? C93 Rh4 C89 N9 -29.1(18) . . . . ? C49 Rh4 C89 N9 62.6(18) . . . . ? P4 Rh4 C89 N9 85.3(19) . . . . ? Rh3 Rh4 C89 N9 155.7(18) . . . . ? C86 N8 C85 Rh3 -19(32) . . . . ? C91 Rh3 C85 N8 -112.7(19) . . . . ? C95 Rh3 C85 N8 -22.8(19) . . . . ? C67 Rh3 C85 N8 69.3(19) . . . . ? P3 Rh3 C85 N8 89(2) . . . . ? Rh4 Rh3 C85 N8 162.7(19) . . . . ? C94 N12 C93 Rh4 17(6) . . . . ? C89 Rh4 C93 N12 -4.9(17) . . . . ? C87 Rh4 C93 N12 89.8(17) . . . . ? C49 Rh4 C93 N12 -89.8(17) . . . . ? P4 Rh4 C93 N12 -175.8(17) . . . . ? Rh3 Rh4 C93 N12 77(2) . . . . ? Rh3 C95 N11 C96 50(6) . . . . ? C92 N7 C91 Rh3 39(7) . . . . ? C85 Rh3 C91 N7 132(5) . . . . ? C95 Rh3 C91 N7 45(5) . . . . ? C67 Rh3 C91 N7 -169(4) . . . . ? P3 Rh3 C91 N7 -52(5) . . . . ? Rh4 Rh3 C91 N7 -135(5) . . . . ? C54 P3 C61 C62 -29.4(2) . . . . ? C55 P3 C61 C62 -139.1(2) . . . . ? Rh3 P3 C61 C62 95.6(2) . . . . ? C54 P3 C61 C66 155.2(2) . . . . ? C55 P3 C61 C66 45.4(2) . . . . ? Rh3 P3 C61 C66 -79.8(2) . . . . ? C46 N5 C45 Rh1 -12(2) . . . . ? C41 Rh1 C45 N5 -33.7(10) . . . . ? C37 Rh1 C45 N5 60.8(10) . . . . ? C1 Rh1 C45 N5 144.7(10) . . . . ? P1 Rh1 C45 N5 -127.1(10) . . . . ? Rh2 Rh1 C45 N5 -42.2(14) . . . . ? C38 N3 C37 Rh1 -143(10) . . . . ? C41 Rh1 C37 N3 125(3) . . . . ? C45 Rh1 C37 N3 39(3) . . . . ? C1 Rh1 C37 N3 -56(3) . . . . ? P1 Rh1 C37 N3 -86(3) . . . . ? Rh2 Rh1 C37 N3 -150(3) . . . . ? C44 N2 C43 Rh2 -2(6) . . . . ? C39 Rh2 C43 N2 90.6(17) . . . . ? C47 Rh2 C43 N2 -0.2(17) . . . . ? C19 Rh2 C43 N2 -94.7(17) . . . . ? P2 Rh2 C43 N2 -106.5(16) . . . . ? Rh1 Rh2 C43 N2 171.6(17) . . . . ? C43 Rh2 C19 C24 -81.2(2) . . . . ? C39 Rh2 C19 C24 -36.3(9) . . . . ? C47 Rh2 C19 C24 -168.7(2) . . . . ? P2 Rh2 C19 C24 97.3(2) . . . . ? Rh1 Rh2 C19 C24 14.8(2) . . . . ? C43 Rh2 C19 C20 96.3(2) . . . . ? C39 Rh2 C19 C20 141.1(7) . . . . ? C47 Rh2 C19 C20 8.7(2) . . . . ? P2 Rh2 C19 C20 -85.2(2) . . . . ? Rh1 Rh2 C19 C20 -167.8(2) . . . . ? C42 N1 C41 Rh1 -71(5) . . . . ? C37 Rh1 C41 N1 -123(4) . . . . ? C45 Rh1 C41 N1 -34(4) . . . . ? C1 Rh1 C41 N1 -160(3) . . . . ? P1 Rh1 C41 N1 62(4) . . . . ? Rh2 Rh1 C41 N1 144(4) . . . . ? C6 P2 C7 C8 -148.9(2) . . . . ? C13 P2 C7 C8 -37.5(2) . . . . ? Rh2 P2 C7 C8 86.0(2) . . . . ? C6 P2 C7 C12 36.2(2) . . . . ? C13 P2 C7 C12 147.6(2) . . . . ? Rh2 P2 C7 C12 -88.9(2) . . . . ? C6 P2 C13 C18 25.3(3) . . . . ? C7 P2 C13 C18 -82.8(2) . . . . ? Rh2 P2 C13 C18 155.2(2) . . . . ? C6 P2 C13 C14 -159.2(2) . . . . ? C7 P2 C13 C14 92.7(2) . . . . ? Rh2 P2 C13 C14 -29.2(2) . . . . ? C20 C19 C24 C23 3.4(4) . . . . ? Rh2 C19 C24 C23 -179.0(2) . . . . ? C20 C19 C24 P1 -172.84(19) . . . . ? Rh2 C19 C24 P1 4.7(3) . . . . ? C25 P1 C24 C19 99.6(2) . . . . ? C36 P1 C24 C19 -152.7(2) . . . . ? Rh1 P1 C24 C19 -27.9(2) . . . . ? C25 P1 C24 C23 -76.6(3) . . . . ? C36 P1 C24 C23 31.0(3) . . . . ? Rh1 P1 C24 C23 155.8(2) . . . . ? C62 C61 C66 C65 -0.6(4) . . . . ? P3 C61 C66 C65 175.0(2) . . . . ? C48 N6 C47 Rh2 -19(5) . . . . ? C43 Rh2 C47 N6 65.3(16) . . . . ? C39 Rh2 C47 N6 -23.3(16) . . . . ? C19 Rh2 C47 N6 151.2(16) . . . . ? P2 Rh2 C47 N6 -121.8(16) . . . . ? Rh1 Rh2 C47 N6 -51.4(19) . . . . ? C24 C19 C20 C21 -4.2(4) . . . . ? Rh2 C19 C20 C21 178.2(2) . . . . ? C81 C82 C83 C84 0.7(4) . . . . ? C79 C84 C83 C82 -0.1(4) . . . . ? P4 C84 C83 C82 179.0(2) . . . . ? C41 Rh1 C1 C6 -36(3) . . . . ? C37 Rh1 C1 C6 -72.9(2) . . . . ? C45 Rh1 C1 C6 -161.1(2) . . . . ? P1 Rh1 C1 C6 102.3(2) . . . . ? Rh2 Rh1 C1 C6 20.0(2) . . . . ? C41 Rh1 C1 C2 140(3) . . . . ? C37 Rh1 C1 C2 103.1(2) . . . . ? C45 Rh1 C1 C2 14.8(2) . . . . ? P1 Rh1 C1 C2 -81.7(2) . . . . ? Rh2 Rh1 C1 C2 -164.0(2) . . . . ? C66 C61 C62 C63 -0.8(4) . . . . ? P3 C61 C62 C63 -176.3(2) . . . . ? C12 C7 C8 C9 -0.3(4) . . . . ? P2 C7 C8 C9 -175.2(2) . . . . ? C32 C31 C36 C35 -0.8(4) . . . . ? C32 C31 C36 P1 -174.8(2) . . . . ? C24 P1 C36 C31 -149.4(2) . . . . ? C25 P1 C36 C31 -40.3(2) . . . . ? Rh1 P1 C36 C31 85.2(2) . . . . ? C24 P1 C36 C35 36.8(2) . . . . ? C25 P1 C36 C35 145.8(2) . . . . ? Rh1 P1 C36 C35 -88.7(2) . . . . ? C24 P1 C25 C26 7.2(3) . . . . ? C36 P1 C25 C26 -102.6(2) . . . . ? Rh1 P1 C25 C26 133.7(2) . . . . ? C24 P1 C25 C30 -174.1(2) . . . . ? C36 P1 C25 C30 76.1(2) . . . . ? Rh1 P1 C25 C30 -47.6(2) . . . . ? C40 N4 C39 Rh2 64(3) . . . . ? C43 Rh2 C39 N4 31.8(17) . . . . ? C47 Rh2 C39 N4 119.7(17) . . . . ? C19 Rh2 C39 N4 -13(2) . . . . ? P2 Rh2 C39 N4 -146.0(17) . . . . ? Rh1 Rh2 C39 N4 -64.7(17) . . . . ? C2 C1 C6 C5 0.8(4) . . . . ? Rh1 C1 C6 C5 176.9(2) . . . . ? C2 C1 C6 P2 178.59(19) . . . . ? Rh1 C1 C6 P2 -5.3(3) . . . . ? C7 P2 C6 C1 -140.8(2) . . . . ? C13 P2 C6 C1 111.8(2) . . . . ? Rh2 P2 C6 C1 -17.7(2) . . . . ? C7 P2 C6 C5 37.0(2) . . . . ? C13 P2 C6 C5 -70.4(2) . . . . ? Rh2 P2 C6 C5 160.08(19) . . . . ? C6 C1 C2 C3 -1.8(4) . . . . ? Rh1 C1 C2 C3 -178.0(2) . . . . ? C31 C36 C35 C34 0.4(4) . . . . ? P1 C36 C35 C34 174.4(2) . . . . ? C65 C64 C63 C62 0.6(4) . . . . ? C61 C62 C63 C64 0.8(4) . . . . ? C16 C17 C18 C13 1.8(5) . . . . ? C14 C13 C18 C17 -2.9(4) . . . . ? P2 C13 C18 C17 172.7(2) . . . . ? C18 C17 C16 C15 1.0(5) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C8 C7 C12 C11 0.2(4) . . . . ? P2 C7 C12 C11 175.1(2) . . . . ? C1 C6 C5 C4 0.4(4) . . . . ? P2 C6 C5 C4 -177.3(2) . . . . ? C6 C5 C4 C3 -0.7(4) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C18 C13 C14 C15 1.3(4) . . . . ? P2 C13 C14 C15 -174.4(2) . . . . ? C55 C60 C59 C58 1.7(4) . . . . ? C57 C58 C59 C60 -1.3(4) . . . . ? C61 C66 C65 C64 2.0(4) . . . . ? C63 C64 C65 C66 -2.0(4) . . . . ? C26 C25 C30 C29 1.8(4) . . . . ? P1 C25 C30 C29 -176.9(2) . . . . ? C7 C8 C9 C10 0.1(4) . . . . ? C36 C35 C34 C33 0.0(4) . . . . ? C7 C12 C11 C10 0.1(4) . . . . ? C12 C11 C10 C9 -0.2(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C35 C34 C33 C32 0.1(4) . . . . ? C34 C33 C32 C31 -0.6(4) . . . . ? C36 C31 C32 C33 0.9(4) . . . . ? C17 C16 C15 C14 -2.6(5) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C19 C24 C23 C22 0.5(5) . . . . ? P1 C24 C23 C22 176.6(2) . . . . ? C20 C21 C22 C23 3.0(5) . . . . ? C24 C23 C22 C21 -3.7(5) . . . . ? C30 C25 C26 C27 -0.9(4) . . . . ? P1 C25 C26 C27 177.8(2) . . . . ? C25 C30 C29 C28 -1.2(5) . . . . ? C25 C26 C27 C28 -0.6(5) . . . . ? C30 C29 C28 C27 -0.4(5) . . . . ? C26 C27 C28 C29 1.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.625 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 932781'