# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cc94 _database_code_depnum_ccdc_archive 'CCDC 886710' #TrackingRef 'cc94z.cif' _audit_update_record ; 2012-06-15 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H53 Cl N4 Rh' _chemical_formula_weight 824.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6281(2) _cell_length_b 11.9529(2) _cell_length_c 33.2439(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.3570(10) _cell_angle_gamma 90.00 _cell_volume 4178.35(12) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9842 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.11 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8496 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34993 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8185 _reflns_number_gt 7875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+3.5628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8185 _refine_ls_number_parameters 527 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.228 _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 0.630028(13) 0.425077(13) 0.902834(4) 0.02114(5) Uani 1 1 d . . . Cl1 Cl 0.84751(4) 0.39923(5) 0.925977(16) 0.03399(12) Uani 1 1 d . . . N1 N 0.68933(17) 0.42080(14) 0.81466(5) 0.0282(4) Uani 1 1 d . . . N2 N 0.73177(15) 0.57921(14) 0.84406(5) 0.0240(3) Uani 1 1 d . . . N4 N 0.58812(15) 0.38007(14) 0.95963(5) 0.0234(3) Uani 1 1 d . . . N3 N 0.43920(15) 0.42545(14) 0.89136(5) 0.0256(3) Uani 1 1 d . . . C1 C 0.67677(17) 0.47733(16) 0.85014(6) 0.0222(4) Uani 1 1 d . . . C2 C 0.7523(2) 0.48503(19) 0.78896(6) 0.0343(5) Uani 1 1 d . . . H2A H 0.7731 0.4628 0.7633 0.041 Uiso 1 1 calc R . . C3 C 0.7780(2) 0.58354(18) 0.80705(6) 0.0306(4) Uani 1 1 d . . . H3A H 0.8200 0.6450 0.7967 0.037 Uiso 1 1 calc R . . C4 C 0.6354(2) 0.31281(18) 0.80237(6) 0.0341(5) Uani 1 1 d . . . C5 C 0.5242(2) 0.3102(2) 0.77396(7) 0.0417(6) Uani 1 1 d . . . C6 C 0.4740(3) 0.2054(2) 0.76193(9) 0.0547(7) Uani 1 1 d . . . H6A H 0.3984 0.2008 0.7429 0.066 Uiso 1 1 calc R . . C7 C 0.5324(3) 0.1091(2) 0.77721(10) 0.0633(9) Uani 1 1 d . . . H7A H 0.4960 0.0386 0.7691 0.076 Uiso 1 1 calc R . . C8 C 0.6432(3) 0.1135(2) 0.80421(9) 0.0580(8) Uani 1 1 d . . . H8A H 0.6821 0.0457 0.8144 0.070 Uiso 1 1 calc R . . C9 C 0.7001(3) 0.2159(2) 0.81702(7) 0.0430(6) Uani 1 1 d . . . C10 C 0.4625(3) 0.4143(2) 0.75395(8) 0.0523(7) Uani 1 1 d . . . H10A H 0.4933 0.4803 0.7711 0.063 Uiso 1 1 calc R . . C11 C 0.3164(3) 0.4128(3) 0.74903(11) 0.0826(11) Uani 1 1 d . . . H11A H 0.2890 0.4031 0.7757 0.124 Uiso 1 1 calc R . . H11B H 0.2840 0.3508 0.7312 0.124 Uiso 1 1 calc R . . H11C H 0.2830 0.4837 0.7370 0.124 Uiso 1 1 calc R . . C12 C 0.5024(4) 0.4301(3) 0.71190(10) 0.0773(10) Uani 1 1 d . . . H12A H 0.5954 0.4343 0.7146 0.116 Uiso 1 1 calc R . . H12B H 0.4653 0.4994 0.6997 0.116 Uiso 1 1 calc R . . H12C H 0.4722 0.3665 0.6945 0.116 Uiso 1 1 calc R . . C13 C 0.8295(3) 0.2223(2) 0.84255(8) 0.0513(7) Uani 1 1 d . . . H13A H 0.8319 0.2921 0.8592 0.062 Uiso 1 1 calc R . . C14 C 0.8591(4) 0.1241(3) 0.87183(10) 0.0794(11) Uani 1 1 d . . . H14A H 0.7923 0.1180 0.8892 0.119 Uiso 1 1 calc R . . H14B H 0.9413 0.1366 0.8888 0.119 Uiso 1 1 calc R . . H14C H 0.8626 0.0548 0.8563 0.119 Uiso 1 1 calc R . . C15 C 0.9326(3) 0.2330(3) 0.81480(9) 0.0596(7) Uani 1 1 d . . . H15A H 0.9201 0.3029 0.7993 0.089 Uiso 1 1 calc R . . H15B H 0.9267 0.1695 0.7960 0.089 Uiso 1 1 calc R . . H15C H 1.0167 0.2337 0.8314 0.089 Uiso 1 1 calc R . . C16 C 0.72601(18) 0.67880(16) 0.86850(6) 0.0234(4) Uani 1 1 d . . . C17 C 0.83443(19) 0.71454(18) 0.89439(6) 0.0286(4) Uani 1 1 d . . . C18 C 0.8256(2) 0.81462(19) 0.91510(7) 0.0360(5) Uani 1 1 d . . . H18A H 0.8973 0.8409 0.9330 0.043 Uiso 1 1 calc R . . C19 C 0.7149(2) 0.8766(2) 0.91022(8) 0.0401(5) Uani 1 1 d . . . H19A H 0.7105 0.9438 0.9252 0.048 Uiso 1 1 calc R . . C20 C 0.6101(2) 0.84099(18) 0.88359(7) 0.0340(5) Uani 1 1 d . . . H20A H 0.5349 0.8850 0.8800 0.041 Uiso 1 1 calc R . . C21 C 0.61359(19) 0.74183(17) 0.86208(6) 0.0269(4) Uani 1 1 d . . . C22 C 0.95931(19) 0.6513(2) 0.89906(7) 0.0323(5) Uani 1 1 d . . . H22A H 0.9415 0.5738 0.8884 0.039 Uiso 1 1 calc R . . C23 C 1.0514(2) 0.7066(3) 0.87373(9) 0.0529(7) Uani 1 1 d . . . H23A H 1.0146 0.7052 0.8449 0.079 Uiso 1 1 calc R . . H23B H 1.1322 0.6657 0.8775 0.079 Uiso 1 1 calc R . . H23C H 1.0664 0.7843 0.8826 0.079 Uiso 1 1 calc R . . C24 C 1.0211(2) 0.6419(2) 0.94341(7) 0.0424(6) Uani 1 1 d . . . H24A H 0.9601 0.6095 0.9596 0.064 Uiso 1 1 calc R . . H24B H 1.0465 0.7164 0.9539 0.064 Uiso 1 1 calc R . . H24C H 1.0962 0.5936 0.9452 0.064 Uiso 1 1 calc R . . C25 C 0.50108(19) 0.70776(19) 0.83113(6) 0.0311(5) Uani 1 1 d . . . H25A H 0.5106 0.6265 0.8250 0.037 Uiso 1 1 calc R . . C26 C 0.5032(3) 0.7730(3) 0.79154(8) 0.0612(8) Uani 1 1 d . . . H26A H 0.5859 0.7630 0.7823 0.092 Uiso 1 1 calc R . . H26B H 0.4892 0.8526 0.7963 0.092 Uiso 1 1 calc R . . H26C H 0.4357 0.7451 0.7707 0.092 Uiso 1 1 calc R . . C27 C 0.3736(2) 0.7232(2) 0.84617(8) 0.0438(6) Uani 1 1 d . . . H27A H 0.3745 0.6835 0.8720 0.066 Uiso 1 1 calc R . . H27B H 0.3057 0.6930 0.8260 0.066 Uiso 1 1 calc R . . H27C H 0.3586 0.8030 0.8502 0.066 Uiso 1 1 calc R . . C28 C 0.3619(2) 0.4406(2) 0.85635(7) 0.0356(5) Uani 1 1 d . . . H28A H 0.3990 0.4568 0.8327 0.043 Uiso 1 1 calc R . . C29 C 0.2295(2) 0.4338(2) 0.85262(8) 0.0435(6) Uani 1 1 d . . . H29A H 0.1796 0.4457 0.8269 0.052 Uiso 1 1 calc R . . C30 C 0.1708(2) 0.4101(2) 0.88570(8) 0.0416(6) Uani 1 1 d . . . H30A H 0.0808 0.4061 0.8833 0.050 Uiso 1 1 calc R . . C31 C 0.24695(19) 0.39198(18) 0.92319(7) 0.0329(5) Uani 1 1 d . . . C32 C 0.1969(2) 0.3669(2) 0.95996(8) 0.0404(6) Uani 1 1 d . . . H32A H 0.1074 0.3626 0.9594 0.049 Uiso 1 1 calc R . . C33 C 0.2740(2) 0.3492(2) 0.99529(8) 0.0395(5) Uani 1 1 d . . . H33A H 0.2380 0.3349 1.0193 0.047 Uiso 1 1 calc R . . C34 C 0.4094(2) 0.35187(18) 0.99715(7) 0.0311(5) Uani 1 1 d . . . C35 C 0.4949(2) 0.3306(2) 1.03248(7) 0.0367(5) Uani 1 1 d . . . H35A H 0.4648 0.3148 1.0574 0.044 Uiso 1 1 calc R . . C36 C 0.6227(2) 0.3331(2) 1.03049(7) 0.0367(5) Uani 1 1 d . . . H36A H 0.6819 0.3177 1.0541 0.044 Uiso 1 1 calc R . . C37 C 0.66641(19) 0.35825(19) 0.99372(6) 0.0305(5) Uani 1 1 d . . . H37A H 0.7555 0.3598 0.9931 0.037 Uiso 1 1 calc R . . C38 C 0.46060(18) 0.37672(16) 0.96144(6) 0.0246(4) Uani 1 1 d . . . C39 C 0.37995(18) 0.39910(16) 0.92458(6) 0.0258(4) Uani 1 1 d . . . C40A C 0.4437(16) 0.1427(12) 0.8855(6) 0.097(9) Uani 0.50 1 d PGD A 1 H40A H 0.4877 0.2013 0.8742 0.117 Uiso 0.50 1 calc PR A 1 C41A C 0.3355(18) 0.1001(11) 0.8644(4) 0.088(6) Uani 0.50 1 d PGD A 1 H41A H 0.3037 0.1289 0.8382 0.105 Uiso 0.50 1 calc PR A 1 C42A C 0.2726(13) 0.0164(11) 0.8806(4) 0.062(3) Uani 0.50 1 d PGD A 1 H42A H 0.1968 -0.0134 0.8658 0.074 Uiso 0.50 1 calc PR A 1 C43A C 0.3180(16) -0.0247(12) 0.9179(5) 0.062(5) Uani 0.50 1 d PGD A 1 H43A H 0.2740 -0.0833 0.9293 0.074 Uiso 0.50 1 calc PR A 1 C44A C 0.4263(17) 0.0179(16) 0.9391(4) 0.087(6) Uani 0.50 1 d PGD A 1 H44A H 0.4581 -0.0108 0.9652 0.104 Uiso 0.50 1 calc PR A 1 C45A C 0.4892(12) 0.1016(16) 0.9229(6) 0.095(8) Uani 0.50 1 d PGD A 1 H45A H 0.5649 0.1315 0.9377 0.114 Uiso 0.50 1 calc PR A 1 C40B C 0.4773(15) 0.1426(12) 0.9011(4) 0.071(5) Uani 0.50 1 d PGD B 2 H40B H 0.5411 0.1958 0.8975 0.086 Uiso 0.50 1 calc PR B 2 C41B C 0.3763(18) 0.1278(13) 0.8717(3) 0.099(8) Uani 0.50 1 d PGD B 2 H41B H 0.3693 0.1706 0.8473 0.119 Uiso 0.50 1 calc PR B 2 C42B C 0.2851(13) 0.0519(16) 0.8769(6) 0.101(8) Uani 0.50 1 d PGD B 2 H42B H 0.2144 0.0416 0.8562 0.121 Uiso 0.50 1 calc PR B 2 C43B C 0.2951(17) -0.0092(14) 0.9116(7) 0.085(7) Uani 0.50 1 d PGD B 2 H43B H 0.2313 -0.0623 0.9152 0.102 Uiso 0.50 1 calc PR B 2 C44B C 0.396(2) 0.0056(14) 0.9410(5) 0.072(4) Uani 0.50 1 d PGD B 2 H44B H 0.4031 -0.0372 0.9653 0.087 Uiso 0.50 1 calc PR B 2 C45B C 0.4873(14) 0.0815(16) 0.9358(4) 0.067(4) Uani 0.50 1 d PGD B 2 H45B H 0.5580 0.0919 0.9565 0.080 Uiso 0.50 1 calc PR B 2 C46 C 0.0884(3) 0.0581(3) 0.98231(10) 0.0662(9) Uani 1 1 d . . . H46A H 0.1501 0.0981 0.9701 0.079 Uiso 1 1 calc R . . C47 C -0.0311(3) 0.1016(3) 0.98177(8) 0.0615(8) Uani 1 1 d . . . H47A H -0.0526 0.1717 0.9692 0.074 Uiso 1 1 calc R . . C48 C -0.1189(3) 0.0433(3) 0.99946(9) 0.0618(8) Uani 1 1 d . . . H48A H -0.2019 0.0731 0.9991 0.074 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 0.01810(8) 0.02467(8) 0.02082(8) 0.00128(6) 0.00348(5) -0.00168(6) Cl1 0.0195(2) 0.0524(3) 0.0303(3) 0.0065(2) 0.00458(18) 0.0006(2) N1 0.0369(9) 0.0256(9) 0.0231(8) -0.0002(7) 0.0073(7) -0.0043(7) N2 0.0237(8) 0.0262(8) 0.0223(8) 0.0005(7) 0.0045(6) -0.0015(7) N4 0.0207(8) 0.0262(8) 0.0237(8) 0.0011(7) 0.0049(6) -0.0013(7) N3 0.0225(8) 0.0248(8) 0.0294(9) -0.0005(7) 0.0030(6) -0.0035(7) C1 0.0199(9) 0.0248(10) 0.0211(9) 0.0009(8) 0.0006(7) 0.0005(7) C2 0.0463(13) 0.0354(12) 0.0233(10) -0.0005(9) 0.0127(9) -0.0052(10) C3 0.0361(11) 0.0317(11) 0.0256(10) 0.0029(9) 0.0102(8) -0.0051(9) C4 0.0505(13) 0.0269(11) 0.0281(11) -0.0060(9) 0.0165(10) -0.0095(10) C5 0.0532(15) 0.0391(13) 0.0341(12) -0.0101(10) 0.0109(11) -0.0138(11) C6 0.0693(19) 0.0460(16) 0.0500(16) -0.0153(13) 0.0132(14) -0.0236(14) C7 0.095(2) 0.0364(15) 0.0638(19) -0.0149(14) 0.0297(18) -0.0283(16) C8 0.101(2) 0.0262(12) 0.0539(17) -0.0012(12) 0.0344(17) -0.0054(14) C9 0.0678(17) 0.0325(12) 0.0333(12) 0.0010(10) 0.0228(11) -0.0010(12) C10 0.0609(17) 0.0461(15) 0.0443(14) -0.0143(12) -0.0108(12) -0.0062(13) C11 0.063(2) 0.102(3) 0.072(2) -0.029(2) -0.0269(17) -0.0020(19) C12 0.110(3) 0.064(2) 0.0510(18) 0.0053(16) -0.0101(18) -0.021(2) C13 0.0781(19) 0.0413(14) 0.0355(13) 0.0008(11) 0.0117(13) 0.0160(14) C14 0.118(3) 0.071(2) 0.0526(19) 0.0214(17) 0.0238(19) 0.036(2) C15 0.0661(19) 0.0549(18) 0.0587(18) 0.0053(14) 0.0118(14) 0.0084(15) C16 0.0249(9) 0.0227(10) 0.0232(9) 0.0008(8) 0.0059(7) -0.0036(8) C17 0.0264(10) 0.0307(11) 0.0285(10) 0.0023(9) 0.0036(8) -0.0038(8) C18 0.0333(11) 0.0336(12) 0.0389(12) -0.0065(10) -0.0024(9) -0.0069(9) C19 0.0451(13) 0.0271(11) 0.0467(14) -0.0097(10) 0.0020(11) -0.0005(10) C20 0.0355(11) 0.0274(11) 0.0383(12) -0.0004(9) 0.0032(9) 0.0059(9) C21 0.0275(10) 0.0267(10) 0.0264(10) 0.0031(8) 0.0038(8) -0.0012(8) C22 0.0226(10) 0.0381(12) 0.0358(12) -0.0037(10) 0.0033(8) -0.0033(9) C23 0.0362(13) 0.0642(18) 0.0606(17) 0.0020(14) 0.0150(12) -0.0100(13) C24 0.0295(11) 0.0506(15) 0.0436(14) -0.0070(11) -0.0062(10) 0.0054(10) C25 0.0283(10) 0.0315(11) 0.0317(11) 0.0006(9) -0.0013(8) 0.0040(9) C26 0.0487(16) 0.096(2) 0.0364(14) 0.0186(15) -0.0014(12) -0.0001(16) C27 0.0290(11) 0.0562(16) 0.0451(14) -0.0028(12) 0.0016(10) 0.0011(11) C28 0.0296(11) 0.0417(13) 0.0341(12) 0.0092(10) -0.0002(9) -0.0032(10) C29 0.0285(11) 0.0529(15) 0.0451(14) 0.0125(12) -0.0085(10) -0.0019(11) C30 0.0206(10) 0.0462(14) 0.0564(15) 0.0067(12) 0.0008(10) -0.0014(10) C31 0.0227(10) 0.0309(11) 0.0452(13) 0.0030(10) 0.0057(9) -0.0005(8) C32 0.0218(10) 0.0458(14) 0.0565(15) 0.0065(12) 0.0153(10) -0.0012(10) C33 0.0306(11) 0.0466(14) 0.0453(14) 0.0059(11) 0.0193(10) -0.0018(10) C34 0.0282(10) 0.0319(11) 0.0353(11) 0.0018(9) 0.0119(9) -0.0018(9) C35 0.0393(12) 0.0443(13) 0.0287(11) 0.0056(10) 0.0128(9) -0.0038(10) C36 0.0359(12) 0.0483(14) 0.0256(11) 0.0075(10) 0.0035(9) -0.0019(10) C37 0.0245(10) 0.0397(12) 0.0269(10) 0.0034(9) 0.0028(8) -0.0018(9) C38 0.0230(9) 0.0233(10) 0.0285(10) -0.0002(8) 0.0068(8) -0.0018(8) C39 0.0226(9) 0.0230(10) 0.0323(11) 0.0011(8) 0.0058(8) -0.0008(8) C40A 0.113(16) 0.045(7) 0.16(2) -0.014(11) 0.095(17) 0.005(8) C41A 0.145(14) 0.047(9) 0.080(9) 0.002(7) 0.045(10) 0.011(8) C42A 0.070(6) 0.049(6) 0.066(7) -0.018(5) 0.008(5) 0.005(4) C43A 0.080(11) 0.058(6) 0.055(8) 0.001(6) 0.035(8) 0.004(6) C44A 0.096(13) 0.106(14) 0.056(7) -0.031(8) 0.003(7) 0.026(11) C45A 0.059(7) 0.052(8) 0.18(2) -0.066(13) 0.020(11) -0.006(6) C40B 0.101(9) 0.024(5) 0.100(11) -0.011(5) 0.049(8) -0.003(5) C41B 0.17(2) 0.055(11) 0.069(7) -0.004(7) 0.011(10) 0.036(12) C42B 0.102(12) 0.092(17) 0.094(12) -0.045(11) -0.032(10) 0.035(10) C43B 0.052(6) 0.102(13) 0.104(16) -0.045(11) 0.023(6) -0.028(8) C44B 0.084(9) 0.081(8) 0.057(7) 0.000(6) 0.029(7) -0.020(7) C45B 0.054(7) 0.078(11) 0.070(5) -0.025(6) 0.012(4) 0.004(6) C46 0.082(2) 0.061(2) 0.0601(19) -0.0103(16) 0.0253(17) -0.0144(17) C47 0.098(3) 0.0513(17) 0.0339(14) -0.0045(12) 0.0070(15) 0.0041(17) C48 0.0615(18) 0.070(2) 0.0522(17) -0.0176(16) 0.0035(14) 0.0027(16) _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 C1 1.9896(19) . ? Rh1 N3 2.0085(16) . ? Rh1 N4 2.0729(16) . ? Rh1 Cl1 2.3480(5) . ? N1 C1 1.382(2) . ? N1 C2 1.390(3) . ? N1 C4 1.447(3) . ? N2 C1 1.378(3) . ? N2 C3 1.391(2) . ? N2 C16 1.448(3) . ? N4 C37 1.331(3) . ? N4 C38 1.366(2) . ? N3 C28 1.336(3) . ? N3 C39 1.385(3) . ? C2 C3 1.332(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.398(3) . ? C4 C5 1.402(3) . ? C5 C6 1.397(3) . ? C5 C10 1.514(4) . ? C6 C7 1.370(4) . ? C6 H6A 0.9500 . ? C7 C8 1.374(5) . ? C7 H7A 0.9500 . ? C8 C9 1.404(4) . ? C8 H8A 0.9500 . ? C9 C13 1.510(4) . ? C10 C12 1.530(4) . ? C10 C11 1.537(4) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.528(4) . ? C13 C15 1.536(4) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.401(3) . ? C16 C21 1.402(3) . ? C17 C18 1.390(3) . ? C17 C22 1.516(3) . ? C18 C19 1.379(3) . ? C18 H18A 0.9500 . ? C19 C20 1.385(3) . ? C19 H19A 0.9500 . ? C20 C21 1.387(3) . ? C20 H20A 0.9500 . ? C21 C25 1.515(3) . ? C22 C24 1.529(3) . ? C22 C23 1.531(3) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.522(3) . ? C25 C26 1.533(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.397(3) . ? C28 H28A 0.9500 . ? C29 C30 1.370(4) . ? C29 H29A 0.9500 . ? C30 C31 1.401(3) . ? C30 H30A 0.9500 . ? C31 C39 1.410(3) . ? C31 C32 1.434(3) . ? C32 C33 1.347(3) . ? C32 H32A 0.9500 . ? C33 C34 1.433(3) . ? C33 H33A 0.9500 . ? C34 C35 1.399(3) . ? C34 C38 1.407(3) . ? C35 C36 1.370(3) . ? C35 H35A 0.9500 . ? C36 C37 1.402(3) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C39 1.415(3) . ? C40A C45A 1.358(4) . ? C40A C41A 1.358(5) . ? C40A H40A 0.9500 . ? C41A C42A 1.358(5) . ? C41A H41A 0.9500 . ? C42A C43A 1.358(4) . ? C42A H42A 0.9500 . ? C43A C44A 1.358(5) . ? C43A H43A 0.9500 . ? C44A C45A 1.357(5) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? C40B C41B 1.356(4) . ? C40B C45B 1.356(5) . ? C40B H40B 0.9500 . ? C41B C42B 1.356(5) . ? C41B H41B 0.9500 . ? C42B C43B 1.356(5) . ? C42B H42B 0.9500 . ? C43B C44B 1.356(4) . ? C43B H43B 0.9500 . ? C44B C45B 1.356(4) . ? C44B H44B 0.9500 . ? C45B H45B 0.9500 . ? C46 C47 1.370(5) . ? C46 C48 1.373(5) 3_557 ? C46 H46A 0.9500 . ? C47 C48 1.364(5) . ? C47 H47A 0.9500 . ? C48 C46 1.373(5) 3_557 ? C48 H48A 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 C1 Rh1 N3 101.92(7) . . ? C1 Rh1 N4 176.04(7) . . ? N3 Rh1 N4 80.14(6) . . ? C1 Rh1 Cl1 88.28(5) . . ? N3 Rh1 Cl1 168.91(5) . . ? N4 Rh1 Cl1 89.94(5) . . ? C1 N1 C2 111.66(17) . . ? C1 N1 C4 126.41(17) . . ? C2 N1 C4 121.69(17) . . ? C1 N2 C3 112.00(17) . . ? C1 N2 C16 126.22(16) . . ? C3 N2 C16 121.01(17) . . ? C37 N4 C38 117.27(17) . . ? C37 N4 Rh1 129.50(13) . . ? C38 N4 Rh1 113.19(13) . . ? C28 N3 C39 115.63(17) . . ? C28 N3 Rh1 129.92(15) . . ? C39 N3 Rh1 114.32(13) . . ? N2 C1 N1 102.19(16) . . ? N2 C1 Rh1 124.88(14) . . ? N1 C1 Rh1 131.69(14) . . ? C3 C2 N1 107.23(18) . . ? C3 C2 H2A 126.4 . . ? N1 C2 H2A 126.4 . . ? C2 C3 N2 106.89(18) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? C9 C4 C5 122.7(2) . . ? C9 C4 N1 119.1(2) . . ? C5 C4 N1 118.1(2) . . ? C6 C5 C4 117.5(3) . . ? C6 C5 C10 119.2(2) . . ? C4 C5 C10 123.1(2) . . ? C7 C6 C5 121.0(3) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 120.6(3) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C7 C8 C9 121.5(3) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C4 C9 C8 116.6(3) . . ? C4 C9 C13 121.0(2) . . ? C8 C9 C13 122.1(3) . . ? C5 C10 C12 110.0(2) . . ? C5 C10 C11 113.8(3) . . ? C12 C10 C11 108.3(3) . . ? C5 C10 H10A 108.2 . . ? C12 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.9(3) . . ? C9 C13 C15 109.7(2) . . ? C14 C13 C15 110.4(2) . . ? C9 C13 H13A 107.5 . . ? C14 C13 H13A 107.5 . . ? C15 C13 H13A 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.42(19) . . ? C17 C16 N2 119.83(17) . . ? C21 C16 N2 117.45(17) . . ? C18 C17 C16 117.25(19) . . ? C18 C17 C22 119.99(19) . . ? C16 C17 C22 122.72(19) . . ? C19 C18 C17 121.4(2) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C18 C19 C20 120.2(2) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 120.8(2) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 117.80(19) . . ? C20 C21 C25 120.13(19) . . ? C16 C21 C25 121.99(18) . . ? C17 C22 C24 112.48(18) . . ? C17 C22 C23 110.4(2) . . ? C24 C22 C23 110.06(19) . . ? C17 C22 H22A 107.9 . . ? C24 C22 H22A 107.9 . . ? C23 C22 H22A 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 113.37(18) . . ? C21 C25 C26 109.74(19) . . ? C27 C25 C26 110.2(2) . . ? C21 C25 H25A 107.8 . . ? C27 C25 H25A 107.8 . . ? C26 C25 H25A 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 123.6(2) . . ? N3 C28 H28A 118.2 . . ? C29 C28 H28A 118.2 . . ? C30 C29 C28 120.7(2) . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C29 C30 C31 118.3(2) . . ? C29 C30 H30A 120.8 . . ? C31 C30 H30A 120.8 . . ? C30 C31 C39 117.8(2) . . ? C30 C31 C32 123.6(2) . . ? C39 C31 C32 118.6(2) . . ? C33 C32 C31 121.4(2) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C32 C33 C34 121.0(2) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C38 117.59(19) . . ? C35 C34 C33 123.9(2) . . ? C38 C34 C33 118.5(2) . . ? C36 C35 C34 118.9(2) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C35 C36 C37 120.2(2) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? N4 C37 C36 122.62(19) . . ? N4 C37 H37A 118.7 . . ? C36 C37 H37A 118.7 . . ? N4 C38 C34 123.43(18) . . ? N4 C38 C39 115.85(17) . . ? C34 C38 C39 120.72(18) . . ? N3 C39 C31 123.89(19) . . ? N3 C39 C38 116.44(17) . . ? C31 C39 C38 119.66(19) . . ? C45A C40A C41A 120.0 . . ? C45A C40A H40A 120.0 . . ? C41A C40A H40A 120.0 . . ? C42A C41A C40A 120.0 . . ? C42A C41A H41A 120.0 . . ? C40A C41A H41A 120.0 . . ? C41A C42A C43A 120.0 . . ? C41A C42A H42A 120.0 . . ? C43A C42A H42A 120.0 . . ? C44A C43A C42A 120.0 . . ? C44A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C45A C44A C43A 120.0 . . ? C45A C44A H44A 120.0 . . ? C43A C44A H44A 120.0 . . ? C44A C45A C40A 120.0 . . ? C44A C45A H45A 120.0 . . ? C40A C45A H45A 120.0 . . ? C41B C40B C45B 120.0 . . ? C41B C40B H40B 120.0 . . ? C45B C40B H40B 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? C42B C41B H41B 120.0 . . ? C41B C42B C43B 120.0 . . ? C41B C42B H42B 120.0 . . ? C43B C42B H42B 120.0 . . ? C44B C43B C42B 120.0 . . ? C44B C43B H43B 120.0 . . ? C42B C43B H43B 120.0 . . ? C43B C44B C45B 120.0 . . ? C43B C44B H44B 120.0 . . ? C45B C44B H44B 120.0 . . ? C40B C45B C44B 120.0 . . ? C40B C45B H45B 120.0 . . ? C44B C45B H45B 120.0 . . ? C47 C46 C48 120.0(3) . 3_557 ? C47 C46 H46A 120.0 . . ? C48 C46 H46A 120.0 3_557 . ? C48 C47 C46 119.4(3) . . ? C48 C47 H47A 120.3 . . ? C46 C47 H47A 120.3 . . ? C47 C48 C46 120.6(3) . 3_557 ? C47 C48 H48A 119.7 . . ? C46 C48 H48A 119.7 3_557 . ? 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 C1 Rh1 N4 C37 -57.9(11) . . . . ? N3 Rh1 N4 C37 -179.57(19) . . . . ? Cl1 Rh1 N4 C37 5.44(18) . . . . ? C1 Rh1 N4 C38 119.8(10) . . . . ? N3 Rh1 N4 C38 -1.90(14) . . . . ? Cl1 Rh1 N4 C38 -176.89(13) . . . . ? C1 Rh1 N3 C28 8.7(2) . . . . ? N4 Rh1 N3 C28 -174.7(2) . . . . ? Cl1 Rh1 N3 C28 -147.8(2) . . . . ? C1 Rh1 N3 C39 -175.77(14) . . . . ? N4 Rh1 N3 C39 0.78(14) . . . . ? Cl1 Rh1 N3 C39 27.7(4) . . . . ? C3 N2 C1 N1 -1.2(2) . . . . ? C16 N2 C1 N1 168.67(17) . . . . ? C3 N2 C1 Rh1 167.31(14) . . . . ? C16 N2 C1 Rh1 -22.8(3) . . . . ? C2 N1 C1 N2 1.6(2) . . . . ? C4 N1 C1 N2 -172.80(19) . . . . ? C2 N1 C1 Rh1 -165.83(16) . . . . ? C4 N1 C1 Rh1 19.8(3) . . . . ? N3 Rh1 C1 N2 111.19(16) . . . . ? N4 Rh1 C1 N2 -9.9(11) . . . . ? Cl1 Rh1 C1 N2 -73.21(15) . . . . ? N3 Rh1 C1 N1 -83.85(19) . . . . ? N4 Rh1 C1 N1 155.1(9) . . . . ? Cl1 Rh1 C1 N1 91.74(18) . . . . ? C1 N1 C2 C3 -1.4(3) . . . . ? C4 N1 C2 C3 173.3(2) . . . . ? N1 C2 C3 N2 0.5(2) . . . . ? C1 N2 C3 C2 0.5(2) . . . . ? C16 N2 C3 C2 -170.04(18) . . . . ? C1 N1 C4 C9 -83.7(3) . . . . ? C2 N1 C4 C9 102.4(2) . . . . ? C1 N1 C4 C5 100.5(2) . . . . ? C2 N1 C4 C5 -73.3(3) . . . . ? C9 C4 C5 C6 3.5(4) . . . . ? N1 C4 C5 C6 179.1(2) . . . . ? C9 C4 C5 C10 -172.1(2) . . . . ? N1 C4 C5 C10 3.5(3) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C10 C5 C6 C7 175.3(3) . . . . ? C5 C6 C7 C8 -1.2(5) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C5 C4 C9 C8 -4.6(3) . . . . ? N1 C4 C9 C8 179.8(2) . . . . ? C5 C4 C9 C13 170.6(2) . . . . ? N1 C4 C9 C13 -5.0(3) . . . . ? C7 C8 C9 C4 2.8(4) . . . . ? C7 C8 C9 C13 -172.4(3) . . . . ? C6 C5 C10 C12 -77.8(3) . . . . ? C4 C5 C10 C12 97.8(3) . . . . ? C6 C5 C10 C11 44.0(3) . . . . ? C4 C5 C10 C11 -140.5(3) . . . . ? C4 C9 C13 C14 152.5(2) . . . . ? C8 C9 C13 C14 -32.6(3) . . . . ? C4 C9 C13 C15 -83.2(3) . . . . ? C8 C9 C13 C15 91.8(3) . . . . ? C1 N2 C16 C17 107.8(2) . . . . ? C3 N2 C16 C17 -83.1(2) . . . . ? C1 N2 C16 C21 -78.3(2) . . . . ? C3 N2 C16 C21 90.8(2) . . . . ? C21 C16 C17 C18 2.3(3) . . . . ? N2 C16 C17 C18 175.91(18) . . . . ? C21 C16 C17 C22 -175.27(19) . . . . ? N2 C16 C17 C22 -1.7(3) . . . . ? C16 C17 C18 C19 -0.4(3) . . . . ? C22 C17 C18 C19 177.3(2) . . . . ? C17 C18 C19 C20 -1.4(4) . . . . ? C18 C19 C20 C21 1.3(4) . . . . ? C19 C20 C21 C16 0.5(3) . . . . ? C19 C20 C21 C25 -176.2(2) . . . . ? C17 C16 C21 C20 -2.4(3) . . . . ? N2 C16 C21 C20 -176.15(18) . . . . ? C17 C16 C21 C25 174.26(19) . . . . ? N2 C16 C21 C25 0.5(3) . . . . ? C18 C17 C22 C24 46.1(3) . . . . ? C16 C17 C22 C24 -136.4(2) . . . . ? C18 C17 C22 C23 -77.3(3) . . . . ? C16 C17 C22 C23 100.2(2) . . . . ? C20 C21 C25 C27 -44.8(3) . . . . ? C16 C21 C25 C27 138.6(2) . . . . ? C20 C21 C25 C26 78.9(3) . . . . ? C16 C21 C25 C26 -97.7(3) . . . . ? C39 N3 C28 C29 1.7(3) . . . . ? Rh1 N3 C28 C29 177.13(18) . . . . ? N3 C28 C29 C30 -0.3(4) . . . . ? C28 C29 C30 C31 -0.6(4) . . . . ? C29 C30 C31 C39 -0.1(3) . . . . ? C29 C30 C31 C32 179.8(2) . . . . ? C30 C31 C32 C33 179.5(2) . . . . ? C39 C31 C32 C33 -0.6(4) . . . . ? C31 C32 C33 C34 -1.7(4) . . . . ? C32 C33 C34 C35 -177.8(2) . . . . ? C32 C33 C34 C38 1.9(4) . . . . ? C38 C34 C35 C36 -1.1(3) . . . . ? C33 C34 C35 C36 178.6(2) . . . . ? C34 C35 C36 C37 1.0(4) . . . . ? C38 N4 C37 C36 -0.3(3) . . . . ? Rh1 N4 C37 C36 177.30(17) . . . . ? C35 C36 C37 N4 -0.3(4) . . . . ? C37 N4 C38 C34 0.1(3) . . . . ? Rh1 N4 C38 C34 -177.85(16) . . . . ? C37 N4 C38 C39 -179.33(18) . . . . ? Rh1 N4 C38 C39 2.7(2) . . . . ? C35 C34 C38 N4 0.6(3) . . . . ? C33 C34 C38 N4 -179.1(2) . . . . ? C35 C34 C38 C39 180.0(2) . . . . ? C33 C34 C38 C39 0.3(3) . . . . ? C28 N3 C39 C31 -2.3(3) . . . . ? Rh1 N3 C39 C31 -178.51(16) . . . . ? C28 N3 C39 C38 176.62(19) . . . . ? Rh1 N3 C39 C38 0.4(2) . . . . ? C30 C31 C39 N3 1.6(3) . . . . ? C32 C31 C39 N3 -178.3(2) . . . . ? C30 C31 C39 C38 -177.3(2) . . . . ? C32 C31 C39 C38 2.8(3) . . . . ? N4 C38 C39 N3 -2.1(3) . . . . ? C34 C38 C39 N3 178.42(18) . . . . ? N4 C38 C39 C31 176.87(18) . . . . ? C34 C38 C39 C31 -2.6(3) . . . . ? C45A C40A C41A C42A 0.0 . . . . ? C40A C41A C42A C43A 0.0 . . . . ? C41A C42A C43A C44A 0.0 . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C43A C44A C45A C40A 0.0 . . . . ? C41A C40A C45A C44A 0.0 . . . . ? C45B C40B C41B C42B 0.0 . . . . ? C40B C41B C42B C43B 0.0 . . . . ? C41B C42B C43B C44B 0.0 . . . . ? C42B C43B C44B C45B 0.0 . . . . ? C41B C40B C45B C44B 0.0 . . . . ? C43B C44B C45B C40B 0.0 . . . . ? C48 C46 C47 C48 0.0(5) 3_557 . . . ? C46 C47 C48 C46 0.0(5) . . . 3_557 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.278 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.050 data_cc119 _database_code_depnum_ccdc_archive 'CCDC 886711' #TrackingRef 'cc119.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H50 Cl N4 Rh' _chemical_formula_weight 761.23 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6065(2) _cell_length_b 12.9410(2) _cell_length_c 15.3621(2) _cell_angle_alpha 76.714(1) _cell_angle_beta 70.664(1) _cell_angle_gamma 79.213(1) _cell_volume 1922.18(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7266 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 27.05 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8527 _exptl_absorpt_correction_T_max 0.9472 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14674 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7498 _reflns_number_gt 6541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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. Disorder Modelling: One of the isopropyl groups is disordered with its two methyl groups. The two methyl groups were thus split into 3 groups. SHELX commands, SUMP, PART, SADI and EADP were applied to refine the disorder. ; _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^)+(0.0350P)^2^+1.2173P] 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 7498 _refine_ls_number_parameters 455 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 0.40838(2) 0.120636(15) 0.278206(13) 0.02441(7) Uani 1 1 d . . . Cl1 Cl 0.22101(7) 0.08059(5) 0.24810(5) 0.03560(15) Uani 1 1 d . . . N1 N 0.3997(2) 0.29341(16) 0.10868(13) 0.0232(4) Uani 1 1 d . . . N2 N 0.3503(2) 0.36365(16) 0.23130(13) 0.0245(4) Uani 1 1 d . . . N3 N 0.5776(2) 0.12932(17) 0.30404(14) 0.0287(5) Uani 1 1 d . . . N4 N 0.4314(2) -0.02710(17) 0.36133(15) 0.0326(5) Uani 1 1 d . . . C1 C 0.3880(2) 0.26610(19) 0.20273(16) 0.0226(5) Uani 1 1 d . . . C2 C 0.3700(3) 0.4022(2) 0.08176(17) 0.0296(6) Uani 1 1 d . . . H2A H 0.3721 0.4388 0.0202 0.036 Uiso 1 1 calc R . . C3 C 0.3380(3) 0.4467(2) 0.15748(17) 0.0311(6) Uani 1 1 d . . . H3A H 0.3118 0.5204 0.1606 0.037 Uiso 1 1 calc R . . C4 C 0.4317(3) 0.22281(19) 0.04114(16) 0.0241(5) Uani 1 1 d . . . C5 C 0.5650(2) 0.17675(19) 0.00729(16) 0.0252(5) Uani 1 1 d . . . C6 C 0.5943(3) 0.1184(2) -0.06437(17) 0.0305(6) Uani 1 1 d . . . H6A H 0.6835 0.0856 -0.0884 0.037 Uiso 1 1 calc R . . C7 C 0.4962(3) 0.1075(2) -0.10103(18) 0.0326(6) Uani 1 1 d . . . H7A H 0.5182 0.0682 -0.1503 0.039 Uiso 1 1 calc R . . C8 C 0.3664(3) 0.1536(2) -0.06619(17) 0.0305(6) Uani 1 1 d . . . H8A H 0.2997 0.1456 -0.0921 0.037 Uiso 1 1 calc R . . C9 C 0.3300(3) 0.2119(2) 0.00608(17) 0.0262(5) Uani 1 1 d . . . C10 C 0.6736(3) 0.1918(2) 0.04555(18) 0.0288(5) Uani 1 1 d . . . H10A H 0.6277 0.2061 0.1107 0.035 Uiso 1 1 calc R . . C11 C 0.7424(4) 0.2898(3) -0.0107(3) 0.0552(9) Uani 1 1 d . . . H11A H 0.6743 0.3520 -0.0142 0.083 Uiso 1 1 calc R . . H11B H 0.7935 0.2773 -0.0742 0.083 Uiso 1 1 calc R . . H11C H 0.8037 0.3033 0.0200 0.083 Uiso 1 1 calc R . . C12 C 0.7754(4) 0.0939(3) 0.0530(3) 0.0622(11) Uani 1 1 d . . . H12A H 0.7286 0.0323 0.0902 0.093 Uiso 1 1 calc R . . H12B H 0.8375 0.1066 0.0835 0.093 Uiso 1 1 calc R . . H12C H 0.8262 0.0794 -0.0099 0.093 Uiso 1 1 calc R . . C13 C 0.1837(3) 0.2599(2) 0.04375(19) 0.0346(6) Uani 1 1 d D . . H13A H 0.1723 0.2807 0.1049 0.042 Uiso 1 1 calc RD . . C14 C 0.0865(3) 0.1786(3) 0.0618(2) 0.0487(8) Uani 1 1 d . . . H14A H 0.1100 0.1144 0.1044 0.073 Uiso 1 1 calc R . . H14B H 0.0927 0.1594 0.0024 0.073 Uiso 1 1 calc R . . H14C H -0.0056 0.2099 0.0904 0.073 Uiso 1 1 calc R . . C15 C 0.1465(3) 0.3606(3) -0.0225(2) 0.0513(8) Uani 1 1 d . . . H15A H 0.2082 0.4132 -0.0335 0.077 Uiso 1 1 calc R . . H15B H 0.0540 0.3912 0.0060 0.077 Uiso 1 1 calc R . . H15C H 0.1534 0.3418 -0.0823 0.077 Uiso 1 1 calc R . . C16 C 0.3227(3) 0.3863(2) 0.32455(16) 0.0272(5) Uani 1 1 d . . . C17 C 0.2103(3) 0.3487(2) 0.39677(18) 0.0320(6) Uani 1 1 d . A . C18 C 0.1829(3) 0.3786(3) 0.4831(2) 0.0430(7) Uani 1 1 d . . . H18A H 0.1093 0.3531 0.5339 0.052 Uiso 1 1 calc R . . C19 C 0.2602(3) 0.4445(3) 0.4967(2) 0.0459(8) Uani 1 1 d . . . H19A H 0.2391 0.4638 0.5564 0.055 Uiso 1 1 calc R . . C20 C 0.3673(3) 0.4825(2) 0.4249(2) 0.0393(7) Uani 1 1 d . . . H20A H 0.4181 0.5291 0.4352 0.047 Uiso 1 1 calc R . . C21 C 0.4030(3) 0.4539(2) 0.33661(17) 0.0304(6) Uani 1 1 d . . . C22 C 0.5229(3) 0.4986(2) 0.2601(2) 0.0361(6) Uani 1 1 d . . . H22A H 0.5451 0.4604 0.2062 0.043 Uiso 1 1 calc R . . C23 C 0.4897(4) 0.6187(2) 0.2250(2) 0.0510(8) Uani 1 1 d . . . H23A H 0.4103 0.6301 0.2033 0.076 Uiso 1 1 calc R . . H23B H 0.5664 0.6447 0.1731 0.076 Uiso 1 1 calc R . . H23C H 0.4714 0.6578 0.2763 0.076 Uiso 1 1 calc R . . C24 C 0.6479(3) 0.4822(3) 0.2937(2) 0.0510(8) Uani 1 1 d . . . H24A H 0.6703 0.4058 0.3158 0.076 Uiso 1 1 calc R . . H24B H 0.6291 0.5214 0.3450 0.076 Uiso 1 1 calc R . . H24C H 0.7239 0.5090 0.2415 0.076 Uiso 1 1 calc R . . C25 C 0.1151(3) 0.2847(2) 0.38333(19) 0.0353(6) Uani 1 1 d D . . H25A H 0.144(3) 0.2501(12) 0.3355(11) 0.042 Uiso 1 1 d D . . C26A C 0.0982(10) 0.1789(6) 0.4592(5) 0.0405(9) Uani 0.518(17) 1 d PD A 1 H26A H 0.1866 0.1456 0.4652 0.061 Uiso 0.518(17) 1 calc PR A 1 H26B H 0.0578 0.1293 0.4399 0.061 Uiso 0.518(17) 1 calc PR A 1 H26C H 0.0398 0.1961 0.5198 0.061 Uiso 0.518(17) 1 calc PR A 1 C27A C -0.0234(6) 0.3473(6) 0.3936(8) 0.0405(9) Uani 0.518(17) 1 d PD A 1 H27A H -0.0834 0.3238 0.4565 0.061 Uiso 0.518(17) 1 calc PR A 1 H27B H -0.0595 0.3348 0.3464 0.061 Uiso 0.518(17) 1 calc PR A 1 H27C H -0.0167 0.4238 0.3847 0.061 Uiso 0.518(17) 1 calc PR A 1 C26B C 0.0298(13) 0.2329(14) 0.4685(7) 0.0405(9) Uani 0.244(9) 1 d PD A 2 H26D H 0.0839 0.1768 0.5002 0.061 Uiso 0.244(9) 1 calc PR A 2 H26E H -0.0367 0.2010 0.4548 0.061 Uiso 0.244(9) 1 calc PR A 2 H26F H -0.0166 0.2853 0.5093 0.061 Uiso 0.244(9) 1 calc PR A 2 C27B C 0.0323(15) 0.3707(9) 0.3207(11) 0.0405(9) Uani 0.244(9) 1 d PD A 2 H27D H 0.0922 0.4210 0.2759 0.061 Uiso 0.244(9) 1 calc PR A 2 H27E H -0.0433 0.4100 0.3618 0.061 Uiso 0.244(9) 1 calc PR A 2 H27F H -0.0021 0.3330 0.2864 0.061 Uiso 0.244(9) 1 calc PR A 2 C26C C 0.061(2) 0.1861(19) 0.4600(11) 0.0405(9) Uani 0.238(15) 1 d PD A 3 H26G H 0.1358 0.1396 0.4776 0.061 Uiso 0.238(15) 1 calc PR A 3 H26H H 0.0157 0.1457 0.4346 0.061 Uiso 0.238(15) 1 calc PR A 3 H26I H -0.0038 0.2115 0.5155 0.061 Uiso 0.238(15) 1 calc PR A 3 C27C C -0.0036(19) 0.3594(12) 0.357(2) 0.0405(9) Uani 0.238(15) 1 d PD A 3 H27G H 0.0042 0.3600 0.2917 0.061 Uiso 0.238(15) 1 calc PR A 3 H27H H -0.0018 0.4321 0.3651 0.061 Uiso 0.238(15) 1 calc PR A 3 H27I H -0.0886 0.3337 0.3981 0.061 Uiso 0.238(15) 1 calc PR A 3 C28 C 0.6545(3) 0.2113(2) 0.27025(17) 0.0299(6) Uani 1 1 d . . . H28A H 0.6189 0.2766 0.2388 0.036 Uiso 1 1 calc R . . C29 C 0.7803(3) 0.2051(3) 0.2789(2) 0.0428(7) Uani 1 1 d . . . H29A H 0.8300 0.2647 0.2529 0.051 Uiso 1 1 calc R . . C30 C 0.8350(3) 0.1123(3) 0.3256(2) 0.0493(8) Uani 1 1 d . . . H30A H 0.9229 0.1058 0.3309 0.059 Uiso 1 1 calc R . . C31 C 0.7571(3) 0.0299(3) 0.3638(2) 0.0468(8) Uani 1 1 d . . . H31A H 0.7905 -0.0340 0.3982 0.056 Uiso 1 1 calc R . . C32 C 0.6303(3) 0.0383(2) 0.35304(18) 0.0344(6) Uani 1 1 d . . . C33 C 0.5443(3) -0.0473(2) 0.38884(18) 0.0370(7) Uani 1 1 d . . . C34 C 0.5708(4) -0.1428(3) 0.4480(2) 0.0524(9) Uani 1 1 d . . . H34A H 0.6498 -0.1558 0.4670 0.063 Uiso 1 1 calc R . . C35 C 0.4823(4) -0.2173(3) 0.4784(2) 0.0591(10) Uani 1 1 d . . . H35A H 0.4992 -0.2825 0.5187 0.071 Uiso 1 1 calc R . . C36 C 0.3685(4) -0.1967(3) 0.4500(2) 0.0551(9) Uani 1 1 d . . . H36A H 0.3063 -0.2478 0.4702 0.066 Uiso 1 1 calc R . . C37 C 0.3454(3) -0.1015(2) 0.3923(2) 0.0426(7) Uani 1 1 d . . . H37A H 0.2660 -0.0877 0.3736 0.051 Uiso 1 1 calc R . . C38 C 0.9516(5) 0.1474(4) 0.7527(3) 0.0773(14) Uani 1 1 d . . . H38A H 0.9233 0.0799 0.7587 0.093 Uiso 1 1 calc R . . C39 C 0.8788(4) 0.2402(4) 0.7213(3) 0.0720(12) Uani 1 1 d . . . H39A H 0.8006 0.2372 0.7052 0.086 Uiso 1 1 calc R . . C40 C 0.9212(4) 0.3378(3) 0.7135(2) 0.0590(10) Uani 1 1 d . . . H40A H 0.8724 0.4024 0.6919 0.071 Uiso 1 1 calc R . . C41 C 1.0333(4) 0.3403(3) 0.7371(2) 0.0561(9) Uani 1 1 d . . . H41A H 1.0620 0.4071 0.7328 0.067 Uiso 1 1 calc R . . C42 C 1.1038(4) 0.2485(3) 0.7667(3) 0.0660(10) Uani 1 1 d . . . H42A H 1.1829 0.2515 0.7817 0.079 Uiso 1 1 calc R . . C43 C 1.0638(5) 0.1525(3) 0.7752(3) 0.0734(12) Uani 1 1 d . . . H43A H 1.1140 0.0887 0.7968 0.088 Uiso 1 1 calc R . . _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 0.02688(12) 0.02160(11) 0.02494(11) -0.00281(7) -0.00930(8) -0.00239(7) Cl1 0.0342(4) 0.0337(4) 0.0435(4) -0.0056(3) -0.0150(3) -0.0107(3) N1 0.0269(11) 0.0223(10) 0.0222(9) -0.0043(8) -0.0091(8) -0.0035(8) N2 0.0309(11) 0.0219(10) 0.0218(10) -0.0041(8) -0.0102(9) -0.0014(8) N3 0.0287(12) 0.0314(12) 0.0249(10) -0.0062(9) -0.0084(9) 0.0010(9) N4 0.0396(13) 0.0254(12) 0.0286(11) -0.0032(9) -0.0071(10) -0.0013(10) C1 0.0206(12) 0.0255(13) 0.0237(11) -0.0061(10) -0.0074(10) -0.0037(10) C2 0.0408(16) 0.0234(13) 0.0259(12) -0.0017(10) -0.0139(11) -0.0034(11) C3 0.0441(16) 0.0217(13) 0.0290(13) -0.0038(10) -0.0164(12) 0.0008(11) C4 0.0304(13) 0.0204(12) 0.0216(11) -0.0031(9) -0.0074(10) -0.0043(10) C5 0.0267(13) 0.0222(12) 0.0252(12) -0.0008(10) -0.0074(10) -0.0046(10) C6 0.0321(14) 0.0260(13) 0.0299(13) -0.0061(11) -0.0050(11) -0.0018(11) C7 0.0444(17) 0.0272(14) 0.0268(13) -0.0080(11) -0.0085(12) -0.0061(12) C8 0.0374(15) 0.0300(14) 0.0297(13) -0.0070(11) -0.0148(12) -0.0074(11) C9 0.0281(13) 0.0249(13) 0.0269(12) -0.0040(10) -0.0090(11) -0.0056(10) C10 0.0250(13) 0.0298(14) 0.0310(13) -0.0052(11) -0.0080(11) -0.0029(10) C11 0.062(2) 0.0444(19) 0.071(2) 0.0089(16) -0.0393(19) -0.0242(16) C12 0.050(2) 0.0395(19) 0.117(3) -0.016(2) -0.054(2) 0.0011(15) C13 0.0284(14) 0.0441(17) 0.0367(14) -0.0155(12) -0.0133(12) -0.0009(12) C14 0.0309(16) 0.073(2) 0.0480(17) -0.0167(16) -0.0126(14) -0.0126(15) C15 0.0433(18) 0.052(2) 0.065(2) -0.0188(16) -0.0287(17) 0.0112(15) C16 0.0345(14) 0.0253(13) 0.0243(12) -0.0062(10) -0.0142(11) 0.0027(10) C17 0.0340(15) 0.0337(15) 0.0289(13) -0.0080(11) -0.0118(11) 0.0018(11) C18 0.0421(17) 0.057(2) 0.0306(14) -0.0147(13) -0.0085(13) -0.0037(14) C19 0.054(2) 0.059(2) 0.0301(14) -0.0196(14) -0.0160(14) 0.0013(16) C20 0.0504(18) 0.0374(16) 0.0411(16) -0.0151(13) -0.0246(14) -0.0018(13) C21 0.0388(15) 0.0255(13) 0.0300(13) -0.0054(10) -0.0162(12) -0.0002(11) C22 0.0429(17) 0.0307(15) 0.0396(15) -0.0090(12) -0.0158(13) -0.0070(12) C23 0.068(2) 0.0313(17) 0.0543(19) -0.0016(14) -0.0188(17) -0.0146(15) C24 0.0472(19) 0.053(2) 0.062(2) -0.0135(16) -0.0224(16) -0.0135(16) C25 0.0362(16) 0.0356(16) 0.0354(14) -0.0116(12) -0.0099(13) -0.0025(12) C26A 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C27A 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C26B 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C27B 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C26C 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C27C 0.036(2) 0.043(2) 0.0417(18) 0.0013(17) -0.013(2) -0.0119(16) C28 0.0285(14) 0.0350(15) 0.0304(13) -0.0060(11) -0.0134(11) -0.0053(11) C29 0.0326(16) 0.055(2) 0.0463(17) -0.0172(15) -0.0122(13) -0.0077(14) C30 0.0343(17) 0.063(2) 0.060(2) -0.0231(17) -0.0248(16) 0.0049(15) C31 0.0446(18) 0.052(2) 0.0475(17) -0.0143(15) -0.0265(15) 0.0142(15) C32 0.0363(15) 0.0359(15) 0.0305(13) -0.0085(11) -0.0136(12) 0.0061(12) C33 0.0426(17) 0.0339(15) 0.0281(13) -0.0054(11) -0.0091(12) 0.0076(12) C34 0.061(2) 0.0420(19) 0.0454(17) 0.0008(14) -0.0199(16) 0.0110(16) C35 0.078(3) 0.0334(18) 0.0471(18) 0.0082(14) -0.0111(18) 0.0066(17) C36 0.070(2) 0.0306(17) 0.0501(19) 0.0020(14) -0.0030(18) -0.0107(16) C37 0.0499(19) 0.0308(16) 0.0419(16) -0.0017(13) -0.0086(14) -0.0082(13) C38 0.100(4) 0.057(3) 0.065(2) -0.031(2) 0.015(2) -0.033(3) C39 0.047(2) 0.115(4) 0.059(2) -0.049(3) 0.0019(18) -0.014(2) C40 0.064(2) 0.061(2) 0.0415(18) -0.0137(16) -0.0064(17) 0.0058(19) C41 0.073(3) 0.049(2) 0.0458(18) -0.0086(16) -0.0109(18) -0.0185(18) C42 0.081(3) 0.073(3) 0.053(2) -0.0185(19) -0.029(2) -0.004(2) C43 0.111(4) 0.051(2) 0.050(2) -0.0099(18) -0.020(2) 0.006(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. ; _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 C1 1.986(2) . ? Rh1 N3 1.990(2) . ? Rh1 N4 2.063(2) . ? Rh1 Cl1 2.3530(7) . ? N1 C1 1.375(3) . ? N1 C2 1.380(3) . ? N1 C4 1.454(3) . ? N2 C1 1.377(3) . ? N2 C3 1.394(3) . ? N2 C16 1.452(3) . ? N3 C28 1.360(3) . ? N3 C32 1.375(3) . ? N4 C37 1.348(4) . ? N4 C33 1.359(4) . ? C2 C3 1.331(4) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.397(3) . ? C4 C5 1.402(3) . ? C5 C6 1.395(3) . ? C5 C10 1.515(3) . ? C6 C7 1.378(4) . ? C6 H6A 0.9500 . ? C7 C8 1.375(4) . ? C7 H7A 0.9500 . ? C8 C9 1.394(3) . ? C8 H8A 0.9500 . ? C9 C13 1.529(4) . ? C10 C12 1.513(4) . ? C10 C11 1.520(4) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.525(4) . ? C13 C15 1.535(4) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.408(4) . ? C16 C21 1.408(4) . ? C17 C18 1.390(4) . ? C17 C25 1.509(4) . ? C18 C19 1.379(4) . ? C18 H18A 0.9500 . ? C19 C20 1.371(4) . ? C19 H19A 0.9500 . ? C20 C21 1.399(4) . ? C20 H20A 0.9500 . ? C21 C22 1.518(4) . ? C22 C24 1.538(4) . ? C22 C23 1.538(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26B 1.421(9) . ? C25 C27A 1.516(6) . ? C25 C27C 1.544(10) . ? C25 C26A 1.577(6) . ? C25 C26C 1.577(14) . ? C25 C27B 1.625(9) . ? C25 H25A 0.886(17) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C26C H26G 0.9800 . ? C26C H26H 0.9800 . ? C26C H26I 0.9800 . ? C27C H27G 0.9800 . ? C27C H27H 0.9800 . ? C27C H27I 0.9800 . ? C28 C29 1.371(4) . ? C28 H28A 0.9500 . ? C29 C30 1.382(5) . ? C29 H29A 0.9500 . ? C30 C31 1.373(5) . ? C30 H30A 0.9500 . ? C31 C32 1.391(4) . ? C31 H31A 0.9500 . ? C32 C33 1.458(4) . ? C33 C34 1.398(4) . ? C34 C35 1.368(5) . ? C34 H34A 0.9500 . ? C35 C36 1.376(5) . ? C35 H35A 0.9500 . ? C36 C37 1.377(4) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C43 1.361(6) . ? C38 C39 1.381(6) . ? C38 H38A 0.9500 . ? C39 C40 1.385(6) . ? C39 H39A 0.9500 . ? C40 C41 1.360(5) . ? C40 H40A 0.9500 . ? C41 C42 1.349(5) . ? C41 H41A 0.9500 . ? C42 C43 1.352(6) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? _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 C1 Rh1 N3 98.50(9) . . ? C1 Rh1 N4 177.18(9) . . ? N3 Rh1 N4 79.57(9) . . ? C1 Rh1 Cl1 89.45(7) . . ? N3 Rh1 Cl1 170.66(6) . . ? N4 Rh1 Cl1 92.65(7) . . ? C1 N1 C2 111.65(19) . . ? C1 N1 C4 128.11(19) . . ? C2 N1 C4 120.18(19) . . ? C1 N2 C3 111.72(19) . . ? C1 N2 C16 128.29(19) . . ? C3 N2 C16 120.0(2) . . ? C28 N3 C32 116.1(2) . . ? C28 N3 Rh1 127.07(17) . . ? C32 N3 Rh1 116.40(18) . . ? C37 N4 C33 118.4(2) . . ? C37 N4 Rh1 126.9(2) . . ? C33 N4 Rh1 114.66(18) . . ? N1 C1 N2 102.48(19) . . ? N1 C1 Rh1 127.95(17) . . ? N2 C1 Rh1 129.44(16) . . ? C3 C2 N1 107.7(2) . . ? C3 C2 H2A 126.1 . . ? N1 C2 H2A 126.1 . . ? C2 C3 N2 106.4(2) . . ? C2 C3 H3A 126.8 . . ? N2 C3 H3A 126.8 . . ? C9 C4 C5 122.6(2) . . ? C9 C4 N1 118.0(2) . . ? C5 C4 N1 119.1(2) . . ? C6 C5 C4 117.4(2) . . ? C6 C5 C10 121.3(2) . . ? C4 C5 C10 121.3(2) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 121.8(2) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C9 C4 117.1(2) . . ? C8 C9 C13 119.8(2) . . ? C4 C9 C13 123.1(2) . . ? C12 C10 C5 113.6(2) . . ? C12 C10 C11 111.2(3) . . ? C5 C10 C11 111.0(2) . . ? C12 C10 H10A 106.9 . . ? C5 C10 H10A 106.9 . . ? C11 C10 H10A 106.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 111.4(2) . . ? C14 C13 C15 109.5(2) . . ? C9 C13 C15 112.1(2) . . ? C14 C13 H13A 107.9 . . ? C9 C13 H13A 107.9 . . ? C15 C13 H13A 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.5(2) . . ? C17 C16 N2 119.3(2) . . ? C21 C16 N2 117.9(2) . . ? C18 C17 C16 117.1(3) . . ? C18 C17 C25 119.2(3) . . ? C16 C17 C25 123.6(2) . . ? C19 C18 C17 121.5(3) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 121.2(3) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 117.1(3) . . ? C20 C21 C22 118.5(2) . . ? C16 C21 C22 124.4(2) . . ? C21 C22 C24 112.1(2) . . ? C21 C22 C23 111.0(2) . . ? C24 C22 C23 108.7(2) . . ? C21 C22 H22A 108.3 . . ? C24 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26B C25 C17 114.0(6) . . ? C26B C25 C27A 74.5(8) . . ? C17 C25 C27A 111.4(3) . . ? C17 C25 C27C 110.5(6) . . ? C17 C25 C26A 110.3(4) . . ? C27A C25 C26A 107.5(4) . . ? C17 C25 C26C 120.6(8) . . ? C27C C25 C26C 109.6(7) . . ? C26B C25 C27B 112.9(7) . . ? C17 C25 C27B 104.2(5) . . ? C26B C25 H25A 116.8(16) . . ? C17 C25 H25A 118.6(19) . . ? C27A C25 H25A 113.5(15) . . ? C27C C25 H25A 99.1(14) . . ? C26A C25 H25A 93.6(11) . . ? C26C C25 H25A 95.7(14) . . ? C27B C25 H25A 85.7(10) . . ? C25 C26A H26A 109.5 . . ? C25 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25 C27A H27A 109.5 . . ? C25 C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25 C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C25 C26B H26D 109.5 . . ? C25 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C25 C27B H27D 109.5 . . ? C25 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C25 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C25 C26C H26G 109.5 . . ? C25 C26C H26H 109.5 . . ? H26G C26C H26H 109.5 . . ? C25 C26C H26I 109.5 . . ? H26G C26C H26I 109.5 . . ? H26H C26C H26I 109.5 . . ? C25 C27C H27G 109.5 . . ? C25 C27C H27H 109.5 . . ? H27G C27C H27H 109.5 . . ? C25 C27C H27I 109.5 . . ? H27G C27C H27I 109.5 . . ? H27H C27C H27I 109.5 . . ? N3 C28 C29 123.7(3) . . ? N3 C28 H28A 118.1 . . ? C29 C28 H28A 118.1 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 117.4(3) . . ? C31 C30 H30A 121.3 . . ? C29 C30 H30A 121.3 . . ? C30 C31 C32 121.2(3) . . ? C30 C31 H31A 119.4 . . ? C32 C31 H31A 119.4 . . ? N3 C32 C31 121.5(3) . . ? N3 C32 C33 114.4(2) . . ? C31 C32 C33 124.1(3) . . ? N4 C33 C34 121.0(3) . . ? N4 C33 C32 114.5(2) . . ? C34 C33 C32 124.5(3) . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? C35 C36 C37 119.5(3) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? N4 C37 C36 122.2(3) . . ? N4 C37 H37A 118.9 . . ? C36 C37 H37A 118.9 . . ? C43 C38 C39 120.0(4) . . ? C43 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 C40 119.1(4) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.4 . . ? C41 C40 C39 119.5(4) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C42 C41 C40 120.4(4) . . ? C42 C41 H41A 119.8 . . ? C40 C41 H41A 119.8 . . ? C41 C42 C43 121.1(4) . . ? C41 C42 H42A 119.5 . . ? C43 C42 H42A 119.5 . . ? C42 C43 C38 119.9(4) . . ? C42 C43 H43A 120.0 . . ? C38 C43 H43A 120.0 . . ? _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 C1 Rh1 N3 C28 -4.5(2) . . . . ? N4 Rh1 N3 C28 177.6(2) . . . . ? C1 Rh1 N3 C32 -176.98(18) . . . . ? N4 Rh1 N3 C32 5.10(18) . . . . ? N3 Rh1 N4 C37 175.7(2) . . . . ? Cl1 Rh1 N4 C37 -9.5(2) . . . . ? N3 Rh1 N4 C33 -2.02(18) . . . . ? Cl1 Rh1 N4 C33 172.77(18) . . . . ? C2 N1 C1 N2 -0.2(3) . . . . ? C4 N1 C1 N2 -177.2(2) . . . . ? C2 N1 C1 Rh1 175.96(18) . . . . ? C4 N1 C1 Rh1 -1.0(4) . . . . ? C3 N2 C1 N1 0.8(3) . . . . ? C16 N2 C1 N1 180.0(2) . . . . ? C3 N2 C1 Rh1 -175.32(18) . . . . ? C16 N2 C1 Rh1 3.9(4) . . . . ? N3 Rh1 C1 N1 111.7(2) . . . . ? Cl1 Rh1 C1 N1 -63.4(2) . . . . ? N3 Rh1 C1 N2 -73.2(2) . . . . ? Cl1 Rh1 C1 N2 111.8(2) . . . . ? C1 N1 C2 C3 -0.4(3) . . . . ? C4 N1 C2 C3 176.8(2) . . . . ? N1 C2 C3 N2 0.9(3) . . . . ? C1 N2 C3 C2 -1.1(3) . . . . ? C16 N2 C3 C2 179.7(2) . . . . ? C1 N1 C4 C9 110.2(3) . . . . ? C2 N1 C4 C9 -66.6(3) . . . . ? C1 N1 C4 C5 -75.7(3) . . . . ? C2 N1 C4 C5 107.5(3) . . . . ? C9 C4 C5 C6 0.2(4) . . . . ? N1 C4 C5 C6 -173.6(2) . . . . ? C9 C4 C5 C10 178.8(2) . . . . ? N1 C4 C5 C10 5.1(3) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C10 C5 C6 C7 -178.0(2) . . . . ? C5 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C4 0.8(4) . . . . ? C7 C8 C9 C13 -178.8(2) . . . . ? C5 C4 C9 C8 -0.8(4) . . . . ? N1 C4 C9 C8 173.0(2) . . . . ? C5 C4 C9 C13 178.7(2) . . . . ? N1 C4 C9 C13 -7.4(3) . . . . ? C6 C5 C10 C12 -38.2(4) . . . . ? C4 C5 C10 C12 143.2(3) . . . . ? C6 C5 C10 C11 87.9(3) . . . . ? C4 C5 C10 C11 -90.7(3) . . . . ? C8 C9 C13 C14 46.7(3) . . . . ? C4 C9 C13 C14 -132.9(3) . . . . ? C8 C9 C13 C15 -76.4(3) . . . . ? C4 C9 C13 C15 104.0(3) . . . . ? C1 N2 C16 C17 -66.4(3) . . . . ? C3 N2 C16 C17 112.7(3) . . . . ? C1 N2 C16 C21 119.3(3) . . . . ? C3 N2 C16 C21 -61.5(3) . . . . ? C21 C16 C17 C18 -1.8(4) . . . . ? N2 C16 C17 C18 -175.8(2) . . . . ? C21 C16 C17 C25 174.2(2) . . . . ? N2 C16 C17 C25 0.2(4) . . . . ? C16 C17 C18 C19 1.7(4) . . . . ? C25 C17 C18 C19 -174.5(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 -1.4(5) . . . . ? C19 C20 C21 C16 1.3(4) . . . . ? C19 C20 C21 C22 -179.9(3) . . . . ? C17 C16 C21 C20 0.4(4) . . . . ? N2 C16 C21 C20 174.4(2) . . . . ? C17 C16 C21 C22 -178.4(2) . . . . ? N2 C16 C21 C22 -4.4(4) . . . . ? C20 C21 C22 C24 50.3(3) . . . . ? C16 C21 C22 C24 -130.9(3) . . . . ? C20 C21 C22 C23 -71.5(3) . . . . ? C16 C21 C22 C23 107.3(3) . . . . ? C18 C17 C25 C26B -18.8(9) . . . . ? C16 C17 C25 C26B 165.2(8) . . . . ? C18 C17 C25 C27A 63.1(6) . . . . ? C16 C17 C25 C27A -112.8(6) . . . . ? C18 C17 C25 C27C 84.3(13) . . . . ? C16 C17 C25 C27C -91.6(13) . . . . ? C18 C17 C25 C26A -56.2(5) . . . . ? C16 C17 C25 C26A 127.8(4) . . . . ? C18 C17 C25 C26C -45.4(13) . . . . ? C16 C17 C25 C26C 138.7(12) . . . . ? C18 C17 C25 C27B 104.7(7) . . . . ? C16 C17 C25 C27B -71.3(7) . . . . ? C32 N3 C28 C29 3.1(4) . . . . ? Rh1 N3 C28 C29 -169.4(2) . . . . ? N3 C28 C29 C30 -1.1(4) . . . . ? C28 C29 C30 C31 -1.6(4) . . . . ? C29 C30 C31 C32 2.2(5) . . . . ? C28 N3 C32 C31 -2.4(4) . . . . ? Rh1 N3 C32 C31 170.9(2) . . . . ? C28 N3 C32 C33 179.5(2) . . . . ? Rh1 N3 C32 C33 -7.2(3) . . . . ? C30 C31 C32 N3 -0.2(4) . . . . ? C30 C31 C32 C33 177.7(3) . . . . ? C37 N4 C33 C34 -0.2(4) . . . . ? Rh1 N4 C33 C34 177.8(2) . . . . ? C37 N4 C33 C32 -179.1(2) . . . . ? Rh1 N4 C33 C32 -1.2(3) . . . . ? N3 C32 C33 N4 5.4(3) . . . . ? C31 C32 C33 N4 -172.7(3) . . . . ? N3 C32 C33 C34 -173.5(3) . . . . ? C31 C32 C33 C34 8.4(4) . . . . ? N4 C33 C34 C35 0.3(5) . . . . ? C32 C33 C34 C35 179.2(3) . . . . ? C33 C34 C35 C36 0.0(5) . . . . ? C34 C35 C36 C37 -0.5(5) . . . . ? C33 N4 C37 C36 -0.3(4) . . . . ? Rh1 N4 C37 C36 -178.0(2) . . . . ? C35 C36 C37 N4 0.6(5) . . . . ? C43 C38 C39 C40 -0.3(6) . . . . ? C38 C39 C40 C41 -0.1(5) . . . . ? C39 C40 C41 C42 0.9(5) . . . . ? C40 C41 C42 C43 -1.2(6) . . . . ? C41 C42 C43 C38 0.8(6) . . . . ? C39 C38 C43 C42 0.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.531 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.060 data_cc126 _database_code_depnum_ccdc_archive 'CCDC 886712' #TrackingRef 'cc126.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.15 H67.15 Cl3 N6 Rh' _chemical_formula_weight 1011.35 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5027(4) _cell_length_b 20.8414(6) _cell_length_c 21.4998(6) _cell_angle_alpha 99.447(2) _cell_angle_beta 104.641(2) _cell_angle_gamma 94.874(2) _cell_volume 5299.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6375 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.20 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9504 _exptl_absorpt_correction_T_max 0.9698 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53751 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 20736 _reflns_number_gt 11824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disorder Modelling: Some of the solvent benzene molecules are disordered. SHELX commands, PART, DFIX, EADP and SAME were applied to resolve the disorder. ; _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^)+(0.0576P)^2^+4.1580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20736 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 0.02792(4) 0.32583(2) 0.05607(2) 0.03943(14) Uani 1 1 d . . . Rh2 Rh 0.78029(4) 0.135349(19) 0.50466(2) 0.03170(12) Uani 1 1 d . . . Cl1 Cl 0.05565(16) 0.22217(7) 0.00585(8) 0.0608(5) Uani 1 1 d . . . Cl2 Cl 0.65505(12) 0.16036(6) 0.56782(7) 0.0422(3) Uani 1 1 d . . . Cl3 Cl 0.20974(16) 0.55811(9) 0.99706(9) 0.0700(5) Uani 1 1 d . . . Cl4 Cl 0.88583(12) 0.87172(7) 0.44130(8) 0.0513(4) Uani 1 1 d . . . Cl5 Cl 0.98475(16) 0.48922(8) 0.23721(8) 0.0630(5) Uani 1 1 d . . . Cl6 Cl 0.95352(14) 0.14590(7) 0.32678(7) 0.0502(4) Uani 1 1 d . . . N1 N 0.1320(4) 0.2903(2) 0.1924(2) 0.0408(12) Uani 1 1 d . . . N2 N -0.0444(4) 0.2571(2) 0.1591(2) 0.0385(11) Uani 1 1 d . . . N3 N 0.0047(4) 0.3544(2) -0.0368(2) 0.0458(12) Uani 1 1 d . . . N4 N -0.1416(4) 0.3013(2) 0.0148(2) 0.0499(13) Uani 1 1 d . . . H4A H -0.1679 0.2678 0.0322 0.060 Uiso 1 1 calc R . . H4B H -0.1774 0.3369 0.0243 0.060 Uiso 1 1 calc R . . N5 N 0.1897(4) 0.3666(2) 0.0806(2) 0.0476(13) Uani 1 1 d . . . N6 N 0.0088(4) 0.4184(2) 0.0991(2) 0.0393(11) Uani 1 1 d . . . H6B H -0.0533 0.4318 0.0740 0.047 Uiso 1 1 calc R . . H6C H -0.0016 0.4175 0.1398 0.047 Uiso 1 1 calc R . . N7 N 0.7637(4) 0.26781(19) 0.4584(2) 0.0340(10) Uani 1 1 d . . . N8 N 0.6363(4) 0.19502(19) 0.3920(2) 0.0336(10) Uani 1 1 d . . . N9 N 0.6791(4) 0.0552(2) 0.4436(2) 0.0347(10) Uani 1 1 d . . . N10 N 0.8866(3) 0.10674(18) 0.4492(2) 0.0317(10) Uani 1 1 d . . . H10B H 0.8875 0.1340 0.4197 0.038 Uiso 1 1 calc R . . H10C H 0.9578 0.1102 0.4761 0.038 Uiso 1 1 calc R . . N11 N 0.8451(4) 0.0725(2) 0.5704(2) 0.0338(10) Uani 1 1 d . . . N12 N 0.9073(4) 0.19817(19) 0.5753(2) 0.0357(11) Uani 1 1 d . . . H12D H 0.9732 0.1965 0.5638 0.043 Uiso 1 1 calc R . . H12E H 0.8909 0.2406 0.5780 0.043 Uiso 1 1 calc R . . C1 C 0.0401(5) 0.2899(2) 0.1410(3) 0.0360(13) Uani 1 1 d . . . C2 C 0.1028(5) 0.2589(3) 0.2393(3) 0.0472(15) Uani 1 1 d . . . H2A H 0.1518 0.2532 0.2791 0.057 Uiso 1 1 calc R . . C3 C -0.0049(5) 0.2386(3) 0.2184(3) 0.0470(15) Uani 1 1 d . . . H3A H -0.0478 0.2154 0.2404 0.056 Uiso 1 1 calc R . . C4 C 0.2520(5) 0.3084(3) 0.2031(3) 0.0493(16) Uani 1 1 d . . . C5 C 0.3023(5) 0.3694(4) 0.2408(3) 0.0564(17) Uani 1 1 d . . . C6 C 0.4170(6) 0.3811(5) 0.2565(4) 0.081(3) Uani 1 1 d . . . H6A H 0.4544 0.4226 0.2811 0.097 Uiso 1 1 calc R . . C7 C 0.4784(8) 0.3331(6) 0.2371(5) 0.104(4) Uani 1 1 d . . . H7A H 0.5575 0.3422 0.2492 0.125 Uiso 1 1 calc R . . C8 C 0.4287(7) 0.2740(5) 0.2015(4) 0.087(3) Uani 1 1 d . . . H8A H 0.4731 0.2423 0.1886 0.105 Uiso 1 1 calc R . . C9 C 0.3105(6) 0.2585(4) 0.1828(3) 0.067(2) Uani 1 1 d . . . C10 C 0.2365(6) 0.4199(3) 0.2658(3) 0.0595(18) Uani 1 1 d . . . H10A H 0.1612 0.4139 0.2338 0.071 Uiso 1 1 calc R . . C11 C 0.2899(7) 0.4914(3) 0.2739(4) 0.084(2) Uani 1 1 d . . . H11A H 0.2992 0.4993 0.2318 0.125 Uiso 1 1 calc R . . H11B H 0.3629 0.4987 0.3063 0.125 Uiso 1 1 calc R . . H11C H 0.2416 0.5215 0.2889 0.125 Uiso 1 1 calc R . . C12 C 0.2207(7) 0.4097(4) 0.3319(3) 0.088(3) Uani 1 1 d . . . H12A H 0.1855 0.3648 0.3276 0.132 Uiso 1 1 calc R . . H12B H 0.1730 0.4409 0.3459 0.132 Uiso 1 1 calc R . . H12C H 0.2934 0.4171 0.3644 0.132 Uiso 1 1 calc R . . C13 C 0.2557(7) 0.1917(4) 0.1460(4) 0.081(3) Uani 1 1 d . . . H13A H 0.1756 0.1952 0.1259 0.097 Uiso 1 1 calc R . . C14 C 0.2588(8) 0.1420(4) 0.1922(4) 0.099(3) Uani 1 1 d . . . H14A H 0.2262 0.1589 0.2276 0.148 Uiso 1 1 calc R . . H14B H 0.3362 0.1356 0.2110 0.148 Uiso 1 1 calc R . . H14C H 0.2159 0.1000 0.1675 0.148 Uiso 1 1 calc R . . C15 C 0.3045(9) 0.1628(5) 0.0904(4) 0.123(4) Uani 1 1 d . . . H15A H 0.3014 0.1930 0.0597 0.184 Uiso 1 1 calc R . . H15B H 0.2610 0.1204 0.0673 0.184 Uiso 1 1 calc R . . H15C H 0.3822 0.1566 0.1087 0.184 Uiso 1 1 calc R . . C16 C -0.1594(5) 0.2352(3) 0.1236(3) 0.0457(15) Uani 1 1 d . . . C17 C -0.1872(6) 0.1702(3) 0.0880(3) 0.0543(17) Uani 1 1 d . . . C18 C -0.3004(7) 0.1497(4) 0.0566(4) 0.071(2) Uani 1 1 d . . . H18A H -0.3227 0.1065 0.0316 0.085 Uiso 1 1 calc R . . C19 C -0.3791(7) 0.1900(4) 0.0610(4) 0.073(2) Uani 1 1 d . . . H19A H -0.4551 0.1746 0.0386 0.088 Uiso 1 1 calc R . . C20 C -0.3504(6) 0.2524(4) 0.0974(3) 0.0623(19) Uani 1 1 d . . . H20A H -0.4067 0.2798 0.1000 0.075 Uiso 1 1 calc R . . C21 C -0.2398(6) 0.2761(3) 0.1306(3) 0.0522(16) Uani 1 1 d . . . C22 C -0.1008(6) 0.1241(3) 0.0854(3) 0.0646(19) Uani 1 1 d . . . H22A H -0.0256 0.1509 0.0996 0.078 Uiso 1 1 calc R . . C23 C -0.1154(8) 0.0839(3) 0.0171(4) 0.091(3) Uani 1 1 d . . . H23A H -0.1095 0.1136 -0.0132 0.137 Uiso 1 1 calc R . . H23B H -0.1889 0.0573 0.0021 0.137 Uiso 1 1 calc R . . H23C H -0.0572 0.0551 0.0185 0.137 Uiso 1 1 calc R . . C24 C -0.1041(7) 0.0771(3) 0.1339(4) 0.081(2) Uani 1 1 d . . . H24A H -0.0472 0.0478 0.1324 0.122 Uiso 1 1 calc R . . H24B H -0.1779 0.0510 0.1215 0.122 Uiso 1 1 calc R . . H24C H -0.0894 0.1028 0.1783 0.122 Uiso 1 1 calc R . . C25 C -0.2091(5) 0.3440(3) 0.1732(3) 0.0527(16) Uani 1 1 d . . . H25A H -0.1335 0.3614 0.1709 0.063 Uiso 1 1 calc R . . C26 C -0.2870(6) 0.3934(3) 0.1523(3) 0.069(2) Uani 1 1 d . . . H26A H -0.2917 0.3965 0.1067 0.104 Uiso 1 1 calc R . . H26B H -0.2582 0.4365 0.1806 0.104 Uiso 1 1 calc R . . H26C H -0.3614 0.3791 0.1561 0.104 Uiso 1 1 calc R . . C27 C -0.1996(6) 0.3399(4) 0.2450(3) 0.078(2) Uani 1 1 d . . . H27A H -0.1489 0.3082 0.2584 0.117 Uiso 1 1 calc R . . H27B H -0.2734 0.3257 0.2497 0.117 Uiso 1 1 calc R . . H27C H -0.1704 0.3832 0.2728 0.117 Uiso 1 1 calc R . . C28 C -0.0913(6) 0.3251(3) -0.0813(3) 0.0523(16) Uani 1 1 d . . . C29 C -0.1175(6) 0.3340(3) -0.1458(3) 0.0614(18) Uani 1 1 d . . . H29A H -0.1846 0.3122 -0.1765 0.074 Uiso 1 1 calc R . . C30 C -0.0432(6) 0.3756(3) -0.1645(3) 0.0635(19) Uani 1 1 d . . . H30A H -0.0581 0.3820 -0.2085 0.076 Uiso 1 1 calc R . . C31 C 0.0509(6) 0.4066(3) -0.1189(3) 0.0569(18) Uani 1 1 d . . . H31A H 0.1009 0.4366 -0.1304 0.068 Uiso 1 1 calc R . . C32 C 0.0741(6) 0.3946(3) -0.0553(3) 0.0540(17) Uani 1 1 d . . . H32A H 0.1413 0.4157 -0.0242 0.065 Uiso 1 1 calc R . . C33 C -0.1653(6) 0.2808(3) -0.0564(3) 0.0618(19) Uani 1 1 d . . . H33A H -0.2445 0.2834 -0.0775 0.074 Uiso 1 1 calc R . . H33B H -0.1513 0.2348 -0.0673 0.074 Uiso 1 1 calc R . . C34 C 0.2063(5) 0.4324(3) 0.1002(3) 0.0532(17) Uani 1 1 d . . . C35 C 0.3109(7) 0.4683(4) 0.1100(4) 0.080(2) Uani 1 1 d . . . H35A H 0.3221 0.5145 0.1248 0.096 Uiso 1 1 calc R . . C36 C 0.3971(7) 0.4363(5) 0.0981(5) 0.099(3) Uani 1 1 d . . . H36A H 0.4685 0.4599 0.1041 0.119 Uiso 1 1 calc R . . C37 C 0.3784(6) 0.3691(5) 0.0774(4) 0.093(3) Uani 1 1 d . . . H37A H 0.4374 0.3460 0.0695 0.112 Uiso 1 1 calc R . . C38 C 0.2728(6) 0.3351(4) 0.0680(3) 0.066(2) Uani 1 1 d . . . H38A H 0.2598 0.2890 0.0525 0.079 Uiso 1 1 calc R . . C39 C 0.1093(5) 0.4661(3) 0.1057(3) 0.0522(16) Uani 1 1 d . . . H39A H 0.0923 0.4928 0.0712 0.063 Uiso 1 1 calc R . . H39B H 0.1276 0.4962 0.1488 0.063 Uiso 1 1 calc R . . C40 C 0.7224(4) 0.2028(2) 0.4482(3) 0.0322(12) Uani 1 1 d . . . C41 C 0.7053(5) 0.2983(3) 0.4107(3) 0.0426(14) Uani 1 1 d . . . H41A H 0.7190 0.3431 0.4077 0.051 Uiso 1 1 calc R . . C42 C 0.6268(5) 0.2536(3) 0.3700(3) 0.0405(14) Uani 1 1 d . . . H42A H 0.5734 0.2604 0.3324 0.049 Uiso 1 1 calc R . . C43 C 0.8450(5) 0.3096(2) 0.5131(3) 0.0364(13) Uani 1 1 d . . . C44 C 0.9555(4) 0.3215(2) 0.5108(3) 0.0377(13) Uani 1 1 d . . . C45 C 1.0290(5) 0.3655(3) 0.5628(3) 0.0507(16) Uani 1 1 d . . . H45A H 1.1051 0.3742 0.5633 0.061 Uiso 1 1 calc R . . C46 C 0.9925(6) 0.3965(3) 0.6134(3) 0.0598(18) Uani 1 1 d . . . H46A H 1.0437 0.4271 0.6479 0.072 Uiso 1 1 calc R . . C47 C 0.8839(5) 0.3843(3) 0.6155(3) 0.0539(17) Uani 1 1 d . . . H47A H 0.8617 0.4060 0.6517 0.065 Uiso 1 1 calc R . . C48 C 0.8062(5) 0.3409(3) 0.5655(3) 0.0431(14) Uani 1 1 d . . . C49 C 0.9942(5) 0.2895(3) 0.4532(3) 0.0427(14) Uani 1 1 d . . . H49A H 0.9423 0.2482 0.4315 0.051 Uiso 1 1 calc R . . C50 C 0.9881(6) 0.3339(3) 0.4031(3) 0.0584(18) Uani 1 1 d . . . H50A H 0.9123 0.3453 0.3898 0.088 Uiso 1 1 calc R . . H50B H 1.0075 0.3110 0.3646 0.088 Uiso 1 1 calc R . . H50C H 1.0407 0.3741 0.4226 0.088 Uiso 1 1 calc R . . C51 C 1.1120(5) 0.2711(3) 0.4733(3) 0.0569(17) Uani 1 1 d . . . H51A H 1.1157 0.2420 0.5049 0.085 Uiso 1 1 calc R . . H51B H 1.1651 0.3110 0.4933 0.085 Uiso 1 1 calc R . . H51C H 1.1309 0.2487 0.4345 0.085 Uiso 1 1 calc R . . C52 C 0.6874(5) 0.3291(3) 0.5679(3) 0.0566(18) Uani 1 1 d . . . H52A H 0.6529 0.2863 0.5379 0.068 Uiso 1 1 calc R . . C53 C 0.6204(6) 0.3822(3) 0.5429(4) 0.075(2) Uani 1 1 d . . . H53A H 0.6253 0.3848 0.4986 0.113 Uiso 1 1 calc R . . H53B H 0.6507 0.4247 0.5721 0.113 Uiso 1 1 calc R . . H53C H 0.5421 0.3713 0.5421 0.113 Uiso 1 1 calc R . . C54 C 0.6772(6) 0.3235(3) 0.6369(3) 0.072(2) Uani 1 1 d . . . H54A H 0.7190 0.2888 0.6523 0.108 Uiso 1 1 calc R . . H54B H 0.5985 0.3127 0.6351 0.108 Uiso 1 1 calc R . . H54C H 0.7076 0.3653 0.6671 0.108 Uiso 1 1 calc R . . C55 C 0.5466(4) 0.1406(3) 0.3606(3) 0.0365(13) Uani 1 1 d . . . C56 C 0.4486(5) 0.1433(3) 0.3800(3) 0.0407(14) Uani 1 1 d . . . C57 C 0.3611(5) 0.0932(3) 0.3468(3) 0.0529(17) Uani 1 1 d . . . H57A H 0.2924 0.0929 0.3581 0.064 Uiso 1 1 calc R . . C58 C 0.3723(5) 0.0454(3) 0.2989(3) 0.0541(17) Uani 1 1 d . . . H58A H 0.3133 0.0104 0.2793 0.065 Uiso 1 1 calc R . . C59 C 0.4680(5) 0.0465(3) 0.2781(3) 0.0514(16) Uani 1 1 d . . . H59A H 0.4726 0.0138 0.2429 0.062 Uiso 1 1 calc R . . C60 C 0.5579(5) 0.0953(3) 0.3083(3) 0.0386(13) Uani 1 1 d . . . C61 C 0.4308(5) 0.1985(3) 0.4311(3) 0.0481(15) Uani 1 1 d . . . H61A H 0.5054 0.2229 0.4567 0.058 Uiso 1 1 calc R . . C62 C 0.3616(6) 0.2466(3) 0.3969(4) 0.071(2) Uani 1 1 d . . . H62A H 0.3988 0.2633 0.3667 0.106 Uiso 1 1 calc R . . H62B H 0.3544 0.2833 0.4298 0.106 Uiso 1 1 calc R . . H62C H 0.2873 0.2238 0.3724 0.106 Uiso 1 1 calc R . . C63 C 0.3727(5) 0.1734(4) 0.4792(3) 0.065(2) Uani 1 1 d . . . H63A H 0.4171 0.1431 0.5015 0.098 Uiso 1 1 calc R . . H63B H 0.2984 0.1504 0.4550 0.098 Uiso 1 1 calc R . . H63C H 0.3656 0.2106 0.5116 0.098 Uiso 1 1 calc R . . C64 C 0.6606(5) 0.1010(3) 0.2823(3) 0.0454(15) Uani 1 1 d . . . H64A H 0.7267 0.1190 0.3205 0.055 Uiso 1 1 calc R . . C65 C 0.6848(6) 0.0365(3) 0.2473(3) 0.0611(18) Uani 1 1 d . . . H65A H 0.6943 0.0052 0.2770 0.092 Uiso 1 1 calc R . . H65B H 0.7532 0.0441 0.2337 0.092 Uiso 1 1 calc R . . H65C H 0.6224 0.0186 0.2086 0.092 Uiso 1 1 calc R . . C66 C 0.6509(6) 0.1493(3) 0.2340(3) 0.0620(19) Uani 1 1 d . . . H66A H 0.6370 0.1919 0.2554 0.093 Uiso 1 1 calc R . . H66B H 0.5889 0.1317 0.1950 0.093 Uiso 1 1 calc R . . H66C H 0.7204 0.1548 0.2212 0.093 Uiso 1 1 calc R . . C67 C 0.7319(4) 0.0145(2) 0.4094(3) 0.0358(13) Uani 1 1 d . . . C68 C 0.6810(5) -0.0474(3) 0.3770(3) 0.0445(15) Uani 1 1 d . . . H68A H 0.7194 -0.0760 0.3540 0.053 Uiso 1 1 calc R . . C69 C 0.5740(6) -0.0675(3) 0.3783(3) 0.0509(16) Uani 1 1 d . . . H69A H 0.5374 -0.1098 0.3556 0.061 Uiso 1 1 calc R . . C70 C 0.5204(5) -0.0256(3) 0.4130(3) 0.0442(15) Uani 1 1 d . . . H70A H 0.4469 -0.0390 0.4148 0.053 Uiso 1 1 calc R . . C71 C 0.5742(4) 0.0353(3) 0.4447(3) 0.0380(13) Uani 1 1 d . . . H71A H 0.5368 0.0643 0.4680 0.046 Uiso 1 1 calc R . . C72 C 0.8503(5) 0.0382(2) 0.4137(3) 0.0418(14) Uani 1 1 d . . . H72A H 0.8994 0.0093 0.4361 0.050 Uiso 1 1 calc R . . H72B H 0.8591 0.0348 0.3688 0.050 Uiso 1 1 calc R . . C73 C 0.9038(5) 0.1057(3) 0.6298(3) 0.0376(13) Uani 1 1 d . . . C74 C 0.9509(5) 0.0736(3) 0.6800(3) 0.0451(15) Uani 1 1 d . . . H74A H 0.9901 0.0979 0.7223 0.054 Uiso 1 1 calc R . . C75 C 0.9391(5) 0.0053(3) 0.6670(3) 0.0445(15) Uani 1 1 d . . . H75A H 0.9704 -0.0179 0.7003 0.053 Uiso 1 1 calc R . . C76 C 0.8824(5) -0.0279(3) 0.6059(3) 0.0403(14) Uani 1 1 d . . . H76A H 0.8761 -0.0744 0.5957 0.048 Uiso 1 1 calc R . . C77 C 0.8341(4) 0.0064(2) 0.5589(3) 0.0341(12) Uani 1 1 d . . . H77A H 0.7917 -0.0173 0.5171 0.041 Uiso 1 1 calc R . . C78 C 0.9190(5) 0.1783(3) 0.6395(3) 0.0453(15) Uani 1 1 d . . . H78A H 0.8623 0.1961 0.6599 0.054 Uiso 1 1 calc R . . H78B H 0.9937 0.1962 0.6690 0.054 Uiso 1 1 calc R . . C79 C 0.4281(6) 0.8176(4) 0.2085(5) 0.134(4) Uani 1 1 d GD . . H79A H 0.4892 0.7940 0.2207 0.161 Uiso 1 1 calc R . . C80 C 0.4199(7) 0.8504(5) 0.1578(5) 0.130(4) Uani 1 1 d GD . . H80A H 0.4754 0.8494 0.1347 0.156 Uiso 1 1 calc R . . C81 C 0.3320(10) 0.8844(4) 0.1403(3) 0.121(4) Uani 1 1 d GD . . H81A H 0.3263 0.9072 0.1050 0.146 Uiso 1 1 calc R . . C82 C 0.2522(6) 0.8858(3) 0.1735(5) 0.118(4) Uani 1 1 d GD . . H82A H 0.1910 0.9095 0.1614 0.142 Uiso 1 1 calc R . . C83 C 0.2603(7) 0.8530(5) 0.2243(5) 0.128(5) Uani 1 1 d GD . . H83A H 0.2048 0.8540 0.2474 0.154 Uiso 1 1 calc R . . C84 C 0.3482(10) 0.8190(4) 0.2418(3) 0.125(5) Uani 1 1 d GD . . H84A H 0.3539 0.7963 0.2771 0.150 Uiso 1 1 calc R . . C85 C 0.8114(7) 0.4757(3) 0.3913(4) 0.088(3) Uani 1 1 d GD . . H85A H 0.8586 0.4543 0.3686 0.106 Uiso 1 1 calc R . . C86 C 0.7226(8) 0.5016(3) 0.3576(3) 0.116(4) Uani 1 1 d GD . . H86A H 0.7082 0.4983 0.3116 0.140 Uiso 1 1 calc R . . C87 C 0.6546(5) 0.5323(3) 0.3902(6) 0.139(5) Uani 1 1 d GD . . H87A H 0.5930 0.5504 0.3669 0.167 Uiso 1 1 calc R . . C88 C 0.6753(7) 0.5371(3) 0.4566(6) 0.150(6) Uani 1 1 d GD . . H88A H 0.6281 0.5584 0.4792 0.180 Uiso 1 1 calc R . . C89 C 0.7640(8) 0.5112(3) 0.4902(3) 0.112(4) Uani 1 1 d GD . . H89A H 0.7784 0.5145 0.5363 0.134 Uiso 1 1 calc R . . C90 C 0.8321(5) 0.4804(3) 0.4576(4) 0.091(3) Uani 1 1 d GD . . H90A H 0.8937 0.4624 0.4810 0.109 Uiso 1 1 calc R . . C91 C 0.2811(10) 0.3720(5) 0.7432(5) 0.145(7) Uiso 0.721(8) 1 d PGD A 1 H91A H 0.2396 0.4000 0.7645 0.174 Uiso 0.721(8) 1 calc PR A 1 C92 C 0.2269(7) 0.3239(5) 0.6901(5) 0.121(5) Uiso 0.721(8) 1 d PGD A 1 H92A H 0.1478 0.3186 0.6747 0.145 Uiso 0.721(8) 1 calc PR A 1 C93 C 0.2868(9) 0.2835(4) 0.6594(4) 0.116(5) Uiso 0.721(8) 1 d PGD A 1 H93A H 0.2492 0.2502 0.6227 0.139 Uiso 0.721(8) 1 calc PR A 1 C94 C 0.4009(9) 0.2912(5) 0.6816(5) 0.139(6) Uiso 0.721(8) 1 d PGD A 1 H94A H 0.4424 0.2632 0.6603 0.167 Uiso 0.721(8) 1 calc PR A 1 C95 C 0.4552(7) 0.3393(6) 0.7347(6) 0.148(6) Uiso 0.721(8) 1 d PGD A 1 H95A H 0.5342 0.3446 0.7501 0.178 Uiso 0.721(8) 1 calc PR A 1 C96 C 0.3953(10) 0.3797(5) 0.7654(5) 0.162(8) Uiso 0.721(8) 1 d PGD A 1 H96A H 0.4329 0.4130 0.8021 0.194 Uiso 0.721(8) 1 calc PR A 1 C97 C 0.1396(6) 0.2209(3) 0.8005(3) 0.138(5) Uani 1 1 d GD . . H97A H 0.1210 0.2612 0.7884 0.166 Uiso 1 1 calc R . . C98 C 0.0958(6) 0.1969(3) 0.8455(3) 0.153(5) Uani 1 1 d GD . . H98A H 0.0467 0.2206 0.8647 0.183 Uiso 1 1 calc R . . C99 C 0.1226(6) 0.1389(3) 0.8630(3) 0.130(4) Uani 1 1 d GD . . H99A H 0.0921 0.1223 0.8943 0.156 Uiso 1 1 calc R . . C100 C 0.1932(5) 0.1049(3) 0.8354(3) 0.092(3) Uani 1 1 d GD . . H10D H 0.2118 0.0646 0.8475 0.111 Uiso 1 1 calc R . . C101 C 0.2370(5) 0.1288(3) 0.7903(3) 0.090(3) Uani 1 1 d GD . . H10E H 0.2861 0.1052 0.7712 0.108 Uiso 1 1 calc R . . C102 C 0.2103(5) 0.1868(3) 0.7729(3) 0.102(3) Uani 1 1 d GD . . H10F H 0.2407 0.2035 0.7416 0.123 Uiso 1 1 calc R . . C103 C 0.3147(7) 0.3368(5) 0.9171(4) 0.077(4) Uani 0.616(7) 1 d PGD B 2 H10G H 0.2359 0.3336 0.9018 0.092 Uiso 0.616(7) 1 calc PR B 2 C104 C 0.3647(9) 0.2811(4) 0.9230(4) 0.088(4) Uani 0.616(7) 1 d PGD B 2 H10H H 0.3204 0.2394 0.9118 0.105 Uiso 0.616(7) 1 calc PR B 2 C105 C 0.4787(9) 0.2857(6) 0.9450(4) 0.107(6) Uani 0.616(7) 1 d PGD B 2 H10I H 0.5132 0.2471 0.9491 0.129 Uiso 0.616(7) 1 calc PR B 2 C106 C 0.5427(7) 0.3459(8) 0.9611(4) 0.107(6) Uani 0.616(7) 1 d PGD B 2 H10J H 0.6216 0.3491 0.9763 0.128 Uiso 0.616(7) 1 calc PR B 2 C107 C 0.4927(10) 0.4016(6) 0.9552(4) 0.104(6) Uani 0.616(7) 1 d PGD B 2 H10K H 0.5370 0.4433 0.9663 0.125 Uiso 0.616(7) 1 calc PR B 2 C108 C 0.3787(11) 0.3970(4) 0.9332(4) 0.092(5) Uani 0.616(7) 1 d PGD B 2 H10L H 0.3442 0.4356 0.9291 0.110 Uiso 0.616(7) 1 calc PR B 2 C109 C 0.4167(6) 0.0384(3) -0.0041(4) 0.067(2) Uani 1 1 d . . . H10M H 0.3578 0.0647 -0.0073 0.080 Uiso 1 1 calc R . . C110 C 0.4557(7) 0.0159(4) 0.0518(4) 0.076(2) Uani 1 1 d . . . H11D H 0.4254 0.0275 0.0878 0.091 Uiso 1 1 calc R . . C111 C 0.5387(7) -0.0236(4) 0.0569(4) 0.078(2) Uani 1 1 d . . . H11E H 0.5651 -0.0405 0.0956 0.094 Uiso 1 1 calc R . . C112 C 0.4436(18) 0.3656(9) 0.7838(11) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11F H 0.4729 0.3420 0.7516 0.123 Uiso 0.290(7) 1 calc PR C 3 C113 C 0.4993(13) 0.3744(9) 0.8488(12) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11G H 0.5674 0.3569 0.8618 0.123 Uiso 0.290(7) 1 calc PR C 3 C114 C 0.4570(16) 0.4085(10) 0.8951(9) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11H H 0.4957 0.4146 0.9402 0.123 Uiso 0.290(7) 1 calc PR C 3 C115 C 0.3588(17) 0.4338(9) 0.8764(11) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11I H 0.3294 0.4574 0.9086 0.123 Uiso 0.290(7) 1 calc PR C 3 C116 C 0.3030(13) 0.4250(9) 0.8114(12) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11J H 0.2349 0.4426 0.7984 0.123 Uiso 0.290(7) 1 calc PR C 3 C117 C 0.3454(18) 0.3909(10) 0.7651(9) 0.102(6) Uani 0.290(7) 1 d PGD C 3 H11K H 0.3067 0.3848 0.7200 0.123 Uiso 0.290(7) 1 calc PR C 3 _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 0.0540(3) 0.0360(3) 0.0398(3) 0.0167(2) 0.0250(2) 0.0137(2) Rh2 0.0388(3) 0.0261(2) 0.0361(3) 0.01078(19) 0.0177(2) 0.00451(18) Cl1 0.1025(14) 0.0461(9) 0.0510(10) 0.0174(8) 0.0398(10) 0.0302(9) Cl2 0.0497(9) 0.0374(7) 0.0492(9) 0.0109(6) 0.0293(7) 0.0053(6) Cl3 0.0848(13) 0.0663(11) 0.0728(12) 0.0358(10) 0.0269(10) 0.0264(10) Cl4 0.0476(9) 0.0438(8) 0.0645(11) 0.0151(8) 0.0144(8) 0.0107(7) Cl5 0.0910(13) 0.0530(10) 0.0471(10) 0.0061(8) 0.0266(9) 0.0046(9) Cl6 0.0768(11) 0.0401(8) 0.0466(9) 0.0210(7) 0.0302(8) 0.0123(7) N1 0.052(3) 0.041(3) 0.042(3) 0.021(2) 0.025(3) 0.018(2) N2 0.052(3) 0.035(3) 0.038(3) 0.016(2) 0.024(2) 0.010(2) N3 0.062(3) 0.045(3) 0.044(3) 0.019(2) 0.028(3) 0.017(3) N4 0.062(3) 0.055(3) 0.039(3) 0.020(2) 0.019(3) 0.007(3) N5 0.043(3) 0.055(3) 0.057(3) 0.030(3) 0.022(3) 0.014(3) N6 0.047(3) 0.035(3) 0.040(3) 0.012(2) 0.016(2) 0.005(2) N7 0.041(3) 0.025(2) 0.042(3) 0.009(2) 0.021(2) 0.004(2) N8 0.034(3) 0.030(2) 0.044(3) 0.013(2) 0.018(2) 0.009(2) N9 0.041(3) 0.032(2) 0.039(3) 0.016(2) 0.019(2) 0.003(2) N10 0.036(3) 0.028(2) 0.037(3) 0.013(2) 0.015(2) 0.0064(19) N11 0.040(3) 0.030(2) 0.036(3) 0.013(2) 0.016(2) 0.004(2) N12 0.049(3) 0.028(2) 0.038(3) 0.015(2) 0.021(2) 0.009(2) C1 0.050(4) 0.030(3) 0.036(3) 0.011(2) 0.022(3) 0.011(3) C2 0.063(4) 0.051(4) 0.041(4) 0.023(3) 0.025(3) 0.019(3) C3 0.061(4) 0.046(4) 0.047(4) 0.023(3) 0.029(3) 0.011(3) C4 0.049(4) 0.074(5) 0.047(4) 0.035(4) 0.030(3) 0.030(4) C5 0.047(4) 0.077(5) 0.054(4) 0.030(4) 0.018(3) 0.005(4) C6 0.050(5) 0.123(7) 0.079(6) 0.059(5) 0.014(4) 0.003(5) C7 0.064(6) 0.175(11) 0.110(9) 0.097(8) 0.039(6) 0.039(7) C8 0.078(7) 0.147(9) 0.080(7) 0.076(6) 0.046(5) 0.077(6) C9 0.068(5) 0.101(6) 0.057(5) 0.045(4) 0.033(4) 0.043(4) C10 0.061(4) 0.062(4) 0.055(4) 0.017(4) 0.014(4) 0.001(4) C11 0.106(6) 0.073(5) 0.066(5) 0.007(4) 0.027(5) -0.015(5) C12 0.115(7) 0.096(6) 0.058(5) 0.014(4) 0.038(5) 0.006(5) C13 0.119(7) 0.091(6) 0.061(5) 0.034(5) 0.044(5) 0.073(5) C14 0.143(8) 0.087(6) 0.096(7) 0.046(5) 0.053(6) 0.067(6) C15 0.183(10) 0.143(8) 0.084(7) 0.046(6) 0.064(7) 0.118(8) C16 0.057(4) 0.045(4) 0.039(4) 0.017(3) 0.018(3) -0.008(3) C17 0.074(5) 0.045(4) 0.048(4) 0.015(3) 0.025(4) -0.004(4) C18 0.089(6) 0.052(4) 0.065(5) 0.012(4) 0.017(5) -0.023(4) C19 0.070(5) 0.065(5) 0.082(6) 0.020(5) 0.019(4) -0.011(4) C20 0.050(4) 0.077(5) 0.064(5) 0.028(4) 0.018(4) 0.000(4) C21 0.058(4) 0.058(4) 0.052(4) 0.023(3) 0.028(4) 0.005(3) C22 0.097(6) 0.043(4) 0.062(5) 0.013(3) 0.036(4) 0.007(4) C23 0.152(8) 0.054(5) 0.070(5) -0.004(4) 0.048(6) 0.005(5) C24 0.122(7) 0.056(5) 0.081(6) 0.028(4) 0.043(5) 0.020(4) C25 0.049(4) 0.062(4) 0.054(4) 0.009(3) 0.026(3) 0.011(3) C26 0.076(5) 0.072(5) 0.078(5) 0.025(4) 0.039(4) 0.025(4) C27 0.076(5) 0.114(6) 0.050(5) 0.012(4) 0.021(4) 0.042(5) C28 0.073(5) 0.044(4) 0.048(4) 0.016(3) 0.027(4) 0.012(3) C29 0.089(5) 0.051(4) 0.046(4) 0.010(3) 0.023(4) 0.007(4) C30 0.095(6) 0.061(4) 0.046(4) 0.019(4) 0.031(4) 0.019(4) C31 0.085(5) 0.054(4) 0.043(4) 0.022(3) 0.028(4) 0.015(4) C32 0.068(4) 0.057(4) 0.054(4) 0.029(3) 0.032(4) 0.015(3) C33 0.063(5) 0.061(4) 0.049(4) -0.008(3) 0.013(4) -0.018(3) C34 0.054(4) 0.064(4) 0.046(4) 0.026(3) 0.014(3) 0.002(3) C35 0.067(5) 0.093(6) 0.081(6) 0.041(5) 0.016(5) -0.010(5) C36 0.061(6) 0.121(8) 0.138(8) 0.087(7) 0.031(6) 0.011(5) C37 0.057(5) 0.133(8) 0.129(8) 0.080(7) 0.049(5) 0.043(5) C38 0.061(5) 0.081(5) 0.082(5) 0.054(4) 0.037(4) 0.028(4) C39 0.063(4) 0.047(4) 0.047(4) 0.013(3) 0.015(3) 0.002(3) C40 0.035(3) 0.028(3) 0.039(3) 0.003(2) 0.022(3) 0.002(2) C41 0.052(4) 0.032(3) 0.055(4) 0.025(3) 0.025(3) 0.011(3) C42 0.049(4) 0.032(3) 0.049(4) 0.023(3) 0.019(3) 0.009(3) C43 0.053(4) 0.020(3) 0.045(3) 0.012(2) 0.023(3) 0.009(2) C44 0.038(3) 0.027(3) 0.052(4) 0.011(3) 0.021(3) 0.001(2) C45 0.053(4) 0.042(4) 0.061(4) 0.010(3) 0.025(3) -0.003(3) C46 0.084(5) 0.039(4) 0.052(4) -0.001(3) 0.023(4) -0.008(3) C47 0.067(5) 0.036(3) 0.067(5) 0.002(3) 0.040(4) 0.003(3) C48 0.052(4) 0.031(3) 0.055(4) 0.011(3) 0.027(3) 0.003(3) C49 0.048(4) 0.036(3) 0.049(4) 0.009(3) 0.023(3) 0.003(3) C50 0.072(5) 0.064(4) 0.054(4) 0.020(3) 0.035(4) 0.020(4) C51 0.053(4) 0.056(4) 0.072(5) 0.015(4) 0.032(4) 0.014(3) C52 0.070(5) 0.039(3) 0.075(5) 0.004(3) 0.048(4) 0.009(3) C53 0.062(5) 0.069(5) 0.108(6) 0.017(4) 0.043(5) 0.017(4) C54 0.095(6) 0.053(4) 0.085(5) 0.001(4) 0.063(5) -0.003(4) C55 0.035(3) 0.038(3) 0.039(3) 0.017(3) 0.007(3) 0.002(3) C56 0.043(4) 0.039(3) 0.044(4) 0.017(3) 0.014(3) 0.005(3) C57 0.043(4) 0.056(4) 0.058(4) 0.025(4) 0.007(3) -0.005(3) C58 0.053(4) 0.044(4) 0.055(4) 0.009(3) 0.004(3) -0.013(3) C59 0.061(4) 0.038(3) 0.050(4) 0.009(3) 0.007(3) 0.003(3) C60 0.047(4) 0.037(3) 0.034(3) 0.013(3) 0.011(3) 0.008(3) C61 0.038(3) 0.059(4) 0.053(4) 0.016(3) 0.019(3) 0.004(3) C62 0.068(5) 0.077(5) 0.093(6) 0.042(4) 0.043(4) 0.036(4) C63 0.059(4) 0.095(5) 0.059(4) 0.029(4) 0.033(4) 0.018(4) C64 0.051(4) 0.050(4) 0.044(4) 0.019(3) 0.019(3) 0.018(3) C65 0.087(5) 0.058(4) 0.046(4) 0.015(3) 0.025(4) 0.021(4) C66 0.077(5) 0.064(4) 0.067(5) 0.038(4) 0.038(4) 0.027(4) C67 0.044(3) 0.032(3) 0.032(3) 0.011(2) 0.009(3) 0.005(3) C68 0.064(4) 0.025(3) 0.044(4) 0.010(3) 0.012(3) 0.004(3) C69 0.066(5) 0.038(3) 0.047(4) 0.015(3) 0.008(3) 0.003(3) C70 0.042(4) 0.047(4) 0.041(4) 0.016(3) 0.006(3) -0.010(3) C71 0.041(3) 0.037(3) 0.041(3) 0.016(3) 0.016(3) 0.001(3) C72 0.054(4) 0.034(3) 0.046(4) 0.011(3) 0.027(3) 0.010(3) C73 0.040(3) 0.037(3) 0.039(3) 0.011(3) 0.014(3) 0.005(3) C74 0.059(4) 0.044(3) 0.037(3) 0.015(3) 0.015(3) 0.010(3) C75 0.053(4) 0.045(4) 0.043(4) 0.021(3) 0.020(3) 0.003(3) C76 0.048(4) 0.034(3) 0.047(4) 0.017(3) 0.021(3) 0.004(3) C77 0.036(3) 0.028(3) 0.042(3) 0.009(2) 0.017(3) 0.002(2) C78 0.061(4) 0.037(3) 0.040(4) 0.009(3) 0.018(3) 0.006(3) C79 0.107(9) 0.121(9) 0.142(12) 0.014(8) -0.008(8) -0.010(7) C80 0.137(11) 0.147(11) 0.111(10) 0.012(8) 0.063(9) -0.011(8) C81 0.162(12) 0.104(9) 0.077(7) 0.012(6) 0.016(8) -0.038(8) C82 0.129(10) 0.076(7) 0.137(11) -0.008(7) 0.038(8) -0.010(6) C83 0.130(11) 0.145(11) 0.105(10) -0.027(8) 0.070(9) -0.023(8) C84 0.143(11) 0.139(10) 0.070(7) 0.013(7) 0.018(8) -0.069(9) C85 0.115(8) 0.041(4) 0.109(8) 0.004(5) 0.041(6) -0.003(5) C86 0.188(13) 0.064(6) 0.077(7) 0.013(5) 0.012(8) -0.020(7) C87 0.104(9) 0.103(9) 0.183(14) 0.020(10) -0.002(10) 0.005(7) C88 0.097(10) 0.116(9) 0.259(19) 0.014(12) 0.099(11) 0.020(8) C89 0.167(12) 0.068(6) 0.113(8) 0.006(6) 0.079(9) -0.019(6) C90 0.115(8) 0.034(4) 0.111(8) 0.020(5) 0.013(7) -0.013(4) C97 0.251(14) 0.103(8) 0.089(7) 0.035(6) 0.061(8) 0.103(9) C98 0.275(15) 0.150(10) 0.101(8) 0.064(7) 0.117(10) 0.127(10) C99 0.229(13) 0.137(9) 0.075(6) 0.051(6) 0.087(8) 0.098(9) C100 0.124(8) 0.085(6) 0.079(6) 0.029(5) 0.028(6) 0.043(6) C101 0.092(6) 0.082(6) 0.092(7) -0.004(5) 0.025(5) 0.032(5) C102 0.157(9) 0.094(7) 0.075(6) 0.027(5) 0.049(6) 0.045(6) C103 0.061(8) 0.091(10) 0.057(8) -0.012(7) -0.004(6) 0.015(8) C104 0.083(10) 0.091(10) 0.069(9) -0.011(8) -0.002(8) 0.019(8) C105 0.087(11) 0.147(15) 0.059(9) -0.039(9) -0.006(8) 0.050(11) C106 0.074(11) 0.166(17) 0.061(10) -0.018(11) 0.014(8) 0.005(12) C107 0.094(13) 0.142(16) 0.075(11) 0.021(10) 0.037(10) -0.033(11) C108 0.112(13) 0.116(13) 0.043(8) 0.010(8) 0.019(8) 0.009(10) C109 0.068(5) 0.051(4) 0.071(5) -0.015(4) 0.020(4) -0.002(4) C110 0.100(7) 0.061(5) 0.068(6) -0.004(4) 0.036(5) 0.002(5) C111 0.096(6) 0.065(5) 0.064(5) 0.000(4) 0.020(5) -0.010(5) C112 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(8) C113 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(8) C114 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(8) C115 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(8) C116 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(8) C117 0.082(11) 0.098(11) 0.146(15) 0.061(11) 0.040(9) 0.020(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. ; _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 2.028(5) . ? Rh1 N6 2.060(4) . ? Rh1 C1 2.061(5) . ? Rh1 N4 2.063(5) . ? Rh1 N3 2.133(4) . ? Rh1 Cl1 2.3460(15) . ? Rh2 N9 2.048(4) . ? Rh2 N10 2.060(4) . ? Rh2 C40 2.065(5) . ? Rh2 N12 2.077(4) . ? Rh2 N11 2.140(4) . ? Rh2 Cl2 2.3555(13) . ? N1 C1 1.377(7) . ? N1 C2 1.392(6) . ? N1 C4 1.465(7) . ? N2 C3 1.376(7) . ? N2 C1 1.381(6) . ? N2 C16 1.442(7) . ? N3 C32 1.331(7) . ? N3 C28 1.354(8) . ? N4 C33 1.466(7) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C38 1.334(7) . ? N5 C34 1.349(8) . ? N6 C39 1.495(7) . ? N6 H6B 0.9200 . ? N6 H6C 0.9200 . ? N7 C40 1.370(6) . ? N7 C41 1.380(6) . ? N7 C43 1.443(7) . ? N8 C40 1.376(6) . ? N8 C42 1.383(6) . ? N8 C55 1.466(7) . ? N9 C71 1.348(6) . ? N9 C67 1.354(6) . ? N10 C72 1.479(6) . ? N10 H10B 0.9200 . ? N10 H10C 0.9200 . ? N11 C73 1.341(7) . ? N11 C77 1.348(6) . ? N12 C78 1.481(6) . ? N12 H12D 0.9200 . ? N12 H12E 0.9200 . ? C2 C3 1.315(8) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.392(9) . ? C4 C9 1.397(9) . ? C5 C6 1.377(9) . ? C5 C10 1.502(9) . ? C6 C7 1.385(12) . ? C6 H6A 0.9500 . ? C7 C8 1.345(12) . ? C7 H7A 0.9500 . ? C8 C9 1.423(11) . ? C8 H8A 0.9500 . ? C9 C13 1.495(10) . ? C10 C12 1.529(9) . ? C10 C11 1.543(9) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.535(9) . ? C13 C14 1.546(9) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.393(8) . ? C16 C17 1.409(8) . ? C17 C18 1.400(9) . ? C17 C22 1.512(9) . ? C18 C19 1.357(10) . ? C18 H18A 0.9500 . ? C19 C20 1.372(9) . ? C19 H19A 0.9500 . ? C20 C21 1.391(9) . ? C20 H20A 0.9500 . ? C21 C25 1.515(8) . ? C22 C23 1.525(9) . ? C22 C24 1.546(8) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.520(8) . ? C25 C27 1.535(8) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.388(8) . ? C28 C33 1.504(8) . ? C29 C30 1.394(8) . ? C29 H29A 0.9500 . ? C30 C31 1.358(9) . ? C30 H30A 0.9500 . ? C31 C32 1.395(8) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.399(9) . ? C34 C39 1.474(8) . ? C35 C36 1.371(11) . ? C35 H35A 0.9500 . ? C36 C37 1.377(12) . ? C36 H36A 0.9500 . ? C37 C38 1.396(10) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 C42 1.318(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.397(7) . ? C43 C48 1.422(7) . ? C44 C45 1.393(8) . ? C44 C49 1.517(7) . ? C45 C46 1.370(8) . ? C45 H45A 0.9500 . ? C46 C47 1.374(8) . ? C46 H46A 0.9500 . ? C47 C48 1.386(8) . ? C47 H47A 0.9500 . ? C48 C52 1.500(8) . ? C49 C50 1.524(7) . ? C49 C51 1.527(8) . ? C49 H49A 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.530(9) . ? C52 C54 1.544(8) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C60 1.388(7) . ? C55 C56 1.392(7) . ? C56 C57 1.401(8) . ? C56 C61 1.527(8) . ? C57 C58 1.354(8) . ? C57 H57A 0.9500 . ? C58 C59 1.378(8) . ? C58 H58A 0.9500 . ? C59 C60 1.392(8) . ? C59 H59A 0.9500 . ? C60 C64 1.529(7) . ? C61 C62 1.537(8) . ? C61 C63 1.538(7) . ? C61 H61A 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.523(8) . ? C64 C66 1.550(7) . ? C64 H64A 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.377(7) . ? C67 C72 1.495(7) . ? C68 C69 1.376(8) . ? C68 H68A 0.9500 . ? C69 C70 1.380(8) . ? C69 H69A 0.9500 . ? C70 C71 1.367(7) . ? C70 H70A 0.9500 . ? C71 H71A 0.9500 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.393(7) . ? C73 C78 1.482(7) . ? C74 C75 1.394(7) . ? C74 H74A 0.9500 . ? C75 C76 1.362(8) . ? C75 H75A 0.9500 . ? C76 C77 1.376(7) . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.366(2) . ? C79 C84 1.366(2) . ? C79 H79A 0.9500 . ? C80 C81 1.366(2) . ? C80 H80A 0.9500 . ? C81 C82 1.366(2) . ? C81 H81A 0.9500 . ? C82 C83 1.366(2) . ? C82 H82A 0.9500 . ? C83 C84 1.366(2) . ? C83 H83A 0.9500 . ? C84 H84A 0.9500 . ? C85 C86 1.368(2) . ? C85 C90 1.368(2) . ? C85 H85A 0.9500 . ? C86 C87 1.369(2) . ? C86 H86A 0.9500 . ? C87 C88 1.368(2) . ? C87 H87A 0.9500 . ? C88 C89 1.368(2) . ? C88 H88A 0.9500 . ? C89 C90 1.369(2) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? C91 C96 1.372(3) . ? C91 C92 1.372(3) . ? C91 H91A 0.9500 . ? C92 C93 1.372(3) . ? C92 H92A 0.9500 . ? C93 C94 1.372(3) . ? C93 H93A 0.9500 . ? C94 C95 1.372(3) . ? C94 H94A 0.9500 . ? C95 C96 1.372(3) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? C97 C98 1.367(3) . ? C97 C102 1.367(3) . ? C97 H97A 0.9500 . ? C98 C99 1.367(3) . ? C98 H98A 0.9500 . ? C99 C100 1.367(3) . ? C99 H99A 0.9500 . ? C100 C101 1.367(3) . ? C100 H10D 0.9500 . ? C101 C102 1.367(3) . ? C101 H10E 0.9500 . ? C102 H10F 0.9500 . ? C103 C104 1.373(4) . ? C103 C108 1.373(4) . ? C103 H10G 0.9500 . ? C104 C105 1.373(4) . ? C104 H10H 0.9500 . ? C105 C106 1.373(4) . ? C105 H10I 0.9500 . ? C106 C107 1.373(4) . ? C106 H10J 0.9500 . ? C107 C108 1.373(4) . ? C107 H10K 0.9500 . ? C108 H10L 0.9500 . ? C109 C110 1.353(10) . ? C109 C111 1.388(10) 2_655 ? C109 H10M 0.9500 . ? C110 C111 1.373(10) . ? C110 H11D 0.9500 . ? C111 C109 1.388(10) 2_655 ? C111 H11E 0.9500 . ? C112 C113 1.369(5) . ? C112 C117 1.370(5) . ? C112 H11F 0.9500 . ? C113 C114 1.370(5) . ? C113 H11G 0.9500 . ? C114 C115 1.370(5) . ? C114 H11H 0.9500 . ? C115 C116 1.370(5) . ? C115 H11I 0.9500 . ? C116 C117 1.370(5) . ? C116 H11J 0.9500 . ? C117 H11K 0.9500 . ? _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 N6 81.85(19) . . ? N5 Rh1 C1 95.4(2) . . ? N6 Rh1 C1 93.04(18) . . ? N5 Rh1 N4 165.10(17) . . ? N6 Rh1 N4 92.18(19) . . ? C1 Rh1 N4 98.6(2) . . ? N5 Rh1 N3 89.05(19) . . ? N6 Rh1 N3 91.03(17) . . ? C1 Rh1 N3 174.4(2) . . ? N4 Rh1 N3 77.36(18) . . ? N5 Rh1 Cl1 96.19(15) . . ? N6 Rh1 Cl1 177.74(12) . . ? C1 Rh1 Cl1 88.26(14) . . ? N4 Rh1 Cl1 89.45(15) . . ? N3 Rh1 Cl1 87.81(13) . . ? N9 Rh2 N10 81.72(16) . . ? N9 Rh2 C40 96.11(18) . . ? N10 Rh2 C40 92.72(17) . . ? N9 Rh2 N12 165.08(16) . . ? N10 Rh2 N12 92.33(16) . . ? C40 Rh2 N12 97.84(18) . . ? N9 Rh2 N11 88.57(16) . . ? N10 Rh2 N11 89.80(15) . . ? C40 Rh2 N11 174.96(19) . . ? N12 Rh2 N11 77.68(16) . . ? N9 Rh2 Cl2 95.22(12) . . ? N10 Rh2 Cl2 176.06(11) . . ? C40 Rh2 Cl2 90.07(13) . . ? N12 Rh2 Cl2 90.04(12) . . ? N11 Rh2 Cl2 87.62(11) . . ? C1 N1 C2 110.7(5) . . ? C1 N1 C4 133.5(4) . . ? C2 N1 C4 115.2(5) . . ? C3 N2 C1 111.4(5) . . ? C3 N2 C16 117.9(4) . . ? C1 N2 C16 130.4(4) . . ? C32 N3 C28 118.5(5) . . ? C32 N3 Rh1 127.7(4) . . ? C28 N3 Rh1 113.7(4) . . ? C33 N4 Rh1 110.1(4) . . ? C33 N4 H4A 109.6 . . ? Rh1 N4 H4A 109.6 . . ? C33 N4 H4B 109.6 . . ? Rh1 N4 H4B 109.6 . . ? H4A N4 H4B 108.2 . . ? C38 N5 C34 119.9(6) . . ? C38 N5 Rh1 124.5(5) . . ? C34 N5 Rh1 114.5(4) . . ? C39 N6 Rh1 110.6(3) . . ? C39 N6 H6B 109.5 . . ? Rh1 N6 H6B 109.5 . . ? C39 N6 H6C 109.5 . . ? Rh1 N6 H6C 109.5 . . ? H6B N6 H6C 108.1 . . ? C40 N7 C41 111.5(5) . . ? C40 N7 C43 131.3(4) . . ? C41 N7 C43 116.6(4) . . ? C40 N8 C42 110.8(4) . . ? C40 N8 C55 130.8(4) . . ? C42 N8 C55 117.5(5) . . ? C71 N9 C67 119.5(5) . . ? C71 N9 Rh2 124.9(4) . . ? C67 N9 Rh2 114.5(3) . . ? C72 N10 Rh2 110.5(3) . . ? C72 N10 H10B 109.6 . . ? Rh2 N10 H10B 109.6 . . ? C72 N10 H10C 109.6 . . ? Rh2 N10 H10C 109.6 . . ? H10B N10 H10C 108.1 . . ? C73 N11 C77 118.7(4) . . ? C73 N11 Rh2 112.9(3) . . ? C77 N11 Rh2 128.4(4) . . ? C78 N12 Rh2 109.4(3) . . ? C78 N12 H12D 109.8 . . ? Rh2 N12 H12D 109.8 . . ? C78 N12 H12E 109.8 . . ? Rh2 N12 H12E 109.8 . . ? H12D N12 H12E 108.2 . . ? N1 C1 N2 102.7(4) . . ? N1 C1 Rh1 129.9(4) . . ? N2 C1 Rh1 127.4(4) . . ? C3 C2 N1 107.6(5) . . ? C3 C2 H2A 126.2 . . ? N1 C2 H2A 126.2 . . ? C2 C3 N2 107.7(5) . . ? C2 C3 H3A 126.2 . . ? N2 C3 H3A 126.2 . . ? C5 C4 C9 124.2(6) . . ? C5 C4 N1 118.9(5) . . ? C9 C4 N1 116.2(6) . . ? C6 C5 C4 116.9(7) . . ? C6 C5 C10 120.7(7) . . ? C4 C5 C10 122.4(6) . . ? C5 C6 C7 121.0(9) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C8 C7 C6 121.5(9) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C7 C8 C9 120.9(8) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C4 C9 C8 115.6(8) . . ? C4 C9 C13 123.6(7) . . ? C8 C9 C13 120.8(7) . . ? C5 C10 C12 110.5(6) . . ? C5 C10 C11 113.9(6) . . ? C12 C10 C11 108.1(6) . . ? C5 C10 H10A 108.1 . . ? C12 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 114.9(8) . . ? C9 C13 C14 111.5(6) . . ? C15 C13 C14 108.0(6) . . ? C9 C13 H13A 107.4 . . ? C15 C13 H13A 107.4 . . ? C14 C13 H13A 107.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.4(6) . . ? C21 C16 N2 119.4(5) . . ? C17 C16 N2 117.9(6) . . ? C18 C17 C16 116.3(6) . . ? C18 C17 C22 121.4(6) . . ? C16 C17 C22 122.3(6) . . ? C19 C18 C17 121.8(7) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 120.8(7) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C21 120.7(7) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 117.8(6) . . ? C20 C21 C25 120.6(6) . . ? C16 C21 C25 121.6(6) . . ? C17 C22 C23 113.2(6) . . ? C17 C22 C24 109.9(5) . . ? C23 C22 C24 109.4(5) . . ? C17 C22 H22A 108.1 . . ? C23 C22 H22A 108.1 . . ? C24 C22 H22A 108.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 115.0(6) . . ? C21 C25 C27 110.2(5) . . ? C26 C25 C27 109.8(5) . . ? C21 C25 H25A 107.1 . . ? C26 C25 H25A 107.1 . . ? C27 C25 H25A 107.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 122.1(6) . . ? N3 C28 C33 115.2(5) . . ? C29 C28 C33 122.7(6) . . ? C28 C29 C30 118.6(7) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? C31 C30 C29 118.9(6) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? C30 C31 C32 120.0(6) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? N3 C32 C31 121.9(6) . . ? N3 C32 H32A 119.1 . . ? C31 C32 H32A 119.1 . . ? N4 C33 C28 109.1(5) . . ? N4 C33 H33A 109.9 . . ? C28 C33 H33A 109.9 . . ? N4 C33 H33B 109.9 . . ? C28 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? N5 C34 C35 121.0(7) . . ? N5 C34 C39 118.2(5) . . ? C35 C34 C39 120.6(7) . . ? C36 C35 C34 119.5(8) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? C35 C36 C37 118.8(8) . . ? C35 C36 H36A 120.6 . . ? C37 C36 H36A 120.6 . . ? C36 C37 C38 120.0(8) . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? N5 C38 C37 120.8(7) . . ? N5 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C34 C39 N6 111.6(5) . . ? C34 C39 H39A 109.3 . . ? N6 C39 H39A 109.3 . . ? C34 C39 H39B 109.3 . . ? N6 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? N7 C40 N8 102.8(4) . . ? N7 C40 Rh2 127.0(4) . . ? N8 C40 Rh2 130.2(3) . . ? C42 C41 N7 107.1(5) . . ? C42 C41 H41A 126.4 . . ? N7 C41 H41A 126.4 . . ? C41 C42 N8 107.8(5) . . ? C41 C42 H42A 126.1 . . ? N8 C42 H42A 126.1 . . ? C44 C43 C48 122.6(5) . . ? C44 C43 N7 119.7(5) . . ? C48 C43 N7 117.5(5) . . ? C45 C44 C43 117.5(5) . . ? C45 C44 C49 120.7(5) . . ? C43 C44 C49 121.8(5) . . ? C46 C45 C44 120.5(6) . . ? C46 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? C45 C46 C47 121.7(6) . . ? C45 C46 H46A 119.1 . . ? C47 C46 H46A 119.1 . . ? C46 C47 C48 120.9(6) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C47 C48 C43 116.8(5) . . ? C47 C48 C52 120.3(5) . . ? C43 C48 C52 122.9(5) . . ? C44 C49 C50 110.6(4) . . ? C44 C49 C51 113.2(5) . . ? C50 C49 C51 109.4(5) . . ? C44 C49 H49A 107.8 . . ? C50 C49 H49A 107.8 . . ? C51 C49 H49A 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 C53 111.7(5) . . ? C48 C52 C54 112.7(6) . . ? C53 C52 C54 109.8(5) . . ? C48 C52 H52A 107.5 . . ? C53 C52 H52A 107.5 . . ? C54 C52 H52A 107.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 124.0(5) . . ? C60 C55 N8 119.0(5) . . ? C56 C55 N8 116.4(5) . . ? C55 C56 C57 116.0(6) . . ? C55 C56 C61 124.0(5) . . ? C57 C56 C61 119.9(5) . . ? C58 C57 C56 121.4(6) . . ? C58 C57 H57A 119.3 . . ? C56 C57 H57A 119.3 . . ? C57 C58 C59 121.0(6) . . ? C57 C58 H58A 119.5 . . ? C59 C58 H58A 119.5 . . ? C58 C59 C60 120.6(6) . . ? C58 C59 H59A 119.7 . . ? C60 C59 H59A 119.7 . . ? C55 C60 C59 116.7(5) . . ? C55 C60 C64 121.9(5) . . ? C59 C60 C64 121.4(5) . . ? C56 C61 C62 109.9(5) . . ? C56 C61 C63 112.9(5) . . ? C62 C61 C63 109.1(5) . . ? C56 C61 H61A 108.3 . . ? C62 C61 H61A 108.3 . . ? C63 C61 H61A 108.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C60 114.7(5) . . ? C65 C64 C66 107.2(5) . . ? C60 C64 C66 111.5(5) . . ? C65 C64 H64A 107.7 . . ? C60 C64 H64A 107.7 . . ? C66 C64 H64A 107.7 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N9 C67 C68 120.9(5) . . ? N9 C67 C72 116.5(5) . . ? C68 C67 C72 122.4(5) . . ? C69 C68 C67 119.4(6) . . ? C69 C68 H68A 120.3 . . ? C67 C68 H68A 120.3 . . ? C68 C69 C70 119.3(6) . . ? C68 C69 H69A 120.3 . . ? C70 C69 H69A 120.3 . . ? C71 C70 C69 119.3(5) . . ? C71 C70 H70A 120.3 . . ? C69 C70 H70A 120.3 . . ? N9 C71 C70 121.5(5) . . ? N9 C71 H71A 119.2 . . ? C70 C71 H71A 119.2 . . ? N10 C72 C67 113.1(4) . . ? N10 C72 H72A 109.0 . . ? C67 C72 H72A 109.0 . . ? N10 C72 H72B 109.0 . . ? C67 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? N11 C73 C74 121.7(5) . . ? N11 C73 C78 117.1(5) . . ? C74 C73 C78 121.2(5) . . ? C73 C74 C75 118.6(6) . . ? C73 C74 H74A 120.7 . . ? C75 C74 H74A 120.7 . . ? C76 C75 C74 119.1(5) . . ? C76 C75 H75A 120.4 . . ? C74 C75 H75A 120.4 . . ? C75 C76 C77 119.6(5) . . ? C75 C76 H76A 120.2 . . ? C77 C76 H76A 120.2 . . ? N11 C77 C76 122.1(5) . . ? N11 C77 H77A 118.9 . . ? C76 C77 H77A 118.9 . . ? N12 C78 C73 109.3(4) . . ? N12 C78 H78A 109.8 . . ? C73 C78 H78A 109.8 . . ? N12 C78 H78B 109.8 . . ? C73 C78 H78B 109.8 . . ? H78A C78 H78B 108.3 . . ? C80 C79 C84 120.0 . . ? C80 C79 H79A 120.0 . . ? C84 C79 H79A 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80A 120.0 . . ? C79 C80 H80A 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81A 120.0 . . ? C82 C81 H81A 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83A 120.0 . . ? C84 C83 H83A 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H84A 120.0 . . ? C79 C84 H84A 120.0 . . ? C86 C85 C90 120.0 . . ? C86 C85 H85A 120.0 . . ? C90 C85 H85A 120.0 . . ? C85 C86 C87 120.0 . . ? C85 C86 H86A 120.0 . . ? C87 C86 H86A 120.0 . . ? C88 C87 C86 120.0 . . ? C88 C87 H87A 120.0 . . ? C86 C87 H87A 120.0 . . ? C87 C88 C89 120.0 . . ? C87 C88 H88A 120.0 . . ? C89 C88 H88A 120.0 . . ? C88 C89 C90 120.0 . . ? C88 C89 H89A 120.0 . . ? C90 C89 H89A 120.0 . . ? C85 C90 C89 120.0 . . ? C85 C90 H90A 120.0 . . ? C89 C90 H90A 120.0 . . ? C96 C91 C92 120.0 . . ? C96 C91 H91A 120.0 . . ? C92 C91 H91A 120.0 . . ? C93 C92 C91 120.0 . . ? C93 C92 H92A 120.0 . . ? C91 C92 H92A 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93A 120.0 . . ? C92 C93 H93A 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94A 120.0 . . ? C95 C94 H94A 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95A 120.0 . . ? C94 C95 H95A 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96A 120.0 . . ? C91 C96 H96A 120.0 . . ? C98 C97 C102 120.0 . . ? C98 C97 H97A 120.0 . . ? C102 C97 H97A 120.0 . . ? C99 C98 C97 120.0 . . ? C99 C98 H98A 120.0 . . ? C97 C98 H98A 120.0 . . ? C98 C99 C100 120.0 . . ? C98 C99 H99A 120.0 . . ? C100 C99 H99A 120.0 . . ? C101 C100 C99 120.0 . . ? C101 C100 H10D 120.0 . . ? C99 C100 H10D 120.0 . . ? C102 C101 C100 120.0 . . ? C102 C101 H10E 120.0 . . ? C100 C101 H10E 120.0 . . ? C101 C102 C97 120.0 . . ? C101 C102 H10F 120.0 . . ? C97 C102 H10F 120.0 . . ? C104 C103 C108 120.0 . . ? C104 C103 H10G 120.0 . . ? C108 C103 H10G 120.0 . . ? C103 C104 C105 120.0 . . ? C103 C104 H10H 120.0 . . ? C105 C104 H10H 120.0 . . ? C106 C105 C104 120.0 . . ? C106 C105 H10I 120.0 . . ? C104 C105 H10I 120.0 . . ? C105 C106 C107 120.0 . . ? C105 C106 H10J 120.0 . . ? C107 C106 H10J 120.0 . . ? C108 C107 C106 120.0 . . ? C108 C107 H10K 120.0 . . ? C106 C107 H10K 120.0 . . ? C107 C108 C103 120.0 . . ? C107 C108 H10L 120.0 . . ? C103 C108 H10L 120.0 . . ? C110 C109 C111 121.1(7) . 2_655 ? C110 C109 H10M 119.5 . . ? C111 C109 H10M 119.5 2_655 . ? C109 C110 C111 120.4(8) . . ? C109 C110 H11D 119.8 . . ? C111 C110 H11D 119.8 . . ? C110 C111 C109 118.5(8) . 2_655 ? C110 C111 H11E 120.7 . . ? C109 C111 H11E 120.7 2_655 . ? C113 C112 C117 120.0 . . ? C113 C112 H11F 120.0 . . ? C117 C112 H11F 120.0 . . ? C112 C113 C114 120.0 . . ? C112 C113 H11G 120.0 . . ? C114 C113 H11G 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H11H 120.0 . . ? C115 C114 H11H 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H11I 120.0 . . ? C116 C115 H11I 120.0 . . ? C115 C116 C117 120.0 . . ? C115 C116 H11J 120.0 . . ? C117 C116 H11J 120.0 . . ? C112 C117 C116 120.0 . . ? C112 C117 H11K 120.0 . . ? C116 C117 H11K 120.0 . . ? _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 N5 Rh1 N3 C32 -11.2(5) . . . . ? N6 Rh1 N3 C32 70.6(5) . . . . ? C1 Rh1 N3 C32 -153.2(18) . . . . ? N4 Rh1 N3 C32 162.6(5) . . . . ? Cl1 Rh1 N3 C32 -107.4(5) . . . . ? N5 Rh1 N3 C28 166.2(4) . . . . ? N6 Rh1 N3 C28 -112.0(4) . . . . ? C1 Rh1 N3 C28 24(2) . . . . ? N4 Rh1 N3 C28 -20.0(4) . . . . ? Cl1 Rh1 N3 C28 70.0(4) . . . . ? N5 Rh1 N4 C33 57.6(10) . . . . ? N6 Rh1 N4 C33 123.5(4) . . . . ? C1 Rh1 N4 C33 -143.1(4) . . . . ? N3 Rh1 N4 C33 33.0(4) . . . . ? Cl1 Rh1 N4 C33 -54.9(4) . . . . ? N6 Rh1 N5 C38 -179.5(5) . . . . ? C1 Rh1 N5 C38 88.2(5) . . . . ? N4 Rh1 N5 C38 -112.4(8) . . . . ? N3 Rh1 N5 C38 -88.3(5) . . . . ? Cl1 Rh1 N5 C38 -0.7(5) . . . . ? N6 Rh1 N5 C34 -11.3(4) . . . . ? C1 Rh1 N5 C34 -103.7(4) . . . . ? N4 Rh1 N5 C34 55.8(10) . . . . ? N3 Rh1 N5 C34 79.8(4) . . . . ? Cl1 Rh1 N5 C34 167.5(4) . . . . ? N5 Rh1 N6 C39 16.0(4) . . . . ? C1 Rh1 N6 C39 111.0(4) . . . . ? N4 Rh1 N6 C39 -150.3(4) . . . . ? N3 Rh1 N6 C39 -72.9(4) . . . . ? Cl1 Rh1 N6 C39 -14(4) . . . . ? N10 Rh2 N9 C71 -178.0(4) . . . . ? C40 Rh2 N9 C71 -86.1(4) . . . . ? N12 Rh2 N9 C71 114.8(7) . . . . ? N11 Rh2 N9 C71 92.0(4) . . . . ? Cl2 Rh2 N9 C71 4.5(4) . . . . ? N10 Rh2 N9 C67 14.5(3) . . . . ? C40 Rh2 N9 C67 106.4(3) . . . . ? N12 Rh2 N9 C67 -52.8(7) . . . . ? N11 Rh2 N9 C67 -75.5(3) . . . . ? Cl2 Rh2 N9 C67 -163.0(3) . . . . ? N9 Rh2 N10 C72 -17.3(3) . . . . ? C40 Rh2 N10 C72 -113.1(4) . . . . ? N12 Rh2 N10 C72 148.9(3) . . . . ? N11 Rh2 N10 C72 71.3(3) . . . . ? Cl2 Rh2 N10 C72 22(2) . . . . ? N9 Rh2 N11 C73 -166.3(4) . . . . ? N10 Rh2 N11 C73 112.0(4) . . . . ? C40 Rh2 N11 C73 -8(2) . . . . ? N12 Rh2 N11 C73 19.5(3) . . . . ? Cl2 Rh2 N11 C73 -71.0(3) . . . . ? N9 Rh2 N11 C77 13.9(4) . . . . ? N10 Rh2 N11 C77 -67.8(4) . . . . ? C40 Rh2 N11 C77 172.1(18) . . . . ? N12 Rh2 N11 C77 -160.2(4) . . . . ? Cl2 Rh2 N11 C77 109.2(4) . . . . ? N9 Rh2 N12 C78 -54.8(8) . . . . ? N10 Rh2 N12 C78 -120.8(3) . . . . ? C40 Rh2 N12 C78 146.1(3) . . . . ? N11 Rh2 N12 C78 -31.5(3) . . . . ? Cl2 Rh2 N12 C78 56.0(3) . . . . ? C2 N1 C1 N2 0.0(6) . . . . ? C4 N1 C1 N2 170.3(6) . . . . ? C2 N1 C1 Rh1 -178.4(4) . . . . ? C4 N1 C1 Rh1 -8.1(9) . . . . ? C3 N2 C1 N1 -0.2(6) . . . . ? C16 N2 C1 N1 -173.7(5) . . . . ? C3 N2 C1 Rh1 178.3(4) . . . . ? C16 N2 C1 Rh1 4.7(8) . . . . ? N5 Rh1 C1 N1 -4.7(5) . . . . ? N6 Rh1 C1 N1 -86.8(5) . . . . ? N4 Rh1 C1 N1 -179.5(5) . . . . ? N3 Rh1 C1 N1 137.1(18) . . . . ? Cl1 Rh1 C1 N1 91.3(5) . . . . ? N5 Rh1 C1 N2 177.3(4) . . . . ? N6 Rh1 C1 N2 95.2(4) . . . . ? N4 Rh1 C1 N2 2.5(5) . . . . ? N3 Rh1 C1 N2 -41(2) . . . . ? Cl1 Rh1 C1 N2 -86.6(4) . . . . ? C1 N1 C2 C3 0.2(6) . . . . ? C4 N1 C2 C3 -172.0(5) . . . . ? N1 C2 C3 N2 -0.3(6) . . . . ? C1 N2 C3 C2 0.3(7) . . . . ? C16 N2 C3 C2 174.7(5) . . . . ? C1 N1 C4 C5 100.7(7) . . . . ? C2 N1 C4 C5 -89.3(6) . . . . ? C1 N1 C4 C9 -88.9(7) . . . . ? C2 N1 C4 C9 81.0(7) . . . . ? C9 C4 C5 C6 2.4(9) . . . . ? N1 C4 C5 C6 171.9(5) . . . . ? C9 C4 C5 C10 -175.3(6) . . . . ? N1 C4 C5 C10 -5.8(9) . . . . ? C4 C5 C6 C7 -1.9(10) . . . . ? C10 C5 C6 C7 175.9(7) . . . . ? C5 C6 C7 C8 1.0(12) . . . . ? C6 C7 C8 C9 -0.4(13) . . . . ? C5 C4 C9 C8 -1.9(9) . . . . ? N1 C4 C9 C8 -171.6(5) . . . . ? C5 C4 C9 C13 175.9(6) . . . . ? N1 C4 C9 C13 6.2(9) . . . . ? C7 C8 C9 C4 0.8(11) . . . . ? C7 C8 C9 C13 -177.0(7) . . . . ? C6 C5 C10 C12 -89.7(7) . . . . ? C4 C5 C10 C12 88.0(8) . . . . ? C6 C5 C10 C11 32.2(9) . . . . ? C4 C5 C10 C11 -150.2(6) . . . . ? C4 C9 C13 C15 139.2(7) . . . . ? C8 C9 C13 C15 -43.1(9) . . . . ? C4 C9 C13 C14 -97.5(8) . . . . ? C8 C9 C13 C14 80.1(8) . . . . ? C3 N2 C16 C21 94.7(6) . . . . ? C1 N2 C16 C21 -92.1(7) . . . . ? C3 N2 C16 C17 -79.1(6) . . . . ? C1 N2 C16 C17 94.1(7) . . . . ? C21 C16 C17 C18 3.5(8) . . . . ? N2 C16 C17 C18 177.1(5) . . . . ? C21 C16 C17 C22 -174.4(5) . . . . ? N2 C16 C17 C22 -0.8(8) . . . . ? C16 C17 C18 C19 -0.9(10) . . . . ? C22 C17 C18 C19 177.1(6) . . . . ? C17 C18 C19 C20 -0.9(11) . . . . ? C18 C19 C20 C21 0.2(11) . . . . ? C19 C20 C21 C16 2.3(9) . . . . ? C19 C20 C21 C25 -177.2(6) . . . . ? C17 C16 C21 C20 -4.2(8) . . . . ? N2 C16 C21 C20 -177.8(5) . . . . ? C17 C16 C21 C25 175.4(5) . . . . ? N2 C16 C21 C25 1.8(8) . . . . ? C18 C17 C22 C23 44.9(8) . . . . ? C16 C17 C22 C23 -137.3(6) . . . . ? C18 C17 C22 C24 -77.7(8) . . . . ? C16 C17 C22 C24 100.1(7) . . . . ? C20 C21 C25 C26 -28.8(8) . . . . ? C16 C21 C25 C26 151.6(5) . . . . ? C20 C21 C25 C27 95.9(7) . . . . ? C16 C21 C25 C27 -83.6(7) . . . . ? C32 N3 C28 C29 2.2(9) . . . . ? Rh1 N3 C28 C29 -175.5(5) . . . . ? C32 N3 C28 C33 -179.6(5) . . . . ? Rh1 N3 C28 C33 2.7(7) . . . . ? N3 C28 C29 C30 -1.3(10) . . . . ? C33 C28 C29 C30 -179.4(6) . . . . ? C28 C29 C30 C31 -1.1(10) . . . . ? C29 C30 C31 C32 2.7(10) . . . . ? C28 N3 C32 C31 -0.6(9) . . . . ? Rh1 N3 C32 C31 176.7(4) . . . . ? C30 C31 C32 N3 -1.9(10) . . . . ? Rh1 N4 C33 C28 -40.7(6) . . . . ? N3 C28 C33 N4 24.7(8) . . . . ? C29 C28 C33 N4 -157.2(6) . . . . ? C38 N5 C34 C35 -2.4(9) . . . . ? Rh1 N5 C34 C35 -171.2(5) . . . . ? C38 N5 C34 C39 172.6(6) . . . . ? Rh1 N5 C34 C39 3.9(7) . . . . ? N5 C34 C35 C36 1.5(11) . . . . ? C39 C34 C35 C36 -173.5(7) . . . . ? C34 C35 C36 C37 -0.7(12) . . . . ? C35 C36 C37 C38 0.9(13) . . . . ? C34 N5 C38 C37 2.6(10) . . . . ? Rh1 N5 C38 C37 170.2(5) . . . . ? C36 C37 C38 N5 -1.8(12) . . . . ? N5 C34 C39 N6 9.8(8) . . . . ? C35 C34 C39 N6 -175.1(5) . . . . ? Rh1 N6 C39 C34 -18.2(6) . . . . ? C41 N7 C40 N8 0.1(5) . . . . ? C43 N7 C40 N8 171.1(5) . . . . ? C41 N7 C40 Rh2 179.5(4) . . . . ? C43 N7 C40 Rh2 -9.5(7) . . . . ? C42 N8 C40 N7 -0.3(5) . . . . ? C55 N8 C40 N7 -168.6(5) . . . . ? C42 N8 C40 Rh2 -179.7(4) . . . . ? C55 N8 C40 Rh2 12.0(8) . . . . ? N9 Rh2 C40 N7 -173.5(4) . . . . ? N10 Rh2 C40 N7 -91.6(4) . . . . ? N12 Rh2 C40 N7 1.2(4) . . . . ? N11 Rh2 C40 N7 28(2) . . . . ? Cl2 Rh2 C40 N7 91.2(4) . . . . ? N9 Rh2 C40 N8 5.8(5) . . . . ? N10 Rh2 C40 N8 87.7(4) . . . . ? N12 Rh2 C40 N8 -179.6(4) . . . . ? N11 Rh2 C40 N8 -152.3(17) . . . . ? Cl2 Rh2 C40 N8 -89.5(4) . . . . ? C40 N7 C41 C42 0.1(6) . . . . ? C43 N7 C41 C42 -172.3(4) . . . . ? N7 C41 C42 N8 -0.3(6) . . . . ? C40 N8 C42 C41 0.3(6) . . . . ? C55 N8 C42 C41 170.4(5) . . . . ? C40 N7 C43 C44 98.1(6) . . . . ? C41 N7 C43 C44 -91.3(6) . . . . ? C40 N7 C43 C48 -86.5(6) . . . . ? C41 N7 C43 C48 84.2(6) . . . . ? C48 C43 C44 C45 0.7(8) . . . . ? N7 C43 C44 C45 175.9(4) . . . . ? C48 C43 C44 C49 -177.8(5) . . . . ? N7 C43 C44 C49 -2.6(7) . . . . ? C43 C44 C45 C46 -1.2(8) . . . . ? C49 C44 C45 C46 177.2(5) . . . . ? C44 C45 C46 C47 1.5(9) . . . . ? C45 C46 C47 C48 -1.2(10) . . . . ? C46 C47 C48 C43 0.5(9) . . . . ? C46 C47 C48 C52 -178.8(6) . . . . ? C44 C43 C48 C47 -0.3(8) . . . . ? N7 C43 C48 C47 -175.6(5) . . . . ? C44 C43 C48 C52 179.0(5) . . . . ? N7 C43 C48 C52 3.7(7) . . . . ? C45 C44 C49 C50 -84.9(7) . . . . ? C43 C44 C49 C50 93.5(6) . . . . ? C45 C44 C49 C51 38.3(7) . . . . ? C43 C44 C49 C51 -143.3(5) . . . . ? C47 C48 C52 C53 82.4(7) . . . . ? C43 C48 C52 C53 -96.9(7) . . . . ? C47 C48 C52 C54 -41.7(8) . . . . ? C43 C48 C52 C54 139.0(5) . . . . ? C40 N8 C55 C60 -98.6(6) . . . . ? C42 N8 C55 C60 93.7(6) . . . . ? C40 N8 C55 C56 90.0(6) . . . . ? C42 N8 C55 C56 -77.7(6) . . . . ? C60 C55 C56 C57 5.2(8) . . . . ? N8 C55 C56 C57 176.2(4) . . . . ? C60 C55 C56 C61 -171.1(5) . . . . ? N8 C55 C56 C61 -0.2(7) . . . . ? C55 C56 C57 C58 0.1(8) . . . . ? C61 C56 C57 C58 176.7(5) . . . . ? C56 C57 C58 C59 -4.3(9) . . . . ? C57 C58 C59 C60 3.3(9) . . . . ? C56 C55 C60 C59 -6.2(8) . . . . ? N8 C55 C60 C59 -176.8(5) . . . . ? C56 C55 C60 C64 170.2(5) . . . . ? N8 C55 C60 C64 -0.5(7) . . . . ? C58 C59 C60 C55 1.7(8) . . . . ? C58 C59 C60 C64 -174.6(5) . . . . ? C55 C56 C61 C62 100.8(6) . . . . ? C57 C56 C61 C62 -75.4(7) . . . . ? C55 C56 C61 C63 -137.1(6) . . . . ? C57 C56 C61 C63 46.7(7) . . . . ? C55 C60 C64 C65 155.1(5) . . . . ? C59 C60 C64 C65 -28.8(7) . . . . ? C55 C60 C64 C66 -82.9(7) . . . . ? C59 C60 C64 C66 93.3(6) . . . . ? C71 N9 C67 C68 -1.6(7) . . . . ? Rh2 N9 C67 C68 166.6(4) . . . . ? C71 N9 C67 C72 -176.5(4) . . . . ? Rh2 N9 C67 C72 -8.3(6) . . . . ? N9 C67 C68 C69 1.5(8) . . . . ? C72 C67 C68 C69 176.1(5) . . . . ? C67 C68 C69 C70 -1.1(8) . . . . ? C68 C69 C70 C71 0.8(8) . . . . ? C67 N9 C71 C70 1.4(7) . . . . ? Rh2 N9 C71 C70 -165.6(4) . . . . ? C69 C70 C71 N9 -1.0(8) . . . . ? Rh2 N10 C72 C67 17.9(5) . . . . ? N9 C67 C72 N10 -6.7(7) . . . . ? C68 C67 C72 N10 178.5(5) . . . . ? C77 N11 C73 C74 -1.7(8) . . . . ? Rh2 N11 C73 C74 178.6(4) . . . . ? C77 N11 C73 C78 176.9(5) . . . . ? Rh2 N11 C73 C78 -2.9(6) . . . . ? N11 C73 C74 C75 2.1(8) . . . . ? C78 C73 C74 C75 -176.4(5) . . . . ? C73 C74 C75 C76 0.0(8) . . . . ? C74 C75 C76 C77 -2.4(8) . . . . ? C73 N11 C77 C76 -0.9(7) . . . . ? Rh2 N11 C77 C76 178.8(4) . . . . ? C75 C76 C77 N11 3.0(8) . . . . ? Rh2 N12 C78 C73 38.9(5) . . . . ? N11 C73 C78 N12 -23.8(7) . . . . ? C74 C73 C78 N12 154.8(5) . . . . ? C84 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C79 0.0 . . . . ? C80 C79 C84 C83 0.0 . . . . ? C90 C85 C86 C87 0.0 . . . . ? C85 C86 C87 C88 0.0 . . . . ? C86 C87 C88 C89 0.0 . . . . ? C87 C88 C89 C90 0.0 . . . . ? C86 C85 C90 C89 0.0 . . . . ? C88 C89 C90 C85 0.0 . . . . ? C96 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C92 C91 C96 C95 0.0 . . . . ? C102 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C100 0.0 . . . . ? C98 C99 C100 C101 0.0 . . . . ? C99 C100 C101 C102 0.0 . . . . ? C100 C101 C102 C97 0.0 . . . . ? C98 C97 C102 C101 0.0 . . . . ? C108 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C107 0.0 . . . . ? C105 C106 C107 C108 0.0 . . . . ? C106 C107 C108 C103 0.0 . . . . ? C104 C103 C108 C107 0.0 . . . . ? C111 C109 C110 C111 -1.7(12) 2_655 . . . ? C109 C110 C111 C109 1.6(12) . . . 2_655 ? C117 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 C117 0.0 . . . . ? C113 C112 C117 C116 0.0 . . . . ? C115 C116 C117 C112 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.791 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.085 data_cc127a _database_code_depnum_ccdc_archive 'CCDC 886713' #TrackingRef 'cc127az.cif' _audit_update_record ; 2012-06-15 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.25 H49.25 Cl N4 Rh' _chemical_formula_weight 667.40 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' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7301(16) _cell_length_b 17.553(3) _cell_length_c 20.621(3) _cell_angle_alpha 65.3250(10) _cell_angle_beta 87.833(2) _cell_angle_gamma 81.848(2) _cell_volume 3492.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1064 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 18.87 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1403 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type TWINABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13703 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1438 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13703 _reflns_number_gt 7663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13703 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _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 0.43556(5) 0.09277(3) 0.55240(2) 0.02648(14) Uani 1 1 d . . . Rh2 Rh 0.54625(5) 0.48149(3) 0.12282(3) 0.03684(17) Uani 1 1 d . . . Cl1 Cl 0.65854(14) 0.07338(10) 0.55327(9) 0.0368(4) Uani 1 1 d . . . Cl2 Cl 0.32656(18) 0.48210(12) 0.11498(11) 0.0580(5) Uani 1 1 d . . . N1 N 0.4237(5) 0.0153(3) 0.7146(2) 0.0294(12) Uani 1 1 d . . . N2 N 0.3824(4) 0.1527(3) 0.6679(2) 0.0272(11) Uani 1 1 d . . . N3 N 0.2469(4) 0.1069(3) 0.5338(3) 0.0282(12) Uani 1 1 d . . . N4 N 0.4379(5) 0.1040(3) 0.4455(2) 0.0342(13) Uani 1 1 d . . . H4A H 0.4990 0.1361 0.4207 0.041 Uiso 1 1 calc R . . H4B H 0.4568 0.0512 0.4455 0.041 Uiso 1 1 calc R . . N5 N 0.5551(5) 0.5317(3) 0.2466(3) 0.0314(12) Uani 1 1 d . . . N6 N 0.5212(5) 0.6423(3) 0.1453(2) 0.0310(12) Uani 1 1 d . . . N7 N 0.7343(6) 0.4628(3) 0.1205(3) 0.0511(17) Uani 1 1 d . . . N8 N 0.5689(6) 0.4040(3) 0.0654(3) 0.0493(16) Uani 1 1 d . . . H8B H 0.5149 0.3641 0.0826 0.059 Uiso 1 1 calc R . . H8C H 0.5488 0.4369 0.0179 0.059 Uiso 1 1 calc R . . C1 C 0.4178(5) 0.0856(4) 0.6490(3) 0.0270(14) Uani 1 1 d . . . C2 C 0.3892(6) 0.0393(4) 0.7707(3) 0.0358(16) Uani 1 1 d . . . H2A H 0.3851 0.0024 0.8198 0.043 Uiso 1 1 calc R . . C3 C 0.3634(6) 0.1235(4) 0.7421(3) 0.0363(16) Uani 1 1 d . . . H3A H 0.3370 0.1577 0.7671 0.044 Uiso 1 1 calc R . . C4 C 0.4785(6) -0.0715(4) 0.7290(3) 0.0297(14) Uani 1 1 d . . . C5 C 0.4003(6) -0.1300(4) 0.7289(3) 0.0320(15) Uani 1 1 d . . . C6 C 0.4580(6) -0.2135(4) 0.7480(3) 0.0388(16) Uani 1 1 d . . . H6A H 0.4098 -0.2541 0.7462 0.047 Uiso 1 1 calc R . . C7 C 0.5827(7) -0.2382(4) 0.7692(3) 0.0421(18) Uani 1 1 d . . . H7A H 0.6194 -0.2953 0.7826 0.051 Uiso 1 1 calc R . . C8 C 0.6548(6) -0.1794(4) 0.7710(3) 0.0387(16) Uani 1 1 d . . . H8A H 0.7404 -0.1975 0.7867 0.046 Uiso 1 1 calc R . . C9 C 0.6054(6) -0.0945(4) 0.7505(3) 0.0311(15) Uani 1 1 d . . . C10 C 0.2626(6) -0.1049(4) 0.7075(3) 0.0434(18) Uani 1 1 d . . . H10A H 0.2393 -0.0439 0.6978 0.052 Uiso 1 1 calc R . . C11 C 0.2338(7) -0.1155(5) 0.6417(4) 0.060(2) Uani 1 1 d . . . H11A H 0.2844 -0.0817 0.6024 0.090 Uiso 1 1 calc R . . H11B H 0.1442 -0.0965 0.6289 0.090 Uiso 1 1 calc R . . H11C H 0.2538 -0.1753 0.6505 0.090 Uiso 1 1 calc R . . C12 C 0.1787(7) -0.1576(6) 0.7684(5) 0.080(3) Uani 1 1 d . . . H12A H 0.1958 -0.1510 0.8120 0.120 Uiso 1 1 calc R . . H12B H 0.1978 -0.2175 0.7774 0.120 Uiso 1 1 calc R . . H12C H 0.0898 -0.1376 0.7542 0.120 Uiso 1 1 calc R . . C13 C 0.6887(6) -0.0321(4) 0.7544(3) 0.0408(17) Uani 1 1 d . . . H13A H 0.6448 0.0264 0.7264 0.049 Uiso 1 1 calc R . . C14 C 0.8175(6) -0.0387(5) 0.7232(4) 0.056(2) Uani 1 1 d . . . H14A H 0.8082 -0.0307 0.6736 0.084 Uiso 1 1 calc R . . H14B H 0.8645 -0.0947 0.7510 0.084 Uiso 1 1 calc R . . H14C H 0.8633 0.0050 0.7247 0.084 Uiso 1 1 calc R . . C15 C 0.7035(7) -0.0437(5) 0.8330(4) 0.055(2) Uani 1 1 d . . . H15A H 0.7561 -0.0031 0.8345 0.082 Uiso 1 1 calc R . . H15B H 0.7435 -0.1015 0.8622 0.082 Uiso 1 1 calc R . . H15C H 0.6204 -0.0339 0.8517 0.082 Uiso 1 1 calc R . . C16 C 0.3857(6) 0.2421(4) 0.6222(3) 0.0290(14) Uani 1 1 d . . . C17 C 0.5054(6) 0.2706(4) 0.6084(3) 0.0278(14) Uani 1 1 d . . . C18 C 0.5066(6) 0.3569(4) 0.5675(3) 0.0392(17) Uani 1 1 d . . . H18A H 0.5852 0.3778 0.5561 0.047 Uiso 1 1 calc R . . C19 C 0.3985(7) 0.4120(4) 0.5435(4) 0.0457(19) Uani 1 1 d . . . H19A H 0.4028 0.4706 0.5163 0.055 Uiso 1 1 calc R . . C20 C 0.2824(6) 0.3835(4) 0.5582(4) 0.0456(18) Uani 1 1 d . . . H20A H 0.2076 0.4226 0.5407 0.055 Uiso 1 1 calc R . . C21 C 0.2743(6) 0.2969(4) 0.5992(3) 0.0387(16) Uani 1 1 d . . . C22 C 0.6274(5) 0.2115(4) 0.6384(3) 0.0315(15) Uani 1 1 d . . . H22A H 0.6169 0.1551 0.6400 0.038 Uiso 1 1 calc R . . C23 C 0.6526(6) 0.1995(4) 0.7154(3) 0.0463(18) Uani 1 1 d . . . H23A H 0.5794 0.1804 0.7445 0.069 Uiso 1 1 calc R . . H23B H 0.6677 0.2535 0.7151 0.069 Uiso 1 1 calc R . . H23C H 0.7269 0.1571 0.7356 0.069 Uiso 1 1 calc R . . C24 C 0.7436(6) 0.2404(4) 0.5942(4) 0.0471(18) Uani 1 1 d . . . H24A H 0.7291 0.2481 0.5451 0.071 Uiso 1 1 calc R . . H24B H 0.8170 0.1975 0.6151 0.071 Uiso 1 1 calc R . . H24C H 0.7591 0.2942 0.5941 0.071 Uiso 1 1 calc R . . C25 C 0.1447(6) 0.2690(4) 0.6126(4) 0.0485(19) Uani 1 1 d . . . H25A H 0.1559 0.2057 0.6358 0.058 Uiso 1 1 calc R . . C26 C 0.0751(7) 0.3014(5) 0.6642(5) 0.081(3) Uani 1 1 d . . . H26A H 0.1251 0.2808 0.7085 0.121 Uiso 1 1 calc R . . H26B H -0.0068 0.2807 0.6748 0.121 Uiso 1 1 calc R . . H26C H 0.0622 0.3634 0.6424 0.121 Uiso 1 1 calc R . . C27 C 0.0681(7) 0.2986(5) 0.5432(4) 0.067(2) Uani 1 1 d . . . H27A H 0.1138 0.2762 0.5114 0.100 Uiso 1 1 calc R . . H27B H 0.0552 0.3606 0.5199 0.100 Uiso 1 1 calc R . . H27C H -0.0137 0.2779 0.5540 0.100 Uiso 1 1 calc R . . C28 C 0.2119(6) 0.1246(4) 0.4654(3) 0.0351(16) Uani 1 1 d . . . C29 C 0.0890(6) 0.1255(4) 0.4468(4) 0.0431(18) Uani 1 1 d . . . H29A H 0.0680 0.1372 0.3989 0.052 Uiso 1 1 calc R . . C30 C -0.0028(6) 0.1094(4) 0.4971(4) 0.0475(19) Uani 1 1 d . . . H30A H -0.0873 0.1101 0.4844 0.057 Uiso 1 1 calc R . . C31 C 0.0300(6) 0.0920(4) 0.5668(4) 0.0415(17) Uani 1 1 d . . . H31A H -0.0312 0.0802 0.6030 0.050 Uiso 1 1 calc R . . C32 C 0.1563(6) 0.0925(4) 0.5825(3) 0.0335(15) Uani 1 1 d . . . H32A H 0.1786 0.0822 0.6298 0.040 Uiso 1 1 calc R . . C33 C 0.3140(6) 0.1443(4) 0.4106(3) 0.0397(17) Uani 1 1 d . . . H33A H 0.2979 0.1233 0.3744 0.048 Uiso 1 1 calc R . . H33B H 0.3132 0.2064 0.3860 0.048 Uiso 1 1 calc R . . C34 C 0.5337(6) 0.5544(4) 0.1739(3) 0.0303(14) Uani 1 1 d . . . C35 C 0.5556(6) 0.6034(4) 0.2601(3) 0.0384(16) Uani 1 1 d . . . H35A H 0.5681 0.6038 0.3053 0.046 Uiso 1 1 calc R . . C36 C 0.5355(6) 0.6700(4) 0.1991(3) 0.0331(15) Uani 1 1 d . . . H36A H 0.5314 0.7272 0.1923 0.040 Uiso 1 1 calc R . . C37 C 0.5459(6) 0.4492(4) 0.3039(3) 0.0311(15) Uani 1 1 d . . . C38 C 0.4248(7) 0.4296(4) 0.3268(3) 0.0370(16) Uani 1 1 d . . . C39 C 0.4182(7) 0.3523(4) 0.3872(3) 0.0440(18) Uani 1 1 d . . . H39A H 0.3380 0.3376 0.4051 0.053 Uiso 1 1 calc R . . C40 C 0.5237(7) 0.2982(4) 0.4206(4) 0.0465(19) Uani 1 1 d . . . H40A H 0.5162 0.2461 0.4603 0.056 Uiso 1 1 calc R . . C41 C 0.6401(7) 0.3191(4) 0.3966(4) 0.0458(18) Uani 1 1 d . . . H41A H 0.7127 0.2806 0.4199 0.055 Uiso 1 1 calc R . . C42 C 0.6557(6) 0.3959(4) 0.3386(3) 0.0339(15) Uani 1 1 d . . . C43 C 0.3055(6) 0.4891(4) 0.2926(4) 0.0458(18) Uani 1 1 d . . . H43A H 0.3251 0.5277 0.2428 0.055 Uiso 1 1 calc R . . C44 C 0.1954(7) 0.4429(5) 0.2883(4) 0.070(2) Uani 1 1 d . . . H44A H 0.1219 0.4847 0.2652 0.105 Uiso 1 1 calc R . . H44B H 0.1740 0.4050 0.3366 0.105 Uiso 1 1 calc R . . H44C H 0.2207 0.4099 0.2605 0.105 Uiso 1 1 calc R . . C45 C 0.2643(7) 0.5434(5) 0.3332(4) 0.071(3) Uani 1 1 d . . . H45A H 0.3334 0.5734 0.3351 0.107 Uiso 1 1 calc R . . H45B H 0.2420 0.5070 0.3818 0.107 Uiso 1 1 calc R . . H45C H 0.1910 0.5845 0.3087 0.107 Uiso 1 1 calc R . . C46 C 0.7868(6) 0.4185(4) 0.3195(4) 0.0412(17) Uani 1 1 d . . . H46A H 0.7807 0.4707 0.2738 0.049 Uiso 1 1 calc R . . C47 C 0.8758(7) 0.3496(5) 0.3087(4) 0.063(2) Uani 1 1 d . . . H47A H 0.8416 0.3377 0.2710 0.095 Uiso 1 1 calc R . . H47B H 0.8850 0.2981 0.3533 0.095 Uiso 1 1 calc R . . H47C H 0.9583 0.3685 0.2948 0.095 Uiso 1 1 calc R . . C48 C 0.8411(7) 0.4390(5) 0.3783(4) 0.061(2) Uani 1 1 d . . . H48A H 0.7839 0.4842 0.3843 0.091 Uiso 1 1 calc R . . H48B H 0.9238 0.4575 0.3641 0.091 Uiso 1 1 calc R . . H48C H 0.8500 0.3882 0.4234 0.091 Uiso 1 1 calc R . . C49 C 0.4766(7) 0.6992(4) 0.0732(3) 0.0339(16) Uani 1 1 d . . . C50 C 0.5647(7) 0.7258(4) 0.0190(4) 0.0427(18) Uani 1 1 d . . . C51 C 0.5150(9) 0.7823(4) -0.0482(4) 0.057(2) Uani 1 1 d . . . H51A H 0.5712 0.8006 -0.0867 0.068 Uiso 1 1 calc R . . C52 C 0.3898(9) 0.8126(5) -0.0615(4) 0.059(2) Uani 1 1 d . . . H52A H 0.3607 0.8509 -0.1083 0.071 Uiso 1 1 calc R . . C53 C 0.3068(8) 0.7877(4) -0.0072(4) 0.052(2) Uani 1 1 d . . . H53A H 0.2199 0.8098 -0.0157 0.062 Uiso 1 1 calc R . . C54 C 0.3503(7) 0.7294(4) 0.0611(4) 0.0415(17) Uani 1 1 d . . . C55 C 0.7032(8) 0.6992(5) 0.0323(4) 0.064(2) Uani 1 1 d . . . H55A H 0.7143 0.6468 0.0780 0.077 Uiso 1 1 calc R . . C56 C 0.7728(8) 0.6768(5) -0.0238(4) 0.085(3) Uani 1 1 d . . . H56A H 0.7336 0.6334 -0.0305 0.128 Uiso 1 1 calc R . . H56B H 0.8609 0.6551 -0.0083 0.128 Uiso 1 1 calc R . . H56C H 0.7690 0.7274 -0.0689 0.128 Uiso 1 1 calc R . . C57 C 0.7639(8) 0.7654(7) 0.0444(5) 0.095(3) Uani 1 1 d . . . H57A H 0.7183 0.7790 0.0811 0.143 Uiso 1 1 calc R . . H57B H 0.7608 0.8166 -0.0002 0.143 Uiso 1 1 calc R . . H57C H 0.8519 0.7432 0.0601 0.143 Uiso 1 1 calc R . . C58 C 0.2516(7) 0.7054(4) 0.1215(4) 0.052(2) Uani 1 1 d . . . H58A H 0.2942 0.6586 0.1651 0.063 Uiso 1 1 calc R . . C59 C 0.2082(7) 0.7818(5) 0.1397(4) 0.071(3) Uani 1 1 d . . . H59A H 0.1467 0.7664 0.1778 0.107 Uiso 1 1 calc R . . H59B H 0.1694 0.8296 0.0972 0.107 Uiso 1 1 calc R . . H59C H 0.2810 0.7980 0.1557 0.107 Uiso 1 1 calc R . . C60 C 0.1393(7) 0.6740(5) 0.1024(5) 0.078(3) Uani 1 1 d . . . H60A H 0.0806 0.6595 0.1419 0.117 Uiso 1 1 calc R . . H60B H 0.1686 0.6237 0.0936 0.117 Uiso 1 1 calc R . . H60C H 0.0966 0.7185 0.0593 0.117 Uiso 1 1 calc R . . C61 C 0.7887(8) 0.4073(5) 0.0930(4) 0.056(2) Uani 1 1 d . . . C62 C 0.9164(8) 0.3904(6) 0.0845(5) 0.083(3) Uani 1 1 d . . . H62A H 0.9484 0.3507 0.0657 0.099 Uiso 1 1 calc R . . C63 C 0.9960(7) 0.4323(6) 0.1040(5) 0.073(3) Uani 1 1 d . . . H63A H 1.0839 0.4232 0.0968 0.088 Uiso 1 1 calc R . . C64 C 0.9504(8) 0.4863(5) 0.1333(4) 0.063(2) Uani 1 1 d . . . H64A H 1.0058 0.5139 0.1482 0.076 Uiso 1 1 calc R . . C65 C 0.8195(7) 0.5010(4) 0.1413(4) 0.0476(19) Uani 1 1 d . . . H65A H 0.7882 0.5390 0.1620 0.057 Uiso 1 1 calc R . . C66 C 0.6977(8) 0.3620(5) 0.0724(5) 0.067(2) Uani 1 1 d . . . H66A H 0.7230 0.3598 0.0265 0.080 Uiso 1 1 calc R . . H66B H 0.7021 0.3031 0.1091 0.080 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 0.0304(3) 0.0259(3) 0.0237(3) -0.0101(2) 0.0003(2) -0.0062(2) Rh2 0.0555(4) 0.0273(3) 0.0296(3) -0.0144(3) 0.0028(3) -0.0039(3) Cl1 0.0294(9) 0.0444(10) 0.0424(10) -0.0236(8) 0.0026(7) -0.0062(8) Cl2 0.0545(13) 0.0639(13) 0.0694(14) -0.0403(11) -0.0034(10) -0.0104(10) N1 0.044(3) 0.025(3) 0.018(3) -0.008(2) -0.002(2) -0.004(2) N2 0.033(3) 0.023(3) 0.028(3) -0.013(2) 0.001(2) -0.004(2) N3 0.019(3) 0.026(3) 0.036(3) -0.009(2) -0.005(2) -0.001(2) N4 0.048(4) 0.027(3) 0.029(3) -0.012(2) 0.003(3) -0.010(3) N5 0.036(3) 0.029(3) 0.029(3) -0.013(2) 0.000(2) 0.000(2) N6 0.049(3) 0.021(3) 0.023(3) -0.010(2) -0.001(2) -0.002(2) N7 0.079(5) 0.031(3) 0.043(4) -0.015(3) 0.018(3) -0.015(3) N8 0.070(5) 0.037(3) 0.042(4) -0.020(3) -0.007(3) -0.002(3) C1 0.026(3) 0.026(3) 0.032(3) -0.014(3) 0.006(3) -0.008(3) C2 0.054(5) 0.027(3) 0.021(3) -0.005(3) 0.005(3) -0.004(3) C3 0.051(4) 0.038(4) 0.027(3) -0.019(3) 0.005(3) -0.010(3) C4 0.040(4) 0.024(3) 0.022(3) -0.007(3) 0.004(3) -0.007(3) C5 0.040(4) 0.030(3) 0.028(3) -0.013(3) -0.001(3) -0.006(3) C6 0.046(4) 0.029(4) 0.042(4) -0.015(3) 0.003(3) -0.008(3) C7 0.058(5) 0.030(4) 0.037(4) -0.016(3) 0.010(4) 0.003(4) C8 0.038(4) 0.038(4) 0.031(4) -0.010(3) 0.003(3) 0.006(3) C9 0.030(4) 0.039(4) 0.019(3) -0.007(3) 0.001(3) -0.006(3) C10 0.053(5) 0.037(4) 0.041(4) -0.014(3) -0.016(4) -0.012(3) C11 0.057(5) 0.071(6) 0.062(5) -0.036(5) -0.014(4) -0.012(4) C12 0.035(5) 0.116(8) 0.089(7) -0.045(6) 0.004(5) -0.005(5) C13 0.047(5) 0.039(4) 0.034(4) -0.012(3) -0.004(3) -0.006(3) C14 0.045(5) 0.074(6) 0.038(4) -0.012(4) 0.000(4) -0.008(4) C15 0.066(5) 0.065(5) 0.047(5) -0.030(4) 0.004(4) -0.032(4) C16 0.032(4) 0.022(3) 0.032(4) -0.009(3) 0.006(3) -0.007(3) C17 0.031(4) 0.030(3) 0.025(3) -0.014(3) 0.004(3) -0.008(3) C18 0.035(4) 0.035(4) 0.047(4) -0.013(3) 0.008(3) -0.018(3) C19 0.065(5) 0.023(3) 0.043(4) -0.006(3) -0.010(4) -0.010(4) C20 0.042(4) 0.033(4) 0.061(5) -0.021(4) -0.019(4) 0.009(3) C21 0.044(4) 0.028(3) 0.046(4) -0.017(3) -0.002(3) -0.005(3) C22 0.033(4) 0.032(3) 0.035(4) -0.017(3) 0.005(3) -0.015(3) C23 0.055(5) 0.050(4) 0.045(4) -0.032(4) -0.003(4) -0.002(4) C24 0.035(4) 0.058(5) 0.054(5) -0.028(4) 0.006(4) -0.009(4) C25 0.041(4) 0.038(4) 0.066(5) -0.020(4) 0.001(4) -0.006(3) C26 0.059(6) 0.074(6) 0.114(8) -0.045(6) 0.035(5) -0.014(5) C27 0.050(5) 0.051(5) 0.093(7) -0.023(5) -0.023(5) -0.005(4) C28 0.042(4) 0.031(3) 0.032(4) -0.011(3) -0.003(3) -0.007(3) C29 0.037(4) 0.055(5) 0.040(4) -0.023(4) -0.013(3) -0.002(4) C30 0.034(4) 0.054(5) 0.059(5) -0.026(4) -0.010(4) -0.008(4) C31 0.031(4) 0.045(4) 0.052(5) -0.024(4) 0.008(3) -0.003(3) C32 0.029(4) 0.041(4) 0.031(4) -0.015(3) 0.000(3) -0.008(3) C33 0.045(4) 0.043(4) 0.031(4) -0.013(3) -0.006(3) -0.010(3) C34 0.035(4) 0.028(3) 0.025(3) -0.008(3) 0.003(3) -0.008(3) C35 0.049(4) 0.037(4) 0.035(4) -0.021(3) 0.005(3) -0.009(3) C36 0.042(4) 0.026(3) 0.038(4) -0.019(3) 0.005(3) -0.011(3) C37 0.044(4) 0.024(3) 0.021(3) -0.005(3) 0.004(3) -0.006(3) C38 0.056(5) 0.035(4) 0.028(4) -0.017(3) 0.008(3) -0.019(3) C39 0.066(5) 0.038(4) 0.035(4) -0.018(3) 0.006(4) -0.020(4) C40 0.073(6) 0.033(4) 0.035(4) -0.014(3) 0.001(4) -0.013(4) C41 0.058(5) 0.033(4) 0.043(4) -0.015(3) -0.007(4) 0.007(4) C42 0.051(4) 0.025(3) 0.030(4) -0.016(3) 0.004(3) -0.004(3) C43 0.045(5) 0.046(4) 0.037(4) -0.008(4) 0.007(3) -0.007(4) C44 0.049(5) 0.093(7) 0.060(5) -0.022(5) 0.004(4) -0.015(5) C45 0.053(5) 0.068(6) 0.090(7) -0.036(5) 0.007(5) 0.011(4) C46 0.039(4) 0.034(4) 0.041(4) -0.007(3) 0.002(3) -0.002(3) C47 0.056(5) 0.054(5) 0.084(6) -0.033(5) 0.011(5) -0.010(4) C48 0.048(5) 0.065(5) 0.084(6) -0.045(5) -0.010(4) -0.010(4) C49 0.055(5) 0.022(3) 0.025(3) -0.009(3) -0.007(3) -0.004(3) C50 0.064(5) 0.029(4) 0.036(4) -0.016(3) 0.007(4) -0.001(3) C51 0.111(8) 0.032(4) 0.027(4) -0.010(3) 0.012(5) -0.019(4) C52 0.093(7) 0.044(5) 0.041(5) -0.015(4) -0.019(5) -0.013(5) C53 0.080(6) 0.036(4) 0.036(4) -0.006(4) -0.003(4) -0.024(4) C54 0.054(5) 0.031(4) 0.041(4) -0.015(3) -0.004(4) -0.010(3) C55 0.070(6) 0.049(5) 0.049(5) -0.001(4) 0.015(4) 0.004(4) C56 0.095(7) 0.074(6) 0.077(6) -0.030(5) 0.051(6) 0.000(5) C57 0.053(6) 0.160(10) 0.082(7) -0.061(7) 0.006(5) -0.010(6) C58 0.054(5) 0.045(4) 0.044(5) -0.008(4) -0.005(4) 0.001(4) C59 0.067(6) 0.101(7) 0.067(6) -0.054(6) 0.016(5) -0.019(5) C60 0.055(6) 0.078(6) 0.112(8) -0.045(6) -0.010(5) -0.021(5) C61 0.069(6) 0.057(5) 0.062(5) -0.041(4) 0.025(4) -0.021(4) C62 0.054(6) 0.103(7) 0.135(9) -0.091(7) 0.043(6) -0.023(5) C63 0.035(5) 0.111(8) 0.105(7) -0.075(7) 0.029(5) -0.019(5) C64 0.076(6) 0.073(6) 0.058(5) -0.036(5) 0.016(5) -0.037(5) C65 0.061(5) 0.040(4) 0.045(4) -0.023(4) 0.006(4) -0.002(4) C66 0.078(6) 0.073(6) 0.080(6) -0.057(5) 0.025(5) -0.030(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 C1 1.947(6) . ? Rh1 N3 2.035(5) . ? Rh1 N4 2.130(5) . ? Rh1 Cl1 2.3681(17) . ? Rh2 C34 1.957(6) . ? Rh2 N7 2.000(6) . ? Rh2 N8 2.130(5) . ? Rh2 Cl2 2.367(2) . ? N1 C1 1.396(7) . ? N1 C2 1.408(7) . ? N1 C4 1.462(7) . ? N2 C1 1.388(7) . ? N2 C3 1.414(7) . ? N2 C16 1.460(7) . ? N3 C32 1.342(7) . ? N3 C28 1.365(7) . ? N4 C33 1.472(7) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C35 1.398(7) . ? N5 C34 1.400(7) . ? N5 C37 1.452(7) . ? N6 C34 1.390(7) . ? N6 C36 1.405(7) . ? N6 C49 1.455(7) . ? N7 C61 1.373(8) . ? N7 C65 1.383(8) . ? N8 C66 1.452(9) . ? N8 H8B 0.9200 . ? N8 H8C 0.9200 . ? C2 C3 1.333(8) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.398(8) . ? C4 C5 1.416(8) . ? C5 C6 1.403(8) . ? C5 C10 1.508(8) . ? C6 C7 1.375(8) . ? C6 H6A 0.9500 . ? C7 C8 1.388(9) . ? C7 H7A 0.9500 . ? C8 C9 1.395(8) . ? C8 H8A 0.9500 . ? C9 C13 1.537(8) . ? C10 C11 1.495(8) . ? C10 C12 1.557(10) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(8) . ? C13 C15 1.558(8) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.383(8) . ? C16 C17 1.420(8) . ? C17 C18 1.395(8) . ? C17 C22 1.520(8) . ? C18 C19 1.361(8) . ? C18 H18A 0.9500 . ? C19 C20 1.384(9) . ? C19 H19A 0.9500 . ? C20 C21 1.412(8) . ? C20 H20A 0.9500 . ? C21 C25 1.517(9) . ? C22 C24 1.533(8) . ? C22 C23 1.542(8) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.529(9) . ? C25 C27 1.529(9) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.384(8) . ? C28 C33 1.512(8) . ? C29 C30 1.372(9) . ? C29 H29A 0.9500 . ? C30 C31 1.388(9) . ? C30 H30A 0.9500 . ? C31 C32 1.407(8) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 C36 1.310(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.402(8) . ? C37 C38 1.405(8) . ? C38 C39 1.417(8) . ? C38 C43 1.517(9) . ? C39 C40 1.365(9) . ? C39 H39A 0.9500 . ? C40 C41 1.369(9) . ? C40 H40A 0.9500 . ? C41 C42 1.406(8) . ? C41 H41A 0.9500 . ? C42 C46 1.508(8) . ? C43 C45 1.524(9) . ? C43 C44 1.549(9) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.518(9) . ? C46 C48 1.554(9) . ? C46 H46A 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C54 1.375(9) . ? C49 C50 1.403(9) . ? C50 C51 1.395(9) . ? C50 C55 1.493(10) . ? C51 C52 1.366(10) . ? C51 H51A 0.9500 . ? C52 C53 1.366(10) . ? C52 H52A 0.9500 . ? C53 C54 1.399(9) . ? C53 H53A 0.9500 . ? C54 C58 1.562(9) . ? C55 C56 1.510(10) . ? C55 C57 1.518(11) . ? C55 H55A 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C60 1.523(9) . ? C58 C59 1.545(9) . ? C58 H58A 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.381(10) . ? C61 C66 1.517(10) . ? C62 C63 1.371(10) . ? C62 H62A 0.9500 . ? C63 C64 1.353(10) . ? C63 H63A 0.9500 . ? C64 C65 1.408(10) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? 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 C1 Rh1 N3 94.4(2) . . ? C1 Rh1 N4 175.1(2) . . ? N3 Rh1 N4 80.7(2) . . ? C1 Rh1 Cl1 96.39(17) . . ? N3 Rh1 Cl1 169.02(15) . . ? N4 Rh1 Cl1 88.46(14) . . ? C34 Rh2 N7 96.7(2) . . ? C34 Rh2 N8 177.1(2) . . ? N7 Rh2 N8 80.7(2) . . ? C34 Rh2 Cl2 95.48(18) . . ? N7 Rh2 Cl2 167.74(17) . . ? N8 Rh2 Cl2 87.18(17) . . ? C1 N1 C2 111.3(5) . . ? C1 N1 C4 126.7(5) . . ? C2 N1 C4 121.2(5) . . ? C1 N2 C3 111.1(5) . . ? C1 N2 C16 126.2(5) . . ? C3 N2 C16 121.8(5) . . ? C32 N3 C28 117.3(5) . . ? C32 N3 Rh1 126.9(4) . . ? C28 N3 Rh1 115.5(4) . . ? C33 N4 Rh1 109.7(4) . . ? C33 N4 H4A 109.7 . . ? Rh1 N4 H4A 109.7 . . ? C33 N4 H4B 109.7 . . ? Rh1 N4 H4B 109.7 . . ? H4A N4 H4B 108.2 . . ? C35 N5 C34 111.0(5) . . ? C35 N5 C37 121.6(5) . . ? C34 N5 C37 125.6(5) . . ? C34 N6 C36 110.5(5) . . ? C34 N6 C49 125.5(5) . . ? C36 N6 C49 123.0(5) . . ? C61 N7 C65 114.1(6) . . ? C61 N7 Rh2 117.6(5) . . ? C65 N7 Rh2 128.3(5) . . ? C66 N8 Rh2 110.8(4) . . ? C66 N8 H8B 109.5 . . ? Rh2 N8 H8B 109.5 . . ? C66 N8 H8C 109.5 . . ? Rh2 N8 H8C 109.5 . . ? H8B N8 H8C 108.1 . . ? N2 C1 N1 102.8(5) . . ? N2 C1 Rh1 126.3(4) . . ? N1 C1 Rh1 130.6(4) . . ? C3 C2 N1 107.2(5) . . ? C3 C2 H2A 126.4 . . ? N1 C2 H2A 126.4 . . ? C2 C3 N2 107.5(5) . . ? C2 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? C9 C4 C5 123.2(6) . . ? C9 C4 N1 116.5(5) . . ? C5 C4 N1 119.9(5) . . ? C6 C5 C4 116.6(6) . . ? C6 C5 C10 120.6(6) . . ? C4 C5 C10 122.7(5) . . ? C7 C6 C5 121.5(6) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 119.9(6) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C7 C8 C9 122.0(6) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C8 C9 C4 116.7(6) . . ? C8 C9 C13 120.0(6) . . ? C4 C9 C13 123.3(6) . . ? C11 C10 C5 112.4(6) . . ? C11 C10 C12 108.3(6) . . ? C5 C10 C12 111.3(6) . . ? C11 C10 H10A 108.2 . . ? C5 C10 H10A 108.2 . . ? C12 C10 H10A 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 113.9(6) . . ? C14 C13 C15 109.5(6) . . ? C9 C13 C15 110.4(5) . . ? C14 C13 H13A 107.6 . . ? C9 C13 H13A 107.6 . . ? C15 C13 H13A 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.4(5) . . ? C21 C16 N2 119.8(5) . . ? C17 C16 N2 117.5(5) . . ? C18 C17 C16 116.8(6) . . ? C18 C17 C22 120.7(5) . . ? C16 C17 C22 122.5(5) . . ? C19 C18 C17 121.9(6) . . ? C19 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? C18 C19 C20 120.6(6) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C19 C20 C21 120.4(6) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C16 C21 C20 117.8(6) . . ? C16 C21 C25 124.0(6) . . ? C20 C21 C25 118.2(6) . . ? C17 C22 C24 114.4(5) . . ? C17 C22 C23 110.5(5) . . ? C24 C22 C23 108.5(5) . . ? C17 C22 H22A 107.7 . . ? C24 C22 H22A 107.7 . . ? C23 C22 H22A 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 109.6(6) . . ? C21 C25 C27 111.9(6) . . ? C26 C25 C27 110.9(6) . . ? C21 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? C27 C25 H25A 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 122.0(6) . . ? N3 C28 C33 116.6(5) . . ? C29 C28 C33 121.4(6) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 118.9(6) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? C30 C31 C32 118.2(6) . . ? C30 C31 H31A 120.9 . . ? C32 C31 H31A 120.9 . . ? N3 C32 C31 123.3(6) . . ? N3 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? N4 C33 C28 110.1(5) . . ? N4 C33 H33A 109.6 . . ? C28 C33 H33A 109.6 . . ? N4 C33 H33B 109.6 . . ? C28 C33 H33B 109.6 . . ? H33A C33 H33B 108.2 . . ? N6 C34 N5 102.5(5) . . ? N6 C34 Rh2 128.0(4) . . ? N5 C34 Rh2 128.8(4) . . ? C36 C35 N5 107.6(5) . . ? C36 C35 H35A 126.2 . . ? N5 C35 H35A 126.2 . . ? C35 C36 N6 108.4(5) . . ? C35 C36 H36A 125.8 . . ? N6 C36 H36A 125.8 . . ? C42 C37 C38 122.5(6) . . ? C42 C37 N5 119.8(6) . . ? C38 C37 N5 117.5(5) . . ? C37 C38 C39 116.6(6) . . ? C37 C38 C43 123.0(6) . . ? C39 C38 C43 120.3(6) . . ? C40 C39 C38 122.0(7) . . ? C40 C39 H39A 119.0 . . ? C38 C39 H39A 119.0 . . ? C39 C40 C41 119.8(7) . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C40 C41 C42 122.1(7) . . ? C40 C41 H41A 119.0 . . ? C42 C41 H41A 119.0 . . ? C37 C42 C41 117.0(6) . . ? C37 C42 C46 123.8(6) . . ? C41 C42 C46 119.1(6) . . ? C38 C43 C45 109.9(6) . . ? C38 C43 C44 113.5(6) . . ? C45 C43 C44 109.4(6) . . ? C38 C43 H43A 108.0 . . ? C45 C43 H43A 108.0 . . ? C44 C43 H43A 108.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 C47 113.2(6) . . ? C42 C46 C48 109.6(5) . . ? C47 C46 C48 110.0(6) . . ? C42 C46 H46A 108.0 . . ? C47 C46 H46A 108.0 . . ? C48 C46 H46A 108.0 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C54 C49 C50 121.9(6) . . ? C54 C49 N6 119.0(6) . . ? C50 C49 N6 119.0(6) . . ? C51 C50 C49 115.6(7) . . ? C51 C50 C55 121.5(7) . . ? C49 C50 C55 122.8(6) . . ? C52 C51 C50 123.4(7) . . ? C52 C51 H51A 118.3 . . ? C50 C51 H51A 118.3 . . ? C51 C52 C53 119.7(7) . . ? C51 C52 H52A 120.2 . . ? C53 C52 H52A 120.2 . . ? C52 C53 C54 119.6(8) . . ? C52 C53 H53A 120.2 . . ? C54 C53 H53A 120.2 . . ? C49 C54 C53 119.7(7) . . ? C49 C54 C58 122.9(6) . . ? C53 C54 C58 117.3(7) . . ? C50 C55 C56 115.4(7) . . ? C50 C55 C57 110.7(7) . . ? C56 C55 C57 110.3(7) . . ? C50 C55 H55A 106.6 . . ? C56 C55 H55A 106.6 . . ? C57 C55 H55A 106.6 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C60 C58 C59 110.8(7) . . ? C60 C58 C54 112.6(6) . . ? C59 C58 C54 109.8(6) . . ? C60 C58 H58A 107.8 . . ? C59 C58 H58A 107.8 . . ? C54 C58 H58A 107.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N7 C61 C62 124.8(7) . . ? N7 C61 C66 115.2(7) . . ? C62 C61 C66 120.0(7) . . ? C63 C62 C61 118.4(7) . . ? C63 C62 H62A 120.8 . . ? C61 C62 H62A 120.8 . . ? C64 C63 C62 120.5(8) . . ? C64 C63 H63A 119.7 . . ? C62 C63 H63A 119.7 . . ? C63 C64 C65 118.9(7) . . ? C63 C64 H64A 120.6 . . ? C65 C64 H64A 120.6 . . ? N7 C65 C64 123.2(7) . . ? N7 C65 H65A 118.4 . . ? C64 C65 H65A 118.4 . . ? N8 C66 C61 111.9(6) . . ? N8 C66 H66A 109.2 . . ? C61 C66 H66A 109.2 . . ? N8 C66 H66B 109.2 . . ? C61 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? 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 C1 Rh1 N3 C32 -14.3(5) . . . . ? N4 Rh1 N3 C32 166.7(5) . . . . ? Cl1 Rh1 N3 C32 156.2(5) . . . . ? C1 Rh1 N3 C28 172.7(4) . . . . ? N4 Rh1 N3 C28 -6.3(4) . . . . ? Cl1 Rh1 N3 C28 -16.8(10) . . . . ? C1 Rh1 N4 C33 9(3) . . . . ? N3 Rh1 N4 C33 19.9(4) . . . . ? Cl1 Rh1 N4 C33 -162.0(4) . . . . ? C34 Rh2 N7 C61 175.0(5) . . . . ? N8 Rh2 N7 C61 -6.2(5) . . . . ? Cl2 Rh2 N7 C61 1.3(11) . . . . ? C34 Rh2 N7 C65 -7.3(6) . . . . ? N8 Rh2 N7 C65 171.5(6) . . . . ? Cl2 Rh2 N7 C65 179.0(5) . . . . ? C34 Rh2 N8 C66 40(5) . . . . ? N7 Rh2 N8 C66 15.4(5) . . . . ? Cl2 Rh2 N8 C66 -163.0(5) . . . . ? C3 N2 C1 N1 -2.0(6) . . . . ? C16 N2 C1 N1 167.2(5) . . . . ? C3 N2 C1 Rh1 172.4(4) . . . . ? C16 N2 C1 Rh1 -18.4(8) . . . . ? C2 N1 C1 N2 1.8(6) . . . . ? C4 N1 C1 N2 -168.0(5) . . . . ? C2 N1 C1 Rh1 -172.2(4) . . . . ? C4 N1 C1 Rh1 18.1(9) . . . . ? N3 Rh1 C1 N2 -76.8(5) . . . . ? N4 Rh1 C1 N2 -66(3) . . . . ? Cl1 Rh1 C1 N2 105.0(5) . . . . ? N3 Rh1 C1 N1 95.9(5) . . . . ? N4 Rh1 C1 N1 107(2) . . . . ? Cl1 Rh1 C1 N1 -82.3(5) . . . . ? C1 N1 C2 C3 -0.9(7) . . . . ? C4 N1 C2 C3 169.4(5) . . . . ? N1 C2 C3 N2 -0.3(7) . . . . ? C1 N2 C3 C2 1.5(7) . . . . ? C16 N2 C3 C2 -168.2(5) . . . . ? C1 N1 C4 C9 91.5(7) . . . . ? C2 N1 C4 C9 -77.2(7) . . . . ? C1 N1 C4 C5 -95.8(7) . . . . ? C2 N1 C4 C5 95.4(7) . . . . ? C9 C4 C5 C6 -3.5(9) . . . . ? N1 C4 C5 C6 -175.7(5) . . . . ? C9 C4 C5 C10 178.2(6) . . . . ? N1 C4 C5 C10 6.1(9) . . . . ? C4 C5 C6 C7 3.3(9) . . . . ? C10 C5 C6 C7 -178.4(6) . . . . ? C5 C6 C7 C8 -1.0(10) . . . . ? C6 C7 C8 C9 -1.2(10) . . . . ? C7 C8 C9 C4 1.0(9) . . . . ? C7 C8 C9 C13 179.2(6) . . . . ? C5 C4 C9 C8 1.5(9) . . . . ? N1 C4 C9 C8 173.9(5) . . . . ? C5 C4 C9 C13 -176.7(5) . . . . ? N1 C4 C9 C13 -4.3(8) . . . . ? C6 C5 C10 C11 -62.6(8) . . . . ? C4 C5 C10 C11 115.6(7) . . . . ? C6 C5 C10 C12 59.1(8) . . . . ? C4 C5 C10 C12 -122.7(7) . . . . ? C8 C9 C13 C14 46.6(8) . . . . ? C4 C9 C13 C14 -135.3(6) . . . . ? C8 C9 C13 C15 -77.1(7) . . . . ? C4 C9 C13 C15 101.1(7) . . . . ? C1 N2 C16 C21 111.8(7) . . . . ? C3 N2 C16 C21 -80.1(8) . . . . ? C1 N2 C16 C17 -73.7(7) . . . . ? C3 N2 C16 C17 94.4(7) . . . . ? C21 C16 C17 C18 -2.6(9) . . . . ? N2 C16 C17 C18 -177.0(5) . . . . ? C21 C16 C17 C22 175.2(6) . . . . ? N2 C16 C17 C22 0.8(8) . . . . ? C16 C17 C18 C19 1.8(9) . . . . ? C22 C17 C18 C19 -176.1(6) . . . . ? C17 C18 C19 C20 -0.9(11) . . . . ? C18 C19 C20 C21 0.7(11) . . . . ? C17 C16 C21 C20 2.5(10) . . . . ? N2 C16 C21 C20 176.7(5) . . . . ? C17 C16 C21 C25 179.7(6) . . . . ? N2 C16 C21 C25 -6.0(10) . . . . ? C19 C20 C21 C16 -1.5(10) . . . . ? C19 C20 C21 C25 -178.9(6) . . . . ? C18 C17 C22 C24 -28.1(8) . . . . ? C16 C17 C22 C24 154.1(5) . . . . ? C18 C17 C22 C23 94.7(7) . . . . ? C16 C17 C22 C23 -83.0(7) . . . . ? C16 C21 C25 C26 112.0(8) . . . . ? C20 C21 C25 C26 -70.7(8) . . . . ? C16 C21 C25 C27 -124.4(7) . . . . ? C20 C21 C25 C27 52.8(8) . . . . ? C32 N3 C28 C29 -1.9(9) . . . . ? Rh1 N3 C28 C29 171.8(5) . . . . ? C32 N3 C28 C33 177.4(5) . . . . ? Rh1 N3 C28 C33 -8.9(7) . . . . ? N3 C28 C29 C30 0.9(10) . . . . ? C33 C28 C29 C30 -178.4(6) . . . . ? C28 C29 C30 C31 -0.2(10) . . . . ? C29 C30 C31 C32 0.5(10) . . . . ? C28 N3 C32 C31 2.3(9) . . . . ? Rh1 N3 C32 C31 -170.6(4) . . . . ? C30 C31 C32 N3 -1.7(10) . . . . ? Rh1 N4 C33 C28 -29.0(6) . . . . ? N3 C28 C33 N4 25.8(7) . . . . ? C29 C28 C33 N4 -154.8(6) . . . . ? C36 N6 C34 N5 0.4(6) . . . . ? C49 N6 C34 N5 -168.9(5) . . . . ? C36 N6 C34 Rh2 -170.6(4) . . . . ? C49 N6 C34 Rh2 20.1(9) . . . . ? C35 N5 C34 N6 -0.2(6) . . . . ? C37 N5 C34 N6 164.8(5) . . . . ? C35 N5 C34 Rh2 170.7(4) . . . . ? C37 N5 C34 Rh2 -24.4(9) . . . . ? N7 Rh2 C34 N6 92.5(5) . . . . ? N8 Rh2 C34 N6 68(5) . . . . ? Cl2 Rh2 C34 N6 -88.8(5) . . . . ? N7 Rh2 C34 N5 -76.1(6) . . . . ? N8 Rh2 C34 N5 -101(4) . . . . ? Cl2 Rh2 C34 N5 102.5(5) . . . . ? C34 N5 C35 C36 -0.1(7) . . . . ? C37 N5 C35 C36 -165.7(6) . . . . ? N5 C35 C36 N6 0.3(7) . . . . ? C34 N6 C36 C35 -0.4(7) . . . . ? C49 N6 C36 C35 169.2(6) . . . . ? C35 N5 C37 C42 -88.9(7) . . . . ? C34 N5 C37 C42 107.6(7) . . . . ? C35 N5 C37 C38 84.9(7) . . . . ? C34 N5 C37 C38 -78.5(7) . . . . ? C42 C37 C38 C39 -0.4(9) . . . . ? N5 C37 C38 C39 -174.1(5) . . . . ? C42 C37 C38 C43 176.2(6) . . . . ? N5 C37 C38 C43 2.5(9) . . . . ? C37 C38 C39 C40 -1.7(9) . . . . ? C43 C38 C39 C40 -178.3(6) . . . . ? C38 C39 C40 C41 1.5(10) . . . . ? C39 C40 C41 C42 0.8(10) . . . . ? C38 C37 C42 C41 2.5(9) . . . . ? N5 C37 C42 C41 176.0(5) . . . . ? C38 C37 C42 C46 -174.4(6) . . . . ? N5 C37 C42 C46 -0.8(9) . . . . ? C40 C41 C42 C37 -2.7(9) . . . . ? C40 C41 C42 C46 174.3(6) . . . . ? C37 C38 C43 C45 -93.8(7) . . . . ? C39 C38 C43 C45 82.6(7) . . . . ? C37 C38 C43 C44 143.3(6) . . . . ? C39 C38 C43 C44 -40.3(8) . . . . ? C37 C42 C46 C47 -129.9(7) . . . . ? C41 C42 C46 C47 53.3(8) . . . . ? C37 C42 C46 C48 107.0(7) . . . . ? C41 C42 C46 C48 -69.8(7) . . . . ? C34 N6 C49 C54 91.8(7) . . . . ? C36 N6 C49 C54 -76.2(8) . . . . ? C34 N6 C49 C50 -92.1(7) . . . . ? C36 N6 C49 C50 99.9(7) . . . . ? C54 C49 C50 C51 -2.2(9) . . . . ? N6 C49 C50 C51 -178.2(5) . . . . ? C54 C49 C50 C55 175.0(6) . . . . ? N6 C49 C50 C55 -1.0(9) . . . . ? C49 C50 C51 C52 1.7(10) . . . . ? C55 C50 C51 C52 -175.5(7) . . . . ? C50 C51 C52 C53 0.3(11) . . . . ? C51 C52 C53 C54 -1.9(11) . . . . ? C50 C49 C54 C53 0.7(9) . . . . ? N6 C49 C54 C53 176.7(5) . . . . ? C50 C49 C54 C58 -175.9(6) . . . . ? N6 C49 C54 C58 0.1(9) . . . . ? C52 C53 C54 C49 1.4(10) . . . . ? C52 C53 C54 C58 178.2(6) . . . . ? C51 C50 C55 C56 -44.6(10) . . . . ? C49 C50 C55 C56 138.5(7) . . . . ? C51 C50 C55 C57 81.6(9) . . . . ? C49 C50 C55 C57 -95.4(8) . . . . ? C49 C54 C58 C60 -128.9(7) . . . . ? C53 C54 C58 C60 54.4(8) . . . . ? C49 C54 C58 C59 107.1(7) . . . . ? C53 C54 C58 C59 -69.6(8) . . . . ? C65 N7 C61 C62 -1.2(11) . . . . ? Rh2 N7 C61 C62 176.8(7) . . . . ? C65 N7 C61 C66 177.8(6) . . . . ? Rh2 N7 C61 C66 -4.2(9) . . . . ? N7 C61 C62 C63 -0.8(14) . . . . ? C66 C61 C62 C63 -179.7(8) . . . . ? C61 C62 C63 C64 2.5(15) . . . . ? C62 C63 C64 C65 -2.1(13) . . . . ? C61 N7 C65 C64 1.6(10) . . . . ? Rh2 N7 C65 C64 -176.1(5) . . . . ? C63 C64 C65 N7 0.0(12) . . . . ? Rh2 N8 C66 C61 -21.4(8) . . . . ? N7 C61 C66 N8 17.5(10) . . . . ? C62 C61 C66 N8 -163.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.789 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.017 0.000 0.000 447 135 ' ' 2 0.085 0.261 0.259 23 2 ' ' 3 0.031 0.512 0.458 8 2 ' ' 4 0.130 0.380 0.772 23 3 ' ' 5 0.171 0.574 0.463 7 1 ' ' 6 0.870 0.620 0.228 22 3 ' ' 7 0.833 0.429 0.537 7 1 ' ' 8 0.915 0.739 0.741 23 2 ' ' 9 0.968 0.488 0.550 7 2 ' ' _platon_squeeze_details ; Difference electron density maps revealed the presence of disordered lattice hexane molecules, which were ultimately modeled through the use of the SQUEEZE subroutine of the PLATON software suite. PLATON Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. One solvent accessible void per lattice were found, comprising a total volume of 447 A3 and contributing a total of 135 electrons. The void was thus assigned to 1.5 disordered hexane molecules, which contribute 1.5 x 86 = 129 electrons, and ocuppy about 180 A3 in space. The larger volume of the void may be a result of the disorder. The contributions have been included in all derived crystal quantities although the precise composition of the lattice solvate is somewhat speculative. ; data_cc110 _database_code_depnum_ccdc_archive 'CCDC 886734' #TrackingRef '- complex 4 (cc110z).cif' _audit_update_record ; 2012-06-15 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H49 Cl N3 Rh' _chemical_formula_weight 662.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.8292(4) _cell_length_b 10.36610(10) _cell_length_c 19.8406(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.6058(4) _cell_angle_gamma 90.00 _cell_volume 6772.56(12) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8380 _exptl_absorpt_correction_T_max 0.8623 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12449 _diffrn_reflns_av_R_equivalents 0.0115 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6613 _reflns_number_gt 6082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+6.9400P] 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 6613 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.088749(3) 0.790941(11) 0.052743(6) 0.02033(5) Uani 1 1 d . . . Cl1 Cl 0.112726(12) 0.58097(4) 0.09780(2) 0.03045(9) Uani 1 1 d . . . N1 N 0.17066(4) 0.92671(12) 0.13601(7) 0.0222(3) Uani 1 1 d . . . N2 N 0.14707(4) 0.86035(13) 0.21118(7) 0.0243(3) Uani 1 1 d . . . N3 N 0.03520(4) 0.69827(12) -0.02856(7) 0.0255(3) Uani 1 1 d . . . C1 C 0.13767(4) 0.86506(14) 0.13571(8) 0.0206(3) Uani 1 1 d . . . C2 C 0.19912(5) 0.95853(18) 0.20852(9) 0.0320(4) Uani 1 1 d . . . H2A H 0.2243 1.0013 0.2224 0.038 Uiso 1 1 calc R . . C3 C 0.18428(5) 0.91727(18) 0.25507(9) 0.0337(4) Uani 1 1 d . . . H3A H 0.1969 0.9255 0.3084 0.040 Uiso 1 1 calc R . . C4 C 0.17890(4) 0.95422(15) 0.07286(8) 0.0219(3) Uani 1 1 d . . . C5 C 0.17657(5) 1.08222(16) 0.04926(9) 0.0271(3) Uani 1 1 d . . . C6 C 0.18900(6) 1.10847(18) -0.00617(10) 0.0358(4) Uani 1 1 d . . . H6A H 0.1878 1.1944 -0.0237 0.043 Uiso 1 1 calc R . . C7 C 0.20299(6) 1.0117(2) -0.03590(10) 0.0407(4) Uani 1 1 d . . . H7A H 0.2123 1.0321 -0.0723 0.049 Uiso 1 1 calc R . . C8 C 0.20368(5) 0.88532(18) -0.01340(9) 0.0337(4) Uani 1 1 d . . . H8A H 0.2124 0.8193 -0.0360 0.040 Uiso 1 1 calc R . . C9 C 0.19181(4) 0.85308(16) 0.04178(8) 0.0245(3) Uani 1 1 d . . . C10 C 0.16144(6) 1.19194(17) 0.08075(11) 0.0363(4) Uani 1 1 d . . . H10A H 0.1500 1.1540 0.1136 0.044 Uiso 1 1 calc R . . C11 C 0.19634(7) 1.28293(19) 0.12925(13) 0.0496(5) Uani 1 1 d . . . H11A H 0.2167 1.2352 0.1722 0.074 Uiso 1 1 calc R . . H11B H 0.1857 1.3541 0.1477 0.074 Uiso 1 1 calc R . . H11C H 0.2089 1.3176 0.0988 0.074 Uiso 1 1 calc R . . C12 C 0.12761(6) 1.26870(19) 0.01760(14) 0.0500(5) Uani 1 1 d . . . H12A H 0.1051 1.2106 -0.0124 0.075 Uiso 1 1 calc R . . H12B H 0.1383 1.3078 -0.0149 0.075 Uiso 1 1 calc R . . H12C H 0.1178 1.3366 0.0398 0.075 Uiso 1 1 calc R . . C13 C 0.19392(5) 0.71465(16) 0.06804(10) 0.0311(4) Uani 1 1 d . . . H13A H 0.1716 0.7027 0.0832 0.037 Uiso 1 1 calc R . . C14 C 0.18726(6) 0.61591(19) 0.00648(12) 0.0433(4) Uani 1 1 d . . . H14A H 0.1632 0.6397 -0.0397 0.065 Uiso 1 1 calc R . . H14B H 0.1833 0.5303 0.0230 0.065 Uiso 1 1 calc R . . H14C H 0.2111 0.6143 -0.0034 0.065 Uiso 1 1 calc R . . C15 C 0.23406(7) 0.6881(2) 0.13754(12) 0.0503(5) Uani 1 1 d . . . H15A H 0.2368 0.7465 0.1784 0.075 Uiso 1 1 calc R . . H15B H 0.2567 0.7021 0.1251 0.075 Uiso 1 1 calc R . . H15C H 0.2345 0.5985 0.1537 0.075 Uiso 1 1 calc R . . C16 C 0.12251(5) 0.80463(16) 0.24408(8) 0.0263(3) Uani 1 1 d . . . C17 C 0.13302(5) 0.68256(17) 0.27811(9) 0.0301(3) Uani 1 1 d . . . C18 C 0.10898(6) 0.63350(19) 0.31013(11) 0.0404(4) Uani 1 1 d . . . H18A H 0.1150 0.5508 0.3331 0.049 Uiso 1 1 calc R . . C19 C 0.07677(7) 0.7022(2) 0.30915(12) 0.0475(5) Uani 1 1 d . . . H19A H 0.0603 0.6653 0.3298 0.057 Uiso 1 1 calc R . . C20 C 0.06828(6) 0.8242(2) 0.27833(11) 0.0417(4) Uani 1 1 d . . . H20A H 0.0465 0.8717 0.2795 0.050 Uiso 1 1 calc R . . C21 C 0.09113(5) 0.87919(17) 0.24550(9) 0.0312(4) Uani 1 1 d . . . C22 C 0.17014(5) 0.60731(18) 0.28625(10) 0.0338(4) Uani 1 1 d . . . H22A H 0.1781 0.6388 0.2471 0.041 Uiso 1 1 calc R . . C23 C 0.20578(6) 0.6321(2) 0.36425(11) 0.0468(5) Uani 1 1 d . . . H23A H 0.2126 0.7242 0.3696 0.070 Uiso 1 1 calc R . . H23B H 0.2294 0.5819 0.3693 0.070 Uiso 1 1 calc R . . H23C H 0.1981 0.6061 0.4035 0.070 Uiso 1 1 calc R . . C24 C 0.16307(7) 0.46128(19) 0.27611(12) 0.0458(5) Uani 1 1 d . . . H24A H 0.1869 0.4198 0.2758 0.069 Uiso 1 1 calc R . . H24B H 0.1392 0.4440 0.2283 0.069 Uiso 1 1 calc R . . H24C H 0.1586 0.4267 0.3178 0.069 Uiso 1 1 calc R . . C25 C 0.08368(6) 1.01788(18) 0.21836(11) 0.0389(4) Uani 1 1 d . . . H25A H 0.0935 1.0278 0.1791 0.047 Uiso 1 1 calc R . . C26 C 0.10863(8) 1.1096(2) 0.28343(15) 0.0689(7) Uani 1 1 d . . . H26A H 0.1376 1.0899 0.3025 0.103 Uiso 1 1 calc R . . H26B H 0.1007 1.0986 0.3241 0.103 Uiso 1 1 calc R . . H26C H 0.1036 1.1989 0.2653 0.103 Uiso 1 1 calc R . . C27 C 0.03911(7) 1.0569(2) 0.18277(13) 0.0536(5) Uani 1 1 d . . . H27A H 0.0230 0.9929 0.1448 0.080 Uiso 1 1 calc R . . H27B H 0.0359 1.1416 0.1588 0.080 Uiso 1 1 calc R . . H27C H 0.0298 1.0613 0.2218 0.080 Uiso 1 1 calc R . . C28 C 0.00252(5) 0.68716(16) -0.01459(10) 0.0299(4) Uani 1 1 d . . . C29 C -0.03260(5) 0.62558(18) -0.06483(11) 0.0405(4) Uani 1 1 d . . . H29A H -0.0553 0.6195 -0.0542 0.049 Uiso 1 1 calc R . . C30 C -0.03467(6) 0.57344(19) -0.12989(12) 0.0457(5) Uani 1 1 d . . . H30A H -0.0588 0.5323 -0.1651 0.055 Uiso 1 1 calc R . . C31 C -0.00133(6) 0.58164(18) -0.14330(10) 0.0409(4) Uani 1 1 d . . . H31A H -0.0021 0.5454 -0.1879 0.049 Uiso 1 1 calc R . . C32 C 0.03373(5) 0.64306(16) -0.09160(9) 0.0311(4) Uani 1 1 d . . . C33 C 0.00559(6) 0.73914(19) 0.05793(11) 0.0376(4) Uani 1 1 d . . . H33A H 0.0327 0.7212 0.0985 0.056 Uiso 1 1 calc R . . H33B H -0.0149 0.6978 0.0694 0.056 Uiso 1 1 calc R . . H33C H 0.0010 0.8325 0.0534 0.056 Uiso 1 1 calc R . . C34 C 0.07148(6) 0.6428(2) -0.10215(11) 0.0436(5) Uani 1 1 d . . . H34A H 0.0858 0.7250 -0.0846 0.065 Uiso 1 1 calc R . . H34B H 0.0642 0.6313 -0.1557 0.065 Uiso 1 1 calc R . . H34C H 0.0892 0.5719 -0.0731 0.065 Uiso 1 1 calc R . . C35 C 0.06132(6) 0.97435(18) 0.02250(10) 0.0333(4) Uani 1 1 d . . . H35A H 0.0719(6) 1.036(2) 0.0571(12) 0.040(6) Uiso 1 1 d . . . H35B H 0.0337(7) 0.968(2) 0.0069(12) 0.050(6) Uiso 1 1 d . . . C36 C 0.07737(5) 0.93968(17) -0.02593(9) 0.0307(4) Uani 1 1 d . . . H36A H 0.0595(6) 0.9096(19) -0.0760(11) 0.037(5) Uiso 1 1 d . . . H36B H 0.1032(7) 0.978(2) -0.0222(12) 0.046(6) Uiso 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 0.01841(7) 0.02033(7) 0.02172(7) -0.00082(4) 0.00853(5) -0.00067(4) Cl1 0.02870(19) 0.02167(19) 0.0370(2) 0.00108(15) 0.01117(16) -0.00097(15) N1 0.0224(6) 0.0256(7) 0.0187(6) -0.0021(5) 0.0094(5) -0.0043(5) N2 0.0271(6) 0.0262(7) 0.0210(6) -0.0005(5) 0.0119(5) -0.0029(5) N3 0.0217(6) 0.0243(7) 0.0281(7) 0.0014(5) 0.0090(5) -0.0005(5) C1 0.0235(7) 0.0181(7) 0.0219(7) -0.0001(6) 0.0116(6) 0.0017(6) C2 0.0287(8) 0.0422(10) 0.0220(7) -0.0060(7) 0.0086(7) -0.0133(7) C3 0.0349(9) 0.0431(10) 0.0201(7) -0.0054(7) 0.0097(7) -0.0109(8) C4 0.0194(7) 0.0268(8) 0.0190(7) 0.0000(6) 0.0079(6) -0.0025(6) C5 0.0268(8) 0.0271(8) 0.0262(7) 0.0006(6) 0.0108(6) -0.0014(6) C6 0.0443(10) 0.0327(9) 0.0326(9) 0.0091(7) 0.0193(8) -0.0008(8) C7 0.0537(11) 0.0487(11) 0.0290(9) 0.0056(8) 0.0267(9) -0.0002(9) C8 0.0393(9) 0.0387(10) 0.0295(8) -0.0022(7) 0.0211(7) 0.0022(8) C9 0.0200(7) 0.0281(8) 0.0240(7) -0.0003(6) 0.0086(6) -0.0004(6) C10 0.0435(10) 0.0261(9) 0.0464(10) -0.0015(8) 0.0265(9) -0.0004(8) C11 0.0602(13) 0.0358(11) 0.0511(12) -0.0116(9) 0.0234(11) -0.0055(9) C12 0.0441(11) 0.0290(10) 0.0729(15) 0.0010(10) 0.0226(11) 0.0060(9) C13 0.0320(9) 0.0264(9) 0.0408(9) 0.0013(7) 0.0216(8) 0.0032(7) C14 0.0406(10) 0.0316(10) 0.0602(12) -0.0094(9) 0.0249(9) -0.0005(8) C15 0.0594(13) 0.0444(12) 0.0406(11) 0.0103(9) 0.0165(10) 0.0184(10) C16 0.0296(8) 0.0311(8) 0.0216(7) 0.0004(6) 0.0147(6) -0.0023(7) C17 0.0338(9) 0.0320(9) 0.0269(8) 0.0022(7) 0.0158(7) 0.0009(7) C18 0.0472(11) 0.0388(10) 0.0436(10) 0.0131(8) 0.0278(9) 0.0029(9) C19 0.0497(12) 0.0572(13) 0.0520(12) 0.0141(10) 0.0373(10) 0.0014(10) C20 0.0407(10) 0.0521(12) 0.0439(10) 0.0074(9) 0.0293(9) 0.0094(9) C21 0.0352(9) 0.0356(9) 0.0258(8) 0.0012(7) 0.0165(7) 0.0027(7) C22 0.0360(9) 0.0355(9) 0.0321(8) 0.0053(7) 0.0171(7) 0.0061(8) C23 0.0400(10) 0.0528(12) 0.0414(10) 0.0019(9) 0.0128(9) 0.0086(9) C24 0.0562(12) 0.0362(10) 0.0426(10) 0.0067(8) 0.0200(9) 0.0101(9) C25 0.0475(11) 0.0354(10) 0.0400(10) 0.0054(8) 0.0251(9) 0.0104(8) C26 0.0745(17) 0.0417(13) 0.0758(17) -0.0084(12) 0.0204(14) 0.0026(12) C27 0.0543(13) 0.0486(12) 0.0568(13) 0.0055(10) 0.0239(11) 0.0200(10) C28 0.0242(8) 0.0249(8) 0.0394(9) 0.0068(7) 0.0131(7) 0.0022(6) C29 0.0243(8) 0.0369(10) 0.0545(11) 0.0052(9) 0.0125(8) -0.0039(7) C30 0.0295(9) 0.0387(11) 0.0509(11) -0.0027(9) 0.0020(8) -0.0089(8) C31 0.0422(10) 0.0352(10) 0.0339(9) -0.0063(8) 0.0069(8) -0.0048(8) C32 0.0319(8) 0.0278(9) 0.0295(8) -0.0016(7) 0.0102(7) -0.0016(7) C33 0.0357(9) 0.0374(10) 0.0479(11) 0.0035(8) 0.0261(8) 0.0019(8) C34 0.0447(11) 0.0505(12) 0.0417(10) -0.0148(9) 0.0247(9) -0.0070(9) C35 0.0319(9) 0.0280(9) 0.0351(9) 0.0023(7) 0.0105(8) 0.0062(7) C36 0.0297(8) 0.0283(9) 0.0280(8) 0.0047(7) 0.0074(7) -0.0012(7) _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 C1 1.9722(15) . ? Rh1 C36 2.0984(16) . ? Rh1 C35 2.1101(17) . ? Rh1 N3 2.1365(13) . ? Rh1 Cl1 2.3685(4) . ? N1 C1 1.3705(19) . ? N1 C2 1.3879(19) . ? N1 C4 1.4437(18) . ? N2 C1 1.3783(18) . ? N2 C3 1.384(2) . ? N2 C16 1.4514(19) . ? N3 C32 1.354(2) . ? N3 C28 1.356(2) . ? C2 C3 1.337(2) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C5 1.397(2) . ? C4 C9 1.403(2) . ? C5 C6 1.394(2) . ? C5 C10 1.519(2) . ? C6 C7 1.375(3) . ? C6 H6A 0.9500 . ? C7 C8 1.381(3) . ? C7 H7A 0.9500 . ? C8 C9 1.389(2) . ? C8 H8A 0.9500 . ? C9 C13 1.517(2) . ? C10 C12 1.535(3) . ? C10 C11 1.536(3) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.527(2) . ? C13 C15 1.529(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.401(2) . ? C16 C17 1.405(2) . ? C17 C18 1.396(2) . ? C17 C22 1.519(2) . ? C18 C19 1.376(3) . ? C18 H18A 0.9500 . ? C19 C20 1.379(3) . ? C19 H19A 0.9500 . ? C20 C21 1.396(2) . ? C20 H20A 0.9500 . ? C21 C25 1.517(3) . ? C22 C24 1.534(3) . ? C22 C23 1.538(3) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.523(3) . ? C25 C26 1.534(3) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.385(2) . ? C28 C33 1.493(3) . ? C29 C30 1.370(3) . ? C29 H29A 0.9500 . ? C30 C31 1.370(3) . ? C30 H30A 0.9500 . ? C31 C32 1.392(2) . ? C31 H31A 0.9500 . ? C32 C34 1.496(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.382(3) . ? C35 H35A 0.89(2) . ? C35 H35B 0.92(2) . ? C36 H36A 0.96(2) . ? C36 H36B 1.00(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 C1 Rh1 C36 97.94(6) . . ? C1 Rh1 C35 91.63(7) . . ? C36 Rh1 C35 38.35(7) . . ? C1 Rh1 N3 174.06(5) . . ? C36 Rh1 N3 87.67(6) . . ? C35 Rh1 N3 91.60(6) . . ? C1 Rh1 Cl1 89.78(4) . . ? C36 Rh1 Cl1 150.75(5) . . ? C35 Rh1 Cl1 170.22(5) . . ? N3 Rh1 Cl1 86.21(4) . . ? C1 N1 C2 111.83(12) . . ? C1 N1 C4 128.24(12) . . ? C2 N1 C4 119.86(12) . . ? C1 N2 C3 111.38(12) . . ? C1 N2 C16 126.77(13) . . ? C3 N2 C16 121.84(13) . . ? C32 N3 C28 118.74(14) . . ? C32 N3 Rh1 121.93(11) . . ? C28 N3 Rh1 119.19(11) . . ? N1 C1 N2 102.76(12) . . ? N1 C1 Rh1 131.45(10) . . ? N2 C1 Rh1 125.74(11) . . ? C3 C2 N1 106.71(14) . . ? C3 C2 H2A 126.6 . . ? N1 C2 H2A 126.6 . . ? C2 C3 N2 107.32(14) . . ? C2 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? C5 C4 C9 123.01(14) . . ? C5 C4 N1 118.24(13) . . ? C9 C4 N1 118.57(13) . . ? C6 C5 C4 117.19(15) . . ? C6 C5 C10 119.27(15) . . ? C4 C5 C10 123.53(14) . . ? C7 C6 C5 120.96(16) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 120.64(16) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C7 C8 C9 121.08(16) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C8 C9 C4 117.05(15) . . ? C8 C9 C13 120.84(15) . . ? C4 C9 C13 122.09(14) . . ? C5 C10 C12 111.44(16) . . ? C5 C10 C11 111.06(16) . . ? C12 C10 C11 109.78(16) . . ? C5 C10 H10A 108.1 . . ? C12 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.22(15) . . ? C9 C13 C15 111.13(15) . . ? C14 C13 C15 110.16(15) . . ? C9 C13 H13A 107.3 . . ? C14 C13 H13A 107.3 . . ? C15 C13 H13A 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.63(15) . . ? C21 C16 N2 118.38(14) . . ? C17 C16 N2 118.81(14) . . ? C18 C17 C16 116.92(16) . . ? C18 C17 C22 119.25(16) . . ? C16 C17 C22 123.70(15) . . ? C19 C18 C17 121.56(17) . . ? C19 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? C18 C19 C20 120.24(17) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 121.15(18) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C20 C21 C16 117.34(16) . . ? C20 C21 C25 120.13(16) . . ? C16 C21 C25 122.37(15) . . ? C17 C22 C24 113.65(16) . . ? C17 C22 C23 110.07(15) . . ? C24 C22 C23 108.38(16) . . ? C17 C22 H22A 108.2 . . ? C24 C22 H22A 108.2 . . ? C23 C22 H22A 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 113.72(17) . . ? C21 C25 C26 110.11(17) . . ? C27 C25 C26 109.93(18) . . ? C21 C25 H25A 107.6 . . ? C27 C25 H25A 107.6 . . ? C26 C25 H25A 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 121.36(17) . . ? N3 C28 C33 118.39(15) . . ? C29 C28 C33 120.21(16) . . ? C30 C29 C28 119.98(17) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 118.82(17) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? C30 C31 C32 120.08(18) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? N3 C32 C31 120.94(16) . . ? N3 C32 C34 118.34(15) . . ? C31 C32 C34 120.63(16) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 Rh1 70.37(10) . . ? C36 C35 H35A 123.1(14) . . ? Rh1 C35 H35A 115.9(13) . . ? C36 C35 H35B 119.9(14) . . ? Rh1 C35 H35B 110.2(14) . . ? H35A C35 H35B 110.3(19) . . ? C35 C36 Rh1 71.28(10) . . ? C35 C36 H36A 119.5(11) . . ? Rh1 C36 H36A 110.2(12) . . ? C35 C36 H36B 122.2(12) . . ? Rh1 C36 H36B 111.6(12) . . ? H36A C36 H36B 113.1(16) . . ? 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 C1 Rh1 N3 C32 -127.3(5) . . . . ? C36 Rh1 N3 C32 71.64(13) . . . . ? C35 Rh1 N3 C32 109.79(13) . . . . ? Cl1 Rh1 N3 C32 -79.75(12) . . . . ? C1 Rh1 N3 C28 48.5(6) . . . . ? C36 Rh1 N3 C28 -112.54(12) . . . . ? C35 Rh1 N3 C28 -74.39(12) . . . . ? Cl1 Rh1 N3 C28 96.07(11) . . . . ? C2 N1 C1 N2 0.00(17) . . . . ? C4 N1 C1 N2 176.96(14) . . . . ? C2 N1 C1 Rh1 -177.48(12) . . . . ? C4 N1 C1 Rh1 -0.5(2) . . . . ? C3 N2 C1 N1 0.10(17) . . . . ? C16 N2 C1 N1 -179.98(14) . . . . ? C3 N2 C1 Rh1 177.78(12) . . . . ? C16 N2 C1 Rh1 -2.3(2) . . . . ? C36 Rh1 C1 N1 -42.25(15) . . . . ? C35 Rh1 C1 N1 -80.23(15) . . . . ? N3 Rh1 C1 N1 156.9(5) . . . . ? Cl1 Rh1 C1 N1 109.45(14) . . . . ? C36 Rh1 C1 N2 140.77(13) . . . . ? C35 Rh1 C1 N2 102.79(14) . . . . ? N3 Rh1 C1 N2 -20.1(6) . . . . ? Cl1 Rh1 C1 N2 -67.54(13) . . . . ? C1 N1 C2 C3 -0.1(2) . . . . ? C4 N1 C2 C3 -177.35(15) . . . . ? N1 C2 C3 N2 0.2(2) . . . . ? C1 N2 C3 C2 -0.2(2) . . . . ? C16 N2 C3 C2 179.91(15) . . . . ? C1 N1 C4 C5 109.17(18) . . . . ? C2 N1 C4 C5 -74.09(19) . . . . ? C1 N1 C4 C9 -75.5(2) . . . . ? C2 N1 C4 C9 101.20(17) . . . . ? C9 C4 C5 C6 -2.0(2) . . . . ? N1 C4 C5 C6 173.05(14) . . . . ? C9 C4 C5 C10 178.07(15) . . . . ? N1 C4 C5 C10 -6.9(2) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C10 C5 C6 C7 179.82(17) . . . . ? C5 C6 C7 C8 2.3(3) . . . . ? C6 C7 C8 C9 -2.5(3) . . . . ? C7 C8 C9 C4 0.5(2) . . . . ? C7 C8 C9 C13 -178.02(16) . . . . ? C5 C4 C9 C8 1.8(2) . . . . ? N1 C4 C9 C8 -173.21(14) . . . . ? C5 C4 C9 C13 -179.70(15) . . . . ? N1 C4 C9 C13 5.2(2) . . . . ? C6 C5 C10 C12 52.8(2) . . . . ? C4 C5 C10 C12 -127.25(18) . . . . ? C6 C5 C10 C11 -69.9(2) . . . . ? C4 C5 C10 C11 110.01(19) . . . . ? C8 C9 C13 C14 -31.0(2) . . . . ? C4 C9 C13 C14 150.64(15) . . . . ? C8 C9 C13 C15 93.64(19) . . . . ? C4 C9 C13 C15 -84.76(19) . . . . ? C1 N2 C16 C21 -82.6(2) . . . . ? C3 N2 C16 C21 97.28(19) . . . . ? C1 N2 C16 C17 102.07(19) . . . . ? C3 N2 C16 C17 -78.0(2) . . . . ? C21 C16 C17 C18 3.9(3) . . . . ? N2 C16 C17 C18 178.99(15) . . . . ? C21 C16 C17 C22 -171.84(16) . . . . ? N2 C16 C17 C22 3.3(2) . . . . ? C16 C17 C18 C19 -0.7(3) . . . . ? C22 C17 C18 C19 175.21(19) . . . . ? C17 C18 C19 C20 -2.2(3) . . . . ? C18 C19 C20 C21 2.0(3) . . . . ? C19 C20 C21 C16 1.0(3) . . . . ? C19 C20 C21 C25 -174.46(19) . . . . ? C17 C16 C21 C20 -4.0(3) . . . . ? N2 C16 C21 C20 -179.16(15) . . . . ? C17 C16 C21 C25 171.32(16) . . . . ? N2 C16 C21 C25 -3.8(2) . . . . ? C18 C17 C22 C24 41.3(2) . . . . ? C16 C17 C22 C24 -143.11(17) . . . . ? C18 C17 C22 C23 -80.5(2) . . . . ? C16 C17 C22 C23 95.1(2) . . . . ? C20 C21 C25 C27 -37.6(2) . . . . ? C16 C21 C25 C27 147.13(17) . . . . ? C20 C21 C25 C26 86.2(2) . . . . ? C16 C21 C25 C26 -89.0(2) . . . . ? C32 N3 C28 C29 -2.7(2) . . . . ? Rh1 N3 C28 C29 -178.67(13) . . . . ? C32 N3 C28 C33 175.22(15) . . . . ? Rh1 N3 C28 C33 -0.7(2) . . . . ? N3 C28 C29 C30 0.5(3) . . . . ? C33 C28 C29 C30 -177.35(18) . . . . ? C28 C29 C30 C31 1.1(3) . . . . ? C29 C30 C31 C32 -0.5(3) . . . . ? C28 N3 C32 C31 3.3(2) . . . . ? Rh1 N3 C32 C31 179.11(13) . . . . ? C28 N3 C32 C34 -173.17(16) . . . . ? Rh1 N3 C32 C34 2.7(2) . . . . ? C30 C31 C32 N3 -1.7(3) . . . . ? C30 C31 C32 C34 174.68(19) . . . . ? C1 Rh1 C35 C36 100.77(11) . . . . ? N3 Rh1 C35 C36 -84.22(11) . . . . ? Cl1 Rh1 C35 C36 -161.1(3) . . . . ? C1 Rh1 C36 C35 -82.53(12) . . . . ? N3 Rh1 C36 C35 95.53(11) . . . . ? Cl1 Rh1 C36 C35 173.52(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.305 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.044