# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name A.L.Balch 'James C. Fettinger' 'Marilyn M. Olmstead' 'David Pham' 'Jay Stork' 'Ngon Tran' _publ_contact_author_name 'A. L. Balch' _publ_contact_author_address ; Department of Chemistry University of California One Shields Avenue Davis California CA 95616 UNITED STATES OF AMERICA ; _publ_contact_author_email ALBALCH@UCDAVIS.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Variation in Crystallization Conditions Allows the Isolation of Trimeric as Well as Dimeric and Monomeric Forms of [(Alkyl Isocyanide)4RhI]+. ; data_jrs102-3 _database_code_depnum_ccdc_archive 'CCDC 285148' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Rh(CNC~6~H~11~)~4~]B(C~6~H~5~)~4~' _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 N4 Rh, C24 H20 B' _chemical_formula_sum 'C52 H64 B N4 Rh' _chemical_formula_weight 858.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9948(7) _cell_length_b 13.9469(8) _cell_length_c 15.4951(9) _cell_angle_alpha 72.1180(10) _cell_angle_beta 86.7140(10) _cell_angle_gamma 66.9070(10) _cell_volume 2263.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6446 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 29.6 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92282 _exptl_absorpt_correction_T_max 0.96544 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30219 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9217 _reflns_number_gt 6911 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All H atoms were located in a difference map, placed in idealized positions, and treated with a riding model. One coordinated cyclohexyl isocyanide group is disordered over two positions. The occupancies of the two orientations refined to 82.4(6) % and 17.6(6) %, based on an assumed occupancy of 100 %. The geometry of the minor orientation was restrained to be similar to the trans cyclohexyl isocyanide, because both involve an equatorial cyclohexyl group. ; _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^)+(0.0182P)^2^+5.4896P] 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 9217 _refine_ls_number_parameters 571 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.140 _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 0.40450(3) 0.67063(3) 0.20082(2) 0.02197(9) Uani 1 1 d D . . C1 C 0.4531(4) 0.5284(4) 0.2967(3) 0.0286(11) Uani 0.825(6) 1 d P A 1 C2 C 0.5223(5) 0.3289(4) 0.4126(3) 0.0258(12) Uani 0.825(6) 1 d P A 1 H2 H 0.6014 0.2827 0.3942 0.031 Uiso 0.825(6) 1 calc PR A 1 C3 C 0.5393(5) 0.3243(4) 0.5110(3) 0.0295(12) Uani 0.825(6) 1 d P A 1 H3A H 0.5790 0.2468 0.5489 0.035 Uiso 0.825(6) 1 calc PR A 1 H3B H 0.5938 0.3614 0.5140 0.035 Uiso 0.825(6) 1 calc PR A 1 C4 C 0.4200(5) 0.3783(5) 0.5495(4) 0.0340(14) Uani 0.825(6) 1 d P A 1 H4A H 0.3872 0.4583 0.5184 0.041 Uiso 0.825(6) 1 calc PR A 1 H4B H 0.4351 0.3659 0.6149 0.041 Uiso 0.825(6) 1 calc PR A 1 C5 C 0.3259(5) 0.3340(5) 0.5381(4) 0.0368(15) Uani 0.825(6) 1 d P A 1 H5A H 0.2479 0.3755 0.5597 0.044 Uiso 0.825(6) 1 calc PR A 1 H5B H 0.3535 0.2561 0.5756 0.044 Uiso 0.825(6) 1 calc PR A 1 C6 C 0.3065(5) 0.3440(5) 0.4382(4) 0.0310(14) Uani 0.825(6) 1 d P A 1 H6A H 0.2484 0.3114 0.4327 0.037 Uiso 0.825(6) 1 calc PR A 1 H6B H 0.2715 0.4224 0.4015 0.037 Uiso 0.825(6) 1 calc PR A 1 C7 C 0.4264(6) 0.2857(5) 0.4021(4) 0.0289(13) Uani 0.825(6) 1 d P A 1 H7A H 0.4126 0.2955 0.3370 0.035 Uiso 0.825(6) 1 calc PR A 1 H7B H 0.4571 0.2062 0.4353 0.035 Uiso 0.825(6) 1 calc PR A 1 N1 N 0.4843(7) 0.4418(5) 0.3520(4) 0.0307(10) Uani 0.825(6) 1 d P A 1 C1A C 0.4531(4) 0.5284(4) 0.2967(3) 0.0286(11) Uani 0.18 1 d PD A 2 C2A C 0.4730(17) 0.3558(12) 0.4256(8) 0.024(6) Uiso 0.175(6) 1 d PD A 2 H2A H 0.5474 0.2889 0.4276 0.028 Uiso 0.175(6) 1 calc PR A 2 C3A C 0.472(2) 0.3789(15) 0.5156(10) 0.021(5) Uiso 0.175(6) 1 d PD A 2 H3A1 H 0.3999 0.4451 0.5155 0.025 Uiso 0.175(6) 1 calc PR A 2 H3A2 H 0.5458 0.3921 0.5243 0.025 Uiso 0.175(6) 1 calc PR A 2 C4A C 0.4710(17) 0.2793(16) 0.5931(8) 0.031(6) Uani 0.175(6) 1 d PD A 2 H4A1 H 0.5474 0.2150 0.5963 0.037 Uiso 0.175(6) 1 calc PR A 2 H4A2 H 0.4661 0.2949 0.6517 0.037 Uiso 0.175(6) 1 calc PR A 2 C5A C 0.3639(17) 0.2530(17) 0.5782(10) 0.032(6) Uani 0.175(6) 1 d PD A 2 H5A1 H 0.3687 0.1855 0.6265 0.039 Uiso 0.175(6) 1 calc PR A 2 H5A2 H 0.2877 0.3135 0.5832 0.039 Uiso 0.175(6) 1 calc PR A 2 C6A C 0.3596(17) 0.2369(15) 0.4867(10) 0.028(6) Uani 0.175(6) 1 d PD A 2 H6A1 H 0.2844 0.2263 0.4784 0.033 Uiso 0.175(6) 1 calc PR A 2 H6A2 H 0.4297 0.1698 0.4850 0.033 Uiso 0.175(6) 1 calc PR A 2 C7A C 0.3625(19) 0.3339(16) 0.4092(9) 0.020(5) Uani 0.175(6) 1 d PD A 2 H7A1 H 0.2874 0.3996 0.4057 0.024 Uiso 0.175(6) 1 calc PR A 2 H7A2 H 0.3667 0.3179 0.3509 0.024 Uiso 0.175(6) 1 calc PR A 2 N1A N 0.478(3) 0.4448(16) 0.3508(13) 0.030 Uiso 0.175(6) 1 d PD A 2 C8 C 0.2729(4) 0.7381(3) 0.2718(3) 0.0286(9) Uani 1 1 d . A . C9 C 0.0911(4) 0.8346(4) 0.3576(3) 0.0354(11) Uani 1 1 d . A . H9 H 0.0874 0.9095 0.3506 0.043 Uiso 1 1 calc R . . C10 C -0.0238(4) 0.8456(3) 0.3125(3) 0.0328(10) Uani 1 1 d . . . H10A H -0.0952 0.8949 0.3350 0.039 Uiso 1 1 calc R . . H10B H -0.0253 0.8791 0.2460 0.039 Uiso 1 1 calc R . . C11 C -0.0322(4) 0.7361(4) 0.3315(3) 0.0346(10) Uani 1 1 d . . . H11A H -0.1120 0.7477 0.3062 0.042 Uiso 1 1 calc R . . H11B H 0.0316 0.6914 0.3001 0.042 Uiso 1 1 calc R . . C12 C -0.0176(5) 0.6741(4) 0.4315(3) 0.0459(12) Uani 1 1 d . . . H12A H -0.0180 0.6010 0.4397 0.055 Uiso 1 1 calc R . . H12B H -0.0873 0.7140 0.4618 0.055 Uiso 1 1 calc R . . C13 C 0.0994(5) 0.6601(4) 0.4758(3) 0.0504(14) Uani 1 1 d . . . H13A H 0.1696 0.6118 0.4513 0.060 Uiso 1 1 calc R . . H13B H 0.1027 0.6246 0.5421 0.060 Uiso 1 1 calc R . . C14 C 0.1080(4) 0.7704(5) 0.4581(3) 0.0480(14) Uani 1 1 d . . . H14A H 0.0451 0.8141 0.4907 0.058 Uiso 1 1 calc R . . H14B H 0.1884 0.7584 0.4827 0.058 Uiso 1 1 calc R . . N2 N 0.1947(3) 0.7793(3) 0.3119(3) 0.0334(9) Uani 1 1 d . . . C15 C 0.3501(4) 0.8114(4) 0.1003(3) 0.0285(10) Uani 1 1 d D A . C16 C 0.2913(4) 0.9829(3) -0.0412(3) 0.0261(9) Uani 1 1 d D A . H16 H 0.2076 1.0024 -0.0665 0.031 Uiso 1 1 calc R . . C17 C 0.2941(4) 1.0821(3) -0.0208(3) 0.0342(10) Uani 1 1 d D . . H17A H 0.3734 1.0619 0.0106 0.041 Uiso 1 1 calc R . . H17B H 0.2295 1.1060 0.0200 0.041 Uiso 1 1 calc R . . C18 C 0.2746(4) 1.1763(3) -0.1092(3) 0.0348(10) Uani 1 1 d D . . H18A H 0.1915 1.2018 -0.1368 0.042 Uiso 1 1 calc R . . H18B H 0.2820 1.2384 -0.0954 0.042 Uiso 1 1 calc R . . C19 C 0.3667(4) 1.1405(4) -0.1764(3) 0.0353(10) Uani 1 1 d D . . H19A H 0.3500 1.2020 -0.2336 0.042 Uiso 1 1 calc R . . H19B H 0.4494 1.1209 -0.1509 0.042 Uiso 1 1 calc R . . C20 C 0.3608(4) 1.0428(3) -0.1964(3) 0.0334(10) Uani 1 1 d D . . H20A H 0.4236 1.0191 -0.2384 0.040 Uiso 1 1 calc R . . H20B H 0.2804 1.0645 -0.2269 0.040 Uiso 1 1 calc R . . C21 C 0.3807(4) 0.9478(3) -0.1100(3) 0.0317(10) Uani 1 1 d D . . H21A H 0.3707 0.8873 -0.1247 0.038 Uiso 1 1 calc R . . H21B H 0.4647 0.9203 -0.0833 0.038 Uiso 1 1 calc R . . N3 N 0.3185(3) 0.8912(3) 0.0409(2) 0.0291(8) Uani 1 1 d D . . C22 C 0.5358(4) 0.6050(3) 0.1274(3) 0.0227(8) Uani 1 1 d . A . C23 C 0.7067(3) 0.5172(3) 0.0293(3) 0.0224(8) Uani 1 1 d . A . H23 H 0.7624 0.4427 0.0677 0.027 Uiso 1 1 calc R . . C24 C 0.6487(3) 0.5059(3) -0.0497(3) 0.0258(9) Uani 1 1 d . . . H24A H 0.5963 0.4650 -0.0258 0.031 Uiso 1 1 calc R . . H24B H 0.7133 0.4628 -0.0817 0.031 Uiso 1 1 calc R . . C25 C 0.5727(4) 0.6165(3) -0.1173(3) 0.0283(9) Uani 1 1 d . . . H25A H 0.5015 0.6560 -0.0879 0.034 Uiso 1 1 calc R . . H25B H 0.5426 0.6051 -0.1699 0.034 Uiso 1 1 calc R . . C26 C 0.6484(4) 0.6859(4) -0.1503(3) 0.0290(9) Uani 1 1 d . . . H26A H 0.7139 0.6505 -0.1859 0.035 Uiso 1 1 calc R . . H26B H 0.5959 0.7592 -0.1907 0.035 Uiso 1 1 calc R . . C27 C 0.7040(4) 0.6990(3) -0.0711(3) 0.0256(9) Uani 1 1 d . . . H27A H 0.7566 0.7398 -0.0945 0.031 Uiso 1 1 calc R . . H27B H 0.6385 0.7424 -0.0400 0.031 Uiso 1 1 calc R . . C28 C 0.7788(3) 0.5887(3) -0.0033(3) 0.0247(9) Uani 1 1 d . . . H28A H 0.8073 0.6007 0.0497 0.030 Uiso 1 1 calc R . . H28B H 0.8512 0.5500 -0.0320 0.030 Uiso 1 1 calc R . . N4 N 0.6108(3) 0.5665(3) 0.0845(2) 0.0232(7) Uani 1 1 d . . . B1 B 0.9739(4) 0.2089(4) 0.2302(3) 0.0225(9) Uani 1 1 d . . . C29 C 1.1159(3) 0.1320(3) 0.2722(3) 0.0241(9) Uani 1 1 d . . . C30 C 1.1678(4) 0.1435(3) 0.3453(3) 0.0276(9) Uani 1 1 d . . . H30 H 1.1181 0.1963 0.3730 0.033 Uiso 1 1 calc R . . C31 C 1.2880(4) 0.0819(4) 0.3793(3) 0.0354(11) Uani 1 1 d . . . H31 H 1.3191 0.0949 0.4277 0.042 Uiso 1 1 calc R . . C32 C 1.3616(4) 0.0025(4) 0.3432(3) 0.0409(12) Uani 1 1 d . . . H32 H 1.4436 -0.0403 0.3666 0.049 Uiso 1 1 calc R . . C33 C 1.3146(4) -0.0144(4) 0.2721(3) 0.0410(12) Uani 1 1 d . . . H33 H 1.3646 -0.0699 0.2471 0.049 Uiso 1 1 calc R . . C34 C 1.1949(4) 0.0491(4) 0.2372(3) 0.0322(10) Uani 1 1 d . . . H34 H 1.1652 0.0363 0.1881 0.039 Uiso 1 1 calc R . . C35 C 0.9662(3) 0.2194(3) 0.1221(2) 0.0200(8) Uani 1 1 d . . . C36 C 0.9464(4) 0.1430(3) 0.0903(3) 0.0272(9) Uani 1 1 d . . . H36 H 0.9360 0.0825 0.1336 0.033 Uiso 1 1 calc R . . C37 C 0.9413(4) 0.1514(4) -0.0009(3) 0.0301(10) Uani 1 1 d . . . H37 H 0.9270 0.0976 -0.0187 0.036 Uiso 1 1 calc R . . C38 C 0.9569(4) 0.2376(4) -0.0661(3) 0.0290(9) Uani 1 1 d . . . H38 H 0.9526 0.2441 -0.1288 0.035 Uiso 1 1 calc R . . C39 C 0.9790(3) 0.3141(3) -0.0382(3) 0.0261(9) Uani 1 1 d . . . H39 H 0.9911 0.3734 -0.0819 0.031 Uiso 1 1 calc R . . C40 C 0.9834(3) 0.3044(3) 0.0531(3) 0.0216(8) Uani 1 1 d . . . H40 H 0.9989 0.3580 0.0702 0.026 Uiso 1 1 calc R . . C41 C 0.9340(3) 0.3310(3) 0.2436(2) 0.0208(8) Uani 1 1 d . . . C42 C 1.0160(4) 0.3822(3) 0.2341(2) 0.0249(9) Uani 1 1 d . . . H42 H 1.0955 0.3464 0.2177 0.030 Uiso 1 1 calc R . . C43 C 0.9857(4) 0.4831(3) 0.2479(3) 0.0301(10) Uani 1 1 d . . . H43 H 1.0447 0.5139 0.2427 0.036 Uiso 1 1 calc R . . C44 C 0.8698(4) 0.5383(3) 0.2692(3) 0.0310(10) Uani 1 1 d . . . H44 H 0.8486 0.6075 0.2784 0.037 Uiso 1 1 calc R . . C45 C 0.7853(4) 0.4933(3) 0.2771(3) 0.0292(9) Uani 1 1 d . . . H45 H 0.7049 0.5316 0.2908 0.035 Uiso 1 1 calc R . . C46 C 0.8174(4) 0.3912(3) 0.2649(3) 0.0262(9) Uani 1 1 d . . . H46 H 0.7578 0.3609 0.2714 0.031 Uiso 1 1 calc R . . C47 C 0.8807(3) 0.1547(3) 0.2852(2) 0.0188(8) Uani 1 1 d . . . C48 C 0.7674(3) 0.1762(3) 0.2465(3) 0.0254(9) Uani 1 1 d . . . H48 H 0.7468 0.2189 0.1844 0.030 Uiso 1 1 calc R . . C49 C 0.6839(4) 0.1385(3) 0.2944(3) 0.0275(9) Uani 1 1 d . . . H49 H 0.6083 0.1550 0.2649 0.033 Uiso 1 1 calc R . . C50 C 0.7104(4) 0.0766(3) 0.3853(3) 0.0261(9) Uani 1 1 d . . . H50 H 0.6538 0.0500 0.4184 0.031 Uiso 1 1 calc R . . C51 C 0.8201(4) 0.0544(3) 0.4270(3) 0.0247(9) Uani 1 1 d . . . H51 H 0.8389 0.0133 0.4896 0.030 Uiso 1 1 calc R . . C52 C 0.9035(3) 0.0922(3) 0.3774(3) 0.0209(8) Uani 1 1 d . . . H52 H 0.9791 0.0748 0.4074 0.025 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 0.01967(15) 0.02369(17) 0.02325(16) -0.01113(13) 0.00578(12) -0.00691(13) C1 0.025(2) 0.050(3) 0.026(2) -0.025(2) 0.0144(18) -0.021(2) C2 0.025(3) 0.019(3) 0.029(3) -0.007(2) 0.006(2) -0.005(2) C3 0.031(3) 0.026(3) 0.031(3) -0.007(2) -0.002(2) -0.012(3) C4 0.036(3) 0.039(4) 0.029(3) -0.017(3) 0.005(3) -0.013(3) C5 0.033(3) 0.051(4) 0.039(3) -0.026(3) 0.017(3) -0.022(3) C6 0.027(3) 0.038(3) 0.036(3) -0.018(3) 0.007(3) -0.017(3) C7 0.034(3) 0.029(3) 0.030(3) -0.015(3) 0.005(3) -0.016(3) N1 0.038(3) 0.028(3) 0.026(2) -0.007(2) 0.005(2) -0.015(2) C1A 0.025(2) 0.050(3) 0.026(2) -0.025(2) 0.0144(18) -0.021(2) C4A 0.042(15) 0.021(14) 0.021(12) 0.000(10) -0.001(11) -0.009(12) C5A 0.027(13) 0.025(15) 0.035(14) -0.001(12) 0.010(11) -0.007(11) C6A 0.030(13) 0.031(14) 0.027(13) -0.014(11) -0.002(10) -0.011(11) C7A 0.005(13) 0.024(14) 0.031(15) -0.020(12) -0.004(11) 0.002(12) C8 0.030(2) 0.028(2) 0.029(2) -0.0093(19) 0.0061(19) -0.013(2) C9 0.030(2) 0.030(2) 0.056(3) -0.028(2) 0.017(2) -0.013(2) C10 0.032(2) 0.030(2) 0.039(3) -0.015(2) 0.005(2) -0.011(2) C11 0.033(2) 0.033(3) 0.040(3) -0.012(2) -0.003(2) -0.014(2) C12 0.050(3) 0.048(3) 0.040(3) -0.004(2) 0.005(2) -0.027(3) C13 0.050(3) 0.059(4) 0.028(3) -0.004(2) 0.001(2) -0.015(3) C14 0.032(3) 0.081(4) 0.045(3) -0.046(3) 0.009(2) -0.018(3) N2 0.031(2) 0.031(2) 0.045(2) -0.0194(18) 0.0139(18) -0.0143(17) C15 0.023(2) 0.042(3) 0.030(2) -0.022(2) 0.0079(18) -0.015(2) C16 0.020(2) 0.029(2) 0.028(2) -0.0078(18) -0.0026(17) -0.0090(18) C17 0.040(3) 0.027(2) 0.033(2) -0.015(2) 0.000(2) -0.006(2) C18 0.039(3) 0.023(2) 0.039(3) -0.013(2) 0.002(2) -0.007(2) C19 0.025(2) 0.031(2) 0.046(3) -0.007(2) 0.004(2) -0.011(2) C20 0.036(2) 0.030(2) 0.035(2) -0.015(2) 0.009(2) -0.012(2) C21 0.031(2) 0.026(2) 0.039(3) -0.014(2) 0.002(2) -0.0099(19) N3 0.0259(19) 0.028(2) 0.028(2) -0.0064(17) -0.0028(15) -0.0067(16) C22 0.026(2) 0.023(2) 0.0187(19) -0.0027(17) 0.0018(17) -0.0124(18) C23 0.0179(19) 0.025(2) 0.022(2) -0.0102(17) 0.0053(16) -0.0053(17) C24 0.024(2) 0.033(2) 0.031(2) -0.0193(19) 0.0098(17) -0.0155(18) C25 0.020(2) 0.040(3) 0.029(2) -0.016(2) 0.0044(17) -0.0130(19) C26 0.023(2) 0.035(2) 0.026(2) -0.0063(19) 0.0008(17) -0.0103(19) C27 0.023(2) 0.024(2) 0.031(2) -0.0082(18) 0.0034(17) -0.0106(18) C28 0.021(2) 0.028(2) 0.027(2) -0.0112(18) 0.0024(16) -0.0087(17) N4 0.0210(17) 0.0257(19) 0.0216(17) -0.0077(15) 0.0007(14) -0.0075(15) B1 0.021(2) 0.024(2) 0.023(2) -0.0038(19) 0.0039(18) -0.0119(19) C29 0.024(2) 0.025(2) 0.024(2) -0.0028(17) 0.0055(16) -0.0140(18) C30 0.026(2) 0.032(2) 0.026(2) -0.0040(18) 0.0017(17) -0.0171(19) C31 0.031(2) 0.049(3) 0.024(2) 0.003(2) -0.0026(18) -0.024(2) C32 0.020(2) 0.048(3) 0.039(3) 0.006(2) 0.001(2) -0.011(2) C33 0.024(2) 0.041(3) 0.048(3) -0.010(2) 0.013(2) -0.006(2) C34 0.027(2) 0.035(3) 0.033(2) -0.008(2) 0.0058(18) -0.013(2) C35 0.0136(18) 0.020(2) 0.0226(19) -0.0044(16) 0.0019(15) -0.0040(16) C36 0.033(2) 0.030(2) 0.024(2) -0.0091(18) 0.0041(18) -0.018(2) C37 0.030(2) 0.040(3) 0.030(2) -0.019(2) 0.0050(18) -0.018(2) C38 0.024(2) 0.043(3) 0.019(2) -0.0125(19) 0.0034(17) -0.011(2) C39 0.022(2) 0.027(2) 0.023(2) -0.0041(17) 0.0049(16) -0.0058(18) C40 0.0185(19) 0.020(2) 0.026(2) -0.0073(16) -0.0006(16) -0.0065(16) C41 0.0223(19) 0.025(2) 0.0156(18) -0.0031(16) 0.0011(15) -0.0117(17) C42 0.032(2) 0.026(2) 0.0191(19) -0.0056(17) 0.0028(17) -0.0150(19) C43 0.045(3) 0.031(2) 0.022(2) -0.0034(18) -0.0002(19) -0.026(2) C44 0.050(3) 0.022(2) 0.018(2) -0.0045(17) -0.0037(19) -0.011(2) C45 0.034(2) 0.031(2) 0.020(2) -0.0095(18) -0.0020(17) -0.008(2) C46 0.031(2) 0.030(2) 0.020(2) -0.0068(17) 0.0007(17) -0.0146(19) C47 0.0219(19) 0.0147(19) 0.0222(19) -0.0090(16) 0.0024(15) -0.0073(16) C48 0.024(2) 0.029(2) 0.0188(19) -0.0030(17) -0.0033(16) -0.0079(18) C49 0.021(2) 0.032(2) 0.031(2) -0.0090(19) -0.0007(17) -0.0117(18) C50 0.023(2) 0.026(2) 0.031(2) -0.0096(18) 0.0063(17) -0.0112(18) C51 0.025(2) 0.023(2) 0.0201(19) -0.0015(16) 0.0033(16) -0.0062(17) C52 0.0181(18) 0.020(2) 0.026(2) -0.0105(17) 0.0039(16) -0.0066(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 C8 1.964(4) . ? Rh1 C1 1.966(5) . ? Rh1 C22 1.979(4) . ? Rh1 C15 1.985(4) . ? C1 N1 1.175(7) . ? C2 N1 1.465(7) . ? C2 C3 1.527(7) . ? C2 C7 1.530(7) . ? C2 H2 1.0000 . ? C3 C4 1.518(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.524(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.535(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.520(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C2A N1A 1.432(9) . ? C2A C7A 1.522(11) . ? C2A C3A 1.524(11) . ? C2A H2A 1.0000 . ? C3A C4A 1.538(11) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C5A 1.514(11) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.508(11) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.519(11) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8 N2 1.152(5) . ? C9 N2 1.457(5) . ? C9 C10 1.514(6) . ? C9 C14 1.518(7) . ? C9 H9 1.0000 . ? C10 C11 1.506(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.514(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.521(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N3 1.144(5) . ? C16 N3 1.443(5) . ? C16 C21 1.517(5) . ? C16 C17 1.524(6) . ? C16 H16 1.0000 . ? C17 C18 1.532(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.520(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.515(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.519(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N4 1.145(5) . ? C23 N4 1.468(4) . ? C23 C24 1.521(5) . ? C23 C28 1.522(5) . ? C23 H23 1.0000 . ? C24 C25 1.524(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.534(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.521(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? B1 C35 1.642(6) . ? B1 C47 1.645(5) . ? B1 C41 1.655(6) . ? B1 C29 1.655(6) . ? C29 C30 1.403(6) . ? C29 C34 1.412(6) . ? C30 C31 1.390(6) . ? C30 H30 0.9500 . ? C31 C32 1.369(7) . ? C31 H31 0.9500 . ? C32 C33 1.387(7) . ? C32 H32 0.9500 . ? C33 C34 1.392(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.403(5) . ? C35 C40 1.406(5) . ? C36 C37 1.385(5) . ? C36 H36 0.9500 . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.383(6) . ? C38 H38 0.9500 . ? C39 C40 1.381(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.401(5) . ? C41 C42 1.404(5) . ? C42 C43 1.390(6) . ? C42 H42 0.9500 . ? C43 C44 1.377(6) . ? C43 H43 0.9500 . ? C44 C45 1.370(6) . ? C44 H44 0.9500 . ? C45 C46 1.392(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.399(5) . ? C47 C52 1.403(5) . ? C48 C49 1.386(5) . ? C48 H48 0.9500 . ? C49 C50 1.385(6) . ? C49 H49 0.9500 . ? C50 C51 1.377(5) . ? C50 H50 0.9500 . ? C51 C52 1.395(5) . ? C51 H51 0.9500 . ? C52 H52 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 C8 Rh1 C1 90.70(16) . . ? C8 Rh1 C22 178.98(19) . . ? C1 Rh1 C22 90.30(15) . . ? C8 Rh1 C15 89.72(17) . . ? C1 Rh1 C15 176.71(18) . . ? C22 Rh1 C15 89.28(16) . . ? N1 C1 Rh1 177.8(5) . . ? N1 C2 C3 110.5(5) . . ? N1 C2 C7 108.5(5) . . ? C3 C2 C7 111.2(4) . . ? N1 C2 H2 108.8 . . ? C3 C2 H2 108.8 . . ? C7 C2 H2 108.8 . . ? C4 C3 C2 112.5(4) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 112.4(4) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 110.8(5) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 110.4(5) . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C2 112.2(4) . . ? C6 C7 H7A 109.2 . . ? C2 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C1 N1 C2 173.6(7) . . ? N1A C2A C7A 109.0(9) . . ? N1A C2A C3A 111.2(10) . . ? C7A C2A C3A 112.1(9) . . ? N1A C2A H2A 108.1 . . ? C7A C2A H2A 108.1 . . ? C3A C2A H2A 108.1 . . ? C2A C3A C4A 108.6(8) . . ? C2A C3A H3A1 110.0 . . ? C4A C3A H3A1 110.0 . . ? C2A C3A H3A2 110.0 . . ? C4A C3A H3A2 110.0 . . ? H3A1 C3A H3A2 108.3 . . ? C5A C4A C3A 111.0(9) . . ? C5A C4A H4A1 109.4 . . ? C3A C4A H4A1 109.4 . . ? C5A C4A H4A2 109.4 . . ? C3A C4A H4A2 109.4 . . ? H4A1 C4A H4A2 108.0 . . ? C6A C5A C4A 112.6(9) . . ? C6A C5A H5A1 109.1 . . ? C4A C5A H5A1 109.1 . . ? C6A C5A H5A2 109.1 . . ? C4A C5A H5A2 109.1 . . ? H5A1 C5A H5A2 107.8 . . ? C5A C6A C7A 112.1(9) . . ? C5A C6A H6A1 109.2 . . ? C7A C6A H6A1 109.2 . . ? C5A C6A H6A2 109.2 . . ? C7A C6A H6A2 109.2 . . ? H6A1 C6A H6A2 107.9 . . ? C6A C7A C2A 109.3(8) . . ? C6A C7A H7A1 109.8 . . ? C2A C7A H7A1 109.8 . . ? C6A C7A H7A2 109.8 . . ? C2A C7A H7A2 109.8 . . ? H7A1 C7A H7A2 108.3 . . ? N2 C8 Rh1 178.7(4) . . ? N2 C9 C10 108.7(4) . . ? N2 C9 C14 109.3(4) . . ? C10 C9 C14 112.3(4) . . ? N2 C9 H9 108.8 . . ? C10 C9 H9 108.8 . . ? C14 C9 H9 108.8 . . ? C11 C10 C9 111.6(4) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 112.8(4) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 111.8(4) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 110.8(4) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C9 C14 C13 112.4(4) . . ? C9 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C9 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C8 N2 C9 176.6(5) . . ? N3 C15 Rh1 178.4(4) . . ? N3 C16 C21 108.5(3) . . ? N3 C16 C17 110.5(3) . . ? C21 C16 C17 112.5(3) . . ? N3 C16 H16 108.4 . . ? C21 C16 H16 108.4 . . ? C17 C16 H16 108.4 . . ? C16 C17 C18 110.2(3) . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C17 111.3(3) . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C18 110.7(3) . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C21 111.4(4) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C16 C21 C20 111.0(3) . . ? C16 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C16 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C15 N3 C16 171.7(4) . . ? N4 C22 Rh1 179.0(4) . . ? N4 C23 C24 108.9(3) . . ? N4 C23 C28 109.0(3) . . ? C24 C23 C28 111.7(3) . . ? N4 C23 H23 109.1 . . ? C24 C23 H23 109.1 . . ? C28 C23 H23 109.1 . . ? C23 C24 C25 112.4(3) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 110.7(3) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 111.4(3) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.6(3) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C23 112.2(3) . . ? C27 C28 H28A 109.2 . . ? C23 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C23 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C22 N4 C23 179.9(4) . . ? C35 B1 C47 110.4(3) . . ? C35 B1 C41 110.8(3) . . ? C47 B1 C41 107.5(3) . . ? C35 B1 C29 108.3(3) . . ? C47 B1 C29 110.8(3) . . ? C41 B1 C29 109.1(3) . . ? C30 C29 C34 114.5(4) . . ? C30 C29 B1 122.9(4) . . ? C34 C29 B1 122.6(4) . . ? C31 C30 C29 123.5(4) . . ? C31 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? C32 C31 C30 120.1(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.0(4) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 120.6(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 122.3(4) . . ? C33 C34 H34 118.8 . . ? C29 C34 H34 118.8 . . ? C36 C35 C40 114.0(3) . . ? C36 C35 B1 123.4(3) . . ? C40 C35 B1 122.6(3) . . ? C37 C36 C35 123.3(4) . . ? C37 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? C38 C37 C36 120.4(4) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 118.6(4) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 120.1(4) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C35 123.6(4) . . ? C39 C40 H40 118.2 . . ? C35 C40 H40 118.2 . . ? C46 C41 C42 114.8(4) . . ? C46 C41 B1 123.4(3) . . ? C42 C41 B1 121.8(3) . . ? C43 C42 C41 122.8(4) . . ? C43 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? C44 C43 C42 119.8(4) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.8(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 122.9(4) . . ? C45 C46 H46 118.6 . . ? C41 C46 H46 118.6 . . ? C48 C47 C52 114.8(3) . . ? C48 C47 B1 122.7(3) . . ? C52 C47 B1 122.3(3) . . ? C49 C48 C47 123.2(4) . . ? C49 C48 H48 118.4 . . ? C47 C48 H48 118.4 . . ? C50 C49 C48 120.1(4) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 119.0(4) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 120.1(4) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C47 122.8(4) . . ? C51 C52 H52 118.6 . . ? C47 C52 H52 118.6 . . ? 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 C8 Rh1 C1 N1 164(13) . . . . ? C22 Rh1 C1 N1 -15(13) . . . . ? C15 Rh1 C1 N1 67(14) . . . . ? N1 C2 C3 C4 69.0(6) . . . . ? C7 C2 C3 C4 -51.6(6) . . . . ? C2 C3 C4 C5 52.7(6) . . . . ? C3 C4 C5 C6 -54.7(7) . . . . ? C4 C5 C6 C7 56.3(6) . . . . ? C5 C6 C7 C2 -56.6(6) . . . . ? N1 C2 C7 C6 -67.7(6) . . . . ? C3 C2 C7 C6 54.1(6) . . . . ? Rh1 C1 N1 C2 -36(18) . . . . ? C3 C2 N1 C1 -177(6) . . . . ? C7 C2 N1 C1 -55(7) . . . . ? N1A C2A C3A C4A -178.5(14) . . . . ? C7A C2A C3A C4A 59.1(16) . . . . ? C2A C3A C4A C5A -56.0(17) . . . . ? C3A C4A C5A C6A 54.6(18) . . . . ? C4A C5A C6A C7A -54.1(18) . . . . ? C5A C6A C7A C2A 54.6(18) . . . . ? N1A C2A C7A C6A 178.0(15) . . . . ? C3A C2A C7A C6A -58.4(16) . . . . ? C1 Rh1 C8 N2 -165(17) . . . . ? C22 Rh1 C8 N2 2(25) . . . . ? C15 Rh1 C8 N2 12(17) . . . . ? N2 C9 C10 C11 69.5(5) . . . . ? C14 C9 C10 C11 -51.5(5) . . . . ? C9 C10 C11 C12 53.0(5) . . . . ? C10 C11 C12 C13 -55.0(6) . . . . ? C11 C12 C13 C14 54.4(6) . . . . ? N2 C9 C14 C13 -68.2(5) . . . . ? C10 C9 C14 C13 52.5(5) . . . . ? C12 C13 C14 C9 -53.5(5) . . . . ? Rh1 C8 N2 C9 30(23) . . . . ? C10 C9 N2 C8 32(7) . . . . ? C14 C9 N2 C8 155(7) . . . . ? C8 Rh1 C15 N3 -125(13) . . . . ? C1 Rh1 C15 N3 -28(15) . . . . ? C22 Rh1 C15 N3 55(13) . . . . ? N3 C16 C17 C18 175.8(3) . . . . ? C21 C16 C17 C18 54.3(5) . . . . ? C16 C17 C18 C19 -55.3(5) . . . . ? C17 C18 C19 C20 57.0(5) . . . . ? C18 C19 C20 C21 -56.8(5) . . . . ? N3 C16 C21 C20 -177.1(3) . . . . ? C17 C16 C21 C20 -54.5(5) . . . . ? C19 C20 C21 C16 55.2(5) . . . . ? Rh1 C15 N3 C16 -47(15) . . . . ? C21 C16 N3 C15 -6(3) . . . . ? C17 C16 N3 C15 -130(3) . . . . ? C8 Rh1 C22 N4 -85(27) . . . . ? C1 Rh1 C22 N4 83(24) . . . . ? C15 Rh1 C22 N4 -94(24) . . . . ? N4 C23 C24 C25 67.2(4) . . . . ? C28 C23 C24 C25 -53.3(4) . . . . ? C23 C24 C25 C26 54.4(4) . . . . ? C24 C25 C26 C27 -55.2(4) . . . . ? C25 C26 C27 C28 55.2(4) . . . . ? C26 C27 C28 C23 -53.9(4) . . . . ? N4 C23 C28 C27 -67.8(4) . . . . ? C24 C23 C28 C27 52.6(4) . . . . ? Rh1 C22 N4 C23 25(100) . . . . ? C24 C23 N4 C22 0(100) . . . . ? C28 C23 N4 C22 122(100) . . . . ? C35 B1 C29 C30 151.1(3) . . . . ? C47 B1 C29 C30 -87.7(4) . . . . ? C41 B1 C29 C30 30.5(5) . . . . ? C35 B1 C29 C34 -29.0(5) . . . . ? C47 B1 C29 C34 92.3(4) . . . . ? C41 B1 C29 C34 -149.6(3) . . . . ? C34 C29 C30 C31 2.2(6) . . . . ? B1 C29 C30 C31 -177.9(4) . . . . ? C29 C30 C31 C32 -2.1(6) . . . . ? C30 C31 C32 C33 0.6(6) . . . . ? C31 C32 C33 C34 0.8(7) . . . . ? C32 C33 C34 C29 -0.6(7) . . . . ? C30 C29 C34 C33 -0.8(6) . . . . ? B1 C29 C34 C33 179.3(4) . . . . ? C47 B1 C35 C36 -34.6(5) . . . . ? C41 B1 C35 C36 -153.6(3) . . . . ? C29 B1 C35 C36 86.9(4) . . . . ? C47 B1 C35 C40 147.9(3) . . . . ? C41 B1 C35 C40 28.9(5) . . . . ? C29 B1 C35 C40 -90.7(4) . . . . ? C40 C35 C36 C37 -1.5(6) . . . . ? B1 C35 C36 C37 -179.2(4) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C36 C37 C38 C39 0.7(6) . . . . ? C37 C38 C39 C40 -0.9(6) . . . . ? C38 C39 C40 C35 -0.2(6) . . . . ? C36 C35 C40 C39 1.3(5) . . . . ? B1 C35 C40 C39 179.1(3) . . . . ? C35 B1 C41 C46 97.9(4) . . . . ? C47 B1 C41 C46 -22.8(5) . . . . ? C29 B1 C41 C46 -143.0(4) . . . . ? C35 B1 C41 C42 -82.1(4) . . . . ? C47 B1 C41 C42 157.2(3) . . . . ? C29 B1 C41 C42 37.0(5) . . . . ? C46 C41 C42 C43 2.1(6) . . . . ? B1 C41 C42 C43 -177.9(4) . . . . ? C41 C42 C43 C44 -1.9(6) . . . . ? C42 C43 C44 C45 0.3(6) . . . . ? C43 C44 C45 C46 1.0(6) . . . . ? C44 C45 C46 C41 -0.7(6) . . . . ? C42 C41 C46 C45 -0.8(6) . . . . ? B1 C41 C46 C45 179.2(4) . . . . ? C35 B1 C47 C48 -35.8(5) . . . . ? C41 B1 C47 C48 85.1(4) . . . . ? C29 B1 C47 C48 -155.8(4) . . . . ? C35 B1 C47 C52 150.8(3) . . . . ? C41 B1 C47 C52 -88.3(4) . . . . ? C29 B1 C47 C52 30.8(5) . . . . ? C52 C47 C48 C49 -0.6(6) . . . . ? B1 C47 C48 C49 -174.5(4) . . . . ? C47 C48 C49 C50 0.4(6) . . . . ? C48 C49 C50 C51 0.5(6) . . . . ? C49 C50 C51 C52 -1.2(6) . . . . ? C50 C51 C52 C47 1.0(6) . . . . ? C48 C47 C52 C51 -0.1(5) . . . . ? B1 C47 C52 C51 173.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.233 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.108 #===END data_jrs93 _database_code_depnum_ccdc_archive 'CCDC 285149' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Rh(i-PrNC)~4~]B(C~6~H~5~)~4~' _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 N4 Rh, C24 H20 B' _chemical_formula_sum 'C40 H48 B N4 Rh' _chemical_formula_weight 698.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 14.2642(6) _cell_length_b 14.2642(6) _cell_length_c 18.6642(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3797.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 30.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8771 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30626 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.53 _reflns_number_total 2913 _reflns_number_gt 2630 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All H atoms were located in a difference map, placed in idealized positions and treated as riding atoms. Atoms Rh1 and B1 occupy special positions with 4-bar site symmetry, such that the asymmetric unit contains 1/4 of a formula unit. One methyl group of the isopropyl group is disordered and was modeled as two positions, C4 and C5, with refined occupancies of 65(3) % and 35(3) %, respectively. ; _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^)+(0.0267P)^2^+4.1786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 2913 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.0000 0.2500 0.6250 0.01491(6) Uani 1 4 d S . . C1 C 0.13442(9) 0.21763(8) 0.62421(6) 0.0185(2) Uani 1 1 d . . . C2 C 0.31310(9) 0.17922(10) 0.61931(8) 0.0260(3) Uani 1 1 d . . . H2 H 0.3426 0.2237 0.5844 0.031 Uiso 1 1 d . . . C3 C 0.32679(13) 0.08097(12) 0.59288(14) 0.0514(5) Uani 1 1 d . A . H3A H 0.3012 0.0367 0.6280 0.077 Uiso 1 1 calc R . . H3B H 0.3939 0.0689 0.5863 0.077 Uiso 1 1 calc R . . H3C H 0.2942 0.0731 0.5470 0.077 Uiso 1 1 calc R . . C4 C 0.3528(4) 0.1837(10) 0.6965(4) 0.056(2) Uani 0.65(3) 1 d P A 1 H4A H 0.3398 0.2455 0.7172 0.084 Uiso 0.65(3) 1 calc PR A 1 H4B H 0.4207 0.1733 0.6953 0.084 Uiso 0.65(3) 1 calc PR A 1 H4C H 0.3231 0.1351 0.7259 0.084 Uiso 0.65(3) 1 calc PR A 1 C5 C 0.3615(6) 0.2262(17) 0.6793(9) 0.059(3) Uani 0.35(3) 1 d P A 2 H5A H 0.3449 0.2929 0.6797 0.088 Uiso 0.35(3) 1 calc PR A 2 H5B H 0.4294 0.2196 0.6734 0.088 Uiso 0.35(3) 1 calc PR A 2 H5C H 0.3423 0.1973 0.7246 0.088 Uiso 0.35(3) 1 calc PR A 2 N1 N 0.21323(7) 0.19967(7) 0.62319(6) 0.0209(2) Uani 1 1 d . A . B1 B 0.5000 0.2500 0.3750 0.0140(4) Uani 1 4 d S . . C6 C 0.42008(8) 0.29678(8) 0.42769(6) 0.0160(2) Uani 1 1 d . . . C7 C 0.32369(8) 0.27889(8) 0.42343(6) 0.0196(2) Uani 1 1 d . . . H7 H 0.3018 0.2362 0.3881 0.023 Uiso 1 1 calc R . . C8 C 0.25830(9) 0.32119(9) 0.46899(7) 0.0239(2) Uani 1 1 d . . . H8 H 0.1935 0.3073 0.4640 0.029 Uiso 1 1 calc R . . C9 C 0.28785(10) 0.38338(9) 0.52141(7) 0.0256(3) Uani 1 1 d . . . H9 H 0.2437 0.4125 0.5524 0.031 Uiso 1 1 calc R . . C10 C 0.38291(10) 0.40254(9) 0.52804(7) 0.0245(2) Uani 1 1 d . . . H10 H 0.4042 0.4448 0.5638 0.029 Uiso 1 1 calc R . . C11 C 0.44704(9) 0.35963(9) 0.48213(6) 0.0206(2) Uani 1 1 d . . . H11 H 0.5118 0.3734 0.4878 0.025 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 0.01284(6) 0.01284(6) 0.01903(9) 0.000 0.000 0.000 C1 0.0203(5) 0.0144(5) 0.0207(5) 0.0003(4) -0.0007(4) -0.0012(4) C2 0.0144(5) 0.0273(6) 0.0361(7) 0.0025(5) 0.0006(5) 0.0039(4) C3 0.0338(8) 0.0291(8) 0.0912(15) -0.0013(9) 0.0269(9) 0.0078(6) C4 0.0301(18) 0.093(5) 0.044(2) -0.014(2) -0.0154(16) 0.020(2) C5 0.026(3) 0.092(8) 0.058(6) -0.005(6) -0.016(3) -0.002(4) N1 0.0176(5) 0.0180(4) 0.0270(5) -0.0001(4) -0.0001(4) 0.0007(3) B1 0.0148(6) 0.0148(6) 0.0126(9) 0.000 0.000 0.000 C6 0.0181(5) 0.0151(5) 0.0149(5) 0.0013(4) 0.0001(4) -0.0003(4) C7 0.0191(5) 0.0210(5) 0.0186(5) -0.0018(4) 0.0011(4) -0.0010(4) C8 0.0191(5) 0.0266(6) 0.0259(6) -0.0002(5) 0.0045(4) 0.0015(4) C9 0.0295(6) 0.0228(6) 0.0244(6) -0.0009(5) 0.0100(5) 0.0040(5) C10 0.0334(7) 0.0201(5) 0.0200(5) -0.0046(4) 0.0041(5) -0.0027(5) C11 0.0221(5) 0.0210(5) 0.0187(5) -0.0020(4) 0.0013(4) -0.0033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.9722(12) 15_556 ? Rh1 C1 1.9722(12) 6_454 ? Rh1 C1 1.9722(12) 12_667 ? Rh1 C1 1.9722(12) . ? C1 N1 1.1532(16) . ? C2 N1 1.4558(16) . ? C2 C5 1.476(10) . ? C2 C3 1.498(2) . ? C2 C4 1.550(5) . ? C2 H2 1.0020 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? B1 C6 1.6467(11) 16_656 ? B1 C6 1.6467(11) . ? B1 C6 1.6467(11) 6_554 ? B1 C6 1.6467(11) 11_666 ? C6 C7 1.4008(16) . ? C6 C11 1.4086(16) . ? C7 C8 1.3990(17) . ? C7 H7 0.9500 . ? C8 C9 1.3863(19) . ? C8 H8 0.9500 . ? C9 C10 1.3888(19) . ? C9 H9 0.9500 . ? C10 C11 1.3949(17) . ? C10 H10 0.9500 . ? C11 H11 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 C1 90.003(1) 15_556 6_454 ? C1 Rh1 C1 179.14(7) 15_556 12_667 ? C1 Rh1 C1 90.003(1) 6_454 12_667 ? C1 Rh1 C1 90.003(1) 15_556 . ? C1 Rh1 C1 179.14(7) 6_454 . ? C1 Rh1 C1 90.003(1) 12_667 . ? N1 C1 Rh1 179.12(12) . . ? N1 C2 C5 109.2(4) . . ? N1 C2 C3 109.35(12) . . ? C5 C2 C3 127.8(9) . . ? N1 C2 C4 107.7(2) . . ? C3 C2 C4 107.3(5) . . ? N1 C2 H2 108.4 . . ? C5 C2 H2 90.6 . . ? C3 C2 H2 108.9 . . ? C4 C2 H2 115.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 N1 C2 177.72(13) . . ? C6 B1 C6 110.89(4) 16_656 . ? C6 B1 C6 110.89(4) 16_656 6_554 ? C6 B1 C6 106.67(8) . 6_554 ? C6 B1 C6 106.67(8) 16_656 11_666 ? C6 B1 C6 110.89(4) . 11_666 ? C6 B1 C6 110.89(4) 6_554 11_666 ? C7 C6 C11 115.14(10) . . ? C7 C6 B1 124.88(9) . . ? C11 C6 B1 119.98(9) . . ? C8 C7 C6 122.78(11) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C9 C8 C7 120.15(12) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.05(12) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C9 C10 C11 119.95(12) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 122.91(11) . . ? C10 C11 H11 118.5 . . ? C6 C11 H11 118.5 . . ? 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 C1 N1 144(9) 15_556 . . . ? C1 Rh1 C1 N1 54(9) 6_454 . . . ? C1 Rh1 C1 N1 -36(9) 12_667 . . . ? Rh1 C1 N1 C2 -21(11) . . . . ? C5 C2 N1 C1 112(4) . . . . ? C3 C2 N1 C1 -104(3) . . . . ? C4 C2 N1 C1 140(3) . . . . ? C6 B1 C6 C7 -6.39(11) 16_656 . . . ? C6 B1 C6 C7 -127.23(12) 6_554 . . . ? C6 B1 C6 C7 111.92(13) 11_666 . . . ? C6 B1 C6 C11 173.34(10) 16_656 . . . ? C6 B1 C6 C11 52.50(8) 6_554 . . . ? C6 B1 C6 C11 -68.34(7) 11_666 . . . ? C11 C6 C7 C8 0.96(17) . . . . ? B1 C6 C7 C8 -179.29(10) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C7 C8 C9 C10 -0.2(2) . . . . ? C8 C9 C10 C11 0.2(2) . . . . ? C9 C10 C11 C6 0.4(2) . . . . ? C7 C6 C11 C10 -0.99(17) . . . . ? B1 C6 C11 C10 179.25(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.591 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.060 #===END data_mn1773 _database_code_depnum_ccdc_archive 'CCDC 285150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Rh(CNCy)4]2(Cl)2.0.5benzene.2H2O' _chemical_melting_point ? _chemical_formula_moiety '2(C28 H44 N4 Rh), 0.5(C6 H6), 2(H2 O), 2(Cl)' _chemical_formula_sum 'C59 H97 Cl2 N8 O2 Rh2' _chemical_formula_weight 1223.13 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5495(4) _cell_length_b 23.1451(7) _cell_length_c 20.2848(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.449(3) _cell_angle_gamma 90.00 _cell_volume 6131.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8251 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 31.5 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 Apex2' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69058 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14059 _reflns_number_gt 12657 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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. One of the cyclohexyl isocyanides is disordered into two orientations with relative occupancies 0.6:0.4 for A:B sets. One of the two water molecules was split into two sites with refined occupancies 0.476(11):0.524(11) for O2A and O2B, respectively. H atoms on the water molecules were not located. ; _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^)+(0.0306P)^2^+5.2064P] 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 14059 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.009 _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 0.545338(10) 0.672665(5) 0.186542(6) 0.01705(4) Uani 1 1 d . A . C1 C 0.47182(13) 0.60351(7) 0.20573(8) 0.0208(3) Uani 1 1 d . . . N1 N 0.43725(11) 0.55986(6) 0.21476(8) 0.0236(3) Uani 1 1 d . . . C2 C 0.40642(13) 0.50154(7) 0.22636(8) 0.0209(3) Uani 1 1 d . . . H2 H 0.3395 0.5031 0.2383 0.025 Uiso 1 1 calc R . . C3 C 0.39327(14) 0.46594(8) 0.16116(9) 0.0243(4) Uani 1 1 d . . . H3A H 0.4585 0.4652 0.1479 0.029 Uiso 1 1 calc R . . H3B H 0.3402 0.4838 0.1234 0.029 Uiso 1 1 calc R . . C4 C 0.36160(14) 0.40435(8) 0.17368(9) 0.0253(4) Uani 1 1 d . . . H4A H 0.2937 0.4052 0.1833 0.030 Uiso 1 1 calc R . . H4B H 0.3555 0.3809 0.1319 0.030 Uiso 1 1 calc R . . C5 C 0.43908(16) 0.37645(8) 0.23340(10) 0.0332(4) Uani 1 1 d . . . H5A H 0.5056 0.3724 0.2223 0.040 Uiso 1 1 calc R . . H5B H 0.4152 0.3374 0.2417 0.040 Uiso 1 1 calc R . . C6 C 0.45283(18) 0.41313(9) 0.29762(10) 0.0379(5) Uani 1 1 d . . . H6A H 0.5049 0.3951 0.3358 0.046 Uiso 1 1 calc R . . H6B H 0.3874 0.4147 0.3106 0.046 Uiso 1 1 calc R . . C7 C 0.48662(15) 0.47461(8) 0.28574(9) 0.0282(4) Uani 1 1 d . . . H7A H 0.4939 0.4981 0.3276 0.034 Uiso 1 1 calc R . . H7B H 0.5537 0.4735 0.2750 0.034 Uiso 1 1 calc R . . C8 C 0.44011(13) 0.72608(7) 0.20179(8) 0.0197(3) Uani 1 1 d . . . N2 N 0.37649(11) 0.75633(6) 0.20893(7) 0.0212(3) Uani 1 1 d . . . C9 C 0.28730(13) 0.78655(7) 0.21821(9) 0.0221(3) Uani 1 1 d . . . H9 H 0.3098 0.8219 0.2466 0.026 Uiso 1 1 calc R . . C10 C 0.21879(15) 0.80417(8) 0.14848(9) 0.0287(4) Uani 1 1 d . . . H10A H 0.1614 0.8280 0.1550 0.034 Uiso 1 1 calc R . . H10B H 0.2587 0.8280 0.1243 0.034 Uiso 1 1 calc R . . C11 C 0.17615(15) 0.75183(10) 0.10492(9) 0.0332(4) Uani 1 1 d . . . H11A H 0.2330 0.7305 0.0938 0.040 Uiso 1 1 calc R . . H11B H 0.1286 0.7648 0.0615 0.040 Uiso 1 1 calc R . . C12 C 0.11945(15) 0.71145(10) 0.14206(10) 0.0365(5) Uani 1 1 d . . . H12A H 0.0575 0.7311 0.1479 0.044 Uiso 1 1 calc R . . H12B H 0.0973 0.6765 0.1140 0.044 Uiso 1 1 calc R . . C13 C 0.18709(15) 0.69381(9) 0.21188(10) 0.0303(4) Uani 1 1 d . . . H13A H 0.2442 0.6696 0.2057 0.036 Uiso 1 1 calc R . . H13B H 0.1465 0.6704 0.2360 0.036 Uiso 1 1 calc R . . C14 C 0.23052(14) 0.74643(8) 0.25529(9) 0.0258(4) Uani 1 1 d . . . H14A H 0.1739 0.7679 0.2665 0.031 Uiso 1 1 calc R . . H14B H 0.2780 0.7334 0.2987 0.031 Uiso 1 1 calc R . . C15 C 0.62151(13) 0.73649(7) 0.15830(8) 0.0206(3) Uani 1 1 d . . . N3 N 0.66770(11) 0.77162(6) 0.13942(7) 0.0227(3) Uani 1 1 d . . . C16 C 0.73078(14) 0.81265(7) 0.11508(8) 0.0215(3) Uani 1 1 d . . . H16 H 0.7628 0.8396 0.1533 0.026 Uiso 1 1 calc R . . C17 C 0.66577(14) 0.84796(8) 0.05545(9) 0.0251(4) Uani 1 1 d . . . H17A H 0.6116 0.8689 0.0702 0.030 Uiso 1 1 calc R . . H17B H 0.6325 0.8219 0.0173 0.030 Uiso 1 1 calc R . . C18 C 0.73457(16) 0.89114(8) 0.03162(9) 0.0293(4) Uani 1 1 d . . . H18A H 0.6933 0.9127 -0.0084 0.035 Uiso 1 1 calc R . . H18B H 0.7623 0.9193 0.0687 0.035 Uiso 1 1 calc R . . C19 C 0.82301(15) 0.86104(8) 0.01232(9) 0.0284(4) Uani 1 1 d . . . H19A H 0.8683 0.8904 0.0001 0.034 Uiso 1 1 calc R . . H19B H 0.7956 0.8363 -0.0283 0.034 Uiso 1 1 calc R . . C20 C 0.88521(15) 0.82395(8) 0.07119(9) 0.0267(4) Uani 1 1 d . . . H20A H 0.9393 0.8030 0.0563 0.032 Uiso 1 1 calc R . . H20B H 0.9188 0.8491 0.1102 0.032 Uiso 1 1 calc R . . C21 C 0.81577(14) 0.78057(8) 0.09382(9) 0.0233(3) Uani 1 1 d . . . H21A H 0.7855 0.7538 0.0557 0.028 Uiso 1 1 calc R . . H21B H 0.8564 0.7575 0.1328 0.028 Uiso 1 1 calc R . . C22 C 0.63936(13) 0.61723(7) 0.16198(9) 0.0221(3) Uani 1 1 d . . . N4 N 0.68878(12) 0.58326(6) 0.14422(8) 0.0247(3) Uani 1 1 d . . . C23 C 0.75247(14) 0.54530(7) 0.11584(9) 0.0243(4) Uani 1 1 d . . . H23 H 0.7339 0.5042 0.1218 0.029 Uiso 1 1 calc R . . C24 C 0.73287(14) 0.55846(8) 0.03977(9) 0.0247(4) Uani 1 1 d . . . H24A H 0.6588 0.5545 0.0172 0.030 Uiso 1 1 calc R . . H24B H 0.7702 0.5302 0.0188 0.030 Uiso 1 1 calc R . . C25 C 0.76772(14) 0.61958(8) 0.02816(9) 0.0246(4) Uani 1 1 d . . . H25A H 0.7249 0.6481 0.0443 0.029 Uiso 1 1 calc R . . H25B H 0.7584 0.6259 -0.0214 0.029 Uiso 1 1 calc R . . C26 C 0.88021(14) 0.62893(8) 0.06620(9) 0.0262(4) Uani 1 1 d . . . H26A H 0.8995 0.6694 0.0601 0.031 Uiso 1 1 calc R . . H26B H 0.9237 0.6034 0.0465 0.031 Uiso 1 1 calc R . . C27 C 0.89940(14) 0.61597(8) 0.14267(9) 0.0269(4) Uani 1 1 d . . . H27A H 0.9734 0.6198 0.1655 0.032 Uiso 1 1 calc R . . H27B H 0.8621 0.6444 0.1635 0.032 Uiso 1 1 calc R . . C28 C 0.86401(15) 0.55531(8) 0.15393(9) 0.0273(4) Uani 1 1 d . . . H28A H 0.8729 0.5491 0.2035 0.033 Uiso 1 1 calc R . . H28B H 0.9073 0.5268 0.1382 0.033 Uiso 1 1 calc R . . Rh2 Rh 0.588646(10) 0.682832(6) 0.353473(6) 0.01790(4) Uani 1 1 d . . . C29A C 0.4690(2) 0.63811(13) 0.35989(15) 0.0200(5) Uiso 0.60 1 d P A 1 N5A N 0.3953(2) 0.61445(11) 0.36347(13) 0.0260(5) Uiso 0.60 1 d P A 1 C30A C 0.2997(2) 0.59075(14) 0.37122(16) 0.0268(6) Uiso 0.60 1 d P A 1 H30A H 0.2545 0.5803 0.3252 0.032 Uiso 0.60 1 calc PR A 1 C31A C 0.3218(3) 0.53717(15) 0.41591(17) 0.0327(7) Uiso 0.60 1 d P A 1 H31A H 0.2561 0.5183 0.4157 0.039 Uiso 0.60 1 calc PR A 1 H31B H 0.3619 0.5097 0.3960 0.039 Uiso 0.60 1 calc PR A 1 C32A C 0.3792(3) 0.54969(16) 0.48780(18) 0.0230(8) Uiso 0.60 1 d P A 1 H32A H 0.4496 0.5622 0.4891 0.028 Uiso 0.60 1 calc PR A 1 H32B H 0.3841 0.5140 0.5155 0.028 Uiso 0.60 1 calc PR A 1 C33A C 0.3258(3) 0.59750(16) 0.51902(17) 0.0327(7) Uiso 0.60 1 d P A 1 H33A H 0.2598 0.5825 0.5242 0.039 Uiso 0.60 1 calc PR A 1 H33B H 0.3692 0.6073 0.5652 0.039 Uiso 0.60 1 calc PR A 1 C34A C 0.3061(3) 0.65156(14) 0.47603(16) 0.0286(6) Uiso 0.60 1 d P A 1 H34A H 0.2666 0.6794 0.4960 0.034 Uiso 0.60 1 calc PR A 1 H34B H 0.3721 0.6698 0.4758 0.034 Uiso 0.60 1 calc PR A 1 C35A C 0.2471(3) 0.63743(18) 0.40390(19) 0.0216(9) Uiso 0.60 1 d P A 1 H35A H 0.2393 0.6730 0.3758 0.026 Uiso 0.60 1 calc PR A 1 H35B H 0.1778 0.6239 0.4039 0.026 Uiso 0.60 1 calc PR A 1 C29B C 0.4995(3) 0.62354(18) 0.3806(2) 0.0163(8) Uiso 0.40 1 d P A 2 N5B N 0.4475(3) 0.59035(15) 0.39669(18) 0.0211(7) Uiso 0.40 1 d P A 2 C30B C 0.3792(4) 0.5522(2) 0.4194(2) 0.0238(9) Uiso 0.40 1 d P A 2 H30B H 0.3949 0.5113 0.4100 0.029 Uiso 0.40 1 calc PR A 2 C31B C 0.3986(4) 0.5611(2) 0.4997(3) 0.0241(12) Uiso 0.40 1 d P A 2 H31C H 0.3628 0.5304 0.5181 0.029 Uiso 0.40 1 calc PR A 2 H31D H 0.4728 0.5577 0.5221 0.029 Uiso 0.40 1 calc PR A 2 C32B C 0.3621(4) 0.6179(2) 0.5159(2) 0.0267(9) Uiso 0.40 1 d P A 2 H32C H 0.4070 0.6483 0.5053 0.032 Uiso 0.40 1 calc PR A 2 H32D H 0.3678 0.6197 0.5655 0.032 Uiso 0.40 1 calc PR A 2 C33B C 0.2512(4) 0.6305(2) 0.4763(2) 0.0273(9) Uiso 0.40 1 d P A 2 H33C H 0.2328 0.6701 0.4873 0.033 Uiso 0.40 1 calc PR A 2 H33D H 0.2051 0.6031 0.4909 0.033 Uiso 0.40 1 calc PR A 2 C34B C 0.2351(5) 0.6252(3) 0.3976(3) 0.0237(15) Uiso 0.40 1 d P A 2 H34C H 0.1620 0.6313 0.3739 0.028 Uiso 0.40 1 calc PR A 2 H34D H 0.2756 0.6553 0.3819 0.028 Uiso 0.40 1 calc PR A 2 C35B C 0.2680(4) 0.5664(2) 0.3803(2) 0.0294(10) Uiso 0.40 1 d P A 2 H35C H 0.2614 0.5645 0.3305 0.035 Uiso 0.40 1 calc PR A 2 H35D H 0.2218 0.5369 0.3912 0.035 Uiso 0.40 1 calc PR A 2 C36 C 0.51292(13) 0.74860(8) 0.37804(8) 0.0215(3) Uani 1 1 d . A . N6 N 0.46814(11) 0.78521(7) 0.39541(7) 0.0238(3) Uani 1 1 d . . . C37 C 0.41221(13) 0.83122(8) 0.41808(9) 0.0229(3) Uani 1 1 d . A . H37 H 0.3802 0.8563 0.3780 0.028 Uiso 1 1 calc R . . C38 C 0.32742(14) 0.80580(9) 0.44602(10) 0.0304(4) Uani 1 1 d . . . H38A H 0.3575 0.7806 0.4857 0.037 Uiso 1 1 calc R A . H38B H 0.2806 0.7822 0.4104 0.037 Uiso 1 1 calc R . . C39 C 0.26812(14) 0.85540(9) 0.46779(10) 0.0302(4) Uani 1 1 d . A . H39A H 0.2344 0.8789 0.4272 0.036 Uiso 1 1 calc R . . H39B H 0.2142 0.8394 0.4872 0.036 Uiso 1 1 calc R . . C40 C 0.33929(15) 0.89367(9) 0.52077(9) 0.0288(4) Uani 1 1 d . . . H40A H 0.2999 0.9264 0.5322 0.035 Uiso 1 1 calc R A . H40B H 0.3676 0.8711 0.5631 0.035 Uiso 1 1 calc R . . C41 C 0.42676(15) 0.91685(9) 0.49439(11) 0.0336(4) Uani 1 1 d . A . H41A H 0.4740 0.9395 0.5309 0.040 Uiso 1 1 calc R . . H41B H 0.3990 0.9430 0.4552 0.040 Uiso 1 1 calc R . . C42 C 0.48577(14) 0.86775(8) 0.47178(10) 0.0284(4) Uani 1 1 d . . . H42A H 0.5397 0.8839 0.4525 0.034 Uiso 1 1 calc R A . H42B H 0.5191 0.8434 0.5117 0.034 Uiso 1 1 calc R . . C43 C 0.69861(12) 0.73459(7) 0.34177(8) 0.0191(3) Uani 1 1 d . A . N7 N 0.76298(11) 0.76406(6) 0.33386(7) 0.0209(3) Uani 1 1 d . . . C44 C 0.84194(13) 0.79892(7) 0.31680(8) 0.0195(3) Uani 1 1 d . A . H44 H 0.8080 0.8285 0.2822 0.023 Uiso 1 1 calc R . . C45 C 0.90577(13) 0.83020(7) 0.38018(9) 0.0213(3) Uani 1 1 d . . . H45A H 0.9496 0.8593 0.3660 0.026 Uiso 1 1 calc R A . H45B H 0.8594 0.8509 0.4025 0.026 Uiso 1 1 calc R . . C46 C 0.97321(14) 0.78898(8) 0.43165(9) 0.0253(4) Uani 1 1 d . A . H46A H 0.9295 0.7626 0.4500 0.030 Uiso 1 1 calc R . . H46B H 1.0164 0.8113 0.4703 0.030 Uiso 1 1 calc R . . C47 C 1.04144(14) 0.75375(9) 0.39770(10) 0.0298(4) Uani 1 1 d . . . H47A H 1.0880 0.7799 0.3817 0.036 Uiso 1 1 calc R A . H47B H 1.0838 0.7267 0.4314 0.036 Uiso 1 1 calc R . . C48 C 0.97582(14) 0.71994(8) 0.33732(10) 0.0271(4) Uani 1 1 d . A . H48A H 1.0208 0.6977 0.3153 0.033 Uiso 1 1 calc R . . H48B H 0.9323 0.6922 0.3540 0.033 Uiso 1 1 calc R . . C49 C 0.90808(13) 0.76009(8) 0.28486(8) 0.0224(3) Uani 1 1 d . . . H49A H 0.8631 0.7367 0.2480 0.027 Uiso 1 1 calc R A . H49B H 0.9517 0.7845 0.2641 0.027 Uiso 1 1 calc R . . C50 C 0.67309(14) 0.61607(7) 0.34179(8) 0.0228(3) Uani 1 1 d . A . N8 N 0.72636(12) 0.57832(7) 0.33847(7) 0.0263(3) Uani 1 1 d . . . C51 C 0.80525(14) 0.53646(7) 0.33656(9) 0.0228(3) Uani 1 1 d . A . H51 H 0.7851 0.5157 0.2918 0.027 Uiso 1 1 calc R . . C52 C 0.90475(15) 0.56898(7) 0.34161(9) 0.0257(4) Uani 1 1 d . . . H52A H 0.8956 0.5958 0.3024 0.031 Uiso 1 1 calc R A . H52B H 0.9229 0.5921 0.3842 0.031 Uiso 1 1 calc R . . C53 C 0.99055(15) 0.52667(8) 0.34161(10) 0.0288(4) Uani 1 1 d . A . H53A H 1.0552 0.5482 0.3462 0.035 Uiso 1 1 calc R . . H53B H 0.9745 0.5056 0.2976 0.035 Uiso 1 1 calc R . . C54 C 1.00440(15) 0.48360(8) 0.40033(9) 0.0299(4) Uani 1 1 d . . . H54A H 1.0589 0.4557 0.3985 0.036 Uiso 1 1 calc R A . H54B H 1.0256 0.5044 0.4445 0.036 Uiso 1 1 calc R . . C55 C 0.90468(16) 0.45142(8) 0.39536(9) 0.0289(4) Uani 1 1 d . A . H55A H 0.9141 0.4250 0.4349 0.035 Uiso 1 1 calc R . . H55B H 0.8876 0.4277 0.3532 0.035 Uiso 1 1 calc R . . C56 C 0.81587(15) 0.49248(8) 0.39414(9) 0.0267(4) Uani 1 1 d . . . H56A H 0.7516 0.4702 0.3871 0.032 Uiso 1 1 calc R A . H56B H 0.8285 0.5128 0.4385 0.032 Uiso 1 1 calc R . . C57 C 1.08758(18) 0.97375(10) 0.54026(14) 0.0440(5) Uani 1 1 d . . . H57 H 1.1475 0.9558 0.5679 0.053 Uiso 1 1 calc R . . C58 C 1.04553(18) 0.95477(9) 0.47442(13) 0.0431(6) Uani 1 1 d . . . H58 H 1.0768 0.9237 0.4568 0.052 Uiso 1 1 calc R . . C59 C 0.95820(18) 0.98041(9) 0.43353(14) 0.0437(5) Uani 1 1 d . . . H59 H 0.9296 0.9671 0.3882 0.052 Uiso 1 1 calc R . . Cl1 Cl 0.71123(4) 0.428445(18) 0.21363(2) 0.02930(10) Uani 1 1 d . . . Cl2 Cl 0.84928(5) 0.92967(2) 0.22763(2) 0.04129(13) Uani 1 1 d . . . O1W O 0.15762(19) 0.54856(10) 0.21796(13) 0.0850(7) Uani 1 1 d . . . O2WA O 1.0843(4) 0.8727(2) 0.2914(4) 0.0637(18) Uiso 0.476(11) 1 d P B 1 O2WB O 1.0628(3) 0.86623(16) 0.2575(3) 0.0488(14) Uiso 0.524(11) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01752(7) 0.01652(6) 0.01787(6) -0.00078(4) 0.00606(5) 0.00003(4) C1 0.0202(8) 0.0222(8) 0.0208(8) -0.0035(6) 0.0068(6) 0.0010(6) N1 0.0241(8) 0.0212(7) 0.0270(7) -0.0032(6) 0.0093(6) -0.0014(6) C2 0.0220(8) 0.0191(8) 0.0234(8) -0.0014(6) 0.0092(6) -0.0040(6) C3 0.0296(9) 0.0231(8) 0.0185(8) 0.0005(6) 0.0036(7) -0.0067(7) C4 0.0288(9) 0.0222(8) 0.0231(8) -0.0015(7) 0.0036(7) -0.0085(7) C5 0.0339(11) 0.0217(9) 0.0379(11) 0.0041(8) -0.0012(8) -0.0053(8) C6 0.0476(13) 0.0330(10) 0.0250(9) 0.0095(8) -0.0047(8) -0.0107(9) C7 0.0329(10) 0.0278(9) 0.0201(8) -0.0020(7) 0.0005(7) -0.0088(8) C8 0.0188(8) 0.0196(8) 0.0197(8) -0.0020(6) 0.0031(6) -0.0041(6) N2 0.0184(7) 0.0206(7) 0.0235(7) -0.0035(5) 0.0033(5) -0.0019(6) C9 0.0223(8) 0.0194(8) 0.0247(8) -0.0038(6) 0.0065(7) 0.0040(6) C10 0.0263(9) 0.0309(9) 0.0289(9) 0.0101(7) 0.0074(7) 0.0078(8) C11 0.0257(9) 0.0512(12) 0.0202(8) 0.0031(8) 0.0015(7) -0.0035(9) C12 0.0243(10) 0.0509(13) 0.0317(10) -0.0016(9) 0.0029(8) -0.0112(9) C13 0.0280(10) 0.0319(10) 0.0319(10) 0.0040(8) 0.0096(8) -0.0058(8) C14 0.0246(9) 0.0338(10) 0.0193(8) 0.0015(7) 0.0065(7) 0.0037(7) C15 0.0210(8) 0.0219(8) 0.0190(7) -0.0004(6) 0.0052(6) 0.0028(6) N3 0.0251(7) 0.0225(7) 0.0211(7) 0.0010(6) 0.0071(6) -0.0006(6) C16 0.0269(9) 0.0191(8) 0.0191(8) 0.0018(6) 0.0072(7) -0.0042(6) C17 0.0308(9) 0.0223(8) 0.0211(8) 0.0026(7) 0.0048(7) 0.0020(7) C18 0.0430(11) 0.0220(9) 0.0216(8) 0.0051(7) 0.0065(8) -0.0029(8) C19 0.0370(10) 0.0289(9) 0.0196(8) 0.0035(7) 0.0080(7) -0.0078(8) C20 0.0277(9) 0.0327(10) 0.0202(8) 0.0023(7) 0.0073(7) -0.0061(7) C21 0.0261(9) 0.0235(8) 0.0208(8) 0.0040(6) 0.0071(7) 0.0001(7) C22 0.0252(9) 0.0218(8) 0.0216(8) 0.0032(6) 0.0101(7) -0.0001(7) N4 0.0299(8) 0.0218(7) 0.0267(7) 0.0034(6) 0.0152(6) 0.0022(6) C23 0.0296(9) 0.0186(8) 0.0289(9) 0.0018(7) 0.0152(7) 0.0053(7) C24 0.0250(9) 0.0263(9) 0.0237(8) -0.0041(7) 0.0081(7) 0.0011(7) C25 0.0235(9) 0.0311(9) 0.0194(8) 0.0036(7) 0.0062(7) 0.0004(7) C26 0.0228(9) 0.0305(9) 0.0272(9) 0.0018(7) 0.0101(7) 0.0002(7) C27 0.0207(8) 0.0351(10) 0.0240(9) -0.0050(7) 0.0043(7) -0.0007(7) C28 0.0322(10) 0.0300(9) 0.0206(8) 0.0038(7) 0.0090(7) 0.0097(8) Rh2 0.01694(7) 0.02007(7) 0.01836(6) -0.00423(4) 0.00763(5) -0.00102(5) C36 0.0158(8) 0.0293(9) 0.0190(8) -0.0048(6) 0.0040(6) -0.0009(7) N6 0.0187(7) 0.0313(8) 0.0207(7) -0.0048(6) 0.0041(6) 0.0039(6) C37 0.0208(8) 0.0281(9) 0.0195(8) -0.0029(6) 0.0046(6) 0.0090(7) C38 0.0233(9) 0.0356(10) 0.0343(10) -0.0125(8) 0.0110(8) 0.0006(8) C39 0.0211(9) 0.0416(11) 0.0292(9) -0.0080(8) 0.0089(7) 0.0063(8) C40 0.0288(9) 0.0335(10) 0.0243(9) -0.0067(7) 0.0074(7) 0.0094(8) C41 0.0309(10) 0.0272(9) 0.0433(11) -0.0118(8) 0.0110(9) 0.0032(8) C42 0.0213(9) 0.0291(9) 0.0348(10) -0.0087(8) 0.0072(7) 0.0019(7) C43 0.0168(8) 0.0219(8) 0.0179(7) -0.0016(6) 0.0036(6) 0.0042(6) N7 0.0188(7) 0.0229(7) 0.0209(7) -0.0007(5) 0.0052(5) 0.0009(6) C44 0.0204(8) 0.0187(7) 0.0194(7) 0.0019(6) 0.0055(6) -0.0012(6) C45 0.0219(8) 0.0198(8) 0.0230(8) -0.0049(6) 0.0075(7) -0.0015(6) C46 0.0249(9) 0.0307(9) 0.0197(8) -0.0031(7) 0.0047(7) 0.0005(7) C47 0.0241(9) 0.0341(10) 0.0295(9) -0.0018(8) 0.0039(7) 0.0069(8) C48 0.0282(9) 0.0226(8) 0.0323(9) -0.0038(7) 0.0109(8) 0.0042(7) C49 0.0241(8) 0.0250(8) 0.0199(8) -0.0035(6) 0.0092(7) -0.0040(7) C50 0.0285(9) 0.0220(8) 0.0178(8) -0.0020(6) 0.0060(7) -0.0004(7) N8 0.0327(8) 0.0237(7) 0.0207(7) -0.0042(6) 0.0039(6) 0.0054(6) C51 0.0295(9) 0.0167(8) 0.0213(8) -0.0047(6) 0.0050(7) 0.0049(7) C52 0.0354(10) 0.0175(8) 0.0232(8) -0.0024(6) 0.0061(7) -0.0013(7) C53 0.0287(10) 0.0288(9) 0.0296(9) 0.0000(7) 0.0088(8) 0.0010(7) C54 0.0321(10) 0.0304(10) 0.0250(9) -0.0010(7) 0.0035(7) 0.0090(8) C55 0.0427(11) 0.0190(8) 0.0252(9) 0.0026(7) 0.0096(8) 0.0067(8) C56 0.0328(10) 0.0222(8) 0.0258(9) 0.0005(7) 0.0092(7) 0.0013(7) C57 0.0382(12) 0.0333(11) 0.0705(16) -0.0023(11) 0.0319(11) -0.0067(9) C58 0.0429(12) 0.0275(10) 0.0721(16) -0.0088(10) 0.0384(12) -0.0091(9) C59 0.0440(13) 0.0313(11) 0.0660(15) -0.0082(10) 0.0322(12) -0.0128(9) Cl1 0.0387(2) 0.01968(19) 0.0259(2) -0.00102(16) 0.00222(18) -0.00695(17) Cl2 0.0573(3) 0.0377(3) 0.0283(2) 0.00102(19) 0.0102(2) -0.0243(2) O1W 0.0735(15) 0.0649(14) 0.1015(18) 0.0098(13) -0.0029(13) -0.0084(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C22 1.9634(17) . ? Rh1 C15 1.9724(17) . ? Rh1 C8 1.9727(17) . ? Rh1 C1 1.9779(17) . ? Rh1 Rh2 3.2874(2) . ? C1 N1 1.149(2) . ? N1 C2 1.451(2) . ? C2 C7 1.524(2) . ? C2 C3 1.528(2) . ? C2 H2 1.0000 . ? C3 C4 1.529(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.533(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N2 1.149(2) . ? N2 C9 1.451(2) . ? C9 C14 1.526(2) . ? C9 C10 1.526(2) . ? C9 H9 1.0000 . ? C10 C11 1.520(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.530(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.524(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N3 1.152(2) . ? N3 C16 1.450(2) . ? C16 C21 1.526(2) . ? C16 C17 1.529(2) . ? C16 H16 1.0000 . ? C17 C18 1.530(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.525(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.528(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N4 1.151(2) . ? N4 C23 1.453(2) . ? C23 C28 1.521(3) . ? C23 C24 1.525(2) . ? C23 H23 1.0000 . ? C24 C25 1.529(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.529(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.533(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.520(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? Rh2 C29A 1.957(3) . ? Rh2 C36 1.9724(17) . ? Rh2 C50 1.9742(18) . ? Rh2 C43 1.9748(17) . ? Rh2 C29B 1.999(4) . ? C29A N5A 1.157(4) . ? N5A C30A 1.453(4) . ? C30A C31A 1.518(5) . ? C30A C35A 1.538(5) . ? C30A H30A 1.0000 . ? C31A C32A 1.487(5) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A C33A 1.547(5) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.508(5) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A C35A 1.504(5) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C29B N5B 1.148(5) . ? N5B C30B 1.441(6) . ? C30B C35B 1.540(6) . ? C30B C31B 1.591(7) . ? C30B H30B 1.0000 . ? C31B C32B 1.471(7) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B C33B 1.532(7) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.556(7) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35B 1.503(8) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36 N6 1.151(2) . ? N6 C37 1.451(2) . ? C37 C42 1.522(2) . ? C37 C38 1.528(3) . ? C37 H37 1.0000 . ? C38 C39 1.532(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.522(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.522(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.529(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N7 1.152(2) . ? N7 C44 1.453(2) . ? C44 C45 1.527(2) . ? C44 C49 1.530(2) . ? C44 H44 1.0000 . ? C45 C46 1.525(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.527(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.524(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.522(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 N8 1.147(2) . ? N8 C51 1.451(2) . ? C51 C52 1.523(3) . ? C51 C56 1.527(2) . ? C51 H51 1.0000 . ? C52 C53 1.520(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.526(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.523(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.528(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.377(4) . ? C57 C59 1.403(3) 3_776 ? C57 H57 0.9500 . ? C58 C59 1.385(4) . ? C58 H58 0.9500 . ? C59 C57 1.403(3) 3_776 ? C59 H59 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 C22 Rh1 C15 89.46(7) . . ? C22 Rh1 C8 173.79(7) . . ? C15 Rh1 C8 91.84(7) . . ? C22 Rh1 C1 85.18(7) . . ? C15 Rh1 C1 173.27(7) . . ? C8 Rh1 C1 93.06(7) . . ? C22 Rh1 Rh2 110.99(5) . . ? C15 Rh1 Rh2 106.37(5) . . ? C8 Rh1 Rh2 74.44(5) . . ? C1 Rh1 Rh2 79.42(5) . . ? N1 C1 Rh1 172.44(15) . . ? C1 N1 C2 172.56(17) . . ? N1 C2 C7 109.47(14) . . ? N1 C2 C3 109.49(13) . . ? C7 C2 C3 110.97(15) . . ? N1 C2 H2 109.0 . . ? C7 C2 H2 109.0 . . ? C3 C2 H2 109.0 . . ? C2 C3 C4 109.40(14) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 111.32(15) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 110.24(17) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 110.86(16) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C2 C7 C6 108.90(15) . . ? C2 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? C2 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N2 C8 Rh1 177.74(15) . . ? C8 N2 C9 171.25(17) . . ? N2 C9 C14 108.50(14) . . ? N2 C9 C10 109.29(14) . . ? C14 C9 C10 110.94(15) . . ? N2 C9 H9 109.4 . . ? C14 C9 H9 109.4 . . ? C10 C9 H9 109.4 . . ? C11 C10 C9 111.66(15) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.32(16) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 111.40(16) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 111.50(17) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C9 C14 C13 111.65(14) . . ? C9 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C9 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N3 C15 Rh1 176.17(15) . . ? C15 N3 C16 175.96(17) . . ? N3 C16 C21 109.59(14) . . ? N3 C16 C17 110.61(15) . . ? C21 C16 C17 110.82(14) . . ? N3 C16 H16 108.6 . . ? C21 C16 H16 108.6 . . ? C17 C16 H16 108.6 . . ? C16 C17 C18 109.14(15) . . ? C16 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? C16 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 111.67(15) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 111.31(15) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 110.38(15) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C16 C21 C20 109.67(14) . . ? C16 C21 H21A 109.7 . . ? C20 C21 H21A 109.7 . . ? C16 C21 H21B 109.7 . . ? C20 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N4 C22 Rh1 175.28(17) . . ? C22 N4 C23 173.28(17) . . ? N4 C23 C28 108.74(15) . . ? N4 C23 C24 108.55(14) . . ? C28 C23 C24 111.42(14) . . ? N4 C23 H23 109.4 . . ? C28 C23 H23 109.4 . . ? C24 C23 H23 109.4 . . ? C23 C24 C25 111.28(14) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.11(15) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 111.14(14) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 110.95(15) . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C23 112.02(15) . . ? C27 C28 H28A 109.2 . . ? C23 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C23 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C29A Rh2 C36 84.00(10) . . ? C29A Rh2 C50 96.37(10) . . ? C36 Rh2 C50 172.52(7) . . ? C29A Rh2 C43 173.65(11) . . ? C36 Rh2 C43 91.27(7) . . ? C50 Rh2 C43 88.88(7) . . ? C29A Rh2 C29B 17.61(12) . . ? C36 Rh2 C29B 93.87(13) . . ? C50 Rh2 C29B 84.69(13) . . ? C43 Rh2 C29B 168.44(14) . . ? C29A Rh2 Rh1 96.14(9) . . ? C36 Rh2 Rh1 110.69(5) . . ? C50 Rh2 Rh1 76.73(5) . . ? C43 Rh2 Rh1 81.55(5) . . ? C29B Rh2 Rh1 106.19(12) . . ? N5A C29A Rh2 176.3(3) . . ? C29A N5A C30A 173.5(3) . . ? N5A C30A C31A 109.5(3) . . ? N5A C30A C35A 108.1(3) . . ? C31A C30A C35A 110.9(3) . . ? N5A C30A H30A 109.5 . . ? C31A C30A H30A 109.5 . . ? C35A C30A H30A 109.5 . . ? C32A C31A C30A 113.3(3) . . ? C32A C31A H31A 108.9 . . ? C30A C31A H31A 108.9 . . ? C32A C31A H31B 108.9 . . ? C30A C31A H31B 108.9 . . ? H31A C31A H31B 107.7 . . ? C31A C32A C33A 111.2(3) . . ? C31A C32A H32A 109.4 . . ? C33A C32A H32A 109.4 . . ? C31A C32A H32B 109.4 . . ? C33A C32A H32B 109.4 . . ? H32A C32A H32B 108.0 . . ? C34A C33A C32A 112.8(3) . . ? C34A C33A H33A 109.0 . . ? C32A C33A H33A 109.0 . . ? C34A C33A H33B 109.0 . . ? C32A C33A H33B 109.0 . . ? H33A C33A H33B 107.8 . . ? C35A C34A C33A 110.4(3) . . ? C35A C34A H34A 109.6 . . ? C33A C34A H34A 109.6 . . ? C35A C34A H34B 109.6 . . ? C33A C34A H34B 109.6 . . ? H34A C34A H34B 108.1 . . ? C34A C35A C30A 112.6(3) . . ? C34A C35A H35A 109.1 . . ? C30A C35A H35A 109.1 . . ? C34A C35A H35B 109.1 . . ? C30A C35A H35B 109.1 . . ? H35A C35A H35B 107.8 . . ? N5B C29B Rh2 178.6(4) . . ? C29B N5B C30B 175.6(4) . . ? N5B C30B C35B 109.1(4) . . ? N5B C30B C31B 107.6(4) . . ? C35B C30B C31B 111.8(4) . . ? N5B C30B H30B 109.4 . . ? C35B C30B H30B 109.4 . . ? C31B C30B H30B 109.4 . . ? C32B C31B C30B 111.8(4) . . ? C32B C31B H31C 109.3 . . ? C30B C31B H31C 109.3 . . ? C32B C31B H31D 109.3 . . ? C30B C31B H31D 109.3 . . ? H31C C31B H31D 107.9 . . ? C31B C32B C33B 113.2(4) . . ? C31B C32B H32C 108.9 . . ? C33B C32B H32C 108.9 . . ? C31B C32B H32D 108.9 . . ? C33B C32B H32D 108.9 . . ? H32C C32B H32D 107.7 . . ? C32B C33B C34B 111.9(4) . . ? C32B C33B H33C 109.2 . . ? C34B C33B H33C 109.2 . . ? C32B C33B H33D 109.2 . . ? C34B C33B H33D 109.2 . . ? H33C C33B H33D 107.9 . . ? C35B C34B C33B 110.0(4) . . ? C35B C34B H34C 109.7 . . ? C33B C34B H34C 109.7 . . ? C35B C34B H34D 109.7 . . ? C33B C34B H34D 109.7 . . ? H34C C34B H34D 108.2 . . ? C34B C35B C30B 112.5(4) . . ? C34B C35B H35C 109.1 . . ? C30B C35B H35C 109.1 . . ? C34B C35B H35D 109.1 . . ? C30B C35B H35D 109.1 . . ? H35C C35B H35D 107.8 . . ? N6 C36 Rh2 176.21(16) . . ? C36 N6 C37 179.39(19) . . ? N6 C37 C42 109.68(14) . . ? N6 C37 C38 110.05(15) . . ? C42 C37 C38 111.23(15) . . ? N6 C37 H37 108.6 . . ? C42 C37 H37 108.6 . . ? C38 C37 H37 108.6 . . ? C37 C38 C39 108.81(16) . . ? C37 C38 H38A 109.9 . . ? C39 C38 H38A 109.9 . . ? C37 C38 H38B 109.9 . . ? C39 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? C40 C39 C38 110.93(15) . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C39 111.29(15) . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 111.22(16) . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 109.43(15) . . ? C37 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? C37 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? N7 C43 Rh2 178.59(15) . . ? C43 N7 C44 174.13(16) . . ? N7 C44 C45 110.52(13) . . ? N7 C44 C49 109.04(13) . . ? C45 C44 C49 111.76(14) . . ? N7 C44 H44 108.5 . . ? C45 C44 H44 108.5 . . ? C49 C44 H44 108.5 . . ? C46 C45 C44 112.41(14) . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? C44 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? C45 C46 C47 110.46(14) . . ? C45 C46 H46A 109.6 . . ? C47 C46 H46A 109.6 . . ? C45 C46 H46B 109.6 . . ? C47 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C46 110.05(15) . . ? C48 C47 H47A 109.6 . . ? C46 C47 H47A 109.6 . . ? C48 C47 H47B 109.6 . . ? C46 C47 H47B 109.6 . . ? H47A C47 H47B 108.2 . . ? C49 C48 C47 111.24(15) . . ? C49 C48 H48A 109.4 . . ? C47 C48 H48A 109.4 . . ? C49 C48 H48B 109.4 . . ? C47 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C48 C49 C44 112.01(14) . . ? C48 C49 H49A 109.2 . . ? C44 C49 H49A 109.2 . . ? C48 C49 H49B 109.2 . . ? C44 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? N8 C50 Rh2 175.93(16) . . ? C50 N8 C51 171.97(19) . . ? N8 C51 C52 108.27(14) . . ? N8 C51 C56 110.17(15) . . ? C52 C51 C56 112.11(15) . . ? N8 C51 H51 108.7 . . ? C52 C51 H51 108.7 . . ? C56 C51 H51 108.7 . . ? C53 C52 C51 110.18(14) . . ? C53 C52 H52A 109.6 . . ? C51 C52 H52A 109.6 . . ? C53 C52 H52B 109.6 . . ? C51 C52 H52B 109.6 . . ? H52A C52 H52B 108.1 . . ? C52 C53 C54 110.84(15) . . ? C52 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 108.1 . . ? C55 C54 C53 110.22(15) . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54B 109.6 . . ? C53 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 112.19(15) . . ? C54 C55 H55A 109.2 . . ? C56 C55 H55A 109.2 . . ? C54 C55 H55B 109.2 . . ? C56 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C51 C56 C55 109.90(15) . . ? C51 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? C51 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C58 C57 C59 119.9(2) . 3_776 ? C58 C57 H57 120.1 . . ? C59 C57 H57 120.1 3_776 . ? C57 C58 C59 120.7(2) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C58 C59 C57 119.4(2) . 3_776 ? C58 C59 H59 120.3 . . ? C57 C59 H59 120.3 3_776 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.272 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.061 #===END data_dp135 _database_code_depnum_ccdc_archive 'CCDC 285151' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Rh3(CN-iPr)12]Cl3.4.5H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H91 Cl3 N12 O4.50 Rh3' _chemical_formula_weight 1323.41 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 21.5193(6) _cell_length_b 22.7979(6) _cell_length_c 14.0456(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6890.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6684 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 23.9 _exptl_crystal_description green _exptl_crystal_colour block _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 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.918 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _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 Apex2' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106793 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6591 _reflns_number_gt 5126 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT 7.12 (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (sheldrick, 1994)' _computing_publication_material SHELXL97 _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. ; _publ_section_exptl_refinement ;The unusually high thermal motion depicted in the thermal ellipsoid plots is a result of an incipient phase change which caused the crystals to crack when they were cooled to the customary 90 K. To avoid this, the cold stream was adjusted to 180 K; however, subsequent refinement of the structure indicates that some instability in the structure was already present at this temperature. All attempts to refine the isopropyl iso- cyanides using split positions failed to yield reasonable geometry or lower the R value. There is disorder in the water molecules and some of the water hydrogen atoms were not located. ; _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^)+(0.0562P)^2^+9.7109P] 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 6591 _refine_ls_number_parameters 369 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.042 _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 0.63433(2) 0.216057(19) 0.0000 0.04140(13) Uani 1 2 d S . . Rh2 Rh 0.77773(2) 0.229645(17) 0.0000 0.03953(13) Uani 1 2 d S . . Rh3 Rh 0.91382(2) 0.270602(19) 0.0000 0.04322(13) Uani 1 2 d S . . N1 N 0.6418(3) 0.0807(2) 0.0000 0.0632(14) Uani 1 2 d SU . . N2 N 0.6308(2) 0.21112(19) 0.2207(3) 0.0713(12) Uani 1 1 d U . . N3 N 0.5965(2) 0.3478(2) 0.0000 0.0595(14) Uani 1 2 d SU . . N4 N 0.80153(18) 0.13892(16) 0.1615(3) 0.0614(10) Uani 1 1 d U . . N5 N 0.75410(18) 0.32154(19) 0.1594(3) 0.0736(12) Uani 1 1 d U . . N6 N 0.9763(3) 0.1479(3) 0.0000 0.0798(19) Uani 1 2 d SU . . N7 N 0.9183(2) 0.2730(2) 0.2205(3) 0.0779(13) Uani 1 1 d U . . N8 N 0.8823(3) 0.4035(2) 0.0000 0.0720(17) Uani 1 2 d SU . . C1 C 0.6415(3) 0.1310(3) 0.0000 0.0489(14) Uani 1 2 d SU . . C2 C 0.6360(4) 0.0171(3) 0.0000 0.093(3) Uani 1 2 d SU . . H2 H 0.6784 -0.0007 0.0000 0.112 Uiso 1 2 calc SR . . C3 C 0.6027(4) -0.0007(3) 0.0899(6) 0.132(3) Uani 1 1 d U . . H3A H 0.6254 0.0144 0.1452 0.198 Uiso 1 1 calc R . . H3B H 0.6005 -0.0436 0.0934 0.198 Uiso 1 1 calc R . . H3C H 0.5605 0.0156 0.0896 0.198 Uiso 1 1 calc R . . C4 C 0.6321(2) 0.21387(19) 0.1392(3) 0.0518(10) Uani 1 1 d U . . C5 C 0.6283(5) 0.2057(4) 0.3243(4) 0.139(3) Uani 1 1 d U . . H5 H 0.6701 0.2041 0.3550 0.166 Uiso 1 1 calc R . . C6 C 0.5878(6) 0.1524(5) 0.3463(7) 0.212(6) Uani 1 1 d U . . H6A H 0.5748 0.1536 0.4131 0.318 Uiso 1 1 calc R . . H6B H 0.6116 0.1164 0.3347 0.318 Uiso 1 1 calc R . . H6C H 0.5510 0.1528 0.3052 0.318 Uiso 1 1 calc R . . C7 C 0.5881(6) 0.2530(5) 0.3621(6) 0.199(5) Uani 1 1 d U . . H7A H 0.5552 0.2618 0.3160 0.298 Uiso 1 1 calc R . . H7B H 0.6131 0.2883 0.3731 0.298 Uiso 1 1 calc R . . H7C H 0.5694 0.2403 0.4223 0.298 Uiso 1 1 calc R . . C8 C 0.6118(3) 0.3001(3) 0.0000 0.0468(13) Uani 1 2 d SU . . C9 C 0.5787(4) 0.4090(3) 0.0000 0.099(3) Uani 1 2 d SU . . H9 H 0.6173 0.4334 0.0000 0.119 Uiso 1 2 calc SR . . C10 C 0.5419(4) 0.4232(3) 0.0884(6) 0.139(3) Uani 1 1 d U . . H10A H 0.5004 0.4058 0.0834 0.208 Uiso 1 1 calc R . . H10B H 0.5381 0.4659 0.0948 0.208 Uiso 1 1 calc R . . H10C H 0.5632 0.4073 0.1443 0.208 Uiso 1 1 calc R . . C11 C 0.79296(19) 0.17120(18) 0.1007(3) 0.0497(10) Uani 1 1 d U . . C12 C 0.8082(3) 0.0976(3) 0.2405(4) 0.0861(17) Uani 1 1 d U . . H12 H 0.8064 0.1203 0.3014 0.103 Uiso 1 1 calc R . . C13 C 0.8704(4) 0.0681(4) 0.2351(6) 0.143(3) Uani 1 1 d U . . H13A H 0.9033 0.0978 0.2373 0.214 Uiso 1 1 calc R . . H13B H 0.8734 0.0461 0.1753 0.214 Uiso 1 1 calc R . . H13C H 0.8751 0.0412 0.2890 0.214 Uiso 1 1 calc R . . C14 C 0.7545(4) 0.0564(3) 0.2385(5) 0.122(2) Uani 1 1 d U . . H14A H 0.7157 0.0787 0.2357 0.182 Uiso 1 1 calc R . . H14B H 0.7549 0.0321 0.2961 0.182 Uiso 1 1 calc R . . H14C H 0.7577 0.0311 0.1823 0.182 Uiso 1 1 calc R . . C15 C 0.76263(19) 0.28843(18) 0.0993(3) 0.0514(10) Uani 1 1 d U . . C16 C 0.7433(3) 0.3630(3) 0.2358(6) 0.115(3) Uani 1 1 d U . . H16 H 0.7429 0.3371 0.2934 0.138 Uiso 1 1 calc R . . C17 C 0.7968(3) 0.3986(3) 0.2517(6) 0.127(3) Uani 1 1 d U . . H17A H 0.8337 0.3736 0.2566 0.190 Uiso 1 1 calc R . . H17B H 0.7916 0.4208 0.3109 0.190 Uiso 1 1 calc R . . H17C H 0.8019 0.4259 0.1983 0.190 Uiso 1 1 calc R . . C18 C 0.6820(3) 0.3859(3) 0.2349(5) 0.0915(18) Uani 1 1 d U . . H18A H 0.6746 0.4082 0.2934 0.137 Uiso 1 1 calc R . . H18B H 0.6521 0.3535 0.2309 0.137 Uiso 1 1 calc R . . H18C H 0.6768 0.4117 0.1797 0.137 Uiso 1 1 calc R . . C19 C 0.9517(3) 0.1921(3) 0.0000 0.0537(15) Uani 1 2 d SU . . C20 C 1.0127(6) 0.0952(5) 0.0000 0.137(5) Uani 1 2 d SU . . H20 H 0.9784 0.0656 0.0000 0.165 Uiso 1 2 calc SR . . C21 C 1.0399(3) 0.0819(3) 0.0891(4) 0.0888(17) Uani 1 1 d U . . H21A H 1.0075 0.0797 0.1378 0.133 Uiso 1 1 calc R . . H21B H 1.0697 0.1127 0.1060 0.133 Uiso 1 1 calc R . . H21C H 1.0615 0.0442 0.0850 0.133 Uiso 1 1 calc R . . C22 C 0.9164(2) 0.27197(19) 0.1396(3) 0.0555(11) Uani 1 1 d U . . C23 C 0.9221(5) 0.2737(4) 0.3248(5) 0.137(3) Uani 1 1 d U . . H23A H 0.8799 0.2748 0.3545 0.165 Uiso 1 1 calc R . . C24 C 0.9578(6) 0.2199(4) 0.3551(6) 0.190(5) Uani 1 1 d U . . H24A H 0.9314 0.1851 0.3483 0.285 Uiso 1 1 calc R . . H24B H 0.9706 0.2240 0.4217 0.285 Uiso 1 1 calc R . . H24C H 0.9948 0.2155 0.3148 0.285 Uiso 1 1 calc R . . C25 C 0.9615(4) 0.3297(4) 0.3526(6) 0.159(4) Uani 1 1 d U . . H25A H 0.9442 0.3643 0.3208 0.238 Uiso 1 1 calc R . . H25B H 1.0047 0.3241 0.3325 0.238 Uiso 1 1 calc R . . H25C H 0.9600 0.3353 0.4217 0.238 Uiso 1 1 calc R . . C26 C 0.8924(3) 0.3541(3) 0.0000 0.0537(15) Uani 1 2 d SU . . C27 C 0.8715(5) 0.4660(3) 0.0000 0.127(4) Uani 1 2 d SU . . H27 H 0.8257 0.4736 0.0000 0.153 Uiso 1 2 calc SR . . C28 C 0.8996(5) 0.4920(3) 0.0876(8) 0.185(5) Uani 1 1 d U . . H28A H 0.8771 0.4780 0.1438 0.278 Uiso 1 1 calc R . . H28B H 0.8968 0.5349 0.0844 0.278 Uiso 1 1 calc R . . H28C H 0.9433 0.4803 0.0920 0.278 Uiso 1 1 calc R . . Cl1 Cl 0.71175(10) 0.50029(9) 0.0000 0.0892(6) Uani 1 2 d S . . Cl2 Cl 0.78159(11) -0.05589(12) 0.0000 0.0981(7) Uani 1 2 d S . . Cl3 Cl 0.78627(19) 0.22603(13) 0.4221(3) 0.1052(11) Uani 0.50 1 d P . . O1 O 0.8778(5) 0.1111(4) 0.5000 0.141(3) Uiso 1 2 d SD . . H1 H 0.865(3) 0.130(2) 0.4538(4) 0.169 Uiso 1 1 d D . . O2 O 0.8349(5) 0.3551(4) 0.5000 0.144(3) Uiso 1 2 d SD . . H2A H 0.820(3) 0.338(3) 0.4538(4) 0.173 Uiso 1 1 d D . . O3 O 0.8674(5) 0.0406(5) 0.0000 0.078(3) Uiso 0.50 2 d SP . . O4 O 0.7058(4) 0.1124(4) 0.4684(6) 0.107(3) Uiso 0.50 1 d PD . . H4 H 0.726(3) 0.134(2) 0.434(4) 0.129 Uiso 1 1 d D . . O5A O 0.8260(7) -0.1792(7) 0.0000 0.109(4) Uiso 0.50 2 d SP . . O5B O 0.8043(10) -0.1979(10) -0.0460(16) 0.122(7) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0459(2) 0.0382(2) 0.0401(2) 0.000 0.000 0.00066(19) Rh2 0.0458(2) 0.0296(2) 0.0432(2) 0.000 0.000 0.00140(18) Rh3 0.0452(3) 0.0405(3) 0.0440(3) 0.000 0.000 0.00722(19) N1 0.062(3) 0.042(3) 0.085(4) 0.000 0.000 -0.001(3) N2 0.087(3) 0.083(3) 0.044(2) 0.006(2) 0.007(2) 0.023(2) N3 0.050(3) 0.044(3) 0.084(4) 0.000 0.000 0.007(2) N4 0.076(3) 0.051(2) 0.058(2) 0.0127(19) 0.005(2) 0.0094(18) N5 0.059(2) 0.076(3) 0.086(3) -0.039(2) 0.003(2) 0.005(2) N6 0.113(5) 0.064(4) 0.062(4) 0.000 0.000 0.042(4) N7 0.089(3) 0.095(4) 0.050(2) -0.009(2) -0.008(2) 0.022(2) N8 0.057(3) 0.046(3) 0.113(5) 0.000 0.000 0.000(3) C1 0.046(3) 0.044(3) 0.057(4) 0.000 0.000 -0.001(3) C2 0.068(5) 0.037(3) 0.174(9) 0.000 0.000 0.006(3) C3 0.127(6) 0.075(4) 0.195(8) 0.058(5) 0.002(6) -0.017(4) C4 0.052(2) 0.052(2) 0.051(2) 0.001(2) 0.000(2) 0.006(2) C5 0.227(10) 0.140(6) 0.048(3) 0.012(4) 0.013(5) 0.072(6) C6 0.319(15) 0.178(8) 0.139(8) 0.100(7) 0.106(9) 0.072(8) C7 0.287(15) 0.207(8) 0.102(6) -0.036(7) 0.077(8) 0.029(9) C8 0.045(3) 0.043(3) 0.052(3) 0.000 0.000 0.002(3) C9 0.072(5) 0.044(4) 0.182(9) 0.000 0.000 0.015(4) C10 0.142(7) 0.109(5) 0.166(7) -0.058(5) -0.028(5) 0.071(5) C11 0.053(2) 0.042(2) 0.055(2) -0.0016(19) 0.005(2) 0.0009(18) C12 0.131(5) 0.072(3) 0.056(3) 0.022(3) 0.000(3) 0.023(3) C13 0.158(6) 0.139(7) 0.132(7) 0.046(6) -0.013(6) 0.074(5) C14 0.179(6) 0.083(4) 0.103(5) 0.040(4) 0.017(5) -0.021(4) C15 0.046(2) 0.045(2) 0.063(3) -0.007(2) 0.000(2) -0.0003(18) C16 0.078(4) 0.132(6) 0.135(6) -0.089(5) 0.002(4) 0.009(4) C17 0.097(4) 0.134(6) 0.150(7) -0.091(6) -0.013(5) -0.003(4) C18 0.084(4) 0.098(4) 0.092(4) -0.031(4) 0.012(3) 0.017(3) C19 0.063(4) 0.049(3) 0.049(3) 0.000 0.000 0.012(3) C20 0.232(13) 0.106(7) 0.074(5) 0.000 0.000 0.119(8) C21 0.091(4) 0.080(4) 0.095(4) 0.005(3) -0.015(3) 0.027(3) C22 0.053(3) 0.059(3) 0.054(3) -0.004(2) -0.006(2) 0.013(2) C23 0.168(8) 0.190(8) 0.055(3) -0.024(5) -0.014(4) 0.027(6) C24 0.285(14) 0.192(8) 0.093(6) 0.050(6) -0.062(8) -0.006(8) C25 0.174(8) 0.198(8) 0.105(6) -0.078(6) -0.050(6) 0.053(6) C26 0.041(3) 0.046(3) 0.075(4) 0.000 0.000 0.000(3) C27 0.093(7) 0.040(4) 0.249(13) 0.000 0.000 0.004(4) C28 0.186(9) 0.089(5) 0.281(12) -0.079(7) 0.025(9) -0.034(6) Cl1 0.0960(15) 0.0674(11) 0.1042(15) 0.000 0.000 -0.0139(10) Cl2 0.0937(16) 0.1074(17) 0.0931(15) 0.000 0.000 0.0104(13) Cl3 0.145(3) 0.075(2) 0.095(2) 0.0006(17) 0.031(2) -0.0134(18) _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 1.946(6) . ? Rh1 C4 1.956(4) . ? Rh1 C4 1.956(4) 6 ? Rh1 C8 1.976(6) . ? Rh1 Rh2 3.1012(6) . ? Rh2 C15 1.962(4) . ? Rh2 C15 1.962(4) 6 ? Rh2 C11 1.970(4) 6 ? Rh2 C11 1.970(4) . ? Rh2 Rh3 3.0739(6) . ? Rh3 C26 1.960(6) . ? Rh3 C22 1.962(5) . ? Rh3 C22 1.962(5) 6 ? Rh3 C19 1.966(6) . ? N1 C1 1.145(7) . ? N1 C2 1.456(8) . ? N2 C4 1.147(6) . ? N2 C5 1.462(7) . ? N3 C8 1.137(7) . ? N3 C9 1.446(8) . ? N4 C11 1.142(5) . ? N4 C12 1.463(6) . ? N5 C15 1.147(5) . ? N5 C16 1.449(7) . ? N6 C19 1.140(8) . ? N6 C20 1.433(9) . ? N7 C22 1.137(6) . ? N7 C23 1.468(8) . ? N8 C26 1.145(8) . ? N8 C27 1.444(9) . ? C2 C3 1.507(8) 6 ? C2 C3 1.507(8) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 C7 1.480(12) . ? C5 C6 1.527(14) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.509(8) . ? C9 C10 1.509(8) 6 ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C14 1.491(9) . ? C12 C13 1.500(9) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C18 1.420(8) . ? C16 C17 1.426(8) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 C21 1.415(7) . ? C20 C21 1.415(7) 6 ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.510(12) . ? C23 C25 1.581(12) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.494(10) . ? C27 C28 1.495(10) 6 ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Cl3 Cl3 2.188(8) 6_556 ? O1 H1 0.826(10) . ? O2 H2A 0.826(10) . ? O4 O4 0.888(18) 6_556 ? O4 H4 0.821(10) . ? O5A O5B 0.90(2) 6 ? O5A O5B 0.90(2) . ? O5B O5B 1.29(4) 6 ? 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 C4 88.65(13) . . ? C1 Rh1 C4 88.65(13) . 6 ? C4 Rh1 C4 175.9(3) . 6 ? C1 Rh1 C8 170.3(2) . . ? C4 Rh1 C8 91.07(12) . . ? C4 Rh1 C8 91.07(12) 6 . ? C1 Rh1 Rh2 91.22(17) . . ? C4 Rh1 Rh2 91.55(13) . . ? C4 Rh1 Rh2 91.54(13) 6 . ? C8 Rh1 Rh2 98.47(17) . . ? C15 Rh2 C15 90.7(3) . 6 ? C15 Rh2 C11 179.46(18) . 6 ? C15 Rh2 C11 88.80(18) 6 6 ? C15 Rh2 C11 88.80(18) . . ? C15 Rh2 C11 179.46(18) 6 . ? C11 Rh2 C11 91.7(2) 6 . ? C15 Rh2 Rh3 87.15(12) . . ? C15 Rh2 Rh3 87.15(12) 6 . ? C11 Rh2 Rh3 92.69(12) 6 . ? C11 Rh2 Rh3 92.69(12) . . ? C15 Rh2 Rh1 84.46(12) . . ? C15 Rh2 Rh1 84.46(12) 6 . ? C11 Rh2 Rh1 95.62(12) 6 . ? C11 Rh2 Rh1 95.62(12) . . ? Rh3 Rh2 Rh1 168.049(18) . . ? C26 Rh3 C22 89.50(13) . . ? C26 Rh3 C22 89.50(13) . 6 ? C22 Rh3 C22 176.2(3) . 6 ? C26 Rh3 C19 169.2(3) . . ? C22 Rh3 C19 90.15(12) . . ? C22 Rh3 C19 90.15(12) 6 . ? C26 Rh3 Rh2 94.05(17) . . ? C22 Rh3 Rh2 91.85(13) . . ? C22 Rh3 Rh2 91.85(13) 6 . ? C19 Rh3 Rh2 96.80(19) . . ? C1 N1 C2 174.7(7) . . ? C4 N2 C5 178.1(7) . . ? C8 N3 C9 178.5(7) . . ? C11 N4 C12 176.3(5) . . ? C15 N5 C16 179.5(7) . . ? C19 N6 C20 174.7(10) . . ? C22 N7 C23 178.6(6) . . ? C26 N8 C27 178.5(7) . . ? N1 C1 Rh1 175.8(5) . . ? N1 C2 C3 108.0(4) . 6 ? N1 C2 C3 108.0(4) . . ? C3 C2 C3 113.9(8) 6 . ? N1 C2 H2 109.0 . . ? C3 C2 H2 109.0 6 . ? C3 C2 H2 109.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 Rh1 178.3(4) . . ? N2 C5 C7 108.5(6) . . ? N2 C5 C6 106.9(8) . . ? C7 C5 C6 100.1(9) . . ? N2 C5 H5 113.5 . . ? C7 C5 H5 113.5 . . ? C6 C5 H5 113.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 Rh1 177.4(5) . . ? N3 C9 C10 110.3(5) . . ? N3 C9 C10 110.3(5) . 6 ? C10 C9 C10 110.7(8) . 6 ? N3 C9 H9 108.5 . . ? C10 C9 H9 108.5 . . ? C10 C9 H9 108.5 6 . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 Rh2 177.5(4) . . ? N4 C12 C14 108.4(5) . . ? N4 C12 C13 109.7(5) . . ? C14 C12 C13 114.0(6) . . ? N4 C12 H12 108.2 . . ? C14 C12 H12 108.2 . . ? C13 C12 H12 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 Rh2 178.0(4) . . ? C18 C16 C17 122.9(6) . . ? C18 C16 N5 112.4(5) . . ? C17 C16 N5 110.9(5) . . ? C18 C16 H16 102.5 . . ? C17 C16 H16 102.5 . . ? N5 C16 H16 102.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 Rh3 176.7(7) . . ? C21 C20 C21 124.4(9) . 6 ? C21 C20 N6 113.9(4) . . ? C21 C20 N6 113.9(4) 6 . ? C21 C20 H20 99.3 . . ? C21 C20 H20 99.3 6 . ? N6 C20 H20 99.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 Rh3 179.5(6) . . ? N7 C23 C24 107.5(7) . . ? N7 C23 C25 106.6(7) . . ? C24 C23 C25 108.3(8) . . ? N7 C23 H23A 111.4 . . ? C24 C23 H23A 111.4 . . ? C25 C23 H23A 111.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N8 C26 Rh3 177.2(6) . . ? N8 C27 C28 109.1(6) . . ? N8 C27 C28 109.1(6) . 6 ? C28 C27 C28 110.8(10) . 6 ? N8 C27 H27 109.3 . . ? C28 C27 H27 109.3 . . ? C28 C27 H27 109.3 6 . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O4 O4 H4 126(5) 6_556 . ? O5B O5A O5B 91(3) 6 . ? O5A O5B O5B 44.4(16) . 6 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 Cl3 0.826(10) 2.80(2) 3.456(9) 137.1(17) . O2 H2A Cl3 0.826(10) 2.69(4) 3.310(9) 134(4) . O4 H4 Cl3 0.821(10) 2.47(4) 3.183(9) 146(6) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.792 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.079 #===END