Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Philip Coppens' _publ_contact_author_address ; Chemistry State University of New York at Buffalo 732 NSC SUNY at Buffalo Buffalo NY 14260 UNITED STATES OF AMERICA ; _publ_contact_author_email COPPENS@BUFFALO.EDU _publ_section_title ; Solid-State Specroscopic Properties and the Geometry of Binuclear Rh(I) Diisocyanoalkane Compelxes ; loop_ _publ_author_name 'Philip Coppens' 'Oksana Gerlits' 'A. Yu Kovalevsky' data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 248488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(dimen)4)(Calix)2x0.64H2O _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C104 H118 N8 O8.64 Rh2' _chemical_formula_weight 1824.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8626(3) _cell_length_b 30.3323(9) _cell_length_c 14.8705(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.1860(10) _cell_angle_gamma 90.00 _cell_volume 4598.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 25.12 _exptl_crystal_description leaves _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1914 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.9020 _exptl_absorpt_correction_T_max 0.9792 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent methanol ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 53652 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.12 _reflns_number_total 8106 _reflns_number_gt 5482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+18.7387P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8106 _refine_ls_number_parameters 589 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.18046(6) 1.027185(16) -0.04826(4) 0.03741(16) Uani 1 1 d . . . N1 N -0.0566(5) 1.10615(17) -0.1193(4) 0.0367(12) Uani 1 1 d . A . N2 N -0.1324(5) 1.08889(18) 0.1270(4) 0.0412(14) Uani 1 1 d . E . N3 N -0.3279(5) 0.95778(16) 0.0295(3) 0.0394(13) Uani 1 1 d . B . N4 N -0.2551(5) 0.96925(17) -0.2327(3) 0.0392(12) Uani 1 1 d . . . O1 O -0.0158(5) 1.23870(17) -0.4664(3) 0.0563(13) Uani 1 1 d . . . H1O H -0.0788 1.2527 -0.4596 0.084 Uiso 1 1 calc R . . O2 O -0.2431(5) 1.25314(15) -0.4532(3) 0.0483(12) Uani 1 1 d . . . O3 O -0.3477(5) 1.16899(18) -0.5415(3) 0.0622(15) Uani 1 1 d . . . H3O H -0.3197 1.1946 -0.5248 0.093 Uiso 1 1 calc R . . O4 O -0.0988(4) 1.16324(15) -0.5205(3) 0.0456(12) Uani 1 1 d . . . H4O H -0.0557 1.1864 -0.5008 0.068 Uiso 1 1 calc R . . C1 C 0.1819(6) 1.20593(19) -0.3708(4) 0.0315(14) Uani 1 1 d . . . C2 C 0.2831(6) 1.2041(2) -0.2829(4) 0.0350(15) Uani 1 1 d . . . H2A H 0.3527 1.1838 -0.2753 0.042 Uiso 1 1 calc R . . C3 C 0.2871(6) 1.2298(2) -0.2072(4) 0.0354(15) Uani 1 1 d . . . H3A H 0.3566 1.2271 -0.1474 0.042 Uiso 1 1 calc R . . C4 C 0.1863(6) 1.26036(19) -0.2195(4) 0.0343(15) Uani 1 1 d . . . H4A H 0.1878 1.2787 -0.1674 0.041 Uiso 1 1 calc R . . C5 C 0.0850(6) 1.26440(18) -0.3055(4) 0.0337(14) Uani 1 1 d . . . C6 C 0.0836(6) 1.2368(2) -0.3818(4) 0.0352(15) Uani 1 1 d . . . C7 C -0.0228(6) 1.2974(2) -0.3156(5) 0.0459(17) Uani 1 1 d . . . H7A H -0.0547 1.3084 -0.3824 0.055 Uiso 1 1 calc R . . H7B H 0.0152 1.3228 -0.2734 0.055 Uiso 1 1 calc R . . C8 C -0.1394(7) 1.28064(19) -0.2922(5) 0.0440(17) Uani 1 1 d . . . C9 C -0.1449(7) 1.2854(2) -0.2015(5) 0.0464(17) Uani 1 1 d . . . H9A H -0.0738 1.2991 -0.1532 0.056 Uiso 1 1 calc R . . C10 C -0.2521(8) 1.2708(2) -0.1793(6) 0.056(2) Uani 1 1 d . . . H10A H -0.2566 1.2754 -0.1174 0.067 Uiso 1 1 calc R . . C11 C -0.3523(7) 1.2492(2) -0.2494(6) 0.0496(18) Uani 1 1 d . . . H11A H -0.4256 1.2389 -0.2346 0.059 Uiso 1 1 calc R . . C12 C -0.3490(7) 1.2422(2) -0.3393(5) 0.0430(16) Uani 1 1 d . . . C13 C -0.2433(6) 1.25875(19) -0.3635(5) 0.0394(16) Uani 1 1 d . . . C14 C -0.4524(6) 1.2136(2) -0.4119(5) 0.0495(18) Uani 1 1 d . . . H14A H -0.5371 1.2165 -0.4012 0.059 Uiso 1 1 calc R . . H14B H -0.4651 1.2240 -0.4776 0.059 Uiso 1 1 calc R . . C15 C -0.4114(6) 1.1657(2) -0.4027(5) 0.0377(15) Uani 1 1 d . . . C16 C -0.4231(6) 1.1397(2) -0.3290(5) 0.0388(15) Uani 1 1 d . . . H16A H -0.4664 1.1515 -0.2887 0.047 Uiso 1 1 calc R . . C17 C -0.3740(7) 1.0975(2) -0.3123(5) 0.0430(16) Uani 1 1 d . . . H17A H -0.3828 1.0806 -0.2610 0.052 Uiso 1 1 calc R . . C18 C -0.3117(7) 1.0800(2) -0.3712(5) 0.0421(16) Uani 1 1 d . . . H18A H -0.2771 1.0509 -0.3595 0.051 Uiso 1 1 calc R . . C19 C -0.2986(6) 1.1038(2) -0.4470(5) 0.0382(15) Uani 1 1 d . . . C20 C -0.3537(6) 1.1464(2) -0.4641(4) 0.0401(16) Uani 1 1 d . . . C21 C -0.2314(7) 1.0839(3) -0.5116(5) 0.0521(19) Uani 1 1 d . . . H21A H -0.2552 1.0523 -0.5209 0.063 Uiso 1 1 calc R . . H21B H -0.2666 1.0984 -0.5750 0.063 Uiso 1 1 calc R . . C22 C -0.0845(7) 1.0876(2) -0.4762(4) 0.0423(17) Uani 1 1 d . . . C23 C -0.0057(8) 1.0515(2) -0.4400(5) 0.0476(18) Uani 1 1 d . . . H23A H -0.0459 1.0241 -0.4356 0.057 Uiso 1 1 calc R . . C24 C 0.1284(8) 1.0536(2) -0.4100(5) 0.0512(19) Uani 1 1 d . . . H24A H 0.1804 1.0281 -0.3868 0.061 Uiso 1 1 calc R . . C25 C 0.1863(7) 1.0939(2) -0.4144(5) 0.0461(18) Uani 1 1 d . . . H25A H 0.2793 1.0958 -0.3926 0.055 Uiso 1 1 calc R . . C26 C 0.1120(7) 1.1315(2) -0.4497(4) 0.0385(16) Uani 1 1 d . . . C27 C -0.0237(7) 1.1280(2) -0.4817(4) 0.0412(17) Uani 1 1 d . . . C28 C 0.1793(7) 1.1748(2) -0.4520(5) 0.0470(17) Uani 1 1 d . . . H28A H 0.1337 1.1896 -0.5139 0.056 Uiso 1 1 calc R . . H28B H 0.2706 1.1689 -0.4483 0.056 Uiso 1 1 calc R . . C29 C -0.0999(6) 1.0753(2) -0.0977(4) 0.0349(15) Uani 1 1 d . . . C30 C 0.0021(6) 1.1464(2) -0.1402(5) 0.0380(15) Uani 1 1 d D . . C31 C -0.0159(12) 1.1840(3) -0.0745(8) 0.043(3) Uani 0.60 1 d P A 1 H31A H 0.0260 1.1755 -0.0072 0.065 Uiso 0.60 1 calc PR A 1 H31B H -0.1097 1.1891 -0.0880 0.065 Uiso 0.60 1 calc PR A 1 H31C H 0.0247 1.2111 -0.0870 0.065 Uiso 0.60 1 calc PR A 1 C32 C 0.1479(10) 1.1376(3) -0.1208(7) 0.033(2) Uani 0.60 1 d P . 1 H32A H 0.1857 1.1648 -0.1388 0.040 Uiso 0.60 1 calc PR . 1 C33 C -0.0694(10) 1.1617(3) -0.2434(7) 0.034(2) Uani 0.60 1 d P A 1 H33A H -0.0658 1.1383 -0.2879 0.051 Uiso 0.60 1 calc PR A 1 H33B H -0.0270 1.1883 -0.2562 0.051 Uiso 0.60 1 calc PR A 1 H33C H -0.1612 1.1682 -0.2521 0.051 Uiso 0.60 1 calc PR A 1 C43 C -0.5267(12) 0.9290(4) 0.0438(11) 0.060(4) Uani 0.60 1 d P B 1 H43A H -0.5725 0.9373 -0.0232 0.090 Uiso 0.60 1 calc PR B 1 H43B H -0.5321 0.9533 0.0857 0.090 Uiso 0.60 1 calc PR B 1 H43C H -0.5676 0.9026 0.0591 0.090 Uiso 0.60 1 calc PR B 1 C44 C -0.3069(12) 0.9100(4) 0.1646(8) 0.045(3) Uani 0.60 1 d P B 1 H44A H -0.3120 0.9360 0.2034 0.054 Uiso 0.60 1 calc PR B 1 H44B H -0.3479 0.8848 0.1861 0.054 Uiso 0.60 1 calc PR B 1 C47 C -0.3678(12) 0.8799(4) -0.0003(9) 0.051(3) Uani 0.60 1 d P B 1 H47A H -0.4053 0.8533 0.0190 0.061 Uiso 0.60 1 calc PR B 1 H47B H -0.4169 0.8853 -0.0690 0.061 Uiso 0.60 1 calc PR B 1 C53 C 0.1064(15) 1.1586(5) -0.0497(11) 0.039(4) Uiso 0.40 1 d P . 2 H53C H 0.0664 1.1607 0.0007 0.047 Uiso 0.40 1 calc PR . 2 H53D H 0.1381 1.1884 -0.0579 0.047 Uiso 0.40 1 calc PR . 2 C54 C 0.0526(19) 1.1330(7) -0.2187(11) 0.061(5) Uiso 0.40 1 d PD . 2 H54C H 0.0820 1.1596 -0.2442 0.074 Uiso 0.40 1 calc PR . 2 H54D H -0.0195 1.1194 -0.2717 0.074 Uiso 0.40 1 calc PR . 2 C55 C -0.108(2) 1.1779(7) -0.1647(16) 0.071(6) Uiso 0.40 1 d P A 2 H55D H -0.1734 1.1699 -0.2268 0.106 Uiso 0.40 1 calc PR A 2 H55E H -0.0757 1.2077 -0.1683 0.106 Uiso 0.40 1 calc PR A 2 H55F H -0.1490 1.1769 -0.1153 0.106 Uiso 0.40 1 calc PR A 2 C56 C -0.443(2) 0.9300(7) 0.1344(14) 0.060(5) Uiso 0.40 1 d P B 2 H56A H -0.3820 0.9487 0.1836 0.090 Uiso 0.40 1 calc PR B 2 H56B H -0.4582 0.9026 0.1638 0.090 Uiso 0.40 1 calc PR B 2 H56C H -0.5263 0.9456 0.1053 0.090 Uiso 0.40 1 calc PR B 2 C57 C -0.4985(16) 0.9050(5) -0.0318(11) 0.043(4) Uiso 0.40 1 d P B 2 H57A H -0.5724 0.9255 -0.0435 0.064 Uiso 0.40 1 calc PR B 2 H57B H -0.5265 0.8752 -0.0224 0.064 Uiso 0.40 1 calc PR B 2 H57C H -0.4688 0.9052 -0.0869 0.064 Uiso 0.40 1 calc PR B 2 C58 C -0.2775(15) 0.8864(5) 0.0918(10) 0.032(3) Uiso 0.40 1 d P B 2 H58A H -0.3181 0.8596 0.1090 0.038 Uiso 0.40 1 calc PR B 2 C34 C -0.1485(6) 1.0648(2) 0.0654(5) 0.0378(15) Uani 1 1 d . . . C35 C -0.1002(8) 1.1206(2) 0.2078(5) 0.054(2) Uani 1 1 d D . . C39 C 0.1358(6) 1.1193(2) 0.2164(4) 0.0414(16) Uani 1 1 d D . . H39A H 0.1305 1.1508 0.1977 0.050 Uiso 1 1 calc R C 1 H39B H 0.1066 1.1015 0.1569 0.050 Uiso 1 1 calc R C 1 C40 C 0.0627(8) 1.0647(2) 0.3124(5) 0.0534(19) Uani 1 1 d D . . H40A H 0.0090 1.0613 0.3539 0.064 Uiso 1 1 calc R D 1 H40B H 0.0299 1.0433 0.2592 0.064 Uiso 1 1 calc R D 1 C49 C -0.2958(7) 0.93847(19) -0.3120(4) 0.0431(17) Uani 1 1 d D . . C36 C -0.1172(11) 1.1673(2) 0.1669(7) 0.052(3) Uani 0.69 1 d PD E 1 H36A H -0.2078 1.1714 0.1238 0.079 Uiso 0.69 1 calc PR E 1 H36B H -0.0573 1.1718 0.1313 0.079 Uiso 0.69 1 calc PR E 1 H36C H -0.0972 1.1887 0.2194 0.079 Uiso 0.69 1 calc PR E 1 C37 C -0.2002(11) 1.1145(4) 0.2552(8) 0.050(3) Uani 0.69 1 d P E 1 H37A H -0.1985 1.0839 0.2765 0.075 Uiso 0.69 1 calc PR E 1 H37B H -0.2875 1.1215 0.2095 0.075 Uiso 0.69 1 calc PR E 1 H37C H -0.1801 1.1343 0.3105 0.075 Uiso 0.69 1 calc PR E 1 C38 C 0.0441(10) 1.1112(2) 0.2711(6) 0.039(2) Uani 0.69 1 d PD E 1 H38A H 0.0681 1.1323 0.3261 0.047 Uiso 0.69 1 calc PR E 1 C50 C -0.2021(11) 0.9464(3) -0.3695(7) 0.050(3) Uani 0.69 1 d P . 1 H50A H -0.2312 0.9281 -0.4283 0.060 Uiso 0.69 1 calc PR . 1 H50B H -0.2075 0.9777 -0.3893 0.060 Uiso 0.69 1 calc PR . 1 C51 C -0.4319(12) 0.9526(4) -0.3726(8) 0.065(3) Uani 0.69 1 d P . 1 H51A H -0.4880 0.9533 -0.3333 0.098 Uiso 0.69 1 calc PR . 1 H51B H -0.4679 0.9316 -0.4253 0.098 Uiso 0.69 1 calc PR . 1 H51C H -0.4285 0.9820 -0.3988 0.098 Uiso 0.69 1 calc PR . 1 C52 C -0.2781(10) 0.8921(2) -0.2734(7) 0.049(3) Uani 0.69 1 d PD . 1 H52A H -0.3115 0.8712 -0.3275 0.059 Uiso 0.69 1 calc PR . 1 H52B H -0.3313 0.8882 -0.2317 0.059 Uiso 0.69 1 calc PR . 1 C62 C -0.1794(19) 0.9100(6) -0.3046(14) 0.032(4) Uiso 0.31 1 d P . 2 H62B H -0.2085 0.8896 -0.3610 0.038 Uiso 0.31 1 calc PR . 2 C63 C -0.361(2) 0.9572(8) -0.4113(9) 0.052(6) Uiso 0.31 1 d PD . 2 H63D H -0.4395 0.9736 -0.4137 0.077 Uiso 0.31 1 calc PR . 2 H63E H -0.3852 0.9331 -0.4580 0.077 Uiso 0.31 1 calc PR . 2 H63F H -0.2996 0.9771 -0.4266 0.077 Uiso 0.31 1 calc PR . 2 C59 C 0.0164(10) 1.1470(4) 0.2069(19) 0.059(7) Uiso 0.31 1 d PD E 2 H59A H 0.0392 1.1686 0.2601 0.071 Uiso 0.31 1 calc PR E 2 H59B H -0.0079 1.1639 0.1462 0.071 Uiso 0.31 1 calc PR E 2 C64 C -0.396(2) 0.9084(7) -0.2932(19) 0.061(7) Uiso 0.31 1 d PD . 2 H64D H -0.4781 0.9246 -0.3045 0.092 Uiso 0.31 1 calc PR . 2 H64E H -0.3624 0.8982 -0.2265 0.092 Uiso 0.31 1 calc PR . 2 H64F H -0.4126 0.8829 -0.3363 0.092 Uiso 0.31 1 calc PR . 2 C61 C -0.0662(17) 1.0886(8) 0.2912(16) 0.081(9) Uiso 0.31 1 d PD E 2 H61A H -0.0640 1.1050 0.3493 0.097 Uiso 0.31 1 calc PR E 2 H61B H -0.1372 1.0664 0.2778 0.097 Uiso 0.31 1 calc PR E 2 C60 C -0.230(4) 1.1385(13) 0.202(3) 0.098(12) Uiso 0.31 1 d P E 2 H60A H -0.2867 1.1412 0.1352 0.146 Uiso 0.31 1 calc PR E 2 H60B H -0.2183 1.1676 0.2330 0.146 Uiso 0.31 1 calc PR E 2 H60C H -0.2711 1.1185 0.2357 0.146 Uiso 0.31 1 calc PR E 2 C41 C -0.2700(6) 0.9833(2) 0.0026(4) 0.0356(15) Uiso 1 1 d . . . C42 C -0.3852(7) 0.9195(2) 0.0586(5) 0.0408(15) Uiso 1 1 d . . . C45 C -0.1666(7) 0.8995(2) 0.1828(5) 0.0419(16) Uiso 1 1 d . . . H45A H -0.1242 0.8913 0.2510 0.050 Uiso 1 1 calc R B 1 H45B H -0.1221 0.9263 0.1711 0.050 Uiso 1 1 calc R B 1 C46 C -0.2242(6) 0.8714(2) 0.0135(4) 0.0375(15) Uiso 1 1 d . . . H46A H -0.1866 0.8974 -0.0080 0.045 Uiso 1 1 calc R B 1 H46B H -0.2167 0.8457 -0.0253 0.045 Uiso 1 1 calc R B 1 C48 C -0.2229(6) 0.9914(2) -0.1648(4) 0.0331(14) Uiso 1 1 d . . . O1W O -0.5886(14) 0.8092(5) 0.0519(10) 0.047(4) Uiso 0.32 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 0.0576(3) 0.0286(2) 0.0301(3) -0.0096(2) 0.0203(2) -0.0127(3) N1 0.038(3) 0.032(3) 0.041(3) -0.001(2) 0.015(3) -0.015(2) N2 0.047(4) 0.046(3) 0.037(3) -0.020(3) 0.022(3) -0.009(3) N3 0.055(4) 0.032(3) 0.035(3) 0.000(2) 0.022(3) -0.008(3) N4 0.056(3) 0.032(3) 0.030(3) -0.010(2) 0.016(2) -0.013(3) O1 0.062(3) 0.066(3) 0.037(3) 0.006(2) 0.011(3) 0.006(3) O2 0.050(3) 0.041(3) 0.051(3) 0.013(2) 0.015(2) -0.005(2) O3 0.067(4) 0.069(3) 0.047(3) 0.021(3) 0.015(3) -0.012(3) O4 0.051(3) 0.049(3) 0.036(3) -0.009(2) 0.013(2) -0.018(2) C1 0.035(4) 0.036(3) 0.031(3) -0.005(3) 0.021(3) -0.013(3) C2 0.032(4) 0.036(3) 0.043(4) -0.001(3) 0.021(3) -0.003(3) C3 0.033(4) 0.041(4) 0.029(3) -0.004(3) 0.008(3) -0.010(3) C4 0.044(4) 0.026(3) 0.036(4) -0.009(3) 0.016(3) -0.007(3) C5 0.041(4) 0.020(3) 0.043(4) 0.006(3) 0.017(3) -0.004(3) C6 0.034(4) 0.046(4) 0.020(3) 0.004(3) 0.003(3) -0.010(3) C7 0.044(4) 0.026(3) 0.067(5) 0.005(3) 0.018(4) -0.002(3) C8 0.051(4) 0.017(3) 0.069(5) 0.008(3) 0.027(4) 0.009(3) C9 0.055(5) 0.028(3) 0.054(4) -0.001(3) 0.017(4) 0.008(3) C10 0.063(5) 0.048(4) 0.066(5) 0.002(4) 0.037(5) 0.012(4) C11 0.048(5) 0.033(4) 0.074(5) 0.004(4) 0.028(4) 0.011(3) C12 0.043(4) 0.029(3) 0.058(5) 0.007(3) 0.018(4) 0.009(3) C13 0.038(4) 0.022(3) 0.052(4) 0.009(3) 0.007(3) 0.002(3) C14 0.030(4) 0.045(4) 0.069(5) 0.016(4) 0.011(4) -0.001(3) C15 0.026(3) 0.033(3) 0.048(4) 0.004(3) 0.005(3) -0.003(3) C16 0.034(4) 0.036(4) 0.049(4) 0.003(3) 0.017(3) -0.004(3) C17 0.046(4) 0.035(4) 0.057(4) 0.004(3) 0.030(4) -0.005(3) C18 0.051(4) 0.029(3) 0.051(4) -0.003(3) 0.023(4) -0.008(3) C19 0.037(4) 0.038(3) 0.036(3) -0.014(3) 0.008(3) -0.011(3) C20 0.034(4) 0.052(4) 0.030(4) 0.008(3) 0.005(3) -0.016(3) C21 0.062(5) 0.062(5) 0.039(4) -0.017(3) 0.025(4) -0.025(4) C22 0.056(5) 0.047(4) 0.032(4) -0.022(3) 0.025(3) -0.022(4) C23 0.066(5) 0.040(4) 0.046(4) -0.023(3) 0.032(4) -0.015(4) C24 0.073(6) 0.047(4) 0.039(4) -0.015(3) 0.026(4) 0.000(4) C25 0.053(5) 0.055(5) 0.036(4) -0.020(3) 0.023(3) -0.003(4) C26 0.051(4) 0.047(4) 0.025(3) -0.018(3) 0.023(3) -0.016(3) C27 0.060(5) 0.046(4) 0.024(3) -0.020(3) 0.023(3) -0.010(4) C28 0.050(4) 0.063(4) 0.038(4) -0.017(4) 0.029(3) -0.016(4) C29 0.032(4) 0.042(4) 0.029(3) -0.019(3) 0.009(3) -0.005(3) C30 0.035(4) 0.031(3) 0.046(4) 0.007(3) 0.010(3) -0.004(3) C31 0.050(7) 0.027(5) 0.055(7) -0.005(5) 0.020(6) -0.006(5) C32 0.031(6) 0.033(6) 0.034(6) 0.007(4) 0.007(5) -0.008(4) C33 0.034(6) 0.033(6) 0.030(6) 0.011(4) 0.004(5) -0.005(5) C43 0.041(8) 0.054(8) 0.089(10) 0.011(7) 0.027(7) 0.009(6) C44 0.063(8) 0.040(6) 0.043(7) 0.011(5) 0.031(6) 0.001(6) C47 0.055(8) 0.037(6) 0.050(7) -0.002(5) 0.005(6) -0.012(6) C34 0.042(4) 0.035(3) 0.039(4) -0.005(3) 0.018(3) -0.007(3) C35 0.068(5) 0.056(5) 0.044(4) -0.029(4) 0.028(4) -0.004(4) C39 0.052(4) 0.034(3) 0.035(4) -0.005(3) 0.010(3) -0.016(3) C40 0.067(5) 0.060(5) 0.039(4) -0.008(3) 0.026(4) -0.017(4) C49 0.059(5) 0.036(4) 0.030(3) -0.014(3) 0.010(3) -0.010(3) C36 0.069(8) 0.037(6) 0.060(7) -0.020(5) 0.035(6) -0.012(5) C37 0.056(7) 0.057(7) 0.048(6) -0.025(5) 0.033(6) -0.009(5) C38 0.056(7) 0.035(5) 0.031(5) -0.021(4) 0.021(5) -0.006(4) C50 0.085(9) 0.035(5) 0.032(5) -0.017(4) 0.022(6) -0.008(5) C51 0.070(8) 0.051(7) 0.056(7) -0.018(6) -0.002(6) -0.011(6) C52 0.053(7) 0.037(6) 0.056(7) -0.015(5) 0.016(6) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C41 1.949(6) . ? Rh1 C48 1.960(6) . ? Rh1 C34 1.968(6) . ? Rh1 C29 1.971(7) . ? N1 C29 1.141(7) . ? N1 C30 1.459(7) . ? N2 C34 1.137(7) . ? N2 C35 1.484(7) . ? N3 C41 1.152(7) . ? N3 C42 1.451(8) . ? N4 C48 1.162(7) . ? N4 C49 1.448(7) . ? O1 C6 1.347(7) . ? O2 C13 1.345(8) . ? O3 C20 1.361(7) . ? O4 C27 1.348(8) . ? C1 C6 1.387(9) . ? C1 C2 1.389(9) . ? C1 C28 1.524(8) . ? C2 C3 1.358(8) . ? C3 C4 1.398(9) . ? C4 C5 1.375(9) . ? C5 C6 1.406(8) . ? C5 C7 1.508(9) . ? C7 C8 1.512(9) . ? C8 C9 1.377(9) . ? C8 C13 1.419(9) . ? C9 C10 1.389(10) . ? C10 C11 1.384(10) . ? C11 C12 1.366(10) . ? C12 C13 1.409(9) . ? C12 C14 1.530(10) . ? C14 C15 1.512(9) . ? C15 C16 1.390(9) . ? C15 C20 1.402(9) . ? C16 C17 1.377(9) . ? C17 C18 1.385(9) . ? C18 C19 1.387(9) . ? C19 C20 1.407(9) . ? C19 C21 1.518(9) . ? C21 C22 1.502(10) . ? C22 C23 1.380(10) . ? C22 C27 1.407(9) . ? C23 C24 1.370(10) . ? C24 C25 1.385(10) . ? C25 C26 1.392(10) . ? C26 C27 1.388(9) . ? C26 C28 1.510(9) . ? C30 C53 1.476(17) . ? C30 C55 1.48(2) . ? C30 C54 1.507(5) . ? C30 C32 1.533(12) . ? C30 C33 1.534(11) . ? C30 C31 1.557(12) . ? C32 C45 1.512(12) 3_575 ? C32 C46 1.548(11) 3_575 ? C43 C42 1.503(13) . ? C44 C45 1.487(13) . ? C44 C42 1.539(12) . ? C47 C46 1.524(14) . ? C47 C42 1.538(13) . ? C53 C46 1.510(16) 3_575 ? C54 C45 1.529(19) 3_575 ? C56 C42 1.501(19) . ? C57 C42 1.540(17) . ? C58 C42 1.491(16) . ? C58 C45 1.522(16) . ? C58 C46 1.538(15) . ? C35 C60 1.49(4) . ? C35 C37 1.495(11) . ? C35 C59 1.504(5) . ? C35 C61 1.516(5) . ? C35 C36 1.528(5) . ? C35 C38 1.551(12) . ? C39 C38 1.508(10) . ? C39 C59 1.511(5) . ? C39 C62 1.518(19) 3_575 ? C39 C52 1.524(12) 3_575 ? C40 C50 1.496(13) 3_575 ? C40 C61 1.511(5) . ? C40 C62 1.52(2) 3_575 ? C40 C38 1.524(5) . ? C49 C51 1.504(13) . ? C49 C62 1.50(2) . ? C49 C52 1.507(5) . ? C49 C63 1.511(5) . ? C49 C64 1.520(5) . ? C49 C50 1.558(12) . ? C50 C40 1.496(13) 3_575 ? C52 C39 1.524(12) 3_575 ? C62 C39 1.518(19) 3_575 ? C62 C40 1.52(2) 3_575 ? C45 C32 1.512(12) 3_575 ? C45 C54 1.529(19) 3_575 ? C46 C53 1.510(16) 3_575 ? C46 C32 1.548(11) 3_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Rh1 C48 88.1(2) . . ? C41 Rh1 C34 91.6(2) . . ? C48 Rh1 C34 176.5(3) . . ? C41 Rh1 C29 175.2(2) . . ? C48 Rh1 C29 94.6(2) . . ? C34 Rh1 C29 85.5(2) . . ? C29 N1 C30 176.2(6) . . ? C34 N2 C35 175.4(7) . . ? C41 N3 C42 169.1(6) . . ? C48 N4 C49 175.0(6) . . ? C6 C1 C2 117.7(5) . . ? C6 C1 C28 121.4(6) . . ? C2 C1 C28 120.9(6) . . ? C3 C2 C1 123.1(6) . . ? C2 C3 C4 118.2(6) . . ? C5 C4 C3 121.4(6) . . ? C4 C5 C6 118.7(6) . . ? C4 C5 C7 119.8(6) . . ? C6 C5 C7 121.6(6) . . ? O1 C6 C1 118.4(6) . . ? O1 C6 C5 120.6(6) . . ? C1 C6 C5 120.9(5) . . ? C5 C7 C8 115.9(5) . . ? C9 C8 C13 119.3(6) . . ? C9 C8 C7 120.8(7) . . ? C13 C8 C7 119.9(6) . . ? C8 C9 C10 121.5(7) . . ? C11 C10 C9 118.6(7) . . ? C12 C11 C10 122.1(7) . . ? C11 C12 C13 119.6(7) . . ? C11 C12 C14 121.1(7) . . ? C13 C12 C14 119.1(6) . . ? O2 C13 C12 119.2(6) . . ? O2 C13 C8 121.8(6) . . ? C12 C13 C8 118.9(7) . . ? C15 C14 C12 111.1(5) . . ? C16 C15 C20 117.3(6) . . ? C16 C15 C14 120.8(6) . . ? C20 C15 C14 121.8(6) . . ? C17 C16 C15 122.3(6) . . ? C16 C17 C18 119.1(6) . . ? C17 C18 C19 121.5(6) . . ? C18 C19 C20 118.0(6) . . ? C18 C19 C21 120.8(6) . . ? C20 C19 C21 121.2(6) . . ? O3 C20 C15 120.2(6) . . ? O3 C20 C19 118.3(6) . . ? C15 C20 C19 121.5(6) . . ? C22 C21 C19 115.7(5) . . ? C23 C22 C27 118.2(7) . . ? C23 C22 C21 121.2(6) . . ? C27 C22 C21 120.5(7) . . ? C24 C23 C22 122.4(7) . . ? C23 C24 C25 118.4(7) . . ? C24 C25 C26 121.8(7) . . ? C27 C26 C25 118.3(6) . . ? C27 C26 C28 121.6(7) . . ? C25 C26 C28 120.0(6) . . ? O4 C27 C26 120.0(6) . . ? O4 C27 C22 119.2(6) . . ? C26 C27 C22 120.8(7) . . ? C26 C28 C1 113.5(5) . . ? N1 C29 Rh1 172.4(5) . . ? N1 C30 C53 105.7(8) . . ? N1 C30 C55 102.5(10) . . ? C53 C30 C55 111.4(12) . . ? N1 C30 C54 104.0(9) . . ? C53 C30 C54 113.8(11) . . ? C55 C30 C54 117.6(12) . . ? N1 C30 C32 108.2(6) . . ? C53 C30 C32 56.9(7) . . ? C55 C30 C32 149.1(10) . . ? C54 C30 C32 58.0(9) . . ? N1 C30 C33 111.0(6) . . ? C53 C30 C33 143.2(8) . . ? C55 C30 C33 58.0(10) . . ? C54 C30 C33 59.9(9) . . ? C32 C30 C33 112.0(7) . . ? N1 C30 C31 108.7(6) . . ? C53 C30 C31 57.8(8) . . ? C55 C30 C31 54.1(10) . . ? C54 C30 C31 147.2(10) . . ? C32 C30 C31 110.8(7) . . ? C33 C30 C31 106.1(7) . . ? C45 C32 C30 111.3(7) 3_575 . ? C45 C32 C46 111.2(7) 3_575 3_575 ? C30 C32 C46 112.0(7) . 3_575 ? C45 C44 C42 113.4(8) . . ? C46 C47 C42 112.1(8) . . ? C30 C53 C46 117.6(11) . 3_575 ? C30 C54 C45 111.8(11) . 3_575 ? C42 C58 C45 114.1(10) . . ? C42 C58 C46 113.9(10) . . ? C45 C58 C46 111.2(10) . . ? N2 C34 Rh1 175.4(6) . . ? N2 C35 C60 103.9(16) . . ? N2 C35 C37 107.2(6) . . ? C60 C35 C37 40.6(14) . . ? N2 C35 C59 107.6(10) . . ? C60 C35 C59 126.2(16) . . ? C37 C35 C59 145.2(10) . . ? N2 C35 C61 99.8(13) . . ? C60 C35 C61 103.7(16) . . ? C37 C35 C61 63.1(6) . . ? C59 C35 C61 112.4(14) . . ? N2 C35 C36 108.4(6) . . ? C60 C35 C36 70.0(16) . . ? C37 C35 C36 107.1(7) . . ? C59 C35 C36 59.2(7) . . ? C61 C35 C36 151.7(13) . . ? N2 C35 C38 106.1(5) . . ? C60 C35 C38 147.2(16) . . ? C37 C35 C38 116.0(7) . . ? C59 C35 C38 54.9(8) . . ? C61 C35 C38 58.4(9) . . ? C36 C35 C38 111.7(7) . . ? C38 C39 C59 55.7(8) . . ? C38 C39 C62 60.3(8) . 3_575 ? C59 C39 C62 114.1(12) . 3_575 ? C38 C39 C52 113.3(7) . 3_575 ? C59 C39 C52 148.4(11) . 3_575 ? C62 C39 C52 55.4(8) 3_575 3_575 ? C50 C40 C61 155.5(13) 3_575 . ? C50 C40 C62 56.6(8) 3_575 3_575 ? C61 C40 C62 118.5(12) . 3_575 ? C50 C40 C38 113.8(7) 3_575 . ? C61 C40 C38 59.1(9) . . ? C62 C40 C38 59.9(8) 3_575 . ? N4 C49 C51 105.4(6) . . ? N4 C49 C62 107.4(9) . . ? C51 C49 C62 146.6(10) . . ? N4 C49 C52 109.2(6) . . ? C51 C49 C52 117.6(7) . . ? C62 C49 C52 56.1(8) . . ? N4 C49 C63 117.5(10) . . ? C51 C49 C63 43.6(10) . . ? C62 C49 C63 112.6(13) . . ? C52 C49 C63 132.8(11) . . ? N4 C49 C64 105.9(11) . . ? C51 C49 C64 70.2(12) . . ? C62 C49 C64 106.2(13) . . ? C52 C49 C64 51.3(11) . . ? C63 C49 C64 106.5(15) . . ? N4 C49 C50 105.9(6) . . ? C51 C49 C50 108.7(7) . . ? C62 C49 C50 55.7(8) . . ? C52 C49 C50 109.4(7) . . ? C63 C49 C50 65.1(11) . . ? C64 C49 C50 147.1(11) . . ? C39 C38 C40 110.4(6) . . ? C39 C38 C35 111.1(6) . . ? C40 C38 C35 112.4(7) . . ? C40 C50 C49 112.3(7) 3_575 . ? C49 C52 C39 113.3(7) . 3_575 ? C49 C62 C39 113.8(12) . 3_575 ? C49 C62 C40 113.9(13) . 3_575 ? C39 C62 C40 110.0(12) 3_575 3_575 ? C35 C59 C39 113.6(8) . . ? C40 C61 C35 115.2(8) . . ? N3 C41 Rh1 177.0(6) . . ? N3 C42 C58 105.6(7) . . ? N3 C42 C56 112.8(9) . . ? C58 C42 C56 112.2(11) . . ? N3 C42 C43 109.0(7) . . ? C58 C42 C43 145.4(9) . . ? C56 C42 C43 53.0(9) . . ? N3 C42 C47 107.8(6) . . ? C58 C42 C47 54.9(7) . . ? C56 C42 C47 139.4(10) . . ? C43 C42 C47 112.7(8) . . ? N3 C42 C44 108.3(6) . . ? C58 C42 C44 56.0(7) . . ? C56 C42 C44 59.8(9) . . ? C43 C42 C44 111.2(8) . . ? C47 C42 C44 107.6(7) . . ? N3 C42 C57 105.3(8) . . ? C58 C42 C57 113.3(10) . . ? C56 C42 C57 107.5(11) . . ? C43 C42 C57 57.2(8) . . ? C47 C42 C57 59.9(8) . . ? C44 C42 C57 146.4(9) . . ? C44 C45 C32 113.1(7) . 3_575 ? C44 C45 C58 56.4(7) . . ? C32 C45 C58 59.7(7) 3_575 . ? C44 C45 C54 149.0(10) . 3_575 ? C32 C45 C54 58.0(7) 3_575 3_575 ? C58 C45 C54 116.0(10) . 3_575 ? C53 C46 C47 148.4(9) 3_575 . ? C53 C46 C58 113.7(9) 3_575 . ? C47 C46 C58 54.3(7) . . ? C53 C46 C32 55.9(7) 3_575 3_575 ? C47 C46 C32 109.1(7) . 3_575 ? C58 C46 C32 58.6(7) . 3_575 ? N4 C48 Rh1 175.7(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 C6 C1 C2 C3 2.4(9) . . . . ? C28 C1 C2 C3 -177.3(6) . . . . ? C1 C2 C3 C4 -1.8(9) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C3 C4 C5 C6 0.4(9) . . . . ? C3 C4 C5 C7 179.2(5) . . . . ? C2 C1 C6 O1 -179.4(5) . . . . ? C28 C1 C6 O1 0.3(8) . . . . ? C2 C1 C6 C5 -1.6(8) . . . . ? C28 C1 C6 C5 178.1(5) . . . . ? C4 C5 C6 O1 178.0(6) . . . . ? C7 C5 C6 O1 -0.8(9) . . . . ? C4 C5 C6 C1 0.3(9) . . . . ? C7 C5 C6 C1 -178.6(5) . . . . ? C4 C5 C7 C8 -90.3(8) . . . . ? C6 C5 C7 C8 88.5(8) . . . . ? C5 C7 C8 C9 93.2(8) . . . . ? C5 C7 C8 C13 -85.3(8) . . . . ? C13 C8 C9 C10 -2.4(9) . . . . ? C7 C8 C9 C10 179.1(6) . . . . ? C8 C9 C10 C11 2.8(10) . . . . ? C9 C10 C11 C12 -0.4(10) . . . . ? C10 C11 C12 C13 -2.4(10) . . . . ? C10 C11 C12 C14 172.6(6) . . . . ? C11 C12 C13 O2 -177.6(6) . . . . ? C14 C12 C13 O2 7.2(9) . . . . ? C11 C12 C13 C8 2.8(9) . . . . ? C14 C12 C13 C8 -172.4(5) . . . . ? C9 C8 C13 O2 180.0(6) . . . . ? C7 C8 C13 O2 -1.5(9) . . . . ? C9 C8 C13 C12 -0.5(9) . . . . ? C7 C8 C13 C12 178.1(5) . . . . ? C11 C12 C14 C15 -88.6(8) . . . . ? C13 C12 C14 C15 86.5(7) . . . . ? C12 C14 C15 C16 77.5(8) . . . . ? C12 C14 C15 C20 -98.9(8) . . . . ? C20 C15 C16 C17 3.6(10) . . . . ? C14 C15 C16 C17 -172.9(6) . . . . ? C15 C16 C17 C18 -0.5(10) . . . . ? C16 C17 C18 C19 -0.5(10) . . . . ? C17 C18 C19 C20 -1.6(10) . . . . ? C17 C18 C19 C21 -179.3(6) . . . . ? C16 C15 C20 O3 175.4(6) . . . . ? C14 C15 C20 O3 -8.2(9) . . . . ? C16 C15 C20 C19 -5.7(9) . . . . ? C14 C15 C20 C19 170.7(6) . . . . ? C18 C19 C20 O3 -176.3(6) . . . . ? C21 C19 C20 O3 1.4(9) . . . . ? C18 C19 C20 C15 4.8(9) . . . . ? C21 C19 C20 C15 -177.5(6) . . . . ? C18 C19 C21 C22 -84.6(8) . . . . ? C20 C19 C21 C22 97.8(8) . . . . ? C19 C21 C22 C23 106.0(7) . . . . ? C19 C21 C22 C27 -75.7(8) . . . . ? C27 C22 C23 C24 -0.4(9) . . . . ? C21 C22 C23 C24 178.0(6) . . . . ? C22 C23 C24 C25 1.6(10) . . . . ? C23 C24 C25 C26 -1.2(9) . . . . ? C24 C25 C26 C27 -0.4(9) . . . . ? C24 C25 C26 C28 179.2(6) . . . . ? C25 C26 C27 O4 -177.0(5) . . . . ? C28 C26 C27 O4 3.5(8) . . . . ? C25 C26 C27 C22 1.6(8) . . . . ? C28 C26 C27 C22 -177.9(5) . . . . ? C23 C22 C27 O4 177.3(5) . . . . ? C21 C22 C27 O4 -1.0(8) . . . . ? C23 C22 C27 C26 -1.2(8) . . . . ? C21 C22 C27 C26 -179.6(5) . . . . ? C27 C26 C28 C1 78.0(8) . . . . ? C25 C26 C28 C1 -101.5(7) . . . . ? C6 C1 C28 C26 -91.8(8) . . . . ? C2 C1 C28 C26 87.9(8) . . . . ? C30 N1 C29 Rh1 38(13) . . . . ? C41 Rh1 C29 N1 32(6) . . . . ? C48 Rh1 C29 N1 156(4) . . . . ? C34 Rh1 C29 N1 -21(4) . . . . ? C29 N1 C30 C53 23(10) . . . . ? C29 N1 C30 C55 -94(10) . . . . ? C29 N1 C30 C54 143(9) . . . . ? C29 N1 C30 C32 83(10) . . . . ? C29 N1 C30 C33 -154(9) . . . . ? C29 N1 C30 C31 -38(10) . . . . ? N1 C30 C32 C45 59.8(8) . . . 3_575 ? C53 C30 C32 C45 157.0(11) . . . 3_575 ? C55 C30 C32 C45 -127(2) . . . 3_575 ? C54 C30 C32 C45 -35.7(10) . . . 3_575 ? C33 C30 C32 C45 -62.9(9) . . . 3_575 ? C31 C30 C32 C45 178.9(7) . . . 3_575 ? N1 C30 C32 C46 -65.4(8) . . . 3_575 ? C53 C30 C32 C46 31.8(9) . . . 3_575 ? C55 C30 C32 C46 108(2) . . . 3_575 ? C54 C30 C32 C46 -160.9(12) . . . 3_575 ? C33 C30 C32 C46 172.0(7) . . . 3_575 ? C31 C30 C32 C46 53.7(9) . . . 3_575 ? N1 C30 C53 C46 67.4(12) . . . 3_575 ? C55 C30 C53 C46 178.0(13) . . . 3_575 ? C54 C30 C53 C46 -46.1(16) . . . 3_575 ? C32 C30 C53 C46 -34.4(9) . . . 3_575 ? C33 C30 C53 C46 -117.2(14) . . . 3_575 ? C31 C30 C53 C46 170.0(15) . . . 3_575 ? N1 C30 C54 C45 -67.6(14) . . . 3_575 ? C53 C30 C54 C45 46.9(17) . . . 3_575 ? C55 C30 C54 C45 179.9(13) . . . 3_575 ? C32 C30 C54 C45 35.4(10) . . . 3_575 ? C33 C30 C54 C45 -173.9(17) . . . 3_575 ? C31 C30 C54 C45 114.0(17) . . . 3_575 ? C35 N2 C34 Rh1 -92(11) . . . . ? C41 Rh1 C34 N2 -136(7) . . . . ? C48 Rh1 C34 N2 -51(10) . . . . ? C29 Rh1 C34 N2 40(7) . . . . ? C34 N2 C35 C60 160(8) . . . . ? C34 N2 C35 C37 -158(8) . . . . ? C34 N2 C35 C59 24(9) . . . . ? C34 N2 C35 C61 -93(8) . . . . ? C34 N2 C35 C36 87(8) . . . . ? C34 N2 C35 C38 -33(8) . . . . ? C48 N4 C49 C51 111(7) . . . . ? C48 N4 C49 C62 -76(8) . . . . ? C48 N4 C49 C52 -16(8) . . . . ? C48 N4 C49 C63 156(7) . . . . ? C48 N4 C49 C64 38(8) . . . . ? C48 N4 C49 C50 -134(7) . . . . ? C59 C39 C38 C40 162.9(12) . . . . ? C62 C39 C38 C40 -33.9(10) 3_575 . . . ? C52 C39 C38 C40 -51.1(8) 3_575 . . . ? C59 C39 C38 C35 37.5(10) . . . . ? C62 C39 C38 C35 -159.4(10) 3_575 . . . ? C52 C39 C38 C35 -176.6(6) 3_575 . . . ? C50 C40 C38 C39 52.2(9) 3_575 . . . ? C61 C40 C38 C39 -154.3(14) . . . . ? C62 C40 C38 C39 34.0(10) 3_575 . . . ? C50 C40 C38 C35 176.9(6) 3_575 . . . ? C61 C40 C38 C35 -29.6(13) . . . . ? C62 C40 C38 C35 158.7(11) 3_575 . . . ? N2 C35 C38 C39 62.3(7) . . . . ? C60 C35 C38 C39 -142(3) . . . . ? C37 C35 C38 C39 -178.7(7) . . . . ? C59 C35 C38 C39 -38.1(11) . . . . ? C61 C35 C38 C39 154.1(14) . . . . ? C36 C35 C38 C39 -55.7(8) . . . . ? N2 C35 C38 C40 -62.0(7) . . . . ? C60 C35 C38 C40 94(3) . . . . ? C37 C35 C38 C40 56.9(9) . . . . ? C59 C35 C38 C40 -162.4(12) . . . . ? C61 C35 C38 C40 29.8(13) . . . . ? C36 C35 C38 C40 -180.0(6) . . . . ? N4 C49 C50 C40 64.2(8) . . . 3_575 ? C51 C49 C50 C40 177.1(7) . . . 3_575 ? C62 C49 C50 C40 -36.2(10) . . . 3_575 ? C52 C49 C50 C40 -53.3(9) . . . 3_575 ? C63 C49 C50 C40 177.6(13) . . . 3_575 ? C64 C49 C50 C40 -101(2) . . . 3_575 ? N4 C49 C52 C39 -62.3(9) . . . 3_575 ? C51 C49 C52 C39 177.7(8) . . . 3_575 ? C62 C49 C52 C39 36.1(10) . . . 3_575 ? C63 C49 C52 C39 126.6(16) . . . 3_575 ? C64 C49 C52 C39 -157.7(16) . . . 3_575 ? C50 C49 C52 C39 53.1(9) . . . 3_575 ? N4 C49 C62 C39 65.4(13) . . . 3_575 ? C51 C49 C62 C39 -126.1(15) . . . 3_575 ? C52 C49 C62 C39 -36.4(10) . . . 3_575 ? C63 C49 C62 C39 -163.7(14) . . . 3_575 ? C64 C49 C62 C39 -47.5(17) . . . 3_575 ? C50 C49 C62 C39 163.1(17) . . . 3_575 ? N4 C49 C62 C40 -61.7(13) . . . 3_575 ? C51 C49 C62 C40 106.7(18) . . . 3_575 ? C52 C49 C62 C40 -163.6(17) . . . 3_575 ? C63 C49 C62 C40 69.1(17) . . . 3_575 ? C64 C49 C62 C40 -174.7(14) . . . 3_575 ? C50 C49 C62 C40 36.0(9) . . . 3_575 ? N2 C35 C59 C39 -58.9(18) . . . . ? C60 C35 C59 C39 178(2) . . . . ? C37 C35 C59 C39 124.7(15) . . . . ? C61 C35 C59 C39 50(2) . . . . ? C36 C35 C59 C39 -160(2) . . . . ? C38 C35 C59 C39 38.8(11) . . . . ? C38 C39 C59 C35 -39.7(12) . . . . ? C62 C39 C59 C35 -56(2) 3_575 . . . ? C52 C39 C59 C35 -118.4(14) 3_575 . . . ? C50 C40 C61 C35 110.8(19) 3_575 . . . ? C62 C40 C61 C35 39(3) 3_575 . . . ? C38 C40 C61 C35 31.1(14) . . . . ? N2 C35 C61 C40 72(2) . . . . ? C60 C35 C61 C40 179(2) . . . . ? C37 C35 C61 C40 177(3) . . . . ? C59 C35 C61 C40 -42(3) . . . . ? C36 C35 C61 C40 -108(2) . . . . ? C38 C35 C61 C40 -30.7(14) . . . . ? C42 N3 C41 Rh1 115(10) . . . . ? C48 Rh1 C41 N3 -64(11) . . . . ? C34 Rh1 C41 N3 112(11) . . . . ? C29 Rh1 C41 N3 60(12) . . . . ? C41 N3 C42 C58 31(4) . . . . ? C41 N3 C42 C56 154(3) . . . . ? C41 N3 C42 C43 -149(3) . . . . ? C41 N3 C42 C47 -26(4) . . . . ? C41 N3 C42 C44 90(3) . . . . ? C41 N3 C42 C57 -89(3) . . . . ? C45 C58 C42 N3 67.0(11) . . . . ? C46 C58 C42 N3 -62.1(11) . . . . ? C45 C58 C42 C56 -56.2(14) . . . . ? C46 C58 C42 C56 174.6(11) . . . . ? C45 C58 C42 C43 -112.7(16) . . . . ? C46 C58 C42 C43 118.2(15) . . . . ? C45 C58 C42 C47 168.1(14) . . . . ? C46 C58 C42 C47 38.9(9) . . . . ? C45 C58 C42 C44 -34.8(9) . . . . ? C46 C58 C42 C44 -163.9(14) . . . . ? C45 C58 C42 C57 -178.2(10) . . . . ? C46 C58 C42 C57 52.6(14) . . . . ? C46 C47 C42 N3 58.1(9) . . . . ? C46 C47 C42 C58 -38.7(9) . . . . ? C46 C47 C42 C56 -122.4(15) . . . . ? C46 C47 C42 C43 178.5(8) . . . . ? C46 C47 C42 C44 -58.5(10) . . . . ? C46 C47 C42 C57 155.8(12) . . . . ? C45 C44 C42 N3 -61.3(9) . . . . ? C45 C44 C42 C58 35.5(9) . . . . ? C45 C44 C42 C56 -167.6(13) . . . . ? C45 C44 C42 C43 178.9(8) . . . . ? C45 C44 C42 C47 54.9(10) . . . . ? C45 C44 C42 C57 116.7(16) . . . . ? C42 C44 C45 C32 -53.9(10) . . . 3_575 ? C42 C44 C45 C58 -34.4(9) . . . . ? C42 C44 C45 C54 -119.7(15) . . . 3_575 ? C42 C58 C45 C44 36.0(9) . . . . ? C46 C58 C45 C44 166.5(13) . . . . ? C42 C58 C45 C32 -164.9(13) . . . 3_575 ? C46 C58 C45 C32 -34.3(8) . . . 3_575 ? C42 C58 C45 C54 -178.9(10) . . . 3_575 ? C46 C58 C45 C54 -48.3(13) . . . 3_575 ? C42 C47 C46 C53 114.8(16) . . . 3_575 ? C42 C47 C46 C58 37.7(9) . . . . ? C42 C47 C46 C32 59.4(10) . . . 3_575 ? C42 C58 C46 C53 174.2(10) . . . 3_575 ? C45 C58 C46 C53 43.6(13) . . . 3_575 ? C42 C58 C46 C47 -39.7(9) . . . . ? C45 C58 C46 C47 -170.4(14) . . . . ? C42 C58 C46 C32 164.5(13) . . . 3_575 ? C45 C58 C46 C32 33.9(8) . . . 3_575 ? C49 N4 C48 Rh1 -52(13) . . . . ? C41 Rh1 C48 N4 29(7) . . . . ? C34 Rh1 C48 N4 -57(10) . . . . ? C29 Rh1 C48 N4 -147(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.999 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.092 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 248489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(diprop)4)(BPh4)2xCH3CN _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C70 H67 B2 N9 Rh2' _chemical_formula_weight 1261.77 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 15.4675(5) _cell_length_b 12.4293(4) _cell_length_c 17.1086(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.8630(10) _cell_angle_gamma 90.00 _cell_volume 3030.73(16) _cell_formula_units_Z 2 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.30 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.8301 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent acetonitrile / diethyl ether ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 49427 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7860 _reflns_number_gt 5461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+3.4830P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7860 _refine_ls_number_parameters 407 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.351670(16) 0.620380(18) 0.057086(14) 0.01406(7) Uani 1 1 d . . . N1 N 0.1991(2) 0.6288(2) 0.13334(18) 0.0275(6) Uani 1 1 d . . . N2 N 0.20815(16) 0.6287(2) -0.13048(15) 0.0158(5) Uani 1 1 d . . . N3 N 0.5017(2) 0.6317(2) -0.02195(18) 0.0253(6) Uani 1 1 d . . . N4 N 0.49811(18) 0.6312(2) 0.24246(16) 0.0245(6) Uani 1 1 d . . . B1 B 0.1756(3) 0.2500 0.3323(3) 0.0137(9) Uani 1 2 d S . . B2 B 0.1542(3) 0.2500 -0.2504(3) 0.0123(9) Uani 1 2 d S . . C1 C 0.2534(2) 0.6215(2) 0.10350(18) 0.0176(6) Uani 1 1 d . . . C2 C 0.1372(3) 0.6455(3) 0.1777(3) 0.0506(13) Uani 1 1 d D . . H2A H 0.1747 0.6412 0.2395 0.061 Uiso 1 1 calc R A 1 H2B H 0.0907 0.5864 0.1627 0.061 Uiso 1 1 calc R A 1 C3A C 0.0858(4) 0.7500 0.1592(4) 0.0195(12) Uani 0.79 2 d SPD . 1 H3AA H 0.0437 0.7500 0.1905 0.023 Uiso 0.79 2 calc SPR . 1 H3AB H 0.0450 0.7500 0.0980 0.023 Uiso 0.79 2 calc SPR . 1 C3B C 0.112(3) 0.7500 0.207(2) 0.066(11) Uiso 0.21 2 d SPD . 2 H3BA H 0.0437 0.7500 0.1914 0.079 Uiso 0.21 2 calc SPR . 2 H3BB H 0.1418 0.7500 0.2700 0.079 Uiso 0.21 2 calc SPR . 2 C4 C 0.2584(2) 0.6213(2) -0.06127(18) 0.0160(6) Uani 1 1 d . . . C5 C 0.1508(2) 0.6471(2) -0.21893(18) 0.0173(6) Uani 1 1 d . . . H5A H 0.0841 0.6523 -0.2265 0.021 Uiso 1 1 calc R . . H5B H 0.1571 0.5854 -0.2529 0.021 Uiso 1 1 calc R . . C6 C 0.1795(3) 0.7500 -0.2506(3) 0.0162(9) Uani 1 2 d S . . H6A H 0.1512 0.7500 -0.3134 0.019 Uiso 1 2 calc SR . . H6B H 0.2485 0.7500 -0.2329 0.019 Uiso 1 2 calc SR . . C7 C 0.4492(2) 0.6243(3) 0.00967(19) 0.0202(6) Uani 1 1 d . . . C8 C 0.5653(3) 0.6481(3) -0.0650(3) 0.0322(8) Uani 1 1 d D . . H8A H 0.5288 0.6488 -0.1271 0.039 Uiso 1 1 calc R B 1 H8B H 0.6100 0.5872 -0.0519 0.039 Uiso 1 1 calc R B 1 C9A C 0.6184(4) 0.7500 -0.0395(4) 0.0223(12) Uani 0.78 2 d SP . 1 H9AA H 0.6677 0.7500 -0.0631 0.027 Uiso 0.78 2 calc SPR . 1 H9AB H 0.6507 0.7500 0.0230 0.027 Uiso 0.78 2 calc SPR . 1 C9B C 0.574(3) 0.7500 -0.1085(14) 0.064(9) Uiso 0.22 2 d SPD . 2 H9BA H 0.5251 0.7500 -0.1667 0.077 Uiso 0.22 2 calc SPR . 2 H9BB H 0.6357 0.7500 -0.1134 0.077 Uiso 0.22 2 calc SPR . 2 C10 C 0.4455(2) 0.6240(3) 0.17350(19) 0.0199(6) Uani 1 1 d . . . C11 C 0.5633(3) 0.6485(3) 0.3287(2) 0.0323(9) Uani 1 1 d . . . H11A H 0.6278 0.6525 0.3299 0.039 Uiso 1 1 calc R . . H11B H 0.5606 0.5863 0.3639 0.039 Uiso 1 1 calc R . . C12 C 0.5427(3) 0.7500 0.3664(3) 0.0235(10) Uani 1 2 d S . . H12A H 0.5804 0.7500 0.4282 0.028 Uiso 1 2 calc SR . . H12B H 0.4756 0.7500 0.3580 0.028 Uiso 1 2 calc SR . . C13 C 0.2461(2) 0.3545(2) 0.35708(18) 0.0161(6) Uani 1 1 d . . . C14 C 0.2817(2) 0.3979(3) 0.3001(2) 0.0267(7) Uani 1 1 d . . . H14A H 0.2620 0.3682 0.2448 0.032 Uiso 1 1 calc R . . C15 C 0.3452(3) 0.4834(3) 0.3220(2) 0.0355(10) Uani 1 1 d . . . H15A H 0.3677 0.5108 0.2816 0.043 Uiso 1 1 calc R . . C16 C 0.3753(3) 0.5284(3) 0.4019(2) 0.0340(9) Uani 1 1 d . . . H16A H 0.4180 0.5871 0.4166 0.041 Uiso 1 1 calc R . . C17 C 0.3428(2) 0.4871(3) 0.4601(2) 0.0250(8) Uani 1 1 d . . . H17A H 0.3634 0.5172 0.5154 0.030 Uiso 1 1 calc R . . C18 C 0.2799(2) 0.4013(2) 0.43822(19) 0.0189(6) Uani 1 1 d . . . H18A H 0.2592 0.3734 0.4796 0.023 Uiso 1 1 calc R . . C19 C 0.1043(3) 0.2500 0.3826(2) 0.0130(8) Uani 1 2 d S . . C20 C 0.0679(2) 0.3451(2) 0.40163(18) 0.0177(6) Uani 1 1 d . . . H20A H 0.0877 0.4121 0.3875 0.021 Uiso 1 1 calc R . . C21 C 0.0039(2) 0.3451(3) 0.44042(19) 0.0235(7) Uani 1 1 d . . . H21A H -0.0187 0.4116 0.4525 0.028 Uiso 1 1 calc R . . C22 C -0.0273(3) 0.2500 0.4615(3) 0.0267(11) Uani 1 2 d S . . H22A H -0.0693 0.2500 0.4899 0.032 Uiso 1 2 calc SR . . C23 C 0.1045(3) 0.2500 0.2319(3) 0.0152(8) Uani 1 2 d S . . C24 C 0.0663(2) 0.3449(3) 0.18923(19) 0.0210(7) Uani 1 1 d . . . H24A H 0.0902 0.4116 0.2161 0.025 Uiso 1 1 calc R . . C25 C -0.0057(2) 0.3460(3) 0.10869(19) 0.0240(7) Uani 1 1 d . . . H25A H -0.0291 0.4125 0.0812 0.029 Uiso 1 1 calc R . . C26 C -0.0429(3) 0.2500 0.0692(3) 0.0270(11) Uani 1 2 d S . . H26A H -0.0936 0.2500 0.0153 0.032 Uiso 1 2 calc SR . . C27 C 0.20709(19) 0.3559(2) -0.26983(17) 0.0125(6) Uani 1 1 d . . . C28 C 0.1785(2) 0.3999(2) -0.35165(18) 0.0159(6) Uani 1 1 d . . . H28A H 0.1273 0.3675 -0.3963 0.019 Uiso 1 1 calc R . . C29 C 0.2216(2) 0.4886(2) -0.3700(2) 0.0202(7) Uani 1 1 d . . . H29A H 0.1993 0.5163 -0.4262 0.024 Uiso 1 1 calc R . . C30 C 0.2975(2) 0.5371(2) -0.3064(2) 0.0219(7) Uani 1 1 d . . . H30A H 0.3267 0.5988 -0.3181 0.026 Uiso 1 1 calc R . . C31 C 0.3297(2) 0.4936(2) -0.2257(2) 0.0205(7) Uani 1 1 d . . . H31A H 0.3825 0.5247 -0.1818 0.025 Uiso 1 1 calc R . . C32 C 0.2855(2) 0.4049(2) -0.20806(18) 0.0168(6) Uani 1 1 d . . . H32A H 0.3094 0.3765 -0.1521 0.020 Uiso 1 1 calc R . . C33 C 0.1579(3) 0.2500 -0.1523(3) 0.0152(8) Uani 1 2 d S . . C34 C 0.1544(2) 0.3452(2) -0.11029(19) 0.0184(6) Uani 1 1 d . . . H34A H 0.1548 0.4120 -0.1372 0.022 Uiso 1 1 calc R . . C35 C 0.1503(2) 0.3461(3) -0.0304(2) 0.0220(7) Uani 1 1 d . . . H35A H 0.1483 0.4126 -0.0038 0.026 Uiso 1 1 calc R . . C36 C 0.1491(3) 0.2500 0.0106(3) 0.0234(10) Uani 1 2 d S . . H36A H 0.1476 0.2500 0.0655 0.028 Uiso 1 2 calc SR . . C37 C 0.0405(3) 0.2500 -0.3079(2) 0.0133(8) Uani 1 2 d S . . C38 C -0.0122(2) 0.3455(2) -0.33005(18) 0.0166(6) Uani 1 1 d . . . H38A H 0.0199 0.4124 -0.3158 0.020 Uiso 1 1 calc R . . C39 C -0.1092(2) 0.3460(2) -0.37190(19) 0.0194(6) Uani 1 1 d . . . H39A H -0.1419 0.4125 -0.3861 0.023 Uiso 1 1 calc R . . C40 C -0.1586(3) 0.2500 -0.3931(3) 0.0204(9) Uani 1 2 d S . . H40A H -0.2250 0.2500 -0.4217 0.024 Uiso 1 2 calc SR . . C1S C 0.4903(4) 0.2500 0.4187(3) 0.0366(13) Uani 1 2 d S . . H1SA H 0.5506 0.2344 0.4650 0.055 Uiso 0.50 1 calc PR . . H1SB H 0.4444 0.1949 0.4174 0.055 Uiso 0.50 1 calc PR . . H1SC H 0.4679 0.3207 0.4279 0.055 Uiso 0.50 1 calc PR . . C2S C 0.5020(4) 0.2500 0.3386(4) 0.0456(15) Uani 1 2 d S . . N1S N 0.5115(4) 0.2500 0.2751(4) 0.0711(19) Uani 1 2 d S . . 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 0.01487(11) 0.01443(11) 0.01279(10) 0.00011(10) 0.00527(8) 0.00208(10) N1 0.0373(16) 0.0174(13) 0.0381(16) 0.0075(13) 0.0257(14) 0.0083(13) N2 0.0175(12) 0.0139(12) 0.0175(12) 0.0008(10) 0.0083(10) 0.0005(10) N3 0.0300(15) 0.0176(13) 0.0358(15) -0.0002(13) 0.0210(13) 0.0004(12) N4 0.0207(14) 0.0332(16) 0.0165(12) -0.0036(12) 0.0039(11) 0.0064(12) B1 0.014(2) 0.014(2) 0.013(2) 0.000 0.0063(18) 0.000 B2 0.013(2) 0.012(2) 0.011(2) 0.000 0.0039(17) 0.000 C1 0.0184(14) 0.0140(13) 0.0202(14) 0.0040(13) 0.0074(12) 0.0063(13) C2 0.073(3) 0.030(2) 0.085(3) 0.012(2) 0.071(3) 0.013(2) C3A 0.026(3) 0.020(3) 0.024(3) 0.000 0.021(3) 0.000 C4 0.0190(14) 0.0137(13) 0.0178(14) -0.0009(13) 0.0097(12) 0.0006(12) C5 0.0176(15) 0.0207(15) 0.0113(13) -0.0024(11) 0.0032(11) -0.0007(12) C6 0.018(2) 0.020(2) 0.0100(18) 0.000 0.0055(16) 0.000 C7 0.0213(15) 0.0161(14) 0.0237(15) 0.0005(14) 0.0093(12) 0.0000(13) C8 0.038(2) 0.0238(18) 0.048(2) -0.0010(16) 0.0306(18) 0.0009(15) C9A 0.015(3) 0.027(3) 0.027(3) 0.000 0.010(2) 0.000 C10 0.0195(15) 0.0198(14) 0.0210(15) -0.0015(14) 0.0086(12) 0.0051(13) C11 0.0286(19) 0.047(2) 0.0131(15) -0.0040(15) -0.0012(14) 0.0134(16) C12 0.020(2) 0.035(3) 0.014(2) 0.000 0.0057(18) 0.000 C13 0.0135(14) 0.0128(13) 0.0186(14) 0.0032(11) 0.0027(11) -0.0001(10) C14 0.0230(16) 0.0328(19) 0.0221(15) 0.0041(14) 0.0064(13) -0.0076(14) C15 0.028(2) 0.045(2) 0.0282(19) 0.0162(17) 0.0055(16) -0.0174(17) C16 0.0263(19) 0.0269(18) 0.038(2) 0.0077(16) -0.0001(16) -0.0137(15) C17 0.0218(18) 0.0191(15) 0.0229(17) -0.0001(13) -0.0035(14) -0.0009(13) C18 0.0179(15) 0.0163(15) 0.0193(14) 0.0037(12) 0.0038(12) 0.0019(12) C19 0.0111(19) 0.0157(19) 0.0088(17) 0.000 0.0002(15) 0.000 C20 0.0151(14) 0.0197(14) 0.0151(13) -0.0018(11) 0.0024(11) -0.0001(11) C21 0.0154(15) 0.0351(18) 0.0157(14) -0.0121(13) 0.0013(12) 0.0023(13) C22 0.013(2) 0.053(3) 0.011(2) 0.000 0.0017(17) 0.000 C23 0.0114(19) 0.022(2) 0.0127(19) 0.000 0.0052(16) 0.000 C24 0.0206(16) 0.0250(16) 0.0173(15) -0.0012(12) 0.0071(13) -0.0026(13) C25 0.0186(16) 0.0378(19) 0.0158(14) 0.0078(13) 0.0069(13) 0.0065(14) C26 0.016(2) 0.051(3) 0.014(2) 0.000 0.0055(18) 0.000 C27 0.0127(13) 0.0102(13) 0.0166(13) -0.0020(10) 0.0079(11) 0.0017(10) C28 0.0143(14) 0.0166(15) 0.0175(13) 0.0012(11) 0.0068(11) 0.0012(11) C29 0.0210(17) 0.0215(15) 0.0223(16) 0.0039(12) 0.0128(14) 0.0045(12) C30 0.0248(17) 0.0142(14) 0.0353(18) -0.0013(13) 0.0211(15) -0.0021(13) C31 0.0161(16) 0.0205(15) 0.0264(17) -0.0083(13) 0.0098(14) -0.0046(12) C32 0.0146(14) 0.0196(15) 0.0157(13) -0.0018(11) 0.0052(11) -0.0003(11) C33 0.013(2) 0.016(2) 0.017(2) 0.000 0.0060(16) 0.000 C34 0.0203(15) 0.0167(14) 0.0193(14) -0.0007(12) 0.0089(12) -0.0019(12) C35 0.0205(16) 0.0239(16) 0.0233(15) -0.0068(13) 0.0104(13) -0.0013(13) C36 0.020(2) 0.035(3) 0.017(2) 0.000 0.0087(19) 0.000 C37 0.015(2) 0.0159(19) 0.0113(18) 0.000 0.0079(16) 0.000 C38 0.0182(15) 0.0136(13) 0.0199(14) 0.0000(11) 0.0095(12) -0.0014(11) C39 0.0180(15) 0.0188(14) 0.0235(15) 0.0033(12) 0.0104(13) 0.0040(12) C40 0.011(2) 0.026(2) 0.024(2) 0.000 0.0066(18) 0.000 C1S 0.026(3) 0.053(3) 0.030(3) 0.000 0.010(2) 0.000 C2S 0.034(3) 0.069(4) 0.036(3) 0.000 0.016(3) 0.000 N1S 0.061(4) 0.109(6) 0.055(4) 0.000 0.036(3) 0.000 _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 C10 1.957(3) . ? Rh1 C1 1.969(3) . ? Rh1 C7 1.971(3) . ? Rh1 C4 1.978(3) . ? N1 C1 1.144(4) . ? N1 C2 1.450(4) . ? N2 C4 1.140(4) . ? N2 C5 1.444(3) . ? N3 C7 1.141(4) . ? N3 C8 1.454(4) . ? N4 C10 1.147(4) . ? N4 C11 1.443(4) . ? B1 C19 1.641(6) . ? B1 C23 1.641(6) . ? B1 C13 1.642(4) . ? B1 C13 1.642(4) 4_565 ? B2 C37 1.649(6) . ? B2 C27 1.650(4) 4_565 ? B2 C27 1.650(4) . ? B2 C33 1.656(6) . ? C2 C3A 1.491(3) . ? C2 C3B 1.496(5) . ? C3A C2 1.491(4) 4_575 ? C3B C2 1.496(5) 4_575 ? C5 C6 1.521(4) . ? C6 C5 1.521(4) 4_575 ? C8 C9A 1.480(5) . ? C8 C9B 1.501(5) . ? C9A C8 1.480(5) 4_575 ? C9B C8 1.501(5) 4_575 ? C11 C12 1.507(4) . ? C12 C11 1.507(4) 4_575 ? C13 C14 1.401(4) . ? C13 C18 1.405(4) . ? C14 C15 1.395(5) . ? C15 C16 1.380(5) . ? C16 C17 1.377(5) . ? C17 C18 1.393(4) . ? C19 C20 1.401(4) . ? C19 C20 1.401(4) 4_565 ? C20 C21 1.390(4) . ? C21 C22 1.377(4) . ? C22 C21 1.377(4) 4_565 ? C23 C24 1.392(4) . ? C23 C24 1.392(4) 4_565 ? C24 C25 1.395(4) . ? C25 C26 1.382(4) . ? C26 C25 1.382(4) 4_565 ? C27 C32 1.401(4) . ? C27 C28 1.405(4) . ? C28 C29 1.386(4) . ? C29 C30 1.391(5) . ? C30 C31 1.383(5) . ? C31 C32 1.391(4) . ? C33 C34 1.397(4) 4_565 ? C33 C34 1.397(4) . ? C34 C35 1.393(4) . ? C35 C36 1.388(4) . ? C36 C35 1.388(4) 4_565 ? C37 C38 1.406(4) . ? C37 C38 1.406(4) 4_565 ? C38 C39 1.389(4) . ? C39 C40 1.387(4) . ? C40 C39 1.388(4) 4_565 ? C1S C2S 1.450(8) . ? C2S N1S 1.152(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Rh1 C1 88.42(12) . . ? C10 Rh1 C7 92.01(12) . . ? C1 Rh1 C7 178.14(12) . . ? C10 Rh1 C4 178.14(13) . . ? C1 Rh1 C4 92.46(12) . . ? C7 Rh1 C4 87.06(12) . . ? C1 N1 C2 174.0(4) . . ? C4 N2 C5 174.0(3) . . ? C7 N3 C8 176.0(3) . . ? C10 N4 C11 175.9(4) . . ? C19 B1 C23 103.6(3) . . ? C19 B1 C13 112.3(2) . . ? C23 B1 C13 112.2(2) . . ? C19 B1 C13 112.3(2) . 4_565 ? C23 B1 C13 112.2(2) . 4_565 ? C13 B1 C13 104.6(3) . 4_565 ? C37 B2 C27 112.1(2) . 4_565 ? C37 B2 C27 112.1(2) . . ? C27 B2 C27 105.8(3) 4_565 . ? C37 B2 C33 102.3(3) . . ? C27 B2 C33 112.3(2) 4_565 . ? C27 B2 C33 112.3(2) . . ? N1 C1 Rh1 175.1(3) . . ? N1 C2 C3A 114.8(4) . . ? N1 C2 C3B 127.5(7) . . ? C3A C2 C3B 29.6(14) . . ? C2 C3A C2 121.1(5) . 4_575 ? C2 C3B C2 120.4(8) 4_575 . ? N2 C4 Rh1 174.7(3) . . ? N2 C5 C6 111.2(3) . . ? C5 C6 C5 114.4(3) . 4_575 ? N3 C7 Rh1 175.1(3) . . ? N3 C8 C9A 112.2(4) . . ? N3 C8 C9B 125.3(10) . . ? C9A C8 C9B 43.7(11) . . ? C8 C9A C8 117.7(5) . 4_575 ? C8 C9B C8 115.1(8) . 4_575 ? N4 C10 Rh1 176.2(3) . . ? N4 C11 C12 112.5(3) . . ? C11 C12 C11 113.8(4) . 4_575 ? C14 C13 C18 115.6(3) . . ? C14 C13 B1 121.8(3) . . ? C18 C13 B1 122.5(3) . . ? C15 C14 C13 122.2(3) . . ? C16 C15 C14 120.4(3) . . ? C17 C16 C15 119.2(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C13 122.4(3) . . ? C20 C19 C20 115.1(4) . 4_565 ? C20 C19 B1 122.31(19) . . ? C20 C19 B1 122.31(19) 4_565 . ? C21 C20 C19 122.4(3) . . ? C22 C21 C20 120.8(3) . . ? C21 C22 C21 118.3(4) . 4_565 ? C24 C23 C24 115.8(4) . 4_565 ? C24 C23 B1 121.62(19) . . ? C24 C23 B1 121.62(19) 4_565 . ? C23 C24 C25 122.7(3) . . ? C26 C25 C24 119.7(3) . . ? C25 C26 C25 119.4(4) . 4_565 ? C32 C27 C28 115.3(3) . . ? C32 C27 B2 123.1(3) . . ? C28 C27 B2 121.5(3) . . ? C29 C28 C27 122.8(3) . . ? C28 C29 C30 120.1(3) . . ? C31 C30 C29 118.6(3) . . ? C30 C31 C32 120.6(3) . . ? C31 C32 C27 122.4(3) . . ? C34 C33 C34 115.9(4) 4_565 . ? C34 C33 B2 121.89(19) 4_565 . ? C34 C33 B2 121.90(19) . . ? C35 C34 C33 122.5(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C35 118.7(4) . 4_565 ? C38 C37 C38 115.2(4) . 4_565 ? C38 C37 B2 122.21(19) . . ? C38 C37 B2 122.21(19) 4_565 . ? C39 C38 C37 122.7(3) . . ? C40 C39 C38 120.4(3) . . ? C39 C40 C39 118.7(4) . 4_565 ? N1S C2S C1S 179.8(7) . . ? 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 C2 N1 C1 Rh1 -21(6) . . . . ? C10 Rh1 C1 N1 57(3) . . . . ? C7 Rh1 C1 N1 -46(6) . . . . ? C4 Rh1 C1 N1 -121(3) . . . . ? C1 N1 C2 C3A 79(3) . . . . ? C1 N1 C2 C3B 47(4) . . . . ? N1 C2 C3A C2 -60.2(8) . . . 4_575 ? C3B C2 C3A C2 62.8(17) . . . 4_575 ? N1 C2 C3B C2 12(4) . . . 4_575 ? C3A C2 C3B C2 -61.7(17) . . . 4_575 ? C5 N2 C4 Rh1 6(5) . . . . ? C10 Rh1 C4 N2 7(6) . . . . ? C1 Rh1 C4 N2 125(3) . . . . ? C7 Rh1 C4 N2 -53(3) . . . . ? C4 N2 C5 C6 -11(3) . . . . ? N2 C5 C6 C5 -73.3(4) . . . 4_575 ? C8 N3 C7 Rh1 18(8) . . . . ? C10 Rh1 C7 N3 -138(3) . . . . ? C1 Rh1 C7 N3 -34(6) . . . . ? C4 Rh1 C7 N3 41(3) . . . . ? C7 N3 C8 C9A 61(5) . . . . ? C7 N3 C8 C9B 13(5) . . . . ? N3 C8 C9A C8 -67.5(6) . . . 4_575 ? C9B C8 C9A C8 50.9(15) . . . 4_575 ? N3 C8 C9B C8 37(3) . . . 4_575 ? C9A C8 C9B C8 -48.5(14) . . . 4_575 ? C11 N4 C10 Rh1 -29(8) . . . . ? C1 Rh1 C10 N4 -56(5) . . . . ? C7 Rh1 C10 N4 122(5) . . . . ? C4 Rh1 C10 N4 62(7) . . . . ? C10 N4 C11 C12 26(5) . . . . ? N4 C11 C12 C11 -70.2(5) . . . 4_575 ? C19 B1 C13 C14 -151.5(3) . . . . ? C23 B1 C13 C14 -35.3(4) . . . . ? C13 B1 C13 C14 86.5(4) 4_565 . . . ? C19 B1 C13 C18 33.2(4) . . . . ? C23 B1 C13 C18 149.4(3) . . . . ? C13 B1 C13 C18 -88.7(4) 4_565 . . . ? C18 C13 C14 C15 -1.2(5) . . . . ? B1 C13 C14 C15 -176.8(3) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -0.3(5) . . . . ? C16 C17 C18 C13 -0.9(5) . . . . ? C14 C13 C18 C17 1.7(4) . . . . ? B1 C13 C18 C17 177.2(3) . . . . ? C23 B1 C19 C20 -86.6(3) . . . . ? C13 B1 C19 C20 34.7(5) . . . . ? C13 B1 C19 C20 152.1(3) 4_565 . . . ? C23 B1 C19 C20 86.6(3) . . . 4_565 ? C13 B1 C19 C20 -152.1(3) . . . 4_565 ? C13 B1 C19 C20 -34.7(5) 4_565 . . 4_565 ? C20 C19 C20 C21 3.1(5) 4_565 . . . ? B1 C19 C20 C21 176.7(3) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C21 -2.3(6) . . . 4_565 ? C19 B1 C23 C24 84.2(3) . . . . ? C13 B1 C23 C24 -37.2(5) . . . . ? C13 B1 C23 C24 -154.5(3) 4_565 . . . ? C19 B1 C23 C24 -84.2(3) . . . 4_565 ? C13 B1 C23 C24 154.5(3) . . . 4_565 ? C13 B1 C23 C24 37.2(5) 4_565 . . 4_565 ? C24 C23 C24 C25 -0.1(6) 4_565 . . . ? B1 C23 C24 C25 -169.1(3) . . . . ? C23 C24 C25 C26 1.3(5) . . . . ? C24 C25 C26 C25 -2.4(6) . . . 4_565 ? C37 B2 C27 C32 147.5(3) . . . . ? C27 B2 C27 C32 -89.9(3) 4_565 . . . ? C33 B2 C27 C32 32.9(4) . . . . ? C37 B2 C27 C28 -35.6(4) . . . . ? C27 B2 C27 C28 86.9(3) 4_565 . . . ? C33 B2 C27 C28 -150.2(3) . . . . ? C32 C27 C28 C29 -2.7(4) . . . . ? B2 C27 C28 C29 -179.8(3) . . . . ? C27 C28 C29 C30 0.9(5) . . . . ? C28 C29 C30 C31 1.3(5) . . . . ? C29 C30 C31 C32 -1.6(5) . . . . ? C30 C31 C32 C27 -0.4(5) . . . . ? C28 C27 C32 C31 2.5(4) . . . . ? B2 C27 C32 C31 179.5(3) . . . . ? C37 B2 C33 C34 86.4(3) . . . 4_565 ? C27 B2 C33 C34 -34.0(5) 4_565 . . 4_565 ? C27 B2 C33 C34 -153.1(3) . . . 4_565 ? C37 B2 C33 C34 -86.4(3) . . . . ? C27 B2 C33 C34 153.1(3) 4_565 . . . ? C27 B2 C33 C34 34.0(5) . . . . ? C34 C33 C34 C35 1.8(6) 4_565 . . . ? B2 C33 C34 C35 175.0(3) . . . . ? C33 C34 C35 C36 -0.3(5) . . . . ? C34 C35 C36 C35 -1.2(6) . . . 4_565 ? C27 B2 C37 C38 -153.1(3) 4_565 . . . ? C27 B2 C37 C38 -34.2(5) . . . . ? C33 B2 C37 C38 86.4(3) . . . . ? C27 B2 C37 C38 34.2(5) 4_565 . . 4_565 ? C27 B2 C37 C38 153.1(3) . . . 4_565 ? C33 B2 C37 C38 -86.4(3) . . . 4_565 ? C38 C37 C38 C39 -0.9(6) 4_565 . . . ? B2 C37 C38 C39 -174.1(3) . . . . ? C37 C38 C39 C40 0.5(5) . . . . ? C38 C39 C40 C39 -0.1(6) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.380 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.103 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 248490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(diprop)4)(BPh4)2x1.6C6H5CNx0.4C6H5Cl _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C81.60 H74 B2 Cl0.40 N9.60 Rh2' _chemical_formula_weight 1430.72 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6380(2) _cell_length_b 12.7472(3) _cell_length_c 15.6755(4) _cell_angle_alpha 67.8980(10) _cell_angle_beta 74.2350(10) _cell_angle_gamma 84.3740(10) _cell_volume 1717.20(7) _cell_formula_units_Z 1 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 870 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.26 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.7935 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent benzonitrile / chlorobenzene ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8763 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4845 _reflns_number_gt 4473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+5.5517P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4845 _refine_ls_number_parameters 389 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.16537(3) 0.02578(2) -0.00825(2) 0.01237(14) Uani 1 1 d . . . B1 B 0.1783(5) -0.2687(4) 0.5928(3) 0.0136(10) Uani 1 1 d . . . N1 N 0.1584(4) 0.1998(3) -0.2097(3) 0.0144(7) Uani 1 1 d . . . N2 N 0.0484(4) 0.2225(3) 0.0628(2) 0.0147(7) Uani 1 1 d . . . N3 N 0.1421(4) -0.1427(3) 0.2010(3) 0.0193(8) Uani 1 1 d . . . N4 N 0.2579(4) -0.1674(3) -0.0894(2) 0.0162(8) Uani 1 1 d . . . C1 C 0.1659(4) 0.1343(3) -0.1367(3) 0.0145(9) Uani 1 1 d . . . C2 C 0.1496(5) 0.2804(4) -0.3023(3) 0.0198(9) Uani 1 1 d . . . H2A H 0.1930 0.2466 -0.3510 0.024 Uiso 1 1 calc R . . H2B H 0.2065 0.3487 -0.3178 0.024 Uiso 1 1 calc R . . C3 C 0.0947(4) 0.1490(4) 0.0384(3) 0.0148(9) Uani 1 1 d . . . C4 C -0.0156(4) 0.3133(3) 0.0943(3) 0.0165(9) Uani 1 1 d . . . H4A H 0.0491 0.3801 0.0610 0.020 Uiso 1 1 calc R . . H4B H -0.0245 0.2894 0.1634 0.020 Uiso 1 1 calc R . . C5 C -0.1633(4) 0.3468(3) 0.0756(3) 0.0159(9) Uani 1 1 d . . . H5A H -0.1532 0.3699 0.0064 0.019 Uiso 1 1 calc R . . H5B H -0.1961 0.4138 0.0930 0.019 Uiso 1 1 calc R . . C6 C 0.1582(4) -0.0807(4) 0.1230(3) 0.0170(9) Uani 1 1 d . . . C7 C 0.1022(5) -0.2231(4) 0.2978(3) 0.0212(10) Uani 1 1 d . . . H7A H 0.0523 -0.1831 0.3408 0.025 Uiso 1 1 calc R . . H7B H 0.1902 -0.2582 0.3175 0.025 Uiso 1 1 calc R . . C8 C 0.0038(5) -0.3150(4) 0.3069(3) 0.0193(9) Uani 1 1 d . . . H8A H 0.0476 -0.3446 0.2556 0.023 Uiso 1 1 calc R . . H8B H 0.0007 -0.3780 0.3683 0.023 Uiso 1 1 calc R . . C9 C 0.2306(4) -0.0963(3) -0.0587(3) 0.0150(9) Uani 1 1 d . . . C10 C 0.2803(4) -0.2558(3) -0.1284(3) 0.0165(9) Uani 1 1 d . . . H10A H 0.3757 -0.2909 -0.1240 0.020 Uiso 1 1 calc R . . H10B H 0.2803 -0.2224 -0.1966 0.020 Uiso 1 1 calc R . . C11 C 0.2914(4) -0.2671(3) 0.4931(3) 0.0138(9) Uani 1 1 d . . . C12 C 0.3286(4) -0.1660(4) 0.4144(3) 0.0170(9) Uani 1 1 d . . . H12A H 0.2914 -0.0969 0.4209 0.020 Uiso 1 1 calc R . . C13 C 0.4178(4) -0.1627(4) 0.3271(3) 0.0186(9) Uani 1 1 d . . . H13A H 0.4410 -0.0922 0.2758 0.022 Uiso 1 1 calc R . . C14 C 0.4730(4) -0.2621(4) 0.3148(3) 0.0195(9) Uani 1 1 d . . . H14A H 0.5341 -0.2601 0.2554 0.023 Uiso 1 1 calc R . . C15 C 0.4379(5) -0.3642(4) 0.3902(3) 0.0207(10) Uani 1 1 d . . . H15A H 0.4741 -0.4332 0.3828 0.025 Uiso 1 1 calc R . . C16 C 0.3489(4) -0.3650(4) 0.4772(3) 0.0183(9) Uani 1 1 d . . . H16A H 0.3264 -0.4359 0.5282 0.022 Uiso 1 1 calc R . . C17 C 0.2004(4) -0.3832(3) 0.6834(3) 0.0130(8) Uani 1 1 d . . . C18 C 0.3385(4) -0.4137(3) 0.6981(3) 0.0138(8) Uani 1 1 d . . . H18A H 0.4182 -0.3675 0.6549 0.017 Uiso 1 1 calc R . . C19 C 0.3637(5) -0.5090(4) 0.7735(3) 0.0179(9) Uani 1 1 d . . . H19A H 0.4588 -0.5262 0.7812 0.022 Uiso 1 1 calc R . . C20 C 0.2488(5) -0.5789(3) 0.8373(3) 0.0174(9) Uani 1 1 d . . . H20A H 0.2650 -0.6456 0.8875 0.021 Uiso 1 1 calc R . . C21 C 0.1114(5) -0.5498(3) 0.8266(3) 0.0164(9) Uani 1 1 d . . . H21A H 0.0320 -0.5959 0.8705 0.020 Uiso 1 1 calc R . . C22 C 0.0877(4) -0.4531(3) 0.7517(3) 0.0135(9) Uani 1 1 d . . . H22A H -0.0085 -0.4341 0.7469 0.016 Uiso 1 1 calc R . . C23 C 0.0180(4) -0.2646(3) 0.5728(3) 0.0131(8) Uani 1 1 d . . . C24 C -0.0403(5) -0.3616(4) 0.5735(3) 0.0173(9) Uani 1 1 d . . . H24A H 0.0133 -0.4298 0.5880 0.021 Uiso 1 1 calc R . . C25 C -0.1714(5) -0.3631(4) 0.5543(3) 0.0202(10) Uani 1 1 d . . . H25A H -0.2071 -0.4315 0.5571 0.024 Uiso 1 1 calc R . . C26 C -0.2519(4) -0.2631(4) 0.5306(3) 0.0207(10) Uani 1 1 d . . . H26A H -0.3430 -0.2629 0.5181 0.025 Uiso 1 1 calc R . . C27 C -0.1952(4) -0.1650(4) 0.5259(3) 0.0181(9) Uani 1 1 d . . . H27A H -0.2466 -0.0960 0.5082 0.022 Uiso 1 1 calc R . . C28 C -0.0640(4) -0.1663(3) 0.5467(3) 0.0131(8) Uani 1 1 d . . . H28A H -0.0282 -0.0975 0.5431 0.016 Uiso 1 1 calc R . . C29 C 0.2113(4) -0.1627(3) 0.6204(3) 0.0129(8) Uani 1 1 d . . . C30 C 0.1071(4) -0.1135(3) 0.6762(3) 0.0148(9) Uani 1 1 d . . . H30A H 0.0091 -0.1356 0.6925 0.018 Uiso 1 1 calc R . . C31 C 0.1408(4) -0.0343(3) 0.7084(3) 0.0145(9) Uani 1 1 d . . . H31A H 0.0668 -0.0033 0.7459 0.017 Uiso 1 1 calc R . . C32 C 0.2839(4) 0.0000(3) 0.6855(3) 0.0147(9) Uani 1 1 d . . . H32A H 0.3081 0.0539 0.7077 0.018 Uiso 1 1 calc R . . C33 C 0.3895(4) -0.0455(3) 0.6304(3) 0.0153(9) Uani 1 1 d . . . H33A H 0.4870 -0.0221 0.6138 0.018 Uiso 1 1 calc R . . C34 C 0.3541(4) -0.1255(3) 0.5989(3) 0.0124(8) Uani 1 1 d . . . H34A H 0.4289 -0.1561 0.5616 0.015 Uiso 1 1 calc R . . N1S N 0.2862(5) 0.5821(4) 0.1393(4) 0.0288(4) Uiso 0.80 1 d PD A 1 C1S C 0.3285(5) 0.3820(3) 0.1368(3) 0.0288(4) Uiso 1 1 d D . . C2S C 0.3813(5) 0.3678(4) 0.0495(4) 0.0288(4) Uiso 1 1 d . . . H2SA H 0.4001 0.4319 -0.0082 0.035 Uiso 1 1 calc R . . C3S C 0.4062(5) 0.2598(4) 0.0476(4) 0.0288(4) Uiso 1 1 d . . . H3SA H 0.4444 0.2500 -0.0115 0.035 Uiso 1 1 calc R A . C4S C 0.3760(5) 0.1662(4) 0.1308(3) 0.0288(4) Uiso 1 1 d . . . H4SA H 0.3912 0.0922 0.1290 0.035 Uiso 1 1 calc R . . C5S C 0.3229(5) 0.1809(4) 0.2179(3) 0.0288(4) Uiso 1 1 d . . . H5SA H 0.3026 0.1165 0.2754 0.035 Uiso 1 1 calc R A . C6S C 0.2997(5) 0.2880(4) 0.2214(4) 0.0288(4) Uiso 1 1 d . . . H6SA H 0.2644 0.2975 0.2808 0.035 Uiso 1 1 calc R . . C7S C 0.3004(9) 0.4945(4) 0.1379(6) 0.0288(4) Uiso 0.80 1 d PD A 1 Cl1S Cl 0.3037(9) 0.5193(5) 0.1406(6) 0.0288(4) Uiso 0.20 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0151(2) 0.0106(2) 0.0124(2) -0.00542(14) -0.00315(13) -0.00041(13) B1 0.017(2) 0.011(2) 0.013(2) -0.0057(19) -0.0022(19) -0.0025(18) N1 0.0147(18) 0.0132(18) 0.017(2) -0.0081(17) -0.0044(14) 0.0024(14) N2 0.0185(18) 0.0141(19) 0.0107(17) -0.0041(15) -0.0019(14) -0.0036(15) N3 0.0185(19) 0.0180(19) 0.022(2) -0.0064(18) -0.0072(16) -0.0002(15) N4 0.0150(18) 0.0171(19) 0.0180(18) -0.0066(16) -0.0060(15) -0.0006(14) C1 0.016(2) 0.015(2) 0.017(2) -0.012(2) -0.0027(17) -0.0031(17) C2 0.029(2) 0.016(2) 0.012(2) -0.0034(18) -0.0032(18) -0.0041(18) C3 0.016(2) 0.017(2) 0.011(2) -0.0027(18) -0.0031(17) -0.0054(18) C4 0.021(2) 0.012(2) 0.017(2) -0.0086(18) -0.0017(18) -0.0012(17) C5 0.022(2) 0.012(2) 0.015(2) -0.0070(17) -0.0036(17) 0.0015(17) C6 0.018(2) 0.016(2) 0.022(3) -0.009(2) -0.0087(18) 0.0002(17) C7 0.026(2) 0.016(2) 0.020(2) -0.0025(19) -0.0093(19) -0.0009(18) C8 0.022(2) 0.016(2) 0.021(2) -0.0049(18) -0.0105(19) 0.0036(18) C9 0.017(2) 0.011(2) 0.015(2) -0.0011(18) -0.0061(17) -0.0008(17) C10 0.017(2) 0.016(2) 0.020(2) -0.0119(18) -0.0033(18) 0.0017(17) C11 0.011(2) 0.019(2) 0.014(2) -0.0082(18) -0.0038(17) -0.0035(16) C12 0.020(2) 0.018(2) 0.017(2) -0.0086(18) -0.0043(18) -0.0058(17) C13 0.016(2) 0.026(2) 0.014(2) -0.0062(19) -0.0036(17) -0.0090(18) C14 0.014(2) 0.030(3) 0.017(2) -0.013(2) -0.0027(17) 0.0025(18) C15 0.020(2) 0.023(2) 0.023(2) -0.016(2) -0.0042(19) 0.0064(18) C16 0.021(2) 0.017(2) 0.017(2) -0.0066(18) -0.0044(18) -0.0008(18) C17 0.017(2) 0.011(2) 0.013(2) -0.0084(17) -0.0013(17) -0.0006(16) C18 0.015(2) 0.013(2) 0.013(2) -0.0052(17) -0.0032(17) 0.0005(16) C19 0.020(2) 0.024(2) 0.018(2) -0.0144(19) -0.0082(18) 0.0028(18) C20 0.031(3) 0.013(2) 0.011(2) -0.0069(17) -0.0064(18) -0.0006(18) C21 0.024(2) 0.014(2) 0.012(2) -0.0072(17) -0.0003(18) -0.0075(17) C22 0.016(2) 0.014(2) 0.014(2) -0.0089(17) -0.0034(17) 0.0002(16) C23 0.016(2) 0.014(2) 0.0071(19) -0.0034(16) 0.0015(16) -0.0037(16) C24 0.022(2) 0.017(2) 0.013(2) -0.0048(17) -0.0048(18) -0.0010(17) C25 0.020(2) 0.025(2) 0.018(2) -0.0075(19) -0.0047(18) -0.0094(19) C26 0.013(2) 0.034(3) 0.013(2) -0.0055(19) -0.0033(17) -0.0012(19) C27 0.018(2) 0.021(2) 0.012(2) -0.0033(18) -0.0043(17) 0.0054(18) C28 0.016(2) 0.010(2) 0.012(2) -0.0031(16) -0.0033(16) 0.0033(16) C29 0.019(2) 0.010(2) 0.0083(19) -0.0013(16) -0.0036(16) -0.0019(16) C30 0.015(2) 0.015(2) 0.012(2) -0.0030(17) -0.0013(17) -0.0024(16) C31 0.020(2) 0.009(2) 0.013(2) -0.0045(17) -0.0036(17) 0.0077(16) C32 0.023(2) 0.011(2) 0.014(2) -0.0063(17) -0.0071(18) 0.0002(17) C33 0.017(2) 0.015(2) 0.012(2) -0.0010(17) -0.0042(17) -0.0057(17) C34 0.014(2) 0.010(2) 0.011(2) -0.0028(16) -0.0037(16) 0.0043(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 C3 1.962(4) . ? Rh1 C1 1.967(4) . ? Rh1 C9 1.977(4) . ? Rh1 C6 1.979(4) . ? B1 C11 1.640(6) . ? B1 C29 1.647(6) . ? B1 C23 1.650(6) . ? B1 C17 1.653(6) . ? N1 C1 1.152(5) . ? N1 C2 1.448(5) . ? N2 C3 1.147(5) . ? N2 C4 1.445(5) . ? N3 C6 1.158(6) . ? N3 C7 1.445(6) . ? N4 C9 1.155(5) . ? N4 C10 1.446(5) . ? C2 C8 1.514(6) 2 ? C4 C5 1.518(6) . ? C5 C10 1.526(6) 2 ? C7 C8 1.518(6) . ? C8 C2 1.514(6) 2 ? C10 C5 1.526(6) 2 ? C11 C16 1.396(6) . ? C11 C12 1.402(6) . ? C12 C13 1.391(6) . ? C13 C14 1.385(6) . ? C14 C15 1.384(6) . ? C15 C16 1.397(6) . ? C17 C22 1.401(6) . ? C17 C18 1.405(6) . ? C18 C19 1.396(6) . ? C19 C20 1.393(6) . ? C20 C21 1.378(6) . ? C21 C22 1.397(6) . ? C23 C28 1.399(6) . ? C23 C24 1.403(6) . ? C24 C25 1.380(6) . ? C25 C26 1.404(6) . ? C26 C27 1.383(6) . ? C27 C28 1.386(6) . ? C29 C30 1.407(6) . ? C29 C34 1.410(6) . ? C30 C31 1.385(6) . ? C31 C32 1.398(6) . ? C32 C33 1.379(6) . ? C33 C34 1.392(6) . ? N1S C7S 1.120(4) . ? C1S C6S 1.393(7) . ? C1S C2S 1.398(7) . ? C1S C7S 1.439(4) . ? C1S Cl1S 1.765(4) . ? C2S C3S 1.384(7) . ? C3S C4S 1.378(7) . ? C4S C5S 1.398(7) . ? C5S C6S 1.380(7) . ? 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 C3 Rh1 C1 87.51(16) . . ? C3 Rh1 C9 177.54(16) . . ? C1 Rh1 C9 90.73(16) . . ? C3 Rh1 C6 90.77(16) . . ? C1 Rh1 C6 177.85(16) . . ? C9 Rh1 C6 90.96(16) . . ? C11 B1 C29 110.8(3) . . ? C11 B1 C23 104.1(3) . . ? C29 B1 C23 114.3(3) . . ? C11 B1 C17 111.1(3) . . ? C29 B1 C17 104.3(3) . . ? C23 B1 C17 112.5(3) . . ? C1 N1 C2 178.8(4) . . ? C3 N2 C4 177.7(4) . . ? C6 N3 C7 171.9(4) . . ? C9 N4 C10 175.4(4) . . ? N1 C1 Rh1 176.0(4) . . ? N1 C2 C8 112.7(3) . 2 ? N2 C3 Rh1 176.4(4) . . ? N2 C4 C5 112.8(3) . . ? C4 C5 C10 115.9(3) . 2 ? N3 C6 Rh1 174.5(4) . . ? N3 C7 C8 111.2(4) . . ? C2 C8 C7 116.3(4) 2 . ? N4 C9 Rh1 174.5(3) . . ? N4 C10 C5 111.5(3) . 2 ? C16 C11 C12 115.0(4) . . ? C16 C11 B1 123.4(4) . . ? C12 C11 B1 121.4(4) . . ? C13 C12 C11 122.8(4) . . ? C14 C13 C12 120.1(4) . . ? C15 C14 C13 119.2(4) . . ? C14 C15 C16 119.5(4) . . ? C11 C16 C15 123.4(4) . . ? C22 C17 C18 115.3(4) . . ? C22 C17 B1 124.3(4) . . ? C18 C17 B1 120.3(3) . . ? C19 C18 C17 122.9(4) . . ? C20 C19 C18 119.7(4) . . ? C21 C20 C19 119.0(4) . . ? C20 C21 C22 120.6(4) . . ? C21 C22 C17 122.4(4) . . ? C28 C23 C24 114.9(4) . . ? C28 C23 B1 124.4(3) . . ? C24 C23 B1 120.5(4) . . ? C25 C24 C23 123.5(4) . . ? C24 C25 C26 119.7(4) . . ? C27 C26 C25 118.3(4) . . ? C26 C27 C28 120.7(4) . . ? C27 C28 C23 122.8(4) . . ? C30 C29 C34 115.3(4) . . ? C30 C29 B1 124.0(4) . . ? C34 C29 B1 120.2(3) . . ? C31 C30 C29 122.9(4) . . ? C30 C31 C32 119.8(4) . . ? C33 C32 C31 119.2(4) . . ? C32 C33 C34 120.3(4) . . ? C33 C34 C29 122.4(4) . . ? C6S C1S C2S 120.3(4) . . ? C6S C1S C7S 120.5(5) . . ? C2S C1S C7S 119.2(5) . . ? C6S C1S Cl1S 119.6(4) . . ? C2S C1S Cl1S 120.1(4) . . ? C7S C1S Cl1S 3.5(5) . . ? C3S C2S C1S 119.6(4) . . ? C4S C3S C2S 120.6(5) . . ? C3S C4S C5S 119.6(5) . . ? C6S C5S C4S 120.7(5) . . ? C5S C6S C1S 119.3(4) . . ? N1S C7S C1S 176.0(8) . . ? 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 C2 N1 C1 Rh1 -127(17) . . . . ? C3 Rh1 C1 N1 -46(5) . . . . ? C9 Rh1 C1 N1 132(5) . . . . ? C6 Rh1 C1 N1 -9(8) . . . . ? C1 N1 C2 C8 107(19) . . . 2 ? C4 N2 C3 Rh1 51(14) . . . . ? C1 Rh1 C3 N2 45(6) . . . . ? C9 Rh1 C3 N2 0(8) . . . . ? C6 Rh1 C3 N2 -134(6) . . . . ? C3 N2 C4 C5 -31(10) . . . . ? N2 C4 C5 C10 63.6(5) . . . 2 ? C7 N3 C6 Rh1 21(6) . . . . ? C3 Rh1 C6 N3 72(4) . . . . ? C1 Rh1 C6 N3 35(7) . . . . ? C9 Rh1 C6 N3 -107(4) . . . . ? C6 N3 C7 C8 33(3) . . . . ? N3 C7 C8 C2 -73.0(5) . . . 2 ? C10 N4 C9 Rh1 -3(8) . . . . ? C3 Rh1 C9 N4 -26(6) . . . . ? C1 Rh1 C9 N4 -70(4) . . . . ? C6 Rh1 C9 N4 108(4) . . . . ? C9 N4 C10 C5 -50(5) . . . 2 ? C29 B1 C11 C16 142.2(4) . . . . ? C23 B1 C11 C16 -94.5(4) . . . . ? C17 B1 C11 C16 26.8(5) . . . . ? C29 B1 C11 C12 -42.6(5) . . . . ? C23 B1 C11 C12 80.6(4) . . . . ? C17 B1 C11 C12 -158.1(4) . . . . ? C16 C11 C12 C13 -0.8(6) . . . . ? B1 C11 C12 C13 -176.3(4) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C12 C11 C16 C15 0.4(6) . . . . ? B1 C11 C16 C15 175.8(4) . . . . ? C14 C15 C16 C11 0.3(7) . . . . ? C11 B1 C17 C22 -132.6(4) . . . . ? C29 B1 C17 C22 108.1(4) . . . . ? C23 B1 C17 C22 -16.3(5) . . . . ? C11 B1 C17 C18 50.0(5) . . . . ? C29 B1 C17 C18 -69.4(4) . . . . ? C23 B1 C17 C18 166.2(3) . . . . ? C22 C17 C18 C19 2.0(6) . . . . ? B1 C17 C18 C19 179.7(4) . . . . ? C17 C18 C19 C20 0.7(6) . . . . ? C18 C19 C20 C21 -2.4(6) . . . . ? C19 C20 C21 C22 1.4(6) . . . . ? C20 C21 C22 C17 1.5(6) . . . . ? C18 C17 C22 C21 -3.1(6) . . . . ? B1 C17 C22 C21 179.3(4) . . . . ? C11 B1 C23 C28 -98.6(4) . . . . ? C29 B1 C23 C28 22.4(5) . . . . ? C17 B1 C23 C28 141.1(4) . . . . ? C11 B1 C23 C24 76.0(4) . . . . ? C29 B1 C23 C24 -163.1(3) . . . . ? C17 B1 C23 C24 -44.3(5) . . . . ? C28 C23 C24 C25 -2.8(6) . . . . ? B1 C23 C24 C25 -177.8(4) . . . . ? C23 C24 C25 C26 1.4(6) . . . . ? C24 C25 C26 C27 0.9(6) . . . . ? C25 C26 C27 C28 -1.8(6) . . . . ? C26 C27 C28 C23 0.3(6) . . . . ? C24 C23 C28 C27 1.9(6) . . . . ? B1 C23 C28 C27 176.7(4) . . . . ? C11 B1 C29 C30 153.8(4) . . . . ? C23 B1 C29 C30 36.6(5) . . . . ? C17 B1 C29 C30 -86.7(4) . . . . ? C11 B1 C29 C34 -34.7(5) . . . . ? C23 B1 C29 C34 -151.9(3) . . . . ? C17 B1 C29 C34 84.8(4) . . . . ? C34 C29 C30 C31 -0.2(6) . . . . ? B1 C29 C30 C31 171.7(4) . . . . ? C29 C30 C31 C32 0.0(6) . . . . ? C30 C31 C32 C33 0.4(6) . . . . ? C31 C32 C33 C34 -0.8(6) . . . . ? C32 C33 C34 C29 0.6(6) . . . . ? C30 C29 C34 C33 -0.1(6) . . . . ? B1 C29 C34 C33 -172.4(4) . . . . ? C6S C1S C2S C3S -0.6(7) . . . . ? C7S C1S C2S C3S -178.8(5) . . . . ? Cl1S C1S C2S C3S 177.2(5) . . . . ? C1S C2S C3S C4S 1.6(7) . . . . ? C2S C3S C4S C5S -1.5(7) . . . . ? C3S C4S C5S C6S 0.4(7) . . . . ? C4S C5S C6S C1S 0.6(7) . . . . ? C2S C1S C6S C5S -0.4(7) . . . . ? C7S C1S C6S C5S 177.7(5) . . . . ? Cl1S C1S C6S C5S -178.3(5) . . . . ? C6S C1S C7S N1S 89(12) . . . . ? C2S C1S C7S N1S -93(12) . . . . ? Cl1S C1S C7S N1S 13(6) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.865 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.111 data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 248491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(diprop)4)(Calix)2 _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C76 H67 N8 O8 Rh2' _chemical_formula_weight 1426.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4914(11) _cell_length_b 27.858(2) _cell_length_c 18.1816(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.975(2) _cell_angle_gamma 90.00 _cell_volume 6499.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 25.01 _exptl_crystal_description leaves _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2932 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.8469 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent acetonitrile / diethyl ether ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 54848 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10921 _reflns_number_gt 7360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+26.4245P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10921 _refine_ls_number_parameters 990 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max <0.002 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.83577(2) 0.859078(11) 0.287744(18) 0.03713(8) Uani 1 1 d . . . Rh2 Rh 0.76078(3) 0.904168(12) 0.115935(19) 0.04057(9) Uani 1 1 d . . . N1 N 0.6863(3) 0.77256(11) 0.2243(2) 0.0597(12) Uani 1 1 d D . . N2 N 0.5948(3) 0.82255(13) 0.0741(2) 0.0438(10) Uani 1 1 d . . . N3 N 0.6570(3) 0.91644(13) 0.3234(2) 0.0425(9) Uani 1 1 d . . . N4 N 0.6152(3) 0.96958(13) 0.1752(2) 0.0491(10) Uani 1 1 d . . . N5 N 0.9649(3) 0.95398(11) 0.3202(2) 0.0511(10) Uani 1 1 d D . . N6 N 0.9096(3) 0.99101(13) 0.1581(2) 0.0452(10) Uani 1 1 d . . . N7 N 1.0162(3) 0.80374(13) 0.2528(2) 0.0507(10) Uani 1 1 d . . . N8 N 0.9252(3) 0.83480(14) 0.0859(2) 0.0565(11) Uani 1 1 d . . . O1 O 0.2818(3) 0.78613(13) 0.3969(2) 0.0709(12) Uani 1 1 d . . . H1A H 0.2544 0.7626 0.4122 0.106 Uiso 1 1 calc R . . O2 O 0.3805(3) 0.74573(14) 0.3188(3) 0.0877(14) Uani 1 1 d . . . H2A H 0.3498 0.7586 0.3475 0.132 Uiso 1 1 calc R . . O3 O 0.3062(3) 0.66511(14) 0.3412(2) 0.0783(13) Uani 1 1 d . . . H3A H 0.3313 0.6930 0.3453 0.117 Uiso 1 1 calc R . . O4 O 0.1781(3) 0.71073(15) 0.4171(2) 0.0892(14) Uani 1 1 d . . . C1 C 0.7432(4) 0.80299(16) 0.2528(3) 0.0478(12) Uani 1 1 d . A . C2A C 0.6003(4) 0.74039(19) 0.1871(4) 0.0441(16) Uiso 0.65 1 d PD A 1 H2AA H 0.5356 0.7519 0.1961 0.053 Uiso 0.65 1 calc PR A 1 H2AB H 0.6156 0.7078 0.2093 0.053 Uiso 0.65 1 calc PR A 1 C3A C 0.5858(5) 0.7390(2) 0.0998(4) 0.0414(15) Uiso 0.65 1 d P A 1 H3AA H 0.6549 0.7380 0.0915 0.050 Uiso 0.65 1 calc PR A 1 H3AB H 0.5477 0.7094 0.0773 0.050 Uiso 0.65 1 calc PR A 1 C2B C 0.6348(4) 0.73200(17) 0.1778(5) 0.043(3) Uiso 0.35 1 d PD A 2 H2BA H 0.6256 0.7050 0.2105 0.052 Uiso 0.35 1 calc PR A 2 H2BB H 0.6734 0.7207 0.1428 0.052 Uiso 0.35 1 calc PR A 2 C3B C 0.5314(5) 0.7544(3) 0.1333(3) 0.064(4) Uiso 0.35 1 d PD A 2 H3BA H 0.5110 0.7769 0.1682 0.076 Uiso 0.35 1 calc PR A 2 H3BB H 0.4784 0.7286 0.1197 0.076 Uiso 0.35 1 calc PR A 2 C4 C 0.5273(4) 0.78137(15) 0.0595(2) 0.0538(14) Uani 1 1 d D . . H4A H 0.5008 0.7751 0.0032 0.065 Uiso 1 1 calc R A 1 H4B H 0.4670 0.7876 0.0782 0.065 Uiso 1 1 calc R A 1 C5 C 0.6554(3) 0.85273(15) 0.0890(2) 0.0414(11) Uani 1 1 d . . . C6 C 0.7225(3) 0.89384(14) 0.3114(2) 0.0362(10) Uani 1 1 d . . . C7 C 0.5848(3) 0.95107(17) 0.3351(3) 0.0502(12) Uani 1 1 d . . . H7A H 0.5980 0.9559 0.3912 0.060 Uiso 1 1 calc R . . H7B H 0.5130 0.9386 0.3130 0.060 Uiso 1 1 calc R . . C8 C 0.5936(4) 0.99874(17) 0.2979(3) 0.0572(13) Uani 1 1 d . . . H8A H 0.6678 1.0084 0.3139 0.069 Uiso 1 1 calc R . . H8B H 0.5550 1.0232 0.3175 0.069 Uiso 1 1 calc R . . C9 C 0.5523(4) 0.99835(19) 0.2102(3) 0.0665(15) Uani 1 1 d . . . H9A H 0.4802 0.9857 0.1939 0.080 Uiso 1 1 calc R . . H9B H 0.5498 1.0317 0.1910 0.080 Uiso 1 1 calc R . . C10 C 0.6646(4) 0.94549(15) 0.1495(2) 0.0446(12) Uani 1 1 d . . . C11 C 0.9206(3) 0.91788(15) 0.3120(2) 0.0396(11) Uani 1 1 d . B . C12A C 1.0023(5) 1.00333(14) 0.3323(4) 0.0393(15) Uiso 0.65 1 d PD B 1 H12A H 1.0555 1.0060 0.3837 0.047 Uiso 0.65 1 calc PR B 1 H12B H 0.9436 1.0248 0.3317 0.047 Uiso 0.65 1 calc PR B 1 C13A C 1.0492(4) 1.0192(2) 0.2705(2) 0.0377(15) Uiso 0.65 1 d PD B 1 H13A H 1.0935 1.0477 0.2897 0.045 Uiso 0.65 1 calc PR B 1 H13B H 1.0951 0.9933 0.2626 0.045 Uiso 0.65 1 calc PR B 1 C12B C 1.0459(8) 0.9896(2) 0.3340(5) 0.051(3) Uiso 0.35 1 d PD B 2 H12C H 1.1071 0.9774 0.3207 0.061 Uiso 0.35 1 calc PR B 2 H12D H 1.0683 1.0004 0.3886 0.061 Uiso 0.35 1 calc PR B 2 C13B C 0.9918(9) 1.0294(3) 0.2800(2) 0.058(4) Uiso 0.35 1 d PD B 2 H13C H 0.9226 1.0329 0.2876 0.070 Uiso 0.35 1 calc PR B 2 H13D H 1.0308 1.0590 0.3008 0.070 Uiso 0.35 1 calc PR B 2 C14 C 0.9718(3) 1.03152(17) 0.19366(18) 0.0583(14) Uani 1 1 d D . . H14A H 0.9255 1.0574 0.2010 0.070 Uiso 1 1 calc R B 1 H14B H 1.0096 1.0438 0.1587 0.070 Uiso 1 1 calc R B 1 C15 C 0.8578(3) 0.95773(16) 0.1395(2) 0.0432(11) Uani 1 1 d . . . C16 C 0.9508(4) 0.82410(15) 0.2670(3) 0.0461(12) Uani 1 1 d . . . C17 C 1.0847(4) 0.77731(17) 0.2203(3) 0.0576(13) Uani 1 1 d . . . H17A H 1.1109 0.7484 0.2521 0.069 Uiso 1 1 calc R . . H17B H 1.1453 0.7976 0.2211 0.069 Uiso 1 1 calc R . . C18 C 1.0289(4) 0.76251(16) 0.1390(3) 0.0606(14) Uani 1 1 d . . . H18A H 0.9620 0.7475 0.1380 0.073 Uiso 1 1 calc R . . H18B H 1.0711 0.7376 0.1237 0.073 Uiso 1 1 calc R . . C19 C 1.0062(4) 0.80193(17) 0.0791(3) 0.0653(14) Uani 1 1 d . . . H19A H 1.0709 0.8203 0.0846 0.078 Uiso 1 1 calc R . . H19B H 0.9840 0.7873 0.0269 0.078 Uiso 1 1 calc R . . C20 C 0.8631(4) 0.86120(16) 0.0926(3) 0.0496(12) Uani 1 1 d . . . C21 C 0.3342(2) 0.81331(9) 0.45843(15) 0.0594(15) Uani 1 1 d G . . C22 C 0.3009(2) 0.81615(11) 0.52343(18) 0.0593(15) Uani 1 1 d G . . C23 C 0.3540(3) 0.84509(12) 0.58531(17) 0.0716(18) Uani 1 1 d G . . H23A H 0.3313 0.8470 0.6297 0.086 Uiso 1 1 calc R . . C24 C 0.4405(3) 0.87118(12) 0.58221(19) 0.0717(12) Uani 1 1 d GU . . H24A H 0.4768 0.8910 0.6245 0.086 Uiso 1 1 calc R . . C25 C 0.4738(2) 0.86833(12) 0.5172(2) 0.0754(12) Uani 1 1 d GU . . H25A H 0.5328 0.8862 0.5151 0.090 Uiso 1 1 calc R . . C26 C 0.4206(2) 0.83940(11) 0.45533(18) 0.0708(18) Uani 1 1 d G . . C27 C 0.4565(5) 0.8367(2) 0.3845(4) 0.097(2) Uani 1 1 d . . . H27A H 0.3948 0.8355 0.3378 0.116 Uiso 1 1 calc R . . H27B H 0.4961 0.8662 0.3815 0.116 Uiso 1 1 calc R . . C28 C 0.4833(2) 0.75025(12) 0.35092(17) 0.0720(16) Uani 1 1 d G . . C29 C 0.5242(3) 0.79351(11) 0.3851(2) 0.0851(18) Uani 1 1 d G . . C30 C 0.6305(3) 0.79779(15) 0.4224(3) 0.111(3) Uani 1 1 d G . . H30A H 0.6585 0.8274 0.4458 0.133 Uiso 1 1 calc R . . C31 C 0.6960(2) 0.75880(19) 0.4255(3) 0.118(3) Uani 1 1 d G . . H31A H 0.7686 0.7617 0.4510 0.142 Uiso 1 1 calc R . . C32 C 0.6551(3) 0.71553(15) 0.3913(3) 0.090(2) Uani 1 1 d G . . H32A H 0.6998 0.6889 0.3935 0.108 Uiso 1 1 calc R . . C33 C 0.5487(3) 0.71125(11) 0.3540(2) 0.0689(15) Uani 1 1 d G . . C34 C 0.5065(4) 0.6646(2) 0.3169(3) 0.0717(16) Uani 1 1 d . . . H34A H 0.5595 0.6490 0.2976 0.086 Uiso 1 1 calc R . . H34B H 0.4443 0.6709 0.2719 0.086 Uiso 1 1 calc R . . C35 C 0.3789(2) 0.63459(8) 0.38194(14) 0.0562(14) Uani 1 1 d G . . C36 C 0.4766(2) 0.63039(10) 0.37202(17) 0.0554(14) Uani 1 1 d G . . C37 C 0.5464(2) 0.59600(13) 0.4133(2) 0.0730(18) Uani 1 1 d G . . H37A H 0.6132 0.5931 0.4065 0.088 Uiso 1 1 calc R . . C38 C 0.5185(3) 0.56579(11) 0.4645(2) 0.079(2) Uani 1 1 d G . . H38A H 0.5662 0.5423 0.4927 0.095 Uiso 1 1 calc R . . C39 C 0.4207(3) 0.56999(10) 0.47438(17) 0.0764(19) Uani 1 1 d G . . H39A H 0.4017 0.5493 0.5094 0.092 Uiso 1 1 calc R . . C40 C 0.3509(2) 0.60438(10) 0.43311(18) 0.0661(16) Uani 1 1 d G . . C41 C 0.2493(5) 0.6126(2) 0.4516(4) 0.0898(19) Uani 1 1 d . . . H41A H 0.2284 0.5823 0.4712 0.108 Uiso 1 1 calc R . . H41B H 0.1939 0.6213 0.4033 0.108 Uiso 1 1 calc R . . C42 C 0.2254(2) 0.69958(11) 0.49125(16) 0.0683(15) Uani 1 1 d G . . C43 C 0.2578(3) 0.65282(10) 0.5124(2) 0.0779(16) Uani 1 1 d G . . C44 C 0.3052(3) 0.64147(12) 0.5897(2) 0.0935(19) Uani 1 1 d G . . H44A H 0.3274 0.6095 0.6042 0.112 Uiso 1 1 calc R . . C45 C 0.3201(3) 0.67688(16) 0.64598(17) 0.092(2) Uani 1 1 d G . . H45A H 0.3525 0.6691 0.6989 0.110 Uiso 1 1 calc R . . C46 C 0.2877(3) 0.72364(14) 0.62485(18) 0.0786(17) Uani 1 1 d G . . H46A H 0.2979 0.7478 0.6633 0.094 Uiso 1 1 calc R . . C47 C 0.2403(3) 0.73499(10) 0.54749(19) 0.0689(16) Uani 1 1 d G . . C48 C 0.2099(4) 0.7870(2) 0.5274(4) 0.0752(17) Uani 1 1 d . . . H48A H 0.1545 0.7884 0.4769 0.090 Uiso 1 1 calc R . . H48B H 0.1817 0.8007 0.5670 0.090 Uiso 1 1 calc R . . O5 O 1.2639(5) 0.3929(3) 0.7053(4) 0.069(2) Uani 0.51 1 d P C 1 O6 O 1.3610(5) 0.4646(3) 0.7819(5) 0.077(2) Uani 0.51 1 d P C 1 O7 O 1.3132(5) 0.4261(2) 0.8920(4) 0.063(2) Uani 0.51 1 d P C 1 O8 O 1.2439(6) 0.3418(3) 0.8351(6) 0.099(3) Uani 0.51 1 d P C 1 C49 C 1.1765(3) 0.40287(19) 0.6471(3) 0.0492(14) Uani 0.51 1 d PGU C 1 C50 C 1.0964(4) 0.36928(19) 0.6296(3) 0.0546(14) Uani 0.51 1 d PGU C 1 C51 C 1.0076(4) 0.3767(2) 0.5670(3) 0.065(3) Uani 0.51 1 d PG C 1 H51A H 0.9529 0.3538 0.5550 0.078 Uiso 0.51 1 calc PR C 1 C52 C 0.9989(4) 0.4178(3) 0.5219(3) 0.070(3) Uani 0.51 1 d PG C 1 H52A H 0.9382 0.4228 0.4791 0.085 Uiso 0.51 1 calc PR C 1 C53 C 1.0790(5) 0.4513(2) 0.5395(3) 0.057(3) Uani 0.51 1 d PG C 1 H53A H 1.0731 0.4794 0.5087 0.068 Uiso 0.51 1 calc PR C 1 C54 C 1.1678(4) 0.44390(19) 0.6021(3) 0.048(3) Uani 0.51 1 d PG C 1 C55 C 1.2531(6) 0.4825(3) 0.6223(5) 0.056(2) Uani 0.51 1 d P C 1 H55A H 1.3221 0.4666 0.6367 0.067 Uiso 0.51 1 calc PR C 1 H55B H 1.2466 0.5023 0.5758 0.067 Uiso 0.51 1 calc PR C 1 C56 C 1.3047(3) 0.50644(15) 0.7653(2) 0.046(2) Uani 0.51 1 d PG C 1 C57 C 1.2484(4) 0.51544(17) 0.6885(2) 0.050(2) Uani 0.51 1 d PG C 1 C58 C 1.1847(4) 0.55569(19) 0.6695(2) 0.061(3) Uani 0.51 1 d PG C 1 H58A H 1.1463 0.5618 0.6170 0.073 Uiso 0.51 1 calc PR C 1 C59 C 1.1773(5) 0.58694(18) 0.7271(3) 0.066(3) Uani 0.51 1 d PG C 1 H59A H 1.1338 0.6145 0.7141 0.079 Uiso 0.51 1 calc PR C 1 C60 C 1.2336(5) 0.57794(17) 0.8039(3) 0.0476(14) Uani 0.51 1 d PGU C 1 H60A H 1.2285 0.5993 0.8433 0.057 Uiso 0.51 1 calc PR C 1 C61 C 1.2973(4) 0.53769(17) 0.8229(2) 0.049(3) Uani 0.51 1 d PGD C 1 C62 C 1.3548(4) 0.5264(3) 0.9059(3) 0.065(3) Uani 0.51 1 d PD C 1 H62A H 1.4168 0.5069 0.9078 0.077 Uiso 0.51 1 calc PR C 1 H62B H 1.3796 0.5569 0.9335 0.077 Uiso 0.51 1 calc PR C 1 C63 C 1.2704(3) 0.45115(19) 0.9372(2) 0.053(3) Uani 0.51 1 d PG C 1 C64 C 1.2913(4) 0.49997(19) 0.9476(3) 0.061(3) Uani 0.51 1 d PGD C 1 C65 C 1.2477(5) 0.52667(19) 0.9944(4) 0.066(3) Uani 0.51 1 d PG C 1 H65A H 1.2620 0.5600 1.0015 0.079 Uiso 0.51 1 calc PR C 1 C66 C 1.1832(5) 0.5045(2) 1.0308(4) 0.059(3) Uani 0.51 1 d PG C 1 H66A H 1.1534 0.5228 1.0628 0.071 Uiso 0.51 1 calc PR C 1 C67 C 1.1622(4) 0.4557(2) 1.0204(3) 0.055(3) Uani 0.51 1 d PG C 1 H67A H 1.1181 0.4406 1.0453 0.067 Uiso 0.51 1 calc PR C 1 C68 C 1.2058(4) 0.42903(19) 0.9736(3) 0.057(3) Uani 0.51 1 d PG C 1 C69 C 1.1816(9) 0.3759(4) 0.9645(6) 0.068(3) Uani 0.51 1 d P C 1 H69A H 1.1517 0.3656 1.0053 0.082 Uiso 0.51 1 calc PR C 1 H69B H 1.2471 0.3579 0.9717 0.082 Uiso 0.51 1 calc PR C 1 C70 C 1.1389(3) 0.34887(15) 0.8240(3) 0.067(3) Uani 0.51 1 d PG C 1 C71 C 1.1049(4) 0.3636(2) 0.8852(3) 0.061(3) Uani 0.51 1 d PG C 1 C72 C 0.9988(4) 0.3678(2) 0.8751(4) 0.059(3) Uani 0.51 1 d PG C 1 H72A H 0.9755 0.3778 0.9169 0.071 Uiso 0.51 1 calc PR C 1 C73 C 0.9268(3) 0.3573(2) 0.8038(4) 0.050(3) Uani 0.51 1 d PG C 1 H73A H 0.8544 0.3601 0.7968 0.059 Uiso 0.51 1 calc PR C 1 C74 C 0.9609(4) 0.3426(2) 0.7426(3) 0.055(3) Uani 0.51 1 d PG C 1 H74A H 0.9117 0.3354 0.6938 0.066 Uiso 0.51 1 calc PR C 1 C75 C 1.0670(4) 0.3384(2) 0.7527(3) 0.046(3) Uani 0.51 1 d PG C 1 C76 C 1.1055(7) 0.3254(3) 0.6850(6) 0.061(3) Uani 0.51 1 d P C 1 H76A H 1.0639 0.2983 0.6559 0.073 Uiso 0.51 1 calc PR C 1 H76B H 1.1792 0.3150 0.7046 0.073 Uiso 0.51 1 calc PR C 1 O9 O 1.2687(5) 0.3852(3) 0.7612(5) 0.062(2) Uani 0.49 1 d P D 2 O10 O 1.3813(6) 0.4531(3) 0.8366(4) 0.066(2) Uani 0.49 1 d P D 2 O11 O 1.3053(6) 0.4211(3) 0.9534(7) 0.090(3) Uani 0.49 1 d P D 2 O12 O 1.2113(6) 0.3507(3) 0.8734(5) 0.077(3) Uani 0.49 1 d P D 2 C77 C 1.1959(3) 0.39293(15) 0.6919(2) 0.047(3) Uani 0.49 1 d PG D 2 C78 C 1.1107(4) 0.36225(17) 0.6678(3) 0.038(2) Uani 0.49 1 d PGD D 2 C79 C 1.0349(4) 0.3698(2) 0.5971(3) 0.043(3) Uani 0.49 1 d PG D 2 H79A H 0.9767 0.3488 0.5805 0.051 Uiso 0.49 1 calc PR D 2 C80 C 1.0443(4) 0.4080(2) 0.5505(2) 0.059(3) Uani 0.49 1 d PG D 2 H80A H 0.9925 0.4131 0.5021 0.071 Uiso 0.49 1 calc PR D 2 C81 C 1.1294(5) 0.4387(2) 0.5746(3) 0.047(3) Uani 0.49 1 d PG D 2 H81A H 1.1358 0.4648 0.5428 0.056 Uiso 0.49 1 calc PR D 2 C82 C 1.2052(4) 0.43113(17) 0.6454(3) 0.047(3) Uani 0.49 1 d PG D 2 C83 C 1.2977(8) 0.4656(4) 0.6729(6) 0.057(3) Uani 0.49 1 d P D 2 H83A H 1.3618 0.4465 0.6956 0.068 Uiso 0.49 1 calc PR D 2 H83B H 1.3058 0.4827 0.6274 0.068 Uiso 0.49 1 calc PR D 2 C84 C 1.3314(4) 0.49342(17) 0.8099(3) 0.054(3) Uani 0.49 1 d PG D 2 C85 C 1.2887(5) 0.5019(2) 0.7311(3) 0.044(3) Uani 0.49 1 d PG D 2 C86 C 1.2389(6) 0.5452(2) 0.7053(4) 0.068(4) Uani 0.49 1 d PG D 2 H86A H 1.2097 0.5511 0.6514 0.082 Uiso 0.49 1 calc PR D 2 C87 C 1.2318(6) 0.58000(19) 0.7583(5) 0.068(4) Uani 0.49 1 d PG D 2 H87A H 1.1977 0.6096 0.7406 0.082 Uiso 0.49 1 calc PR D 2 C88 C 1.2745(6) 0.57148(19) 0.8371(4) 0.059(3) Uani 0.49 1 d PG D 2 H88A H 1.2696 0.5952 0.8733 0.071 Uiso 0.49 1 calc PR D 2 C89 C 1.3243(5) 0.5282(2) 0.8629(3) 0.058(3) Uani 0.49 1 d PG D 2 C90 C 1.3633(10) 0.5172(5) 0.9490(7) 0.071(4) Uani 0.49 1 d P D 2 H90A H 1.3981 0.5460 0.9773 0.085 Uiso 0.49 1 calc PR D 2 H90B H 1.4154 0.4911 0.9585 0.085 Uiso 0.49 1 calc PR D 2 C91 C 1.2468(4) 0.45398(18) 0.9749(3) 0.055(3) Uani 0.49 1 d PG D 2 C92 C 1.2743(5) 0.50224(19) 0.9800(4) 0.054(3) Uani 0.49 1 d PG D 2 C93 C 1.2172(6) 0.53533(18) 1.0076(4) 0.061(4) Uani 0.49 1 d PG D 2 H93A H 1.2360 0.5683 1.0111 0.074 Uiso 0.49 1 calc PR D 2 C94 C 1.1327(6) 0.5202(2) 1.0299(4) 0.066(3) Uani 0.49 1 d PG D 2 H94A H 1.0937 0.5428 1.0488 0.079 Uiso 0.49 1 calc PR D 2 C95 C 1.1052(5) 0.4719(2) 1.0248(4) 0.057(3) Uani 0.49 1 d PG D 2 H95A H 1.0474 0.4615 1.0401 0.069 Uiso 0.49 1 calc PR D 2 C96 C 1.1623(5) 0.43881(19) 0.9973(4) 0.049(3) Uani 0.49 1 d PG D 2 C97 C 1.1258(9) 0.3862(3) 0.9918(6) 0.053(3) Uani 0.49 1 d P D 2 H97A H 1.1877 0.3651 1.0101 0.064 Uiso 0.49 1 calc PR D 2 H97B H 1.0830 0.3815 1.0267 0.064 Uiso 0.49 1 calc PR D 2 C98 C 1.1060(3) 0.35345(17) 0.8555(2) 0.050(3) Uani 0.49 1 d PG D 2 C99 C 1.0626(4) 0.3710(2) 0.9103(2) 0.049(3) Uani 0.49 1 d PG D 2 C100 C 0.9552(4) 0.3762(2) 0.8916(3) 0.044(3) Uani 0.49 1 d PG D 2 H10C H 0.9255 0.3882 0.9291 0.053 Uiso 0.49 1 calc PR D 2 C101 C 0.8912(3) 0.3639(2) 0.8182(3) 0.051(3) Uani 0.49 1 d PG D 2 H10D H 0.8178 0.3675 0.8055 0.061 Uiso 0.49 1 calc PR D 2 C102 C 0.9346(3) 0.3464(3) 0.7635(3) 0.042(3) Uani 0.49 1 d PG D 2 H10E H 0.8909 0.3380 0.7133 0.050 Uiso 0.49 1 calc PR D 2 C103 C 1.0420(3) 0.3412(2) 0.7821(2) 0.043(3) Uani 0.49 1 d PGD D 2 C104 C 1.0880(5) 0.3254(2) 0.7208(3) 0.056(3) Uani 0.49 1 d PD D 2 H10A H 1.0401 0.3014 0.6881 0.067 Uiso 0.49 1 calc PR D 2 H10B H 1.1541 0.3085 0.7469 0.067 Uiso 0.49 1 calc PR D 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 0.04509(16) 0.03073(16) 0.03922(16) -0.00155(13) 0.01835(13) -0.00764(14) Rh2 0.04981(17) 0.03559(17) 0.04238(17) 0.00024(14) 0.02313(14) -0.00358(15) N1 0.084(3) 0.039(2) 0.048(2) 0.0037(17) 0.009(2) -0.028(2) N2 0.0488(19) 0.0363(19) 0.0473(19) -0.0032(16) 0.0163(16) 0.0006(16) N3 0.0399(17) 0.046(2) 0.0441(19) 0.0076(16) 0.0163(15) -0.0059(16) N4 0.063(2) 0.045(2) 0.0437(19) 0.0101(17) 0.0225(17) 0.0124(18) N5 0.066(2) 0.048(2) 0.0406(19) -0.0027(16) 0.0178(17) -0.0271(18) N6 0.0518(19) 0.043(2) 0.0454(19) 0.0022(16) 0.0214(16) -0.0084(17) N7 0.061(2) 0.0355(19) 0.063(2) 0.0011(17) 0.0312(18) 0.0022(17) N8 0.071(2) 0.043(2) 0.070(2) 0.0015(18) 0.0434(18) 0.0009(19) O1 0.071(2) 0.058(2) 0.074(2) -0.0075(19) 0.0091(19) -0.0090(18) O2 0.102(3) 0.063(2) 0.101(3) 0.013(2) 0.034(2) 0.004(2) O3 0.064(2) 0.067(2) 0.098(3) 0.015(2) 0.017(2) 0.0023(19) O4 0.103(3) 0.072(2) 0.091(3) -0.026(2) 0.027(2) -0.032(2) C1 0.066(3) 0.037(2) 0.043(2) 0.0055(19) 0.021(2) -0.001(2) C4 0.055(3) 0.046(3) 0.056(3) -0.011(2) 0.011(2) -0.017(2) C5 0.057(2) 0.038(2) 0.034(2) -0.0005(18) 0.0209(18) 0.006(2) C6 0.042(2) 0.036(2) 0.030(2) 0.0071(17) 0.0101(17) -0.0103(18) C7 0.044(2) 0.064(3) 0.048(2) 0.008(2) 0.0221(19) 0.011(2) C8 0.068(3) 0.051(3) 0.061(3) 0.000(2) 0.033(2) 0.014(2) C9 0.086(3) 0.063(3) 0.062(3) 0.015(2) 0.038(2) 0.033(3) C10 0.059(2) 0.036(2) 0.042(2) 0.0076(19) 0.020(2) 0.002(2) C11 0.046(2) 0.043(2) 0.032(2) -0.0011(18) 0.0168(17) -0.0007(19) C14 0.074(3) 0.045(3) 0.065(3) -0.003(2) 0.036(2) -0.022(2) C15 0.056(2) 0.043(2) 0.038(2) 0.0061(18) 0.0248(18) 0.003(2) C16 0.057(2) 0.030(2) 0.055(3) 0.0013(19) 0.022(2) -0.004(2) C17 0.065(3) 0.041(3) 0.078(3) -0.001(2) 0.039(2) -0.001(2) C18 0.082(3) 0.035(2) 0.082(3) 0.003(2) 0.051(2) 0.002(2) C19 0.087(3) 0.042(3) 0.089(3) 0.002(2) 0.060(2) 0.012(2) C20 0.064(2) 0.041(2) 0.054(2) -0.002(2) 0.032(2) -0.005(2) C21 0.056(3) 0.039(3) 0.076(3) -0.003(2) 0.009(3) 0.005(2) C22 0.048(3) 0.048(3) 0.073(3) -0.007(3) 0.006(2) -0.001(2) C23 0.076(3) 0.053(3) 0.075(4) -0.008(3) 0.008(3) 0.017(3) C24 0.0695(16) 0.0616(16) 0.0755(17) -0.0019(13) 0.0095(12) 0.0033(13) C25 0.0729(16) 0.0666(17) 0.0813(17) 0.0014(13) 0.0158(12) -0.0009(13) C26 0.063(3) 0.032(2) 0.109(4) 0.013(3) 0.013(3) 0.002(2) C27 0.120(5) 0.046(3) 0.138(5) 0.032(3) 0.060(4) -0.005(3) C28 0.088(3) 0.064(3) 0.077(3) 0.014(3) 0.044(3) -0.012(3) C29 0.102(4) 0.065(3) 0.108(4) 0.023(3) 0.060(3) -0.019(3) C30 0.105(4) 0.078(4) 0.165(6) 0.009(4) 0.064(4) -0.039(4) C31 0.085(4) 0.116(6) 0.175(7) -0.014(5) 0.071(4) -0.044(4) C32 0.083(3) 0.092(5) 0.120(4) -0.002(4) 0.068(3) -0.008(3) C33 0.085(3) 0.066(3) 0.075(3) 0.004(3) 0.053(2) -0.008(3) C34 0.086(3) 0.079(4) 0.063(3) -0.004(3) 0.043(2) 0.006(3) C35 0.068(3) 0.043(3) 0.054(3) -0.004(2) 0.013(2) -0.011(2) C36 0.074(3) 0.047(3) 0.046(2) -0.013(2) 0.018(2) 0.000(2) C37 0.076(3) 0.061(3) 0.068(3) -0.026(3) 0.000(3) 0.019(3) C38 0.119(5) 0.037(3) 0.056(3) -0.015(2) -0.010(3) 0.017(3) C39 0.132(5) 0.035(3) 0.057(3) -0.010(2) 0.023(3) -0.015(3) C40 0.089(4) 0.037(3) 0.070(3) -0.010(2) 0.020(3) -0.018(3) C41 0.117(4) 0.056(3) 0.118(4) -0.022(3) 0.068(3) -0.045(3) C42 0.070(3) 0.050(3) 0.101(4) -0.002(3) 0.050(3) -0.017(2) C43 0.088(3) 0.072(4) 0.097(3) -0.004(3) 0.063(3) -0.033(3) C44 0.121(4) 0.066(4) 0.123(4) 0.016(3) 0.081(3) -0.025(3) C45 0.121(4) 0.100(5) 0.083(3) 0.017(3) 0.072(3) 0.010(4) C46 0.073(3) 0.074(4) 0.108(4) 0.005(3) 0.056(3) -0.007(3) C47 0.059(3) 0.075(4) 0.086(3) 0.003(3) 0.042(2) -0.015(3) C48 0.064(3) 0.068(3) 0.103(4) -0.024(3) 0.038(3) -0.004(3) O5 0.048(3) 0.075(5) 0.092(5) -0.008(4) 0.033(3) 0.007(3) O6 0.053(4) 0.086(5) 0.083(5) -0.028(4) 0.011(4) 0.014(4) O7 0.051(4) 0.055(4) 0.074(4) 0.001(4) 0.005(3) 0.001(3) O8 0.063(4) 0.103(6) 0.142(7) -0.028(6) 0.046(4) 0.007(4) C49 0.0485(18) 0.0498(18) 0.0501(19) -0.0027(14) 0.0162(13) 0.0004(14) C50 0.0549(18) 0.0547(19) 0.0549(19) -0.0012(14) 0.0179(13) 0.0001(14) C51 0.092(6) 0.065(6) 0.058(5) -0.009(5) 0.052(4) -0.025(5) C52 0.063(6) 0.115(8) 0.037(5) -0.039(5) 0.021(4) -0.036(6) C53 0.075(6) 0.066(6) 0.034(4) -0.008(4) 0.024(4) -0.015(5) C54 0.036(4) 0.068(6) 0.047(5) -0.023(4) 0.024(4) -0.012(4) C55 0.056(4) 0.065(6) 0.064(5) -0.021(4) 0.045(4) -0.028(4) C56 0.043(4) 0.055(5) 0.048(5) -0.021(4) 0.025(4) -0.019(4) C57 0.047(4) 0.046(5) 0.073(5) -0.006(4) 0.042(4) -0.021(4) C58 0.105(7) 0.036(5) 0.051(5) 0.002(4) 0.036(5) -0.013(5) C59 0.098(7) 0.036(5) 0.071(6) 0.000(5) 0.037(6) -0.010(5) C60 0.0489(18) 0.0467(18) 0.0473(19) -0.0011(14) 0.0152(13) -0.0013(14) C61 0.043(4) 0.048(5) 0.058(5) 0.000(4) 0.016(4) -0.017(4) C62 0.047(5) 0.078(7) 0.065(7) -0.006(6) 0.012(5) -0.029(5) C63 0.045(5) 0.076(7) 0.038(5) -0.009(5) 0.012(4) -0.007(5) C64 0.047(5) 0.082(7) 0.053(6) -0.021(5) 0.013(5) -0.012(5) C65 0.067(6) 0.057(6) 0.077(7) -0.011(5) 0.026(5) -0.027(5) C66 0.059(6) 0.072(7) 0.045(5) -0.008(5) 0.013(4) -0.003(5) C67 0.052(5) 0.080(7) 0.034(5) 0.013(5) 0.013(4) 0.008(5) C68 0.047(5) 0.061(6) 0.051(6) 0.019(5) -0.001(5) -0.002(5) C69 0.063(6) 0.066(6) 0.062(6) 0.025(5) 0.000(5) 0.010(5) C70 0.073(6) 0.034(5) 0.112(7) 0.029(5) 0.053(5) 0.018(4) C71 0.067(6) 0.024(4) 0.088(7) 0.019(5) 0.017(6) 0.004(4) C72 0.078(6) 0.047(5) 0.069(5) 0.018(4) 0.047(5) 0.014(5) C73 0.057(5) 0.031(4) 0.055(6) -0.007(4) 0.010(5) -0.004(4) C74 0.065(6) 0.023(4) 0.081(7) 0.001(4) 0.027(5) -0.003(4) C75 0.062(5) 0.028(4) 0.063(5) 0.014(4) 0.039(4) -0.003(4) C76 0.056(5) 0.037(5) 0.101(7) -0.035(5) 0.041(5) -0.005(4) O9 0.045(4) 0.058(4) 0.076(5) 0.020(4) 0.010(4) -0.002(3) O10 0.071(4) 0.059(4) 0.072(5) 0.012(4) 0.030(4) 0.014(4) O11 0.050(4) 0.053(5) 0.163(9) 0.010(6) 0.030(5) 0.004(4) O12 0.043(4) 0.117(7) 0.071(5) 0.002(5) 0.018(4) -0.007(4) C77 0.037(4) 0.046(5) 0.061(6) 0.012(4) 0.018(4) 0.020(4) C78 0.045(4) 0.028(4) 0.047(5) -0.005(4) 0.021(4) 0.002(4) C79 0.053(5) 0.046(5) 0.032(4) -0.018(4) 0.016(4) 0.006(4) C80 0.070(6) 0.085(8) 0.023(5) 0.001(5) 0.016(5) 0.018(6) C81 0.070(6) 0.049(6) 0.029(4) 0.005(4) 0.025(4) -0.009(5) C82 0.033(4) 0.059(6) 0.057(5) 0.007(5) 0.026(4) 0.008(4) C83 0.060(5) 0.068(7) 0.051(5) 0.013(5) 0.029(4) -0.003(5) C84 0.045(5) 0.056(6) 0.071(6) 0.022(5) 0.032(4) -0.009(5) C85 0.038(5) 0.038(5) 0.064(6) 0.006(5) 0.026(4) -0.003(4) C86 0.071(7) 0.067(7) 0.067(7) 0.030(6) 0.022(6) -0.015(6) C87 0.084(8) 0.031(5) 0.087(8) 0.010(5) 0.021(7) -0.012(5) C88 0.045(5) 0.027(5) 0.097(8) 0.003(5) 0.008(5) -0.009(4) C89 0.051(6) 0.037(5) 0.087(8) 0.004(6) 0.025(6) -0.003(5) C90 0.069(7) 0.062(7) 0.064(8) -0.008(6) -0.004(6) -0.009(6) C91 0.061(6) 0.039(5) 0.061(7) -0.004(5) 0.011(5) 0.002(5) C92 0.058(6) 0.040(6) 0.056(7) -0.013(5) 0.006(5) -0.008(5) C93 0.085(8) 0.050(6) 0.037(5) -0.009(5) 0.002(6) -0.018(6) C94 0.104(8) 0.051(6) 0.049(6) -0.009(5) 0.034(6) -0.006(6) C95 0.085(7) 0.046(6) 0.046(5) -0.014(4) 0.029(5) -0.016(5) C96 0.064(7) 0.043(6) 0.036(5) -0.004(5) 0.007(5) -0.006(5) C97 0.069(6) 0.041(5) 0.049(5) 0.009(4) 0.020(5) 0.003(5) C98 0.047(6) 0.047(6) 0.051(6) 0.009(5) 0.006(5) -0.020(5) C99 0.058(6) 0.038(5) 0.055(6) 0.013(4) 0.023(5) -0.001(5) C100 0.065(6) 0.035(5) 0.037(5) -0.002(4) 0.022(4) -0.019(4) C101 0.050(5) 0.041(6) 0.067(6) 0.006(5) 0.027(5) -0.002(5) C102 0.061(6) 0.024(5) 0.037(5) -0.008(4) 0.009(5) -0.021(4) C103 0.061(5) 0.040(5) 0.040(5) 0.000(4) 0.032(4) -0.022(4) C104 0.065(6) 0.068(7) 0.050(5) -0.009(5) 0.041(5) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C6 1.966(4) . ? Rh1 C16 1.966(5) . ? Rh1 C11 1.969(4) . ? Rh1 C1 1.979(5) . ? Rh2 C15 1.943(4) . ? Rh2 C10 1.967(5) . ? Rh2 C20 1.969(5) . ? Rh2 C5 1.971(4) . ? N1 C1 1.154(5) . ? N1 C2B 1.453(4) . ? N1 C2A 1.457(4) . ? N2 C5 1.145(5) . ? N2 C4 1.437(5) . ? N3 C6 1.159(5) . ? N3 C7 1.433(6) . ? N4 C10 1.143(6) . ? N4 C9 1.449(6) . ? N5 C11 1.156(5) . ? N5 C12B 1.439(10) . ? N5 C12A 1.457(4) . ? N6 C15 1.148(5) . ? N6 C14 1.436(5) . ? N7 C16 1.142(6) . ? N7 C17 1.444(6) . ? N8 C20 1.150(6) . ? N8 C19 1.459(6) . ? O1 C21 1.355(4) . ? O2 C28 1.334(5) . ? O3 C35 1.335(4) . ? O4 C42 1.338(5) . ? C2A C3A 1.540(9) . ? C3A C4 1.481(8) . ? C2B C3B 1.514(5) . ? C3B C4 1.524(5) . ? C7 C8 1.512(7) . ? C8 C9 1.518(7) . ? C12A C13A 1.517(8) . ? C13A C14 1.503(4) . ? C12B C13B 1.511(5) . ? C13B C14 1.509(4) . ? C17 C18 1.495(7) . ? C18 C19 1.510(7) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C48 1.492(6) . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.511(8) . ? C27 C29 1.508(7) . ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.495(6) . ? C34 C36 1.524(6) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.526(7) . ? C41 C43 1.553(7) . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.518(6) . ? O5 C49 1.347(8) . ? O6 C56 1.373(9) . ? O7 C63 1.337(9) . ? O8 C70 1.382(9) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 C76 1.564(11) . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.536(10) . ? C55 C57 1.530(10) . ? C56 C57 1.3900 . ? C56 C61 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.501(4) . ? C62 C64 1.500(4) . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.513(12) . ? C69 C71 1.533(11) . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.521(12) . ? O9 C77 1.354(8) . ? O10 C84 1.322(9) . ? O11 C91 1.342(11) . ? O12 C98 1.359(8) . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 C104 1.503(4) . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.530(11) . ? C83 C85 1.498(12) . ? C84 C85 1.3900 . ? C84 C89 1.3900 . ? C85 C86 1.3900 . ? C86 C87 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.520(13) . ? C90 C92 1.533(15) . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.540(11) . ? C97 C99 1.525(10) . ? C98 C99 1.3900 . ? C98 C103 1.3900 . ? C99 C100 1.3900 . ? C100 C101 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.500(4) . ? 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 C6 Rh1 C16 178.53(17) . . ? C6 Rh1 C11 88.78(17) . . ? C16 Rh1 C11 90.94(18) . . ? C6 Rh1 C1 90.14(18) . . ? C16 Rh1 C1 90.28(19) . . ? C11 Rh1 C1 174.06(17) . . ? C15 Rh2 C10 86.90(18) . . ? C15 Rh2 C20 92.61(19) . . ? C10 Rh2 C20 174.65(18) . . ? C15 Rh2 C5 176.41(17) . . ? C10 Rh2 C5 90.45(18) . . ? C20 Rh2 C5 90.26(18) . . ? C1 N1 C2B 165.0(5) . . ? C1 N1 C2A 169.9(5) . . ? C2B N1 C2A 23.4(4) . . ? C5 N2 C4 174.1(4) . . ? C6 N3 C7 170.5(4) . . ? C10 N4 C9 177.4(5) . . ? C11 N5 C12B 163.1(5) . . ? C11 N5 C12A 168.9(5) . . ? C12B N5 C12A 27.7(4) . . ? C15 N6 C14 170.3(4) . . ? C16 N7 C17 169.0(4) . . ? C20 N8 C19 178.5(5) . . ? N1 C1 Rh1 172.2(4) . . ? N1 C2A C3A 108.9(5) . . ? C4 C3A C2A 111.6(5) . . ? N1 C2B C3B 100.8(4) . . ? C2B C3B C4 116.8(6) . . ? N2 C4 C3A 109.5(4) . . ? N2 C4 C3B 112.5(4) . . ? C3A C4 C3B 45.8(4) . . ? N2 C5 Rh2 179.2(4) . . ? N3 C6 Rh1 176.4(4) . . ? N3 C7 C8 112.0(4) . . ? C7 C8 C9 114.2(4) . . ? N4 C9 C8 113.0(4) . . ? N4 C10 Rh2 174.0(4) . . ? N5 C11 Rh1 174.1(4) . . ? N5 C12A C13A 111.6(5) . . ? C14 C13A C12A 115.2(4) . . ? N5 C12B C13B 101.8(7) . . ? C14 C13B C12B 126.9(7) . . ? N6 C14 C13A 112.5(4) . . ? N6 C14 C13B 109.2(5) . . ? C13A C14 C13B 34.4(5) . . ? N6 C15 Rh2 173.3(4) . . ? N7 C16 Rh1 178.2(4) . . ? N7 C17 C18 110.8(4) . . ? C17 C18 C19 116.1(4) . . ? N8 C19 C18 112.7(4) . . ? N8 C20 Rh2 173.8(4) . . ? O1 C21 C22 120.7(3) . . ? O1 C21 C26 119.3(3) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 C48 120.2(3) . . ? C21 C22 C48 119.8(3) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C27 119.9(3) . . ? C21 C26 C27 120.1(3) . . ? C29 C27 C26 112.7(4) . . ? O2 C28 C29 119.5(3) . . ? O2 C28 C33 120.4(3) . . ? C29 C28 C33 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 C27 122.2(3) . . ? C30 C29 C27 117.8(3) . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C28 120.0 . . ? C32 C33 C34 119.2(3) . . ? C28 C33 C34 120.8(3) . . ? C33 C34 C36 112.8(4) . . ? O3 C35 C36 123.0(3) . . ? O3 C35 C40 116.9(3) . . ? C36 C35 C40 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 C34 119.1(3) . . ? C37 C36 C34 120.9(3) . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 C41 119.4(3) . . ? C35 C40 C41 120.2(3) . . ? C40 C41 C43 113.0(4) . . ? O4 C42 C43 120.5(3) . . ? O4 C42 C47 119.5(3) . . ? C43 C42 C47 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 C41 117.8(3) . . ? C42 C43 C41 122.1(3) . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 C48 117.8(3) . . ? C42 C47 C48 122.2(3) . . ? C22 C48 C47 111.5(4) . . ? O5 C49 C50 118.1(5) . . ? O5 C49 C54 121.7(5) . . ? C50 C49 C54 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 C76 118.5(5) . . ? C51 C50 C76 121.4(5) . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 C55 119.0(5) . . ? C49 C54 C55 121.0(5) . . ? C57 C55 C54 113.4(6) . . ? O6 C56 C57 117.9(4) . . ? O6 C56 C61 122.0(4) . . ? C57 C56 C61 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 C55 117.3(4) . . ? C56 C57 C55 122.7(4) . . ? C57 C58 C59 120.0 . . ? C58 C59 C60 120.0 . . ? C61 C60 C59 120.0 . . ? C60 C61 C56 120.0 . . ? C60 C61 C62 120.5(4) . . ? C56 C61 C62 119.4(4) . . ? C64 C62 C61 114.3(4) . . ? O7 C63 C64 119.1(4) . . ? O7 C63 C68 120.9(4) . . ? C64 C63 C68 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 C62 122.4(5) . . ? C65 C64 C62 117.5(5) . . ? C64 C65 C66 120.0 . . ? C67 C66 C65 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C63 120.0 . . ? C67 C68 C69 118.2(6) . . ? C63 C68 C69 121.8(6) . . ? C68 C69 C71 112.5(7) . . ? O8 C70 C71 120.2(5) . . ? O8 C70 C75 119.7(5) . . ? C71 C70 C75 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 C69 118.3(6) . . ? C70 C71 C69 121.7(6) . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C70 120.0 . . ? C74 C75 C76 120.5(4) . . ? C70 C75 C76 119.3(4) . . ? C75 C76 C50 110.9(6) . . ? O9 C77 C78 119.2(4) . . ? O9 C77 C82 120.8(4) . . ? C78 C77 C82 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 C104 122.0(4) . . ? C79 C78 C104 117.3(4) . . ? C80 C79 C78 120.0 . . ? C79 C80 C81 120.0 . . ? C82 C81 C80 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 C83 120.0(5) . . ? C77 C82 C83 119.9(5) . . ? C85 C83 C82 114.8(7) . . ? O10 C84 C85 121.6(5) . . ? O10 C84 C89 118.3(5) . . ? C85 C84 C89 120.0 . . ? C86 C85 C84 120.0 . . ? C86 C85 C83 119.0(5) . . ? C84 C85 C83 121.0(5) . . ? C87 C86 C85 120.0 . . ? C86 C87 C88 120.0 . . ? C89 C88 C87 120.0 . . ? C88 C89 C84 120.0 . . ? C88 C89 C90 120.0(6) . . ? C84 C89 C90 119.8(6) . . ? C89 C90 C92 111.9(8) . . ? O11 C91 C92 120.7(5) . . ? O11 C91 C96 119.2(5) . . ? C92 C91 C96 120.0 . . ? C91 C92 C93 120.0 . . ? C91 C92 C90 117.5(6) . . ? C93 C92 C90 122.4(6) . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C96 C95 C94 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 C97 117.0(6) . . ? C91 C96 C97 123.0(6) . . ? C99 C97 C96 113.5(7) . . ? O12 C98 C99 119.3(5) . . ? O12 C98 C103 120.6(4) . . ? C99 C98 C103 120.0 . . ? C98 C99 C100 120.0 . . ? C98 C99 C97 124.1(5) . . ? C100 C99 C97 115.9(5) . . ? C101 C100 C99 120.0 . . ? C102 C101 C100 120.0 . . ? C103 C102 C101 120.0 . . ? C102 C103 C98 120.0 . . ? C102 C103 C104 119.3(3) . . ? C98 C103 C104 120.6(3) . . ? C103 C104 C78 119.3(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 C2B N1 C1 Rh1 65(4) . . . . ? C2A N1 C1 Rh1 -72(5) . . . . ? C6 Rh1 C1 N1 92(3) . . . . ? C16 Rh1 C1 N1 -89(3) . . . . ? C11 Rh1 C1 N1 12(5) . . . . ? C1 N1 C2A C3A 97(3) . . . . ? C2B N1 C2A C3A -56.3(10) . . . . ? N1 C2A C3A C4 -79.9(6) . . . . ? C1 N1 C2B C3B -121.2(16) . . . . ? C2A N1 C2B C3B 41.3(8) . . . . ? N1 C2B C3B C4 85.1(7) . . . . ? C5 N2 C4 C3A 5(5) . . . . ? C5 N2 C4 C3B 54(4) . . . . ? C2A C3A C4 N2 76.4(6) . . . . ? C2A C3A C4 C3B -26.3(5) . . . . ? C2B C3B C4 N2 -63.4(7) . . . . ? C2B C3B C4 C3A 32.4(5) . . . . ? C4 N2 C5 Rh2 -23(41) . . . . ? C15 Rh2 C5 N2 -153(36) . . . . ? C10 Rh2 C5 N2 -111(37) . . . . ? C20 Rh2 C5 N2 64(37) . . . . ? C7 N3 C6 Rh1 -15(7) . . . . ? C16 Rh1 C6 N3 119(7) . . . . ? C11 Rh1 C6 N3 40(6) . . . . ? C1 Rh1 C6 N3 -135(6) . . . . ? C6 N3 C7 C8 17(3) . . . . ? N3 C7 C8 C9 71.6(5) . . . . ? C10 N4 C9 C8 50(10) . . . . ? C7 C8 C9 N4 -68.2(6) . . . . ? C9 N4 C10 Rh2 -64(12) . . . . ? C15 Rh2 C10 N4 -62(4) . . . . ? C20 Rh2 C10 N4 23(5) . . . . ? C5 Rh2 C10 N4 121(4) . . . . ? C12B N5 C11 Rh1 -128(4) . . . . ? C12A N5 C11 Rh1 68(5) . . . . ? C6 Rh1 C11 N5 -73(4) . . . . ? C16 Rh1 C11 N5 108(4) . . . . ? C1 Rh1 C11 N5 6(5) . . . . ? C11 N5 C12A C13A -130(2) . . . . ? C12B N5 C12A C13A 60.3(9) . . . . ? N5 C12A C13A C14 76.9(6) . . . . ? C11 N5 C12B C13B 144.5(15) . . . . ? C12A N5 C12B C13B -42.1(7) . . . . ? N5 C12B C13B C14 -78.3(12) . . . . ? C15 N6 C14 C13A 49(3) . . . . ? C15 N6 C14 C13B 12(3) . . . . ? C12A C13A C14 N6 -63.1(6) . . . . ? C12A C13A C14 C13B 28.4(7) . . . . ? C12B C13B C14 N6 59.5(12) . . . . ? C12B C13B C14 C13A -42.4(9) . . . . ? C14 N6 C15 Rh2 36(5) . . . . ? C10 Rh2 C15 N6 21(3) . . . . ? C20 Rh2 C15 N6 -154(3) . . . . ? C5 Rh2 C15 N6 63(5) . . . . ? C17 N7 C16 Rh1 -6(14) . . . . ? C6 Rh1 C16 N7 170(10) . . . . ? C11 Rh1 C16 N7 -111(12) . . . . ? C1 Rh1 C16 N7 63(12) . . . . ? C16 N7 C17 C18 -5(3) . . . . ? N7 C17 C18 C19 73.0(6) . . . . ? C20 N8 C19 C18 78(20) . . . . ? C17 C18 C19 N8 -71.3(6) . . . . ? C19 N8 C20 Rh2 -54(22) . . . . ? C15 Rh2 C20 N8 93(4) . . . . ? C10 Rh2 C20 N8 9(5) . . . . ? C5 Rh2 C20 N8 -89(4) . . . . ? O1 C21 C22 C23 -178.5(3) . . . . ? C26 C21 C22 C23 0.0 . . . . ? O1 C21 C22 C48 3.3(4) . . . . ? C26 C21 C22 C48 -178.2(3) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C48 C22 C23 C24 178.2(3) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C24 C25 C26 C27 179.5(3) . . . . ? O1 C21 C26 C25 178.5(3) . . . . ? C22 C21 C26 C25 0.0 . . . . ? O1 C21 C26 C27 -1.1(4) . . . . ? C22 C21 C26 C27 -179.5(3) . . . . ? C25 C26 C27 C29 97.5(4) . . . . ? C21 C26 C27 C29 -82.9(5) . . . . ? O2 C28 C29 C30 176.5(3) . . . . ? C33 C28 C29 C30 0.0 . . . . ? O2 C28 C29 C27 -2.5(5) . . . . ? C33 C28 C29 C27 -179.0(4) . . . . ? C26 C27 C29 C28 92.3(5) . . . . ? C26 C27 C29 C30 -86.8(4) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C27 C29 C30 C31 179.1(4) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C28 0.0 . . . . ? C31 C32 C33 C34 179.4(4) . . . . ? O2 C28 C33 C32 -176.5(3) . . . . ? C29 C28 C33 C32 0.0 . . . . ? O2 C28 C33 C34 4.2(4) . . . . ? C29 C28 C33 C34 -179.4(4) . . . . ? C32 C33 C34 C36 89.0(4) . . . . ? C28 C33 C34 C36 -91.6(4) . . . . ? O3 C35 C36 C37 -176.4(3) . . . . ? C40 C35 C36 C37 0.0 . . . . ? O3 C35 C36 C34 4.9(4) . . . . ? C40 C35 C36 C34 -178.7(3) . . . . ? C33 C34 C36 C35 84.6(4) . . . . ? C33 C34 C36 C37 -94.1(4) . . . . ? C35 C36 C37 C38 0.0 . . . . ? C34 C36 C37 C38 178.7(3) . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C35 0.0 . . . . ? C38 C39 C40 C41 -172.7(3) . . . . ? O3 C35 C40 C39 176.6(3) . . . . ? C36 C35 C40 C39 0.0 . . . . ? O3 C35 C40 C41 -10.7(4) . . . . ? C36 C35 C40 C41 172.7(3) . . . . ? C39 C40 C41 C43 92.3(4) . . . . ? C35 C40 C41 C43 -80.4(5) . . . . ? O4 C42 C43 C44 -178.9(3) . . . . ? C47 C42 C43 C44 0.0 . . . . ? O4 C42 C43 C41 5.0(4) . . . . ? C47 C42 C43 C41 -176.1(4) . . . . ? C40 C41 C43 C44 -78.8(4) . . . . ? C40 C41 C43 C42 97.4(4) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C41 C43 C44 C45 176.3(4) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C42 0.0 . . . . ? C45 C46 C47 C48 -177.9(4) . . . . ? O4 C42 C47 C46 178.9(3) . . . . ? C43 C42 C47 C46 0.0 . . . . ? O4 C42 C47 C48 -3.3(4) . . . . ? C43 C42 C47 C48 177.8(4) . . . . ? C23 C22 C48 C47 -100.1(4) . . . . ? C21 C22 C48 C47 78.1(5) . . . . ? C46 C47 C48 C22 81.2(5) . . . . ? C42 C47 C48 C22 -96.6(4) . . . . ? O5 C49 C50 C51 -176.0(5) . . . . ? C54 C49 C50 C51 0.0 . . . . ? O5 C49 C50 C76 8.3(7) . . . . ? C54 C49 C50 C76 -175.8(6) . . . . ? C49 C50 C51 C52 0.0 . . . . ? C76 C50 C51 C52 175.6(6) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C49 0.0 . . . . ? C52 C53 C54 C55 -177.5(6) . . . . ? O5 C49 C54 C53 175.8(5) . . . . ? C50 C49 C54 C53 0.0 . . . . ? O5 C49 C54 C55 -6.8(7) . . . . ? C50 C49 C54 C55 177.4(6) . . . . ? C53 C54 C55 C57 99.2(6) . . . . ? C49 C54 C55 C57 -78.3(7) . . . . ? O6 C56 C57 C58 175.7(5) . . . . ? C61 C56 C57 C58 0.0 . . . . ? O6 C56 C57 C55 -4.3(7) . . . . ? C61 C56 C57 C55 180.0(5) . . . . ? C54 C55 C57 C58 -87.4(7) . . . . ? C54 C55 C57 C56 92.7(7) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C55 C57 C58 C59 -180.0(5) . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C56 0.0 . . . . ? C59 C60 C61 C62 -177.3(5) . . . . ? O6 C56 C61 C60 -175.5(5) . . . . ? C57 C56 C61 C60 0.0 . . . . ? O6 C56 C61 C62 1.8(6) . . . . ? C57 C56 C61 C62 177.4(4) . . . . ? C60 C61 C62 C64 83.3(6) . . . . ? C56 C61 C62 C64 -94.1(6) . . . . ? O7 C63 C64 C65 -179.9(4) . . . . ? C68 C63 C64 C65 0.0 . . . . ? O7 C63 C64 C62 4.1(5) . . . . ? C68 C63 C64 C62 -176.0(5) . . . . ? C61 C62 C64 C63 77.0(7) . . . . ? C61 C62 C64 C65 -99.1(6) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C62 C64 C65 C66 176.2(4) . . . . ? C64 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C63 0.0 . . . . ? C66 C67 C68 C69 179.5(6) . . . . ? O7 C63 C68 C67 179.9(4) . . . . ? C64 C63 C68 C67 0.0 . . . . ? O7 C63 C68 C69 0.4(7) . . . . ? C64 C63 C68 C69 -179.5(6) . . . . ? C67 C68 C69 C71 106.0(8) . . . . ? C63 C68 C69 C71 -74.5(9) . . . . ? O8 C70 C71 C72 -175.9(6) . . . . ? C75 C70 C71 C72 0.0 . . . . ? O8 C70 C71 C69 4.6(8) . . . . ? C75 C70 C71 C69 -179.5(6) . . . . ? C68 C69 C71 C72 -85.0(9) . . . . ? C68 C69 C71 C70 94.4(8) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C69 C71 C72 C73 179.5(6) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C73 C74 C75 C76 -176.1(6) . . . . ? O8 C70 C75 C74 176.0(6) . . . . ? C71 C70 C75 C74 0.0 . . . . ? O8 C70 C75 C76 -7.9(7) . . . . ? C71 C70 C75 C76 176.1(6) . . . . ? C74 C75 C76 C50 75.2(7) . . . . ? C70 C75 C76 C50 -100.9(6) . . . . ? C49 C50 C76 C75 84.4(7) . . . . ? C51 C50 C76 C75 -91.3(6) . . . . ? O9 C77 C78 C79 179.7(5) . . . . ? C82 C77 C78 C79 0.0 . . . . ? O9 C77 C78 C104 9.5(6) . . . . ? C82 C77 C78 C104 -170.2(5) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C104 C78 C79 C80 170.6(5) . . . . ? C78 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C77 0.0 . . . . ? C80 C81 C82 C83 -178.6(6) . . . . ? O9 C77 C82 C81 -179.7(5) . . . . ? C78 C77 C82 C81 0.0 . . . . ? O9 C77 C82 C83 -1.1(7) . . . . ? C78 C77 C82 C83 178.6(6) . . . . ? C81 C82 C83 C85 100.6(7) . . . . ? C77 C82 C83 C85 -77.9(8) . . . . ? O10 C84 C85 C86 -178.6(6) . . . . ? C89 C84 C85 C86 0.0 . . . . ? O10 C84 C85 C83 -0.1(8) . . . . ? C89 C84 C85 C83 178.4(7) . . . . ? C82 C83 C85 C86 -87.8(7) . . . . ? C82 C83 C85 C84 93.7(8) . . . . ? C84 C85 C86 C87 0.0 . . . . ? C83 C85 C86 C87 -178.5(6) . . . . ? C85 C86 C87 C88 0.0 . . . . ? C86 C87 C88 C89 0.0 . . . . ? C87 C88 C89 C84 0.0 . . . . ? C87 C88 C89 C90 -175.0(8) . . . . ? O10 C84 C89 C88 178.6(5) . . . . ? C85 C84 C89 C88 0.0 . . . . ? O10 C84 C89 C90 -6.4(8) . . . . ? C85 C84 C89 C90 175.0(8) . . . . ? C88 C89 C90 C92 77.2(9) . . . . ? C84 C89 C90 C92 -97.8(9) . . . . ? O11 C91 C92 C93 -175.4(7) . . . . ? C96 C91 C92 C93 0.0 . . . . ? O11 C91 C92 C90 8.9(8) . . . . ? C96 C91 C92 C90 -175.7(6) . . . . ? C89 C90 C92 C91 86.7(9) . . . . ? C89 C90 C92 C93 -88.8(8) . . . . ? C91 C92 C93 C94 0.0 . . . . ? C90 C92 C93 C94 175.5(7) . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C94 C95 C96 C97 -178.9(6) . . . . ? O11 C91 C96 C95 175.5(6) . . . . ? C92 C91 C96 C95 0.0 . . . . ? O11 C91 C96 C97 -5.7(8) . . . . ? C92 C91 C96 C97 178.8(6) . . . . ? C95 C96 C97 C99 100.4(7) . . . . ? C91 C96 C97 C99 -78.4(9) . . . . ? O12 C98 C99 C100 176.9(6) . . . . ? C103 C98 C99 C100 0.0 . . . . ? O12 C98 C99 C97 -2.1(8) . . . . ? C103 C98 C99 C97 -179.0(6) . . . . ? C96 C97 C99 C98 87.0(8) . . . . ? C96 C97 C99 C100 -92.0(8) . . . . ? C98 C99 C100 C101 0.0 . . . . ? C97 C99 C100 C101 179.0(6) . . . . ? C99 C100 C101 C102 0.0 . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C98 0.0 . . . . ? C101 C102 C103 C104 -175.9(5) . . . . ? O12 C98 C103 C102 -176.9(6) . . . . ? C99 C98 C103 C102 0.0 . . . . ? O12 C98 C103 C104 -1.0(7) . . . . ? C99 C98 C103 C104 175.9(5) . . . . ? C102 C103 C104 C78 85.2(5) . . . . ? C98 C103 C104 C78 -90.7(6) . . . . ? C77 C78 C104 C103 75.7(6) . . . . ? C79 C78 C104 C103 -94.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.998 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.099 data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 248492' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(dihex)4)(PF6)2 _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 F12 N8 P2 Rh2' _chemical_formula_weight 1040.54 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/mnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 13.01390(10) _cell_length_b 13.01390(10) _cell_length_c 26.2806(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4450.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.02 _exptl_crystal_description plate _exptl_crystal_colour maroon _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.8773 _exptl_absorpt_correction_T_max 0.9358 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent acetonitrile/methylene chloride/diethyl ether ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 73815 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.02 _reflns_number_total 3315 _reflns_number_gt 2236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+27.5274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3315 _refine_ls_number_parameters 168 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.41581(2) 0.08419(2) 0.2500 0.01712(11) Uani 1 2 d S . . P1 P 0.4355(3) 0.1913(3) 0.5000 0.0287(7) Uani 0.50 2 d SP . . F1 F 0.4360(9) 0.0693(7) 0.5000 0.055(2) Uani 0.50 2 d SP . . F2 F 0.4354(5) 0.1914(5) 0.4394(2) 0.0440(15) Uani 0.50 1 d P . . F3 F 0.4391(8) 0.3154(9) 0.5000 0.060(3) Uani 0.50 2 d SP . . F4 F 0.3152(6) 0.1924(7) 0.5000 0.0390(18) Uani 0.50 2 d SP . . F5 F 0.5583(7) 0.1882(9) 0.5000 0.050(2) Uani 0.50 2 d SP . . P2 P 0.0000 0.0000 0.30917(9) 0.0256(4) Uani 1 4 d S . . F6 F 0.0000 0.0000 0.37002(19) 0.0323(11) Uani 1 4 d S A . F7 F 0.0000 0.0000 0.2476(2) 0.0312(10) Uani 1 4 d S A . F8A F 0.0302(4) -0.1191(3) 0.30712(15) 0.0349(9) Uani 0.70 1 d P A 1 F8B F 0.0902(8) -0.0829(7) 0.3138(4) 0.0356(19) Uani 0.30 1 d P A 2 N1 N 0.2535(3) -0.0781(2) 0.21628(14) 0.0242(7) Uani 1 1 d . . . N2A N 0.3678(5) 0.0267(5) 0.3628(2) 0.0306(14) Uani 0.70 1 d P B 1 C6A C 0.3402(5) -0.0079(6) 0.4132(3) 0.0354(14) Uiso 0.70 1 d P B 1 H6AA H 0.3280 0.0525 0.4352 0.043 Uiso 0.70 1 calc PR B 1 H6AB H 0.3981 -0.0475 0.4278 0.043 Uiso 0.70 1 calc PR B 1 C7A C 0.2446(6) -0.0748(6) 0.4128(3) 0.0382(15) Uiso 0.70 1 d P B 1 H7AA H 0.1850 -0.0320 0.4028 0.046 Uiso 0.70 1 calc PR B 1 H7AB H 0.2319 -0.1001 0.4478 0.046 Uiso 0.70 1 calc PR B 1 C8A C 0.2511(6) -0.1680(5) 0.3765(3) 0.0320(13) Uiso 0.70 1 d P B 1 H8AA H 0.2572 -0.1426 0.3411 0.038 Uiso 0.70 1 calc PR B 1 H8AB H 0.1864 -0.2076 0.3790 0.038 Uiso 0.70 1 calc PR B 1 N2B N 0.3250(9) 0.0426(11) 0.3562(3) 0.021(2) Uani 0.30 1 d PD B 2 C6B C 0.2735(10) 0.0106(11) 0.4028(4) 0.027(3) Uiso 0.30 1 d PD B 2 H6BA H 0.1990 0.0024 0.3963 0.033 Uiso 0.30 1 calc PR B 2 H6BB H 0.2823 0.0640 0.4292 0.033 Uiso 0.30 1 calc PR B 2 C7B C 0.3174(11) -0.0892(10) 0.4213(5) 0.026(3) Uiso 0.30 1 d P B 2 H7BA H 0.2867 -0.1061 0.4547 0.031 Uiso 0.30 1 calc PR B 2 H7BB H 0.3924 -0.0812 0.4262 0.031 Uiso 0.30 1 calc PR B 2 C8B C 0.2977(11) -0.1798(10) 0.3838(5) 0.024(3) Uiso 0.30 1 d P B 2 H8BA H 0.2258 -0.2033 0.3882 0.029 Uiso 0.30 1 calc PR B 2 H8BB H 0.3047 -0.1538 0.3486 0.029 Uiso 0.30 1 calc PR B 2 C1 C 0.3132(3) -0.0169(3) 0.22783(16) 0.0220(7) Uani 1 1 d . . . C2 C 0.3777(4) 0.0518(3) 0.32103(18) 0.0322(9) Uani 1 1 d D . . C3 C 0.1819(3) -0.1568(3) 0.20170(18) 0.0302(9) Uani 1 1 d . . . H3A H 0.1175 -0.1485 0.2213 0.036 Uiso 1 1 calc R . . H3B H 0.2111 -0.2251 0.2100 0.036 Uiso 1 1 calc R . . C4 C 0.1580(4) -0.1518(5) 0.14518(18) 0.0427(12) Uani 1 1 d . . . H4A H 0.1179 -0.0887 0.1382 0.051 Uiso 1 1 calc R . . H4B H 0.1147 -0.2114 0.1359 0.051 Uiso 1 1 calc R . . C5 C 0.2544(5) -0.1516(5) 0.1116(2) 0.0499(13) Uani 1 1 d U . . H5A H 0.2922 -0.0865 0.1169 0.060 Uiso 1 1 calc R . . H5B H 0.2332 -0.1543 0.0754 0.060 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 0.01143(13) 0.01143(13) 0.0285(2) -0.00038(11) -0.00038(11) -0.00095(12) P1 0.0258(15) 0.0410(18) 0.0193(13) 0.000 0.000 0.0010(13) F1 0.080(7) 0.040(5) 0.044(5) 0.000 0.000 0.012(5) F2 0.038(3) 0.071(4) 0.023(2) 0.010(3) -0.002(2) -0.006(3) F3 0.059(6) 0.060(6) 0.062(6) 0.000 0.000 0.006(5) F4 0.030(4) 0.053(5) 0.033(4) 0.000 0.000 0.002(3) F5 0.033(4) 0.092(8) 0.023(4) 0.000 0.000 0.002(5) P2 0.0239(6) 0.0239(6) 0.0291(10) 0.000 0.000 0.000 F6 0.0351(17) 0.0351(17) 0.027(2) 0.000 0.000 0.000 F7 0.0327(16) 0.0327(16) 0.028(2) 0.000 0.000 0.000 F8A 0.048(2) 0.0220(18) 0.035(2) 0.0011(16) 0.0041(19) 0.0049(17) F8B 0.039(5) 0.028(5) 0.040(5) 0.003(4) 0.006(4) 0.011(4) N1 0.0200(15) 0.0191(15) 0.0336(17) -0.0020(13) 0.0014(14) -0.0006(12) N2A 0.031(3) 0.027(3) 0.034(3) 0.001(2) -0.009(3) 0.003(3) N2B 0.024(6) 0.022(6) 0.016(5) 0.003(4) -0.006(5) -0.011(5) C1 0.0151(15) 0.0183(17) 0.0326(18) 0.0000(15) 0.0008(14) 0.0018(13) C2 0.037(2) 0.0220(19) 0.037(2) -0.0030(17) 0.000(2) -0.0090(18) C3 0.0248(19) 0.0238(19) 0.042(2) -0.0060(17) 0.0029(17) -0.0077(16) C4 0.035(3) 0.051(3) 0.042(3) 0.002(2) -0.010(2) -0.022(2) C5 0.048(2) 0.056(2) 0.0448(19) -0.0005(16) -0.0010(16) -0.0137(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.963(4) . ? Rh1 C1 1.963(4) 8 ? Rh1 C2 1.977(5) . ? Rh1 C2 1.977(5) 8 ? Rh1 Rh1 3.0989(7) 2_655 ? P1 F4 1.566(9) . ? P1 F1 1.588(10) . ? P1 F2 1.593(5) 10_556 ? P1 F2 1.593(5) . ? P1 F5 1.598(9) . ? P1 F3 1.616(12) . ? P2 F8B 1.599(9) 2 ? P2 F8B 1.599(9) 4 ? P2 F8B 1.599(9) 3 ? P2 F8B 1.599(9) . ? P2 F6 1.599(5) . ? P2 F8A 1.599(4) 4 ? P2 F8A 1.599(4) 3 ? P2 F8A 1.599(4) 2 ? P2 F8A 1.599(4) . ? P2 F7 1.619(6) . ? N1 C1 1.153(5) . ? N1 C3 1.437(5) . ? N2A C2 1.153(8) . ? N2A C6A 1.444(9) . ? C6A C7A 1.518(10) . ? C7A C8A 1.545(10) . ? C8A C5 1.650(9) 7_545 ? N2B C2 1.156(5) . ? N2B C6B 1.458(5) . ? C6B C7B 1.501(19) . ? C7B C8B 1.557(19) . ? C8B C5 1.088(15) 7_545 ? C3 C4 1.519(6) . ? C4 C5 1.534(8) . ? C5 C8B 1.088(15) 7_545 ? C5 C8A 1.650(9) 7_545 ? 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 179.2(2) . 8 ? C1 Rh1 C2 88.10(17) . . ? C1 Rh1 C2 91.88(17) 8 . ? C1 Rh1 C2 91.88(17) . 8 ? C1 Rh1 C2 88.10(17) 8 8 ? C2 Rh1 C2 176.9(3) . 8 ? C1 Rh1 Rh1 90.42(11) . 2_655 ? C1 Rh1 Rh1 90.42(11) 8 2_655 ? C2 Rh1 Rh1 91.53(14) . 2_655 ? C2 Rh1 Rh1 91.53(14) 8 2_655 ? F4 P1 F1 90.8(6) . . ? F4 P1 F2 89.9(2) . 10_556 ? F1 P1 F2 90.1(3) . 10_556 ? F4 P1 F2 89.9(2) . . ? F1 P1 F2 90.1(3) . . ? F2 P1 F2 179.8(6) 10_556 . ? F4 P1 F5 179.1(6) . . ? F1 P1 F5 88.4(6) . . ? F2 P1 F5 90.1(2) 10_556 . ? F2 P1 F5 90.1(2) . . ? F4 P1 F3 91.1(5) . . ? F1 P1 F3 178.1(6) . . ? F2 P1 F3 89.9(3) 10_556 . ? F2 P1 F3 89.9(3) . . ? F5 P1 F3 89.8(6) . . ? F8B P2 F8B 89.67(6) 2 4 ? F8B P2 F8B 89.67(6) 2 3 ? F8B P2 F8B 171.3(7) 4 3 ? F8B P2 F8B 171.3(7) 2 . ? F8B P2 F8B 89.67(5) 4 . ? F8B P2 F8B 89.67(5) 3 . ? F8B P2 F6 85.6(4) 2 . ? F8B P2 F6 85.6(4) 4 . ? F8B P2 F6 85.6(4) 3 . ? F8B P2 F6 85.6(4) . . ? F8B P2 F8A 57.1(4) 2 4 ? F8B P2 F8A 33.7(4) 4 4 ? F8B P2 F8A 146.8(4) 3 4 ? F8B P2 F8A 123.2(4) . 4 ? F6 P2 F8A 91.93(17) . 4 ? F8B P2 F8A 123.2(4) 2 3 ? F8B P2 F8A 146.8(4) 4 3 ? F8B P2 F8A 33.7(4) 3 3 ? F8B P2 F8A 57.1(4) . 3 ? F6 P2 F8A 91.93(17) . 3 ? F8A P2 F8A 176.1(3) 4 3 ? F8B P2 F8A 33.7(4) 2 2 ? F8B P2 F8A 123.2(4) 4 2 ? F8B P2 F8A 57.1(4) 3 2 ? F8B P2 F8A 146.8(4) . 2 ? F6 P2 F8A 91.93(17) . 2 ? F8A P2 F8A 89.935(12) 4 2 ? F8A P2 F8A 89.935(12) 3 2 ? F8B P2 F8A 146.8(4) 2 . ? F8B P2 F8A 57.1(4) 4 . ? F8B P2 F8A 123.2(4) 3 . ? F8B P2 F8A 33.7(4) . . ? F6 P2 F8A 91.93(17) . . ? F8A P2 F8A 89.934(12) 4 . ? F8A P2 F8A 89.936(12) 3 . ? F8A P2 F8A 176.1(3) 2 . ? F8B P2 F7 94.4(4) 2 . ? F8B P2 F7 94.4(4) 4 . ? F8B P2 F7 94.4(4) 3 . ? F8B P2 F7 94.4(4) . . ? F6 P2 F7 180.000(1) . . ? F8A P2 F7 88.07(17) 4 . ? F8A P2 F7 88.07(17) 3 . ? F8A P2 F7 88.07(17) 2 . ? F8A P2 F7 88.07(17) . . ? C1 N1 C3 178.1(4) . . ? C2 N2A C6A 171.7(7) . . ? N2A C6A C7A 112.1(6) . . ? C6A C7A C8A 114.1(6) . . ? C7A C8A C5 113.9(6) . 7_545 ? C2 N2B C6B 166.9(14) . . ? N2B C6B C7B 110.1(11) . . ? C6B C7B C8B 112.8(11) . . ? C5 C8B C7B 115.2(13) 7_545 . ? N1 C1 Rh1 177.7(4) . . ? N2A C2 N2B 31.1(6) . . ? N2A C2 Rh1 171.0(5) . . ? N2B C2 Rh1 157.7(8) . . ? N1 C3 C4 111.3(4) . . ? C3 C4 C5 113.3(4) . . ? C8B C5 C4 125.3(9) 7_545 . ? C8B C5 C8A 14.4(8) 7_545 7_545 ? C4 C5 C8A 113.0(5) . 7_545 ? 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 C2 N2A C6A C7A 21(5) . . . . ? N2A C6A C7A C8A 54.7(8) . . . . ? C6A C7A C8A C5 57.8(8) . . . 7_545 ? C2 N2B C6B C7B -5(6) . . . . ? N2B C6B C7B C8B -64.5(15) . . . . ? C6B C7B C8B C5 160.0(12) . . . 7_545 ? C3 N1 C1 Rh1 -67(19) . . . . ? C1 Rh1 C1 N1 -120(9) 8 . . . ? C2 Rh1 C1 N1 -31(9) . . . . ? C2 Rh1 C1 N1 152(9) 8 . . . ? Rh1 Rh1 C1 N1 60(9) 2_655 . . . ? C6A N2A C2 N2B 29(4) . . . . ? C6A N2A C2 Rh1 -140(4) . . . . ? C6B N2B C2 N2A -32(5) . . . . ? C6B N2B C2 Rh1 143(5) . . . . ? C1 Rh1 C2 N2A 108(3) . . . . ? C1 Rh1 C2 N2A -73(3) 8 . . . ? C2 Rh1 C2 N2A -162(3) 8 . . . ? Rh1 Rh1 C2 N2A 18(3) 2_655 . . . ? C1 Rh1 C2 N2B -57(2) . . . . ? C1 Rh1 C2 N2B 122(2) 8 . . . ? C2 Rh1 C2 N2B 32.4(19) 8 . . . ? Rh1 Rh1 C2 N2B -148(2) 2_655 . . . ? C1 N1 C3 C4 -95(13) . . . . ? N1 C3 C4 C5 52.5(6) . . . . ? C3 C4 C5 C8B 45.5(12) . . . 7_545 ? C3 C4 C5 C8A 53.9(6) . . . 7_545 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.251 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.130 data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 248493' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(dihex)4)(Calix)2x0.5C2H5OH _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C89 H97 N8 O8.50 Rh2' _chemical_formula_weight 1620.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 19.021(11) _cell_length_b 19.021(11) _cell_length_c 45.85(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16589(16) _cell_formula_units_Z 8 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 750 _cell_measurement_theta_min 1.05 _cell_measurement_theta_max 20.00 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6760 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9556 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent methylene chloride/DMSO/diethyl ether ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.64300 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 53255 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 20.00 _reflns_number_total 10477 _reflns_number_gt 9226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+90.6901P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.133(16) _refine_ls_number_reflns 10477 _refine_ls_number_parameters 940 _refine_ls_number_restraints 332 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_restrained_S_all 1.210 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh2 Rh 0.511521(13) 0.627697(13) 0.007585(5) 0.01349(6) Uani 1 1 d . . . Rh1 Rh 0.398264(13) 0.733609(14) 0.035031(5) 0.01557(6) Uani 1 1 d . . . O1 O 0.52802(11) 0.89078(12) 0.19868(5) 0.0213(7) Uani 1 1 d . . . O2 O 0.49040(12) 0.77263(12) 0.22057(5) 0.0249(7) Uani 1 1 d . . . H2A H 0.5141 0.8094 0.2180 0.037 Uiso 1 1 calc R . . O3 O 0.34254(12) 0.78869(12) 0.20025(4) 0.0226(5) Uani 1 1 d U . . H3A H 0.3634 0.8267 0.1968 0.034 Uiso 1 1 calc R . . O4 O 0.41058(12) 0.90243(12) 0.17577(5) 0.0210(7) Uani 1 1 d . . . H4A H 0.4524 0.9036 0.1816 0.032 Uiso 1 1 calc R . . O5 O 0.38885(12) 0.45012(12) 0.13762(5) 0.0233(6) Uani 1 1 d U . . H5A H 0.3490 0.4458 0.1299 0.035 Uiso 1 1 calc R . . O6 O 0.45661(14) 0.32769(13) 0.10647(5) 0.0383(8) Uani 1 1 d . . . H6A H 0.4175 0.3251 0.0980 0.058 Uiso 1 1 calc R . . O7 O 0.32720(17) 0.30906(13) 0.08825(5) 0.0423(9) Uani 1 1 d . . . H7C H 0.3093 0.3380 0.0999 0.063 Uiso 1 1 calc R . . O8 O 0.27252(14) 0.41102(13) 0.11335(5) 0.0363(6) Uani 1 1 d U . . N1 N 0.27990(15) 0.73823(17) -0.01145(6) 0.0326(9) Uani 1 1 d . . . N2 N 0.50284(14) 0.72862(15) -0.04570(6) 0.0212(8) Uani 1 1 d . . . N3 N 0.46210(14) 0.86919(15) 0.00742(6) 0.0249(8) Uani 1 1 d . . . N4 N 0.62721(14) 0.72079(13) 0.03642(6) 0.0210(8) Uani 1 1 d . . . N5 N 0.48859(13) 0.75770(13) 0.09126(5) 0.0136(4) Uani 1 1 d U . . N6 N 0.50452(14) 0.53157(13) 0.06303(6) 0.0165(4) Uani 1 1 d U . . N7 N 0.33216(14) 0.59539(15) 0.05907(6) 0.0202(4) Uani 1 1 d U . . N8 N 0.38592(14) 0.55728(16) -0.02475(6) 0.0247(9) Uani 1 1 d . . . C1 C 0.57985(17) 0.93203(17) 0.15444(7) 0.0191(10) Uani 1 1 d . . . C2 C 0.63030(17) 0.92412(16) 0.13342(7) 0.0144(4) Uani 1 1 d U . . H2B H 0.6299 0.9549 0.1171 0.017 Uiso 1 1 calc R . . C3 C 0.68167(17) 0.87309(18) 0.13506(8) 0.0209(10) Uani 1 1 d . . . H3B H 0.7151 0.8675 0.1198 0.025 Uiso 1 1 calc R . . C4 C 0.68339(17) 0.82980(17) 0.15964(7) 0.0178(4) Uani 1 1 d U . . H4B H 0.7192 0.7953 0.1615 0.021 Uiso 1 1 calc R . . C5 C 0.63312(18) 0.83690(17) 0.18133(7) 0.0193(4) Uani 1 1 d U . . C6 C 0.57929(16) 0.88638(17) 0.17889(7) 0.0157(10) Uani 1 1 d . . . C7 C 0.63867(18) 0.78869(19) 0.20859(6) 0.0218(10) Uani 1 1 d . . . H7A H 0.6889 0.7794 0.2127 0.026 Uiso 1 1 calc R . . H7B H 0.6189 0.8139 0.2256 0.026 Uiso 1 1 calc R . . C8 C 0.60058(18) 0.71859(18) 0.20525(7) 0.0226(4) Uani 1 1 d U . . C9 C 0.63503(18) 0.65876(17) 0.19637(7) 0.0179(4) Uani 1 1 d U . . H9A H 0.6839 0.6604 0.1922 0.021 Uiso 1 1 calc R . . C10 C 0.5979(2) 0.5951(2) 0.19345(8) 0.0302(4) Uani 1 1 d U . . H10A H 0.6225 0.5539 0.1877 0.036 Uiso 1 1 calc R . . C11 C 0.52651(18) 0.59097(19) 0.19867(7) 0.0265(4) Uani 1 1 d U . . H11A H 0.5023 0.5474 0.1970 0.032 Uiso 1 1 calc R . . C12 C 0.49044(17) 0.65254(16) 0.20649(6) 0.0171(4) Uani 1 1 d U . . C13 C 0.52765(18) 0.71541(18) 0.21037(7) 0.0216(4) Uani 1 1 d U . . C14 C 0.40989(18) 0.65265(18) 0.20985(7) 0.0211(4) Uani 1 1 d U . . H14A H 0.3929 0.6049 0.2148 0.025 Uiso 1 1 calc R . . H14B H 0.3956 0.6852 0.2256 0.025 Uiso 1 1 calc R . . C15 C 0.37919(18) 0.67624(19) 0.18105(7) 0.0232(10) Uani 1 1 d . . . C16 C 0.38489(16) 0.63211(17) 0.15709(7) 0.0146(4) Uani 1 1 d U . . H16A H 0.4026 0.5858 0.1597 0.018 Uiso 1 1 calc R . . C17 C 0.36546(17) 0.65387(17) 0.12969(7) 0.0176(4) Uani 1 1 d U . . H17A H 0.3696 0.6227 0.1136 0.021 Uiso 1 1 calc R . . C18 C 0.33968(17) 0.72189(18) 0.12552(7) 0.0205(4) Uani 1 1 d U . . H18A H 0.3283 0.7379 0.1065 0.025 Uiso 1 1 calc R . . C19 C 0.33067(16) 0.76624(18) 0.14943(7) 0.0161(4) Uani 1 1 d U . . C20 C 0.35063(16) 0.74363(17) 0.17668(7) 0.0141(4) Uani 1 1 d U . . C21 C 0.30147(18) 0.83983(18) 0.14409(8) 0.0249(10) Uani 1 1 d . . . H21A H 0.2592 0.8361 0.1316 0.030 Uiso 1 1 calc R . . H21B H 0.2867 0.8602 0.1630 0.030 Uiso 1 1 calc R . . C22 C 0.35355(17) 0.88961(17) 0.12964(7) 0.0177(10) Uani 1 1 d . . . C23 C 0.35017(18) 0.90397(19) 0.10047(7) 0.0213(10) Uani 1 1 d . . . H23A H 0.3128 0.8852 0.0892 0.026 Uiso 1 1 calc R . . C24 C 0.4004(2) 0.94544(19) 0.08724(8) 0.0278(11) Uani 1 1 d . . . H24A H 0.3977 0.9554 0.0670 0.033 Uiso 1 1 calc R . . C25 C 0.45474(18) 0.97239(18) 0.10386(7) 0.0215(4) Uani 1 1 d U . . H25A H 0.4895 1.0006 0.0947 0.026 Uiso 1 1 calc R . . C26 C 0.46011(17) 0.95955(17) 0.13349(7) 0.0160(4) Uani 1 1 d U . . C27 C 0.40864(17) 0.91760(17) 0.14698(7) 0.0170(4) Uani 1 1 d U . . C28 C 0.52359(17) 0.98770(18) 0.15065(7) 0.0197(4) Uani 1 1 d U . . H28A H 0.5438 1.0286 0.1402 0.024 Uiso 1 1 calc R . . H28B H 0.5077 1.0040 0.1701 0.024 Uiso 1 1 calc R . . C29 C 0.32564(8) 0.46119(7) 0.18261(3) 0.0171(4) Uani 1 1 d GU . . C30 C 0.32523(10) 0.45436(11) 0.21279(3) 0.0283(4) Uani 1 1 d GU . . H30A H 0.2856 0.4695 0.2237 0.034 Uiso 1 1 calc R . . C31 C 0.38286(12) 0.42533(14) 0.22702(4) 0.0359(13) Uani 1 1 d G . . H31A H 0.3826 0.4207 0.2477 0.043 Uiso 1 1 calc R . . C32 C 0.44090(10) 0.40313(14) 0.21107(5) 0.0307(11) Uani 1 1 d G . . H32A H 0.4803 0.3833 0.2208 0.037 Uiso 1 1 calc R . . C33 C 0.44132(9) 0.40996(12) 0.18089(5) 0.0238(10) Uani 1 1 d G . . C34 C 0.38369(9) 0.43899(10) 0.16666(4) 0.0103(4) Uani 1 1 d GU . . C35 C 0.50035(19) 0.37627(18) 0.16317(8) 0.0329(11) Uani 1 1 d . . . H35A H 0.5447 0.3792 0.1744 0.040 Uiso 1 1 calc R . . H35B H 0.5068 0.4030 0.1448 0.040 Uiso 1 1 calc R . . C36 C 0.48516(8) 0.29821(8) 0.15568(4) 0.0335(12) Uani 1 1 d G . . C37 C 0.49272(11) 0.24820(9) 0.17756(4) 0.0381(13) Uani 1 1 d G . . H37A H 0.5103 0.2616 0.1961 0.046 Uiso 1 1 calc R . . C38 C 0.47452(14) 0.17858(9) 0.17226(6) 0.0432(14) Uani 1 1 d G . . H38A H 0.4797 0.1444 0.1872 0.052 Uiso 1 1 calc R . . C39 C 0.44877(14) 0.15898(9) 0.14508(6) 0.0301(4) Uani 1 1 d GU . . H39A H 0.4363 0.1114 0.1415 0.036 Uiso 1 1 calc R . . C40 C 0.44121(15) 0.20900(11) 0.12320(5) 0.0306(4) Uani 1 1 d GU . . C41 C 0.45941(12) 0.27861(10) 0.12850(4) 0.0239(10) Uani 1 1 d G . . C42 C 0.4128(2) 0.1862(2) 0.09439(9) 0.0445(4) Uani 1 1 d U . . H42A H 0.4320 0.1392 0.0896 0.053 Uiso 1 1 calc R . . H42B H 0.4293 0.2193 0.0792 0.053 Uiso 1 1 calc R . . C43 C 0.3303(2) 0.1828(2) 0.09352(8) 0.0302(4) Uani 1 1 d U . . C44 C 0.2952(2) 0.1210(2) 0.09582(8) 0.0416(13) Uani 1 1 d . . . H44A H 0.3213 0.0784 0.0964 0.050 Uiso 1 1 calc R . . C45 C 0.2233(2) 0.1177(2) 0.09736(8) 0.0368(12) Uani 1 1 d . . . H45A H 0.2003 0.0738 0.0997 0.044 Uiso 1 1 calc R . . C46 C 0.1846(2) 0.1790(2) 0.09548(9) 0.0450(4) Uani 1 1 d U . . H46A H 0.1347 0.1772 0.0961 0.054 Uiso 1 1 calc R . . C47 C 0.2191(3) 0.2445(2) 0.09271(10) 0.0619(15) Uani 1 1 d . . . C48 C 0.2941(2) 0.2461(2) 0.09080(9) 0.0353(4) Uani 1 1 d U . . C49 C 0.1767(3) 0.3123(3) 0.09186(12) 0.0753(5) Uani 1 1 d U . . H49A H 0.1995 0.3451 0.0780 0.090 Uiso 1 1 calc R . . H49B H 0.1292 0.3017 0.0842 0.090 Uiso 1 1 calc R . . C50 C 0.16892(10) 0.34867(10) 0.12074(4) 0.0692(17) Uani 1 1 d G . . C51 C 0.11197(11) 0.33186(13) 0.13841(5) 0.0691(5) Uani 1 1 d GU . . H51A H 0.0787 0.2978 0.1322 0.083 Uiso 1 1 calc R . . C52 C 0.10371(14) 0.36490(16) 0.16523(5) 0.0594(5) Uani 1 1 d GU . . H52A H 0.0648 0.3534 0.1773 0.071 Uiso 1 1 calc R . . C53 C 0.15239(18) 0.41473(16) 0.17439(5) 0.067(2) Uani 1 1 d G . . H53A H 0.1467 0.4373 0.1927 0.080 Uiso 1 1 calc R . . C54 C 0.20934(16) 0.43154(14) 0.15671(6) 0.0339(4) Uani 1 1 d GU . . C55 C 0.21760(12) 0.39851(12) 0.12989(5) 0.0316(4) Uani 1 1 d GU . . C56 C 0.26118(18) 0.48969(19) 0.16691(8) 0.0283(11) Uani 1 1 d . . . H56A H 0.2767 0.5170 0.1497 0.034 Uiso 1 1 calc R . . H56B H 0.2360 0.5223 0.1801 0.034 Uiso 1 1 calc R . . C57 C 0.32358(17) 0.73485(19) 0.00513(7) 0.0216(4) Uani 1 1 d U . . C58 C 0.50887(18) 0.69193(17) -0.02572(7) 0.0196(10) Uani 1 1 d . . . C59 C 0.2206(2) 0.7527(2) -0.03032(9) 0.0409(4) Uani 1 1 d U . . H59A H 0.1845 0.7790 -0.0193 0.049 Uiso 1 1 calc R . . H59B H 0.1995 0.7077 -0.0368 0.049 Uiso 1 1 calc R . . C60 C 0.24275(19) 0.7957(2) -0.05719(8) 0.0358(12) Uani 1 1 d . . . H60A H 0.2730 0.8350 -0.0506 0.043 Uiso 1 1 calc R . . H60B H 0.2001 0.8164 -0.0661 0.043 Uiso 1 1 calc R . . C61 C 0.2829(2) 0.7534(2) -0.08095(9) 0.0387(4) Uani 1 1 d U . . H61A H 0.2560 0.7100 -0.0852 0.046 Uiso 1 1 calc R . . H61B H 0.2841 0.7817 -0.0990 0.046 Uiso 1 1 calc R . . C62 C 0.35862(19) 0.7326(2) -0.07307(8) 0.0334(12) Uani 1 1 d . . . H62A H 0.3577 0.7053 -0.0547 0.040 Uiso 1 1 calc R . . H62B H 0.3771 0.7013 -0.0885 0.040 Uiso 1 1 calc R . . C63 C 0.40858(18) 0.79366(18) -0.06941(7) 0.0224(10) Uani 1 1 d . . . H63A H 0.3998 0.8276 -0.0854 0.027 Uiso 1 1 calc R . . H63B H 0.3974 0.8176 -0.0508 0.027 Uiso 1 1 calc R . . C64 C 0.48526(18) 0.77552(19) -0.06936(7) 0.0237(4) Uani 1 1 d U . . H64A H 0.4977 0.7530 -0.0881 0.028 Uiso 1 1 calc R . . H64B H 0.5133 0.8192 -0.0675 0.028 Uiso 1 1 calc R . . C65 C 0.43783(18) 0.81959(18) 0.01752(7) 0.0195(4) Uani 1 1 d U . . C66 C 0.58534(16) 0.68568(16) 0.02613(7) 0.0143(4) Uani 1 1 d U . . C67 C 0.49951(19) 0.93037(18) -0.00323(8) 0.0265(4) Uani 1 1 d U . . H67A H 0.4651 0.9662 -0.0096 0.032 Uiso 1 1 calc R . . H67B H 0.5280 0.9168 -0.0204 0.032 Uiso 1 1 calc R . . C68 C 0.5460(2) 0.9614(2) 0.01915(8) 0.0295(11) Uani 1 1 d . . . H68A H 0.5165 0.9855 0.0339 0.035 Uiso 1 1 calc R . . H68B H 0.5759 0.9975 0.0097 0.035 Uiso 1 1 calc R . . C69 C 0.5943(2) 0.90838(19) 0.03502(9) 0.0381(12) Uani 1 1 d . . . H69A H 0.6243 0.9337 0.0492 0.046 Uiso 1 1 calc R . . H69B H 0.5652 0.8741 0.0459 0.046 Uiso 1 1 calc R . . C70 C 0.63975(19) 0.8702(2) 0.01353(7) 0.0253(10) Uani 1 1 d . . . H70A H 0.6609 0.9051 0.0001 0.030 Uiso 1 1 calc R . . H70B H 0.6095 0.8388 0.0017 0.030 Uiso 1 1 calc R . . C71 C 0.6985(2) 0.8265(2) 0.02688(9) 0.0357(12) Uani 1 1 d . . . H71A H 0.7329 0.8587 0.0361 0.043 Uiso 1 1 calc R . . H71B H 0.7231 0.8010 0.0111 0.043 Uiso 1 1 calc R . . C72 C 0.67414(19) 0.7729(2) 0.04981(9) 0.0377(13) Uani 1 1 d . . . H72A H 0.7155 0.7489 0.0583 0.045 Uiso 1 1 calc R . . H72B H 0.6491 0.7976 0.0657 0.045 Uiso 1 1 calc R . . C73 C 0.45686(17) 0.74714(17) 0.07089(7) 0.0183(4) Uani 1 1 d U . . C74 C 0.50642(18) 0.56612(17) 0.04293(7) 0.0171(10) Uani 1 1 d . . . C75 C 0.52561(18) 0.76061(19) 0.11930(7) 0.0242(4) Uani 1 1 d U . . H75A H 0.4920 0.7527 0.1355 0.029 Uiso 1 1 calc R . . H75B H 0.5473 0.8075 0.1219 0.029 Uiso 1 1 calc R . . C76 C 0.58221(17) 0.70400(17) 0.11967(7) 0.0169(4) Uani 1 1 d U . . H76A H 0.6151 0.7123 0.1033 0.020 Uiso 1 1 calc R . . H76B H 0.6093 0.7078 0.1380 0.020 Uiso 1 1 calc R . . C77 C 0.55272(18) 0.63038(18) 0.11719(8) 0.0221(4) Uani 1 1 d U . . H77A H 0.5116 0.6311 0.1040 0.026 Uiso 1 1 calc R . . H77B H 0.5363 0.6148 0.1366 0.026 Uiso 1 1 calc R . . C78 C 0.60715(18) 0.57686(18) 0.10550(7) 0.0200(10) Uani 1 1 d . . . H78A H 0.6217 0.5912 0.0857 0.024 Uiso 1 1 calc R . . H78B H 0.6493 0.5780 0.1181 0.024 Uiso 1 1 calc R . . C79 C 0.57885(19) 0.50100(19) 0.10433(9) 0.0328(12) Uani 1 1 d . . . H79A H 0.6123 0.4716 0.0931 0.039 Uiso 1 1 calc R . . H79B H 0.5768 0.4821 0.1244 0.039 Uiso 1 1 calc R . . C80 C 0.50607(18) 0.49460(18) 0.09049(7) 0.0231(4) Uani 1 1 d U . . H80A H 0.4947 0.4444 0.0873 0.028 Uiso 1 1 calc R . . H80B H 0.4703 0.5146 0.1038 0.028 Uiso 1 1 calc R . . C81 C 0.35596(17) 0.64661(16) 0.05208(7) 0.0139(4) Uani 1 1 d U . . C82 C 0.43228(17) 0.57841(17) -0.01196(7) 0.0183(4) Uani 1 1 d U . . C83 C 0.3043(2) 0.52885(17) 0.06995(7) 0.0262(11) Uani 1 1 d . . . H83A H 0.2929 0.5337 0.0909 0.031 Uiso 1 1 calc R . . H83B H 0.3407 0.4919 0.0680 0.031 Uiso 1 1 calc R . . C84 C 0.23832(19) 0.50623(19) 0.05342(7) 0.0267(11) Uani 1 1 d . . . H84A H 0.2255 0.4580 0.0596 0.032 Uiso 1 1 calc R . . H84B H 0.1991 0.5378 0.0590 0.032 Uiso 1 1 calc R . . C85 C 0.24593(19) 0.5072(2) 0.02053(8) 0.0375(12) Uani 1 1 d . . . H85A H 0.2586 0.5555 0.0144 0.045 Uiso 1 1 calc R . . H85B H 0.1997 0.4961 0.0118 0.045 Uiso 1 1 calc R . . C86 C 0.3003(2) 0.4564(2) 0.00803(8) 0.0415(13) Uani 1 1 d . . . H86A H 0.3466 0.4686 0.0165 0.050 Uiso 1 1 calc R . . H86B H 0.2884 0.4085 0.0149 0.050 Uiso 1 1 calc R . . C87 C 0.3086(3) 0.4534(2) -0.02388(9) 0.0542(4) Uani 1 1 d U . . H87A H 0.2652 0.4337 -0.0325 0.065 Uiso 1 1 calc R . . H87B H 0.3478 0.4212 -0.0287 0.065 Uiso 1 1 calc R . . C88 C 0.3234(2) 0.5259(2) -0.03781(9) 0.0381(4) Uani 1 1 d U . . H88A H 0.3306 0.5202 -0.0591 0.046 Uiso 1 1 calc R . . H88B H 0.2825 0.5572 -0.0348 0.046 Uiso 1 1 calc R . . C2S C 0.34300(9) 1.02407(8) 0.01256(15) 0.035(2) Uiso 0.50 1 d PD . . H2SA H 0.3605 1.0076 -0.0066 0.043 Uiso 0.50 1 calc PR . . H2SB H 0.3725 1.0000 0.0273 0.043 Uiso 0.50 1 calc PR . . O1S O 0.27645(9) 0.99193(19) 0.01538(15) 0.088(2) Uiso 0.50 1 d PD . . H1SD H 0.2793 0.9496 0.0103 0.132 Uiso 0.50 1 calc PR . . C1S C 0.3660(3) 1.10007(9) 0.0141(2) 0.076(3) Uiso 0.50 1 d PD . . H1SA H 0.4159 1.1023 0.0192 0.114 Uiso 0.50 1 calc PR . . H1SB H 0.3383 1.1247 0.0289 0.114 Uiso 0.50 1 calc PR . . H1SC H 0.3586 1.1225 -0.0049 0.114 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh2 0.01648(11) 0.01685(12) 0.00713(10) 0.00136(11) -0.00075(11) 0.00100(11) Rh1 0.01578(12) 0.02325(13) 0.00769(10) 0.00546(12) -0.00122(11) -0.00086(12) O1 0.0216(12) 0.0213(12) 0.0211(12) 0.0014(10) 0.0034(10) -0.0032(11) O2 0.0224(12) 0.0239(12) 0.0285(13) -0.0072(11) 0.0071(11) -0.0010(11) O3 0.0258(10) 0.0269(10) 0.0152(9) -0.0035(8) 0.0041(8) 0.0002(8) O4 0.0153(11) 0.0213(12) 0.0265(12) -0.0020(11) 0.0007(10) 0.0063(11) O5 0.0262(10) 0.0246(10) 0.0189(9) -0.0011(8) 0.0038(8) -0.0041(8) O6 0.0546(16) 0.0269(14) 0.0335(13) -0.0035(12) 0.0304(12) -0.0116(12) O7 0.097(2) 0.0244(14) 0.0053(12) 0.0021(11) -0.0017(14) -0.0155(15) O8 0.0445(11) 0.0323(10) 0.0320(10) 0.0076(9) -0.0132(9) -0.0026(9) N1 0.0133(15) 0.0508(19) 0.0336(17) 0.0268(15) -0.0087(14) -0.0095(15) N2 0.0187(15) 0.0281(16) 0.0168(13) 0.0022(13) -0.0020(12) -0.0042(14) N3 0.0192(14) 0.0277(15) 0.0276(15) 0.0111(15) -0.0040(14) 0.0045(13) N4 0.0218(14) 0.0099(13) 0.0314(15) 0.0026(13) 0.0024(14) 0.0057(12) N5 0.0141(7) 0.0145(7) 0.0123(7) -0.0005(5) 0.0001(6) -0.0004(6) N6 0.0169(7) 0.0172(7) 0.0154(7) -0.0007(6) 0.0023(6) 0.0000(6) N7 0.0207(7) 0.0205(7) 0.0192(7) -0.0007(6) 0.0006(6) 0.0002(6) N8 0.0152(15) 0.0436(18) 0.0154(14) -0.0084(13) -0.0014(12) -0.0069(14) C1 0.0185(18) 0.0140(17) 0.0247(18) -0.0058(15) -0.0031(15) -0.0009(15) C2 0.0143(7) 0.0155(7) 0.0135(7) 0.0010(6) 0.0006(6) -0.0011(6) C3 0.0127(16) 0.0201(18) 0.0299(19) -0.0043(17) 0.0005(15) -0.0109(15) C4 0.0171(7) 0.0183(7) 0.0181(7) 0.0005(6) -0.0008(6) -0.0006(6) C5 0.0196(7) 0.0194(7) 0.0190(7) -0.0006(6) -0.0007(6) -0.0002(6) C6 0.0099(16) 0.0237(19) 0.0136(16) -0.0038(15) -0.0005(13) -0.0027(14) C7 0.0141(17) 0.043(2) 0.0088(16) 0.0039(15) -0.0046(14) 0.0069(16) C8 0.0233(7) 0.0228(7) 0.0216(7) 0.0011(6) -0.0005(6) 0.0005(6) C9 0.0185(7) 0.0194(7) 0.0157(7) 0.0007(6) -0.0010(6) 0.0010(6) C10 0.0312(7) 0.0301(7) 0.0293(7) 0.0010(6) 0.0001(6) 0.0012(6) C11 0.0272(7) 0.0267(7) 0.0256(7) 0.0005(6) -0.0017(6) -0.0009(6) C12 0.0185(7) 0.0183(7) 0.0144(7) 0.0017(6) 0.0004(6) 0.0006(6) C13 0.0214(7) 0.0231(7) 0.0202(7) 0.0014(6) 0.0005(6) 0.0004(6) C14 0.0215(7) 0.0218(7) 0.0201(7) 0.0004(6) 0.0004(6) -0.0005(6) C15 0.0194(18) 0.034(2) 0.0160(17) 0.0033(16) 0.0039(15) -0.0096(17) C16 0.0146(7) 0.0141(7) 0.0152(7) 0.0005(6) -0.0003(6) -0.0009(6) C17 0.0173(7) 0.0178(7) 0.0176(7) -0.0015(6) -0.0011(6) -0.0010(6) C18 0.0204(7) 0.0215(7) 0.0195(7) 0.0007(6) -0.0007(6) -0.0012(6) C19 0.0156(7) 0.0169(7) 0.0156(7) -0.0002(6) 0.0003(6) -0.0008(6) C20 0.0145(7) 0.0152(7) 0.0128(7) 0.0001(6) 0.0015(6) -0.0013(6) C21 0.0121(17) 0.031(2) 0.0312(19) -0.0092(17) -0.0080(16) 0.0078(16) C22 0.0189(17) 0.0147(17) 0.0195(17) 0.0107(15) 0.0029(15) 0.0057(15) C23 0.0212(18) 0.0252(18) 0.0174(17) -0.0024(16) -0.0069(15) -0.0012(16) C24 0.035(2) 0.030(2) 0.0181(18) -0.0021(16) 0.0004(18) 0.0140(18) C25 0.0224(7) 0.0212(7) 0.0211(7) 0.0013(6) 0.0014(6) 0.0005(6) C26 0.0156(7) 0.0157(7) 0.0167(7) 0.0000(6) -0.0002(6) 0.0028(6) C27 0.0168(7) 0.0171(7) 0.0171(7) 0.0011(6) -0.0004(6) 0.0010(6) C28 0.0200(7) 0.0194(7) 0.0196(7) 0.0011(6) 0.0019(6) 0.0000(6) C29 0.0175(7) 0.0165(7) 0.0173(7) 0.0002(6) 0.0013(6) -0.0004(6) C30 0.0295(7) 0.0277(7) 0.0277(7) 0.0017(6) 0.0024(6) 0.0002(6) C31 0.062(3) 0.035(2) 0.0107(17) -0.0064(17) 0.0084(19) -0.012(2) C32 0.038(2) 0.0179(18) 0.037(2) 0.0126(18) -0.0053(18) -0.0111(17) C33 0.0226(18) 0.0128(17) 0.036(2) -0.0121(16) 0.0080(16) -0.0128(15) C34 0.0119(7) 0.0095(7) 0.0094(7) -0.0010(6) 0.0024(6) 0.0003(6) C35 0.028(2) 0.0152(17) 0.056(2) -0.0039(18) 0.0012(18) -0.0031(16) C36 0.0052(16) 0.0091(17) 0.086(3) -0.0014(19) 0.003(2) -0.0052(15) C37 0.026(2) 0.021(2) 0.067(3) 0.002(2) -0.008(2) 0.0015(17) C38 0.020(2) 0.022(2) 0.088(3) 0.016(2) 0.010(2) 0.0121(17) C39 0.0297(7) 0.0289(7) 0.0318(7) -0.0007(6) 0.0018(6) -0.0007(6) C40 0.0306(7) 0.0308(7) 0.0304(7) -0.0013(6) 0.0026(6) -0.0004(6) C41 0.0199(18) 0.0148(17) 0.037(2) -0.0168(16) 0.0136(16) -0.0025(15) C42 0.0453(7) 0.0437(7) 0.0445(7) -0.0003(6) 0.0037(6) -0.0018(6) C43 0.0324(7) 0.0302(7) 0.0281(7) -0.0010(6) 0.0001(6) -0.0003(6) C44 0.064(3) 0.023(2) 0.038(2) -0.0008(19) -0.005(2) -0.015(2) C45 0.044(2) 0.026(2) 0.040(2) 0.0003(18) -0.011(2) -0.0141(18) C46 0.0449(7) 0.0447(7) 0.0453(7) -0.0007(6) -0.0030(6) -0.0009(6) C47 0.095(3) 0.020(2) 0.071(3) 0.014(2) -0.066(2) -0.008(2) C48 0.0366(7) 0.0354(7) 0.0339(7) -0.0013(6) -0.0021(6) -0.0010(6) C49 0.0751(8) 0.0748(8) 0.0760(8) 0.0000(6) -0.0030(6) -0.0004(6) C50 0.052(3) 0.027(2) 0.129(4) 0.009(3) -0.059(3) 0.006(2) C51 0.0679(7) 0.0679(8) 0.0713(8) 0.0009(6) -0.0018(6) 0.0002(6) C52 0.0579(7) 0.0588(7) 0.0615(8) 0.0028(6) 0.0001(6) 0.0002(6) C53 0.010(2) 0.026(2) 0.163(5) 0.008(3) 0.007(3) -0.0033(19) C54 0.0329(7) 0.0328(7) 0.0358(7) 0.0020(6) -0.0013(6) 0.0013(6) C55 0.0312(7) 0.0309(7) 0.0327(7) 0.0001(6) -0.0036(6) 0.0006(6) C56 0.0205(18) 0.0177(18) 0.047(2) -0.0089(18) 0.0005(18) -0.0030(17) C57 0.0212(7) 0.0224(7) 0.0212(7) -0.0001(6) 0.0019(6) -0.0004(6) C58 0.0153(17) 0.0150(17) 0.0286(19) 0.0065(15) 0.0064(16) -0.0006(15) C59 0.0401(7) 0.0420(7) 0.0406(7) 0.0016(6) -0.0010(6) 0.0006(6) C60 0.0167(19) 0.064(3) 0.026(2) 0.019(2) -0.0125(17) -0.0162(18) C61 0.0385(7) 0.0398(7) 0.0379(7) 0.0015(6) -0.0014(6) -0.0004(6) C62 0.028(2) 0.056(2) 0.0160(17) 0.0151(18) -0.0034(16) -0.011(2) C63 0.0255(19) 0.0237(19) 0.0179(17) 0.0060(15) -0.0013(16) -0.0050(16) C64 0.0240(7) 0.0240(7) 0.0231(7) 0.0018(6) -0.0005(6) -0.0004(6) C65 0.0193(7) 0.0207(7) 0.0184(7) 0.0010(6) -0.0017(6) -0.0014(6) C66 0.0142(7) 0.0143(7) 0.0144(7) 0.0002(6) -0.0007(6) 0.0002(6) C67 0.0271(7) 0.0267(7) 0.0255(7) 0.0013(6) -0.0007(6) -0.0006(6) C68 0.032(2) 0.039(2) 0.0171(18) 0.0039(17) 0.0127(17) -0.0046(19) C69 0.038(2) 0.0181(18) 0.059(2) -0.013(2) 0.001(2) -0.0113(18) C70 0.0286(19) 0.033(2) 0.0140(17) 0.0105(16) 0.0132(15) -0.0063(18) C71 0.033(2) 0.026(2) 0.048(2) -0.0037(19) 0.0081(19) -0.0127(17) C72 0.021(2) 0.030(2) 0.062(3) 0.011(2) -0.0084(19) 0.0028(18) C73 0.0176(7) 0.0179(7) 0.0194(7) 0.0002(6) 0.0002(6) -0.0004(6) C74 0.0245(19) 0.0145(16) 0.0123(16) 0.0054(14) 0.0003(15) -0.0014(15) C75 0.0248(7) 0.0248(7) 0.0229(7) -0.0008(6) -0.0004(6) -0.0011(6) C76 0.0168(7) 0.0192(7) 0.0147(7) -0.0015(6) -0.0003(6) -0.0001(6) C77 0.0220(7) 0.0227(7) 0.0214(7) 0.0007(6) 0.0004(6) 0.0002(6) C78 0.0180(18) 0.035(2) 0.0073(15) 0.0019(15) -0.0018(15) 0.0052(16) C79 0.027(2) 0.028(2) 0.043(2) 0.0196(18) -0.0060(18) 0.0019(17) C80 0.0235(7) 0.0229(7) 0.0228(7) -0.0001(6) 0.0000(6) 0.0006(6) C81 0.0146(7) 0.0144(7) 0.0128(7) -0.0006(6) -0.0025(6) -0.0002(6) C82 0.0183(7) 0.0191(7) 0.0175(7) 0.0001(6) 0.0009(6) -0.0001(6) C83 0.051(2) 0.0171(19) 0.0104(16) -0.0068(15) 0.0010(17) -0.0104(18) C84 0.0302(19) 0.0190(18) 0.0308(19) -0.0061(16) -0.0017(17) -0.0140(17) C85 0.0193(19) 0.053(2) 0.041(2) -0.022(2) -0.0175(17) 0.0100(19) C86 0.038(2) 0.057(3) 0.030(2) -0.019(2) 0.001(2) -0.001(2) C87 0.0544(7) 0.0544(7) 0.0538(7) -0.0023(6) 0.0000(6) -0.0007(6) C88 0.0379(7) 0.0399(7) 0.0364(7) -0.0010(6) -0.0008(6) -0.0015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh2 C58 1.956(3) . ? Rh2 C66 1.978(3) . ? Rh2 C82 1.988(3) . ? Rh2 C74 2.002(3) . ? Rh1 C65 1.971(4) . ? Rh1 C57 1.974(3) . ? Rh1 C81 1.999(3) . ? Rh1 C73 2.003(3) . ? O1 C6 1.335(4) . ? O2 C13 1.380(4) . ? O3 C20 1.388(4) . ? O4 C27 1.352(4) . ? O5 C34 1.352(3) . ? O6 C41 1.377(3) . ? O7 C48 1.358(5) . ? O8 C55 1.313(3) . ? N1 C57 1.128(4) . ? N1 C59 1.447(5) . ? N2 C58 1.158(4) . ? N2 C64 1.444(4) . ? N3 C65 1.148(4) . ? N3 C67 1.449(5) . ? N4 C66 1.141(4) . ? N4 C72 1.469(5) . ? N5 C73 1.130(4) . ? N5 C75 1.467(4) . ? N6 C74 1.132(4) . ? N6 C80 1.442(4) . ? N7 C81 1.121(4) . ? N7 C83 1.460(4) . ? N8 C82 1.133(4) . ? N8 C88 1.459(5) . ? C1 C2 1.368(5) . ? C1 C6 1.418(5) . ? C1 C28 1.515(5) . ? C2 C3 1.379(5) . ? C3 C4 1.396(5) . ? C4 C5 1.386(5) . ? C5 C6 1.395(5) . ? C5 C7 1.554(5) . ? C7 C8 1.525(5) . ? C8 C9 1.375(5) . ? C8 C13 1.408(5) . ? C9 C10 1.409(5) . ? C10 C11 1.380(5) . ? C11 C12 1.404(5) . ? C12 C13 1.401(5) . ? C12 C14 1.540(5) . ? C14 C15 1.512(5) . ? C15 C16 1.387(5) . ? C15 C20 1.407(5) . ? C16 C17 1.373(5) . ? C17 C18 1.397(5) . ? C18 C19 1.394(5) . ? C19 C20 1.375(4) . ? C19 C21 1.526(5) . ? C21 C22 1.522(5) . ? C22 C23 1.367(5) . ? C22 C27 1.419(5) . ? C23 C24 1.379(5) . ? C24 C25 1.383(5) . ? C25 C26 1.384(5) . ? C26 C27 1.406(5) . ? C26 C28 1.537(5) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C29 C56 1.522(4) . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 C35 1.527(4) . ? C35 C36 1.551(4) . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C40 C42 1.492(5) . ? C42 C43 1.572(6) . ? C43 C44 1.357(6) . ? C43 C48 1.394(6) . ? C44 C45 1.371(6) . ? C45 C46 1.382(6) . ? C46 C47 1.413(6) . ? C47 C48 1.429(6) . ? C47 C49 1.523(7) . ? C49 C50 1.501(6) . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C54 C56 1.554(4) . ? C59 C60 1.538(6) . ? C60 C61 1.556(6) . ? C61 C62 1.536(5) . ? C62 C63 1.511(5) . ? C63 C64 1.499(5) . ? C67 C68 1.478(5) . ? C68 C69 1.546(6) . ? C69 C70 1.499(5) . ? C70 C71 1.521(5) . ? C71 C72 1.536(6) . ? C75 C76 1.523(5) . ? C76 C77 1.513(5) . ? C77 C78 1.548(5) . ? C78 C79 1.541(5) . ? C79 C80 1.528(5) . ? C83 C84 1.527(5) . ? C84 C85 1.515(5) . ? C85 C86 1.527(6) . ? C86 C87 1.472(6) . ? C87 C88 1.544(6) . ? C2S O1S 1.412(3) . ? C2S C1S 1.512(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C58 Rh2 C66 90.32(14) . . ? C58 Rh2 C82 85.59(14) . . ? C66 Rh2 C82 174.22(13) . . ? C58 Rh2 C74 174.90(14) . . ? C66 Rh2 C74 90.72(13) . . ? C82 Rh2 C74 93.00(14) . . ? C65 Rh1 C57 88.96(14) . . ? C65 Rh1 C81 178.49(14) . . ? C57 Rh1 C81 89.54(14) . . ? C65 Rh1 C73 90.88(14) . . ? C57 Rh1 C73 165.66(14) . . ? C81 Rh1 C73 90.53(13) . . ? C57 N1 C59 170.9(4) . . ? C58 N2 C64 172.0(3) . . ? C65 N3 C67 173.6(3) . . ? C66 N4 C72 172.7(3) . . ? C73 N5 C75 170.9(3) . . ? C74 N6 C80 173.0(3) . . ? C81 N7 C83 176.1(3) . . ? C82 N8 C88 172.8(3) . . ? C2 C1 C6 119.7(3) . . ? C2 C1 C28 119.4(3) . . ? C6 C1 C28 120.9(3) . . ? C1 C2 C3 122.4(3) . . ? C2 C3 C4 118.4(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 121.0(3) . . ? C4 C5 C7 118.2(3) . . ? C6 C5 C7 120.8(3) . . ? O1 C6 C5 121.6(3) . . ? O1 C6 C1 120.3(3) . . ? C5 C6 C1 118.1(3) . . ? C8 C7 C5 113.8(3) . . ? C9 C8 C13 118.9(3) . . ? C9 C8 C7 121.8(3) . . ? C13 C8 C7 119.3(3) . . ? C8 C9 C10 120.0(3) . . ? C11 C10 C9 121.7(3) . . ? C10 C11 C12 118.5(3) . . ? C13 C12 C11 119.8(3) . . ? C13 C12 C14 119.3(3) . . ? C11 C12 C14 120.9(3) . . ? O2 C13 C12 117.2(3) . . ? O2 C13 C8 121.9(3) . . ? C12 C13 C8 120.9(3) . . ? C15 C14 C12 107.3(3) . . ? C16 C15 C20 118.0(3) . . ? C16 C15 C14 118.8(3) . . ? C20 C15 C14 123.0(3) . . ? C17 C16 C15 121.4(3) . . ? C16 C17 C18 119.9(3) . . ? C19 C18 C17 119.8(3) . . ? C20 C19 C18 119.4(3) . . ? C20 C19 C21 122.2(3) . . ? C18 C19 C21 118.3(3) . . ? C19 C20 O3 118.9(3) . . ? C19 C20 C15 121.4(3) . . ? O3 C20 C15 119.6(3) . . ? C22 C21 C19 113.8(3) . . ? C23 C22 C27 120.5(3) . . ? C23 C22 C21 121.3(3) . . ? C27 C22 C21 118.0(3) . . ? C22 C23 C24 120.8(3) . . ? C23 C24 C25 119.2(3) . . ? C24 C25 C26 122.0(3) . . ? C25 C26 C27 118.7(3) . . ? C25 C26 C28 119.9(3) . . ? C27 C26 C28 121.3(3) . . ? O4 C27 C26 122.1(3) . . ? O4 C27 C22 119.2(3) . . ? C26 C27 C22 118.7(3) . . ? C1 C28 C26 111.7(3) . . ? C30 C29 C34 120.0 . . ? C30 C29 C56 119.98(16) . . ? C34 C29 C56 119.95(17) . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 C35 119.65(19) . . ? C34 C33 C35 119.79(19) . . ? O5 C34 C33 117.86(14) . . ? O5 C34 C29 121.89(14) . . ? C33 C34 C29 120.0 . . ? C33 C35 C36 112.5(2) . . ? C37 C36 C41 120.0 . . ? C37 C36 C35 118.43(16) . . ? C41 C36 C35 121.39(16) . . ? C36 C37 C38 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 C42 121.4(2) . . ? C39 C40 C42 118.6(2) . . ? O6 C41 C40 120.54(15) . . ? O6 C41 C36 119.32(15) . . ? C40 C41 C36 120.0 . . ? C40 C42 C43 113.3(3) . . ? C44 C43 C48 120.8(4) . . ? C44 C43 C42 121.7(4) . . ? C48 C43 C42 117.4(3) . . ? C43 C44 C45 122.3(4) . . ? C44 C45 C46 119.4(4) . . ? C45 C46 C47 120.1(4) . . ? C46 C47 C48 119.3(4) . . ? C46 C47 C49 120.2(4) . . ? C48 C47 C49 120.5(4) . . ? O7 C48 C43 122.7(4) . . ? O7 C48 C47 119.2(4) . . ? C43 C48 C47 118.0(4) . . ? C50 C49 C47 114.8(4) . . ? C51 C50 C55 120.0 . . ? C51 C50 C49 119.0(2) . . ? C55 C50 C49 121.0(2) . . ? C50 C51 C52 120.0 . . ? C51 C52 C53 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 C56 121.1(2) . . ? C53 C54 C56 118.9(2) . . ? O8 C55 C54 121.28(17) . . ? O8 C55 C50 118.65(17) . . ? C54 C55 C50 120.0 . . ? C29 C56 C54 113.6(3) . . ? N1 C57 Rh1 177.0(3) . . ? N2 C58 Rh2 175.6(3) . . ? N1 C59 C60 111.5(3) . . ? C59 C60 C61 114.8(3) . . ? C62 C61 C60 115.4(3) . . ? C63 C62 C61 114.7(3) . . ? C64 C63 C62 115.8(3) . . ? N2 C64 C63 111.6(3) . . ? N3 C65 Rh1 178.7(3) . . ? N4 C66 Rh2 178.0(3) . . ? N3 C67 C68 112.4(3) . . ? C67 C68 C69 115.0(3) . . ? C70 C69 C68 110.4(3) . . ? C69 C70 C71 115.1(3) . . ? C70 C71 C72 114.6(3) . . ? N4 C72 C71 110.2(3) . . ? N5 C73 Rh1 176.9(3) . . ? N6 C74 Rh2 179.0(3) . . ? N5 C75 C76 108.8(3) . . ? C77 C76 C75 113.1(3) . . ? C76 C77 C78 112.8(3) . . ? C79 C78 C77 113.2(3) . . ? C80 C79 C78 113.9(3) . . ? N6 C80 C79 110.0(3) . . ? N7 C81 Rh1 173.5(3) . . ? N8 C82 Rh2 172.2(3) . . ? N7 C83 C84 111.9(3) . . ? C85 C84 C83 114.3(3) . . ? C84 C85 C86 115.5(3) . . ? C87 C86 C85 118.0(4) . . ? C86 C87 C88 113.4(4) . . ? N8 C88 C87 110.1(3) . . ? O1S C2S C1S 132.0(3) . . ? 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 C6 C1 C2 C3 -0.3(5) . . . . ? C28 C1 C2 C3 -177.9(3) . . . . ? C1 C2 C3 C4 -2.3(5) . . . . ? C2 C3 C4 C5 2.0(5) . . . . ? C3 C4 C5 C6 1.1(5) . . . . ? C3 C4 C5 C7 -178.4(3) . . . . ? C4 C5 C6 O1 175.7(3) . . . . ? C7 C5 C6 O1 -4.9(5) . . . . ? C4 C5 C6 C1 -3.7(5) . . . . ? C7 C5 C6 C1 175.8(3) . . . . ? C2 C1 C6 O1 -176.0(3) . . . . ? C28 C1 C6 O1 1.5(5) . . . . ? C2 C1 C6 C5 3.3(5) . . . . ? C28 C1 C6 C5 -179.1(3) . . . . ? C4 C5 C7 C8 -88.6(4) . . . . ? C6 C5 C7 C8 91.9(4) . . . . ? C5 C7 C8 C9 95.2(4) . . . . ? C5 C7 C8 C13 -82.5(4) . . . . ? C13 C8 C9 C10 -2.1(5) . . . . ? C7 C8 C9 C10 -179.8(3) . . . . ? C8 C9 C10 C11 1.5(5) . . . . ? C9 C10 C11 C12 1.3(5) . . . . ? C10 C11 C12 C13 -3.5(5) . . . . ? C10 C11 C12 C14 174.4(3) . . . . ? C11 C12 C13 O2 -174.4(3) . . . . ? C14 C12 C13 O2 7.8(4) . . . . ? C11 C12 C13 C8 2.9(5) . . . . ? C14 C12 C13 C8 -175.0(3) . . . . ? C9 C8 C13 O2 177.0(3) . . . . ? C7 C8 C13 O2 -5.2(5) . . . . ? C9 C8 C13 C12 -0.1(5) . . . . ? C7 C8 C13 C12 177.7(3) . . . . ? C13 C12 C14 C15 83.6(4) . . . . ? C11 C12 C14 C15 -94.2(4) . . . . ? C12 C14 C15 C16 68.9(4) . . . . ? C12 C14 C15 C20 -105.2(4) . . . . ? C20 C15 C16 C17 2.0(5) . . . . ? C14 C15 C16 C17 -172.3(3) . . . . ? C15 C16 C17 C18 0.4(5) . . . . ? C16 C17 C18 C19 -3.0(5) . . . . ? C17 C18 C19 C20 3.2(5) . . . . ? C17 C18 C19 C21 -179.2(3) . . . . ? C18 C19 C20 O3 178.9(3) . . . . ? C21 C19 C20 O3 1.4(5) . . . . ? C18 C19 C20 C15 -0.8(5) . . . . ? C21 C19 C20 C15 -178.3(3) . . . . ? C16 C15 C20 C19 -1.8(5) . . . . ? C14 C15 C20 C19 172.3(3) . . . . ? C16 C15 C20 O3 178.5(3) . . . . ? C14 C15 C20 O3 -7.4(5) . . . . ? C20 C19 C21 C22 104.6(4) . . . . ? C18 C19 C21 C22 -72.9(4) . . . . ? C19 C21 C22 C23 100.9(4) . . . . ? C19 C21 C22 C27 -75.4(4) . . . . ? C27 C22 C23 C24 0.5(5) . . . . ? C21 C22 C23 C24 -175.7(3) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C24 C25 C26 C27 0.2(5) . . . . ? C24 C25 C26 C28 176.9(3) . . . . ? C25 C26 C27 O4 179.6(3) . . . . ? C28 C26 C27 O4 2.9(5) . . . . ? C25 C26 C27 C22 0.5(5) . . . . ? C28 C26 C27 C22 -176.2(3) . . . . ? C23 C22 C27 O4 -180.0(3) . . . . ? C21 C22 C27 O4 -3.7(4) . . . . ? C23 C22 C27 C26 -0.8(5) . . . . ? C21 C22 C27 C26 175.4(3) . . . . ? C2 C1 C28 C26 87.9(4) . . . . ? C6 C1 C28 C26 -89.7(4) . . . . ? C25 C26 C28 C1 -97.4(4) . . . . ? C27 C26 C28 C1 79.3(4) . . . . ? C34 C29 C30 C31 0.0 . . . . ? C56 C29 C30 C31 177.05(18) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C35 -171.4(2) . . . . ? C32 C33 C34 O5 174.45(17) . . . . ? C35 C33 C34 O5 -14.2(2) . . . . ? C32 C33 C34 C29 0.0 . . . . ? C35 C33 C34 C29 171.4(2) . . . . ? C30 C29 C34 O5 -174.22(18) . . . . ? C56 C29 C34 O5 8.7(2) . . . . ? C30 C29 C34 C33 0.0 . . . . ? C56 C29 C34 C33 -177.05(18) . . . . ? C32 C33 C35 C36 85.8(3) . . . . ? C34 C33 C35 C36 -85.7(3) . . . . ? C33 C35 C36 C37 -75.5(3) . . . . ? C33 C35 C36 C41 99.6(3) . . . . ? C41 C36 C37 C38 0.0 . . . . ? C35 C36 C37 C38 175.19(18) . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C38 C39 C40 C42 -179.5(3) . . . . ? C39 C40 C41 O6 175.7(2) . . . . ? C42 C40 C41 O6 -4.9(3) . . . . ? C39 C40 C41 C36 0.0 . . . . ? C42 C40 C41 C36 179.5(3) . . . . ? C37 C36 C41 O6 -175.7(2) . . . . ? C35 C36 C41 O6 9.3(3) . . . . ? C37 C36 C41 C40 0.0 . . . . ? C35 C36 C41 C40 -175.04(18) . . . . ? C41 C40 C42 C43 -96.3(3) . . . . ? C39 C40 C42 C43 83.2(3) . . . . ? C40 C42 C43 C44 -101.3(4) . . . . ? C40 C42 C43 C48 77.6(4) . . . . ? C48 C43 C44 C45 -4.0(6) . . . . ? C42 C43 C44 C45 174.8(4) . . . . ? C43 C44 C45 C46 2.4(6) . . . . ? C44 C45 C46 C47 -1.5(6) . . . . ? C45 C46 C47 C48 2.3(6) . . . . ? C45 C46 C47 C49 -177.5(4) . . . . ? C44 C43 C48 O7 -179.6(3) . . . . ? C42 C43 C48 O7 1.6(5) . . . . ? C44 C43 C48 C47 4.6(6) . . . . ? C42 C43 C48 C47 -174.3(4) . . . . ? C46 C47 C48 O7 -179.7(4) . . . . ? C49 C47 C48 O7 0.0(6) . . . . ? C46 C47 C48 C43 -3.7(6) . . . . ? C49 C47 C48 C43 176.1(4) . . . . ? C46 C47 C49 C50 95.0(5) . . . . ? C48 C47 C49 C50 -84.7(5) . . . . ? C47 C49 C50 C51 -89.9(4) . . . . ? C47 C49 C50 C55 90.1(4) . . . . ? C55 C50 C51 C52 0.0 . . . . ? C49 C50 C51 C52 -180.0(3) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C52 C53 C54 C56 177.5(3) . . . . ? C53 C54 C55 O8 -176.9(2) . . . . ? C56 C54 C55 O8 5.7(2) . . . . ? C53 C54 C55 C50 0.0 . . . . ? C56 C54 C55 C50 -177.4(3) . . . . ? C51 C50 C55 O8 177.0(2) . . . . ? C49 C50 C55 O8 -3.1(3) . . . . ? C51 C50 C55 C54 0.0 . . . . ? C49 C50 C55 C54 179.9(3) . . . . ? C30 C29 C56 C54 -92.1(3) . . . . ? C34 C29 C56 C54 84.9(3) . . . . ? C55 C54 C56 C29 -87.1(3) . . . . ? C53 C54 C56 C29 95.5(3) . . . . ? C59 N1 C57 Rh1 -2(8) . . . . ? C65 Rh1 C57 N1 -64(6) . . . . ? C81 Rh1 C57 N1 115(6) . . . . ? C73 Rh1 C57 N1 25(7) . . . . ? C64 N2 C58 Rh2 33(6) . . . . ? C66 Rh2 C58 N2 -153(4) . . . . ? C82 Rh2 C58 N2 23(4) . . . . ? C74 Rh2 C58 N2 -51(5) . . . . ? C57 N1 C59 C60 93(2) . . . . ? N1 C59 C60 C61 75.2(4) . . . . ? C59 C60 C61 C62 -72.3(4) . . . . ? C60 C61 C62 C63 -65.0(4) . . . . ? C61 C62 C63 C64 -164.9(3) . . . . ? C58 N2 C64 C63 -5(3) . . . . ? C62 C63 C64 N2 -60.9(4) . . . . ? C67 N3 C65 Rh1 -27(16) . . . . ? C57 Rh1 C65 N3 -142(14) . . . . ? C81 Rh1 C65 N3 -149(12) . . . . ? C73 Rh1 C65 N3 52(14) . . . . ? C72 N4 C66 Rh2 37(11) . . . . ? C58 Rh2 C66 N4 27(9) . . . . ? C82 Rh2 C66 N4 -18(10) . . . . ? C74 Rh2 C66 N4 -148(9) . . . . ? C65 N3 C67 C68 -31(3) . . . . ? N3 C67 C68 C69 48.8(4) . . . . ? C67 C68 C69 C70 57.8(4) . . . . ? C68 C69 C70 C71 169.3(3) . . . . ? C69 C70 C71 C72 54.5(4) . . . . ? C66 N4 C72 C71 -77(3) . . . . ? C70 C71 C72 N4 62.8(4) . . . . ? C75 N5 C73 Rh1 129(5) . . . . ? C65 Rh1 C73 N5 57(6) . . . . ? C57 Rh1 C73 N5 -33(6) . . . . ? C81 Rh1 C73 N5 -123(6) . . . . ? C80 N6 C74 Rh2 43(20) . . . . ? C58 Rh2 C74 N6 -125(18) . . . . ? C66 Rh2 C74 N6 -23(18) . . . . ? C82 Rh2 C74 N6 161(93) . . . . ? C73 N5 C75 C76 67(2) . . . . ? N5 C75 C76 C77 -62.3(3) . . . . ? C75 C76 C77 C78 157.3(3) . . . . ? C76 C77 C78 C79 177.1(3) . . . . ? C77 C78 C79 C80 47.3(4) . . . . ? C74 N6 C80 C79 -48(3) . . . . ? C78 C79 C80 N6 49.5(4) . . . . ? C83 N7 C81 Rh1 140(4) . . . . ? C65 Rh1 C81 N7 56(7) . . . . ? C57 Rh1 C81 N7 49(3) . . . . ? C73 Rh1 C81 N7 -145(3) . . . . ? C88 N8 C82 Rh2 -138(2) . . . . ? C58 Rh2 C82 N8 -21(2) . . . . ? C66 Rh2 C82 N8 24(3) . . . . ? C74 Rh2 C82 N8 154(2) . . . . ? C81 N7 C83 C84 168(5) . . . . ? N7 C83 C84 C85 50.4(4) . . . . ? C83 C84 C85 C86 63.3(4) . . . . ? C84 C85 C86 C87 178.2(4) . . . . ? C85 C86 C87 C88 54.5(5) . . . . ? C82 N8 C88 C87 -35(3) . . . . ? C86 C87 C88 N8 56.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.581 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.139 data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 248494' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(dimen)4)(PF6)2xCH3CN _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C50 H75 F12 N9 P2 Rh2' _chemical_formula_weight 1297.95 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4476(2) _cell_length_b 13.4410(3) _cell_length_c 13.6704(3) _cell_angle_alpha 61.9180(10) _cell_angle_beta 84.8570(10) _cell_angle_gamma 75.2360(10) _cell_volume 1480.07(6) _cell_formula_units_Z 1 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.05 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.9342 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent acetonitrile / diethyl ether ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 25586 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 30.05 _reflns_number_total 8482 _reflns_number_gt 7266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.1774P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8482 _refine_ls_number_parameters 394 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.706842(17) 0.509080(14) 0.562977(12) 0.01491(5) Uani 1 1 d . . . P1 P 0.88815(7) 0.91052(5) 0.81961(5) 0.02193(12) Uani 1 1 d . . . F1 F 0.9416(3) 0.77239(15) 0.88962(16) 0.0556(5) Uani 1 1 d . . . F2 F 1.05196(17) 0.91691(16) 0.78021(15) 0.0384(4) Uani 1 1 d . . . F3 F 0.72448(19) 0.90424(16) 0.85828(14) 0.0391(4) Uani 1 1 d . . . F4 F 0.85595(17) 0.89689(14) 0.71371(12) 0.0327(3) Uani 1 1 d . . . F5 F 0.83558(17) 1.04810(12) 0.74886(11) 0.0300(3) Uani 1 1 d . . . F6 F 0.92025(18) 0.92475(14) 0.92461(12) 0.0337(3) Uani 1 1 d . . . N1 N 0.7899(2) 0.69270(19) 0.33602(16) 0.0283(4) Uani 1 1 d . A . N2 N 0.8735(2) 0.33334(17) 0.47869(16) 0.0223(4) Uani 1 1 d . . . N3 N 0.6283(2) 0.32583(17) 0.79343(15) 0.0226(4) Uani 1 1 d . C . N4 N 0.5480(2) 0.69662(17) 0.63430(16) 0.0221(4) Uani 1 1 d . B . C1 C 0.7586(2) 0.6271(2) 0.42094(18) 0.0221(4) Uani 1 1 d . . . C2 C 0.8200(3) 0.7675(2) 0.22030(19) 0.0310(5) Uani 1 1 d D . . C3 C 0.9643(3) 0.7020(4) 0.1938(3) 0.0511(12) Uani 0.80 1 d PD A 1 H3A H 1.0459 0.7017 0.2335 0.077 Uiso 0.80 1 calc PR A 1 H3B H 0.9789 0.7409 0.1138 0.077 Uiso 0.80 1 calc PR A 1 H3C H 0.9599 0.6219 0.2172 0.077 Uiso 0.80 1 calc PR A 1 C4 C 0.8377(6) 0.8796(4) 0.2097(3) 0.0545(13) Uani 0.80 1 d P A 1 H4A H 0.9272 0.8650 0.2504 0.082 Uiso 0.80 1 calc PR A 1 H4B H 0.7530 0.9135 0.2405 0.082 Uiso 0.80 1 calc PR A 1 H4C H 0.8446 0.9336 0.1312 0.082 Uiso 0.80 1 calc PR A 1 C5 C 0.6918(3) 0.7848(2) 0.1458(2) 0.0220(5) Uani 0.80 1 d PD . 1 H5A H 0.7107 0.8386 0.0677 0.026 Uiso 0.80 1 calc PR . 1 C6 C 0.5448(3) 0.84157(19) 0.17525(18) 0.0228(4) Uani 1 1 d D . . H6A H 0.5507 0.9160 0.1711 0.027 Uiso 1 1 calc R A 1 H6B H 0.5230 0.7903 0.2525 0.027 Uiso 1 1 calc R A 1 C7 C 0.8109(2) 0.39338(19) 0.51435(17) 0.0197(4) Uani 1 1 d . . . C8 C 0.9522(2) 0.2657(2) 0.42370(18) 0.0215(4) Uani 1 1 d D . . C9 C 0.8408(3) 0.2299(2) 0.3790(2) 0.0183(4) Uani 0.86 1 d P . 1 H9A H 0.8982 0.1763 0.3500 0.022 Uiso 0.86 1 calc PR . 1 C10 C 1.0364(3) 0.3459(3) 0.3289(2) 0.0272(5) Uani 0.86 1 d P . 1 H10A H 1.1037 0.3690 0.3603 0.041 Uiso 0.86 1 calc PR . 1 H10B H 0.9665 0.4153 0.2767 0.041 Uiso 0.86 1 calc PR . 1 H10C H 1.0922 0.3040 0.2899 0.041 Uiso 0.86 1 calc PR . 1 C11 C 1.0618(3) 0.1619(3) 0.5081(2) 0.0279(6) Uani 0.86 1 d P . 1 H11A H 1.0104 0.1179 0.5738 0.042 Uiso 0.86 1 calc PR . 1 H11B H 1.1347 0.1891 0.5296 0.042 Uiso 0.86 1 calc PR . 1 H11C H 1.1110 0.1117 0.4752 0.042 Uiso 0.86 1 calc PR . 1 C20 C 0.5572(3) 0.8211(3) 0.7159(3) 0.0327(6) Uani 0.86 1 d P B 1 H20A H 0.6206 0.7555 0.7769 0.049 Uiso 0.86 1 calc PR B 1 H20B H 0.4974 0.8740 0.7427 0.049 Uiso 0.86 1 calc PR B 1 H20C H 0.6177 0.8628 0.6558 0.049 Uiso 0.86 1 calc PR B 1 C21 C 0.3605(3) 0.8770(2) 0.5729(2) 0.0251(5) Uani 0.86 1 d P B 1 H21A H 0.3039 0.9353 0.5955 0.030 Uiso 0.86 1 calc PR B 1 H21B H 0.4243 0.9152 0.5124 0.030 Uiso 0.86 1 calc PR B 1 C23 C 0.3601(3) 0.7098(3) 0.7620(2) 0.0244(5) Uani 0.86 1 d P B 1 H23A H 0.3013 0.7609 0.7921 0.029 Uiso 0.86 1 calc PR B 1 H23B H 0.4228 0.6421 0.8235 0.029 Uiso 0.86 1 calc PR B 1 C12 C 0.6568(2) 0.39090(19) 0.70698(17) 0.0191(4) Uani 1 1 d . . . C13 C 0.5887(3) 0.2478(2) 0.90401(18) 0.0250(5) Uani 1 1 d D . . C14 C 0.7139(4) 0.2182(4) 0.9864(3) 0.0392(8) Uani 0.80 1 d P C 1 H14A H 0.7240 0.2897 0.9848 0.059 Uiso 0.80 1 calc PR C 1 H14B H 0.8059 0.1811 0.9650 0.059 Uiso 0.80 1 calc PR C 1 H14C H 0.6909 0.1650 1.0615 0.059 Uiso 0.80 1 calc PR C 1 C15 C 0.5798(3) 0.1354(2) 0.9031(2) 0.0251(6) Uani 0.80 1 d P . 1 H15A H 0.6740 0.1023 0.8791 0.030 Uiso 0.80 1 calc PR . 1 H15B H 0.5634 0.0776 0.9792 0.030 Uiso 0.80 1 calc PR . 1 C16 C 0.4438(3) 0.3054(3) 0.9302(2) 0.0239(5) Uani 0.80 1 d PD C 1 H16A H 0.4503 0.3803 0.9246 0.029 Uiso 0.80 1 calc PR C 1 H16B H 0.4211 0.2556 1.0076 0.029 Uiso 0.80 1 calc PR C 1 C17 C 0.3172(2) 0.32837(19) 0.85156(19) 0.0247(4) Uani 1 1 d D . . H17A H 0.2233 0.3627 0.8749 0.030 Uiso 1 1 calc R C 1 H17B H 0.3340 0.3846 0.7749 0.030 Uiso 1 1 calc R C 1 C18 C 0.6064(2) 0.62836(19) 0.60679(17) 0.0194(4) Uani 1 1 d . . . C19 C 0.4572(2) 0.7762(2) 0.6726(2) 0.0236(4) Uani 1 1 d D . . C22 C 0.2559(2) 0.83789(19) 0.52981(18) 0.0220(4) Uani 1 1 d D . . H22A H 0.3124 0.7879 0.4978 0.026 Uiso 1 1 calc R B 1 H22B H 0.1925 0.9067 0.4697 0.026 Uiso 1 1 calc R B 1 C24 C 0.2565(2) 0.6673(2) 0.71789(18) 0.0228(4) Uani 1 1 d D . . H24A H 0.3148 0.6117 0.6926 0.027 Uiso 1 1 calc R B 1 H24B H 0.1943 0.6263 0.7782 0.027 Uiso 1 1 calc R B 1 C25 C 0.6861(8) 0.8731(9) 0.1820(9) 0.0181(18) Uiso 0.20 1 d PD A 2 H25A H 0.6746 0.9058 0.2345 0.022 Uiso 0.20 1 calc PR A 2 H25B H 0.7043 0.9338 0.1081 0.022 Uiso 0.20 1 calc PR A 2 C26 C 0.8395(12) 0.6982(8) 0.1584(8) 0.0200(19) Uiso 0.20 1 d PD . 2 H26A H 0.9135 0.6240 0.1980 0.024 Uiso 0.20 1 calc PR . 2 H26B H 0.8747 0.7421 0.0833 0.024 Uiso 0.20 1 calc PR . 2 C27 C 0.5684(11) 0.7702(9) 0.1109(9) 0.0185(19) Uiso 0.20 1 d P . 2 H27A H 0.5946 0.8231 0.0346 0.022 Uiso 0.20 1 calc PR . 2 C28 C 0.9544(10) 0.8084(11) 0.2258(11) 0.030(2) Uiso 0.20 1 d PD A 2 H28A H 1.0367 0.7408 0.2620 0.045 Uiso 0.20 1 calc PR A 2 H28B H 0.9325 0.8518 0.2685 0.045 Uiso 0.20 1 calc PR A 2 H28C H 0.9801 0.8588 0.1505 0.045 Uiso 0.20 1 calc PR A 2 C29 C 0.7095(13) 0.1398(9) 0.9551(12) 0.041(3) Uiso 0.20 1 d PD C 2 H29A H 0.7859 0.1545 0.9870 0.061 Uiso 0.20 1 calc PR C 2 H29B H 0.7512 0.1173 0.8981 0.061 Uiso 0.20 1 calc PR C 2 H29C H 0.6704 0.0769 1.0136 0.061 Uiso 0.20 1 calc PR C 2 C30 C 0.5539(18) 0.3243(12) 0.9614(12) 0.043(3) Uiso 0.20 1 d PD C 2 H30A H 0.6452 0.3351 0.9793 0.065 Uiso 0.20 1 calc PR C 2 H30B H 0.5029 0.2869 1.0298 0.065 Uiso 0.20 1 calc PR C 2 H30C H 0.4912 0.4000 0.9120 0.065 Uiso 0.20 1 calc PR C 2 C36 C 0.0953(17) 0.8603(13) 0.5162(13) 0.019(3) Uiso 0.14 1 d P . 2 H36A H 0.0663 0.9021 0.4364 0.023 Uiso 0.14 1 calc PR . 2 H36B H 0.0446 0.9094 0.5508 0.023 Uiso 0.14 1 calc PR . 2 C35 C 0.3012(15) 0.7808(8) 0.6520(5) 0.018(3) Uiso 0.14 1 d PD B 2 H35A H 0.2403 0.8340 0.6802 0.022 Uiso 0.14 1 calc PR B 2 C32 C 0.8983(15) 0.3284(12) 0.3043(6) 0.017(3) Uiso 0.14 1 d PD . 2 H32A H 0.9085 0.4093 0.2721 0.020 Uiso 0.14 1 calc PR . 2 H32B H 0.9638 0.2910 0.2640 0.020 Uiso 0.14 1 calc PR . 2 C31 C 1.1146(7) 0.2407(16) 0.4447(15) 0.028(3) Uiso 0.14 1 d PD . 2 H31A H 1.1453 0.3140 0.4116 0.042 Uiso 0.14 1 calc PR . 2 H31B H 1.1676 0.1920 0.4113 0.042 Uiso 0.14 1 calc PR . 2 H31C H 1.1366 0.1998 0.5248 0.042 Uiso 0.14 1 calc PR . 2 C33 C 0.508(3) 0.715(2) 0.7937(7) 0.046(5) Uiso 0.14 1 d PD B 2 H33A H 0.4945 0.6353 0.8289 0.069 Uiso 0.14 1 calc PR B 2 H33B H 0.4512 0.7570 0.8317 0.069 Uiso 0.14 1 calc PR B 2 H33C H 0.6124 0.7115 0.7985 0.069 Uiso 0.14 1 calc PR B 2 C34 C 0.511(2) 0.8844(19) 0.6142(18) 0.039(4) Uiso 0.14 1 d P B 2 H34A H 0.6175 0.8641 0.6085 0.058 Uiso 0.14 1 calc PR B 2 H34B H 0.4855 0.9287 0.6559 0.058 Uiso 0.14 1 calc PR B 2 H34C H 0.4649 0.9316 0.5396 0.058 Uiso 0.14 1 calc PR B 2 N1S N 1.2704(7) 0.4883(8) 1.0571(7) 0.082(2) Uiso 0.50 1 d PD D 2 C1S C 1.1530(6) 0.4924(8) 1.0346(7) 0.062(2) Uiso 0.50 1 d PD D 2 C2S C 1.0000 0.5000 1.0000 0.0755(17) Uiso 1 2 d SD . 2 H2SA H 0.9866 0.4231 1.0267 0.113 Uiso 0.50 1 d PR . 2 H2SB H 0.9282 0.5410 1.0310 0.113 Uiso 0.50 1 d PR . 2 H2SC H 0.9889 0.5407 0.9206 0.113 Uiso 0.50 1 d PR . 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 0.01759(8) 0.01566(8) 0.01218(7) -0.00687(6) 0.00361(5) -0.00541(5) P1 0.0303(3) 0.0189(3) 0.0179(2) -0.0097(2) 0.0048(2) -0.0069(2) F1 0.0918(16) 0.0189(8) 0.0440(10) -0.0080(7) -0.0047(10) -0.0046(9) F2 0.0270(7) 0.0544(10) 0.0468(10) -0.0360(9) 0.0088(7) -0.0084(7) F3 0.0420(9) 0.0563(10) 0.0362(8) -0.0293(8) 0.0206(7) -0.0307(8) F4 0.0398(8) 0.0419(9) 0.0295(7) -0.0259(7) 0.0080(6) -0.0148(7) F5 0.0424(8) 0.0213(7) 0.0218(7) -0.0082(5) 0.0039(6) -0.0049(6) F6 0.0457(9) 0.0380(8) 0.0204(7) -0.0157(6) 0.0013(6) -0.0110(7) N1 0.0330(11) 0.0309(11) 0.0178(9) -0.0052(8) 0.0016(8) -0.0149(9) N2 0.0227(9) 0.0279(10) 0.0229(9) -0.0167(8) 0.0026(7) -0.0076(7) N3 0.0241(9) 0.0267(9) 0.0187(8) -0.0104(7) 0.0051(7) -0.0106(8) N4 0.0195(8) 0.0242(9) 0.0255(9) -0.0141(8) 0.0030(7) -0.0059(7) C1 0.0250(10) 0.0241(10) 0.0185(10) -0.0093(8) 0.0019(8) -0.0095(8) C2 0.0317(12) 0.0375(14) 0.0170(10) -0.0013(9) 0.0022(9) -0.0208(11) C3 0.0262(16) 0.081(3) 0.0238(16) -0.0032(17) 0.0012(13) -0.0199(18) C4 0.085(3) 0.060(3) 0.0243(16) -0.0035(16) -0.0050(18) -0.057(3) C5 0.0241(13) 0.0240(13) 0.0160(11) -0.0059(10) 0.0028(10) -0.0104(11) C6 0.0308(11) 0.0178(9) 0.0208(10) -0.0099(8) 0.0062(8) -0.0075(8) C7 0.0210(10) 0.0222(10) 0.0180(9) -0.0103(8) 0.0025(7) -0.0077(8) C8 0.0211(10) 0.0279(11) 0.0224(10) -0.0187(9) 0.0041(8) -0.0043(8) C9 0.0189(11) 0.0204(11) 0.0185(11) -0.0127(9) 0.0009(8) -0.0020(9) C10 0.0247(13) 0.0369(15) 0.0267(13) -0.0189(12) 0.0055(10) -0.0114(11) C11 0.0240(13) 0.0345(15) 0.0266(13) -0.0186(12) -0.0046(10) 0.0013(11) C20 0.0285(14) 0.0373(16) 0.0452(17) -0.0297(14) -0.0010(12) -0.0069(12) C21 0.0258(12) 0.0199(12) 0.0319(14) -0.0135(11) -0.0003(10) -0.0057(10) C23 0.0238(12) 0.0332(14) 0.0185(11) -0.0151(11) 0.0014(9) -0.0045(10) C12 0.0203(9) 0.0214(10) 0.0183(9) -0.0113(8) 0.0037(7) -0.0064(8) C13 0.0283(11) 0.0319(12) 0.0138(9) -0.0072(9) 0.0059(8) -0.0147(9) C14 0.0310(16) 0.059(2) 0.0188(14) -0.0060(14) -0.0034(12) -0.0186(16) C15 0.0275(14) 0.0191(12) 0.0211(13) -0.0051(10) 0.0051(10) -0.0034(10) C16 0.0302(14) 0.0244(13) 0.0225(13) -0.0146(11) 0.0085(11) -0.0105(11) C17 0.0272(11) 0.0199(10) 0.0247(11) -0.0106(9) 0.0091(9) -0.0043(8) C18 0.0199(9) 0.0204(10) 0.0187(9) -0.0093(8) 0.0030(7) -0.0069(8) C19 0.0205(10) 0.0275(11) 0.0308(11) -0.0204(10) 0.0013(8) -0.0049(8) C22 0.0242(10) 0.0191(10) 0.0209(10) -0.0079(8) 0.0015(8) -0.0055(8) C24 0.0235(10) 0.0253(11) 0.0169(9) -0.0069(8) 0.0014(8) -0.0078(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.962(2) . ? Rh1 C18 1.964(2) . ? Rh1 C12 1.973(2) . ? Rh1 C7 1.976(2) . ? P1 F5 1.5924(15) . ? P1 F1 1.5980(18) . ? P1 F6 1.5984(15) . ? P1 F3 1.5985(17) . ? P1 F2 1.6023(17) . ? P1 F4 1.6059(15) . ? N1 C1 1.149(3) . ? N1 C2 1.470(3) . ? N2 C7 1.146(3) . ? N2 C8 1.464(3) . ? N3 C12 1.151(3) . ? N3 C13 1.460(3) . ? N4 C18 1.148(3) . ? N4 C19 1.460(3) . ? C2 C4 1.496(5) . ? C2 C26 1.498(5) . ? C2 C28 1.527(5) . ? C2 C3 1.537(4) . ? C2 C25 1.547(10) . ? C2 C5 1.554(3) . ? C5 C6 1.524(4) . ? C5 C17 1.528(4) 2_666 ? C6 C25 1.523(5) . ? C6 C15 1.535(4) 2_666 ? C6 C27 1.547(11) . ? C8 C32 1.506(5) . ? C8 C31 1.508(5) . ? C8 C11 1.521(4) . ? C8 C9 1.538(3) . ? C8 C10 1.553(4) . ? C8 C36 1.661(15) 2_666 ? C9 C24 1.535(3) 2_666 ? C9 C22 1.540(3) 2_666 ? C20 C19 1.528(3) . ? C21 C22 1.503(3) . ? C21 C19 1.544(4) . ? C23 C19 1.524(4) . ? C23 C24 1.538(3) . ? C13 C16 1.494(4) . ? C13 C29 1.497(5) . ? C13 C30 1.523(5) . ? C13 C15 1.541(4) . ? C13 C14 1.550(4) . ? C13 C27 1.609(11) 2_666 ? C15 C6 1.535(4) 2_666 ? C16 C17 1.553(3) . ? C17 C27 1.384(11) 2_666 ? C17 C5 1.528(4) 2_666 ? C17 C26 1.640(11) 2_666 ? C19 C34 1.49(2) . ? C19 C35 1.506(11) . ? C19 C33 1.519(5) . ? C22 C36 1.481(15) . ? C22 C35 1.522(5) . ? C22 C9 1.540(3) 2_666 ? C24 C32 1.501(13) 2_666 ? C24 C35 1.512(5) . ? C24 C9 1.535(3) 2_666 ? C26 C17 1.640(10) 2_666 ? C27 C17 1.384(11) 2_666 ? C27 C13 1.609(11) 2_666 ? C36 C8 1.661(15) 2_666 ? C32 C24 1.501(13) 2_666 ? N1S C1S 1.158(5) . ? C1S C2S 1.525(4) . ? C2S C1S 1.525(4) 2_767 ? 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 C18 91.42(9) . . ? C1 Rh1 C12 179.13(9) . . ? C18 Rh1 C12 88.27(9) . . ? C1 Rh1 C7 86.54(9) . . ? C18 Rh1 C7 177.92(9) . . ? C12 Rh1 C7 93.77(9) . . ? F5 P1 F1 179.47(10) . . ? F5 P1 F6 89.87(8) . . ? F1 P1 F6 90.55(10) . . ? F5 P1 F3 90.18(9) . . ? F1 P1 F3 90.13(11) . . ? F6 P1 F3 90.05(9) . . ? F5 P1 F2 89.74(9) . . ? F1 P1 F2 89.94(11) . . ? F6 P1 F2 90.25(9) . . ? F3 P1 F2 179.69(9) . . ? F5 P1 F4 89.85(8) . . ? F1 P1 F4 89.72(10) . . ? F6 P1 F4 179.71(9) . . ? F3 P1 F4 90.06(9) . . ? F2 P1 F4 89.64(8) . . ? C1 N1 C2 171.1(2) . . ? C7 N2 C8 175.0(2) . . ? C12 N3 C13 177.4(2) . . ? C18 N4 C19 172.3(2) . . ? N1 C1 Rh1 177.0(2) . . ? N1 C2 C4 109.2(2) . . ? N1 C2 C26 108.0(5) . . ? C4 C2 C26 142.2(5) . . ? N1 C2 C28 105.7(5) . . ? C4 C2 C28 47.6(5) . . ? C26 C2 C28 115.0(7) . . ? N1 C2 C3 106.5(2) . . ? C4 C2 C3 109.8(3) . . ? C26 C2 C3 52.2(4) . . ? C28 C2 C3 65.6(5) . . ? N1 C2 C25 103.6(4) . . ? C4 C2 C25 61.1(3) . . ? C26 C2 C25 115.4(6) . . ? C28 C2 C25 108.2(6) . . ? C3 C2 C25 149.8(4) . . ? N1 C2 C5 107.80(19) . . ? C4 C2 C5 112.7(3) . . ? C26 C2 C5 60.4(4) . . ? C28 C2 C5 145.8(5) . . ? C3 C2 C5 110.5(2) . . ? C25 C2 C5 56.8(3) . . ? C6 C5 C17 109.8(2) . 2_666 ? C6 C5 C2 112.2(2) . . ? C17 C5 C2 112.7(2) 2_666 . ? C25 C6 C5 57.9(4) . . ? C25 C6 C15 144.3(4) . 2_666 ? C5 C6 C15 111.7(2) . 2_666 ? C25 C6 C27 110.1(6) . . ? C5 C6 C27 53.7(4) . . ? C15 C6 C27 62.0(4) 2_666 . ? N2 C7 Rh1 174.7(2) . . ? N2 C8 C32 108.1(6) . . ? N2 C8 C31 109.2(7) . . ? C32 C8 C31 116.8(9) . . ? N2 C8 C11 107.65(19) . . ? C32 C8 C11 144.1(6) . . ? C31 C8 C11 46.8(7) . . ? N2 C8 C9 108.93(18) . . ? C32 C8 C9 56.6(6) . . ? C31 C8 C9 141.1(7) . . ? C11 C8 C9 112.6(2) . . ? N2 C8 C10 106.34(19) . . ? C32 C8 C10 57.7(6) . . ? C31 C8 C10 63.8(7) . . ? C11 C8 C10 109.2(2) . . ? C9 C8 C10 111.84(19) . . ? N2 C8 C36 106.9(6) . 2_666 ? C32 C8 C36 107.7(8) . 2_666 ? C31 C8 C36 107.8(9) . 2_666 ? C11 C8 C36 63.4(5) . 2_666 ? C9 C8 C36 52.8(5) . 2_666 ? C10 C8 C36 146.6(6) . 2_666 ? C24 C9 C8 113.2(2) 2_666 . ? C24 C9 C22 109.59(19) 2_666 2_666 ? C8 C9 C22 112.51(19) . 2_666 ? C22 C21 C19 112.9(2) . . ? C19 C23 C24 112.4(2) . . ? N3 C12 Rh1 176.24(19) . . ? N3 C13 C16 109.0(2) . . ? N3 C13 C29 109.7(6) . . ? C16 C13 C29 141.2(6) . . ? N3 C13 C30 102.8(6) . . ? C16 C13 C30 50.3(6) . . ? C29 C13 C30 117.1(9) . . ? N3 C13 C15 107.70(19) . . ? C16 C13 C15 110.6(2) . . ? C29 C13 C15 59.0(6) . . ? C30 C13 C15 148.5(7) . . ? N3 C13 C14 107.6(2) . . ? C16 C13 C14 113.1(2) . . ? C29 C13 C14 51.3(6) . . ? C30 C13 C14 68.2(6) . . ? C15 C13 C14 108.7(2) . . ? N3 C13 C27 106.2(4) . 2_666 ? C16 C13 C27 53.6(4) . 2_666 ? C29 C13 C27 116.1(7) . 2_666 ? C30 C13 C27 103.6(7) . 2_666 ? C15 C13 C27 60.5(4) . 2_666 ? C14 C13 C27 146.2(4) . 2_666 ? C6 C15 C13 111.3(2) 2_666 . ? C13 C16 C17 112.9(2) . . ? C27 C17 C5 56.7(4) 2_666 2_666 ? C27 C17 C16 56.8(4) 2_666 . ? C5 C17 C16 110.5(2) 2_666 . ? C27 C17 C26 112.7(6) 2_666 2_666 ? C5 C17 C26 57.9(3) 2_666 2_666 ? C16 C17 C26 146.3(4) . 2_666 ? N4 C18 Rh1 178.8(2) . . ? N4 C19 C34 105.0(9) . . ? N4 C19 C35 105.7(5) . . ? C34 C19 C35 119.1(9) . . ? N4 C19 C33 100.5(10) . . ? C34 C19 C33 108.7(13) . . ? C35 C19 C33 115.5(10) . . ? N4 C19 C23 107.7(2) . . ? C34 C19 C23 146.9(9) . . ? C35 C19 C23 55.8(2) . . ? C33 C19 C23 60.3(10) . . ? N4 C19 C20 108.8(2) . . ? C34 C19 C20 50.4(9) . . ? C35 C19 C20 145.6(5) . . ? C33 C19 C20 58.4(10) . . ? C23 C19 C20 112.3(2) . . ? N4 C19 C21 107.66(19) . . ? C34 C19 C21 64.4(9) . . ? C35 C19 C21 56.7(2) . . ? C33 C19 C21 151.8(10) . . ? C23 C19 C21 109.4(2) . . ? C20 C19 C21 110.8(2) . . ? C36 C22 C21 137.3(6) . . ? C36 C22 C35 110.6(8) . . ? C21 C22 C35 57.2(3) . . ? C36 C22 C9 56.3(6) . 2_666 ? C21 C22 C9 112.4(2) . 2_666 ? C35 C22 C9 58.8(4) . 2_666 ? C32 C24 C35 114.9(7) 2_666 . ? C32 C24 C9 56.7(4) 2_666 2_666 ? C35 C24 C9 59.1(4) . 2_666 ? C32 C24 C23 147.6(6) 2_666 . ? C35 C24 C23 55.4(3) . . ? C9 C24 C23 110.5(2) 2_666 . ? C6 C25 C2 112.6(6) . . ? C2 C26 C17 109.5(6) . 2_666 ? C17 C27 C6 116.7(7) 2_666 . ? C17 C27 C13 115.9(7) 2_666 2_666 ? C6 C27 C13 107.2(6) . 2_666 ? C22 C36 C8 109.0(9) . 2_666 ? C19 C35 C24 114.9(7) . . ? C19 C35 C22 114.1(7) . . ? C24 C35 C22 111.8(4) . . ? C24 C32 C8 117.1(8) 2_666 . ? N1S C1S C2S 177.7(9) . . ? C1S C2S C1S 179.999(1) . 2_767 ? 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 C2 N1 C1 Rh1 32(5) . . . . ? C18 Rh1 C1 N1 -161(4) . . . . ? C12 Rh1 C1 N1 130(6) . . . . ? C7 Rh1 C1 N1 19(4) . . . . ? C1 N1 C2 C4 157.9(16) . . . . ? C1 N1 C2 C26 -28.8(18) . . . . ? C1 N1 C2 C28 -152.3(17) . . . . ? C1 N1 C2 C3 -83.6(17) . . . . ? C1 N1 C2 C25 94.1(17) . . . . ? C1 N1 C2 C5 35.0(17) . . . . ? N1 C2 C5 C6 59.8(3) . . . . ? C4 C2 C5 C6 -60.8(3) . . . . ? C26 C2 C5 C6 160.8(5) . . . . ? C28 C2 C5 C6 -107.6(10) . . . . ? C3 C2 C5 C6 175.9(2) . . . . ? C25 C2 C5 C6 -35.1(4) . . . . ? N1 C2 C5 C17 -64.7(3) . . . 2_666 ? C4 C2 C5 C17 174.6(3) . . . 2_666 ? C26 C2 C5 C17 36.3(5) . . . 2_666 ? C28 C2 C5 C17 127.9(10) . . . 2_666 ? C3 C2 C5 C17 51.3(3) . . . 2_666 ? C25 C2 C5 C17 -159.6(5) . . . 2_666 ? C17 C5 C6 C25 161.3(5) 2_666 . . . ? C2 C5 C6 C25 35.2(5) . . . . ? C17 C5 C6 C15 -57.2(3) 2_666 . . 2_666 ? C2 C5 C6 C15 176.7(2) . . . 2_666 ? C17 C5 C6 C27 -33.9(5) 2_666 . . . ? C2 C5 C6 C27 -160.0(5) . . . . ? C8 N2 C7 Rh1 -15(4) . . . . ? C1 Rh1 C7 N2 0(2) . . . . ? C18 Rh1 C7 N2 -11(4) . . . . ? C12 Rh1 C7 N2 -179(100) . . . . ? C7 N2 C8 C32 -28(3) . . . . ? C7 N2 C8 C31 100(3) . . . . ? C7 N2 C8 C11 149(2) . . . . ? C7 N2 C8 C9 -88(2) . . . . ? C7 N2 C8 C10 32(3) . . . . ? C7 N2 C8 C36 -144(2) . . . 2_666 ? N2 C8 C9 C24 68.8(2) . . . 2_666 ? C32 C8 C9 C24 -30.9(7) . . . 2_666 ? C31 C8 C9 C24 -123.4(12) . . . 2_666 ? C11 C8 C9 C24 -171.9(2) . . . 2_666 ? C10 C8 C9 C24 -48.5(3) . . . 2_666 ? C36 C8 C9 C24 165.9(7) 2_666 . . 2_666 ? N2 C8 C9 C22 -56.2(2) . . . 2_666 ? C32 C8 C9 C22 -155.8(7) . . . 2_666 ? C31 C8 C9 C22 111.6(12) . . . 2_666 ? C11 C8 C9 C22 63.2(3) . . . 2_666 ? C10 C8 C9 C22 -173.4(2) . . . 2_666 ? C36 C8 C9 C22 41.0(7) 2_666 . . 2_666 ? C13 N3 C12 Rh1 34(7) . . . . ? C1 Rh1 C12 N3 37(8) . . . . ? C18 Rh1 C12 N3 -32(3) . . . . ? C7 Rh1 C12 N3 147(3) . . . . ? C12 N3 C13 C16 33(5) . . . . ? C12 N3 C13 C29 -144(5) . . . . ? C12 N3 C13 C30 -19(5) . . . . ? C12 N3 C13 C15 153(5) . . . . ? C12 N3 C13 C14 -90(5) . . . . ? C12 N3 C13 C27 90(5) . . . 2_666 ? N3 C13 C15 C6 -65.0(3) . . . 2_666 ? C16 C13 C15 C6 54.0(3) . . . 2_666 ? C29 C13 C15 C6 -167.8(7) . . . 2_666 ? C30 C13 C15 C6 100.1(13) . . . 2_666 ? C14 C13 C15 C6 178.7(2) . . . 2_666 ? C27 C13 C15 C6 34.0(5) 2_666 . . 2_666 ? N3 C13 C16 C17 63.8(3) . . . . ? C29 C13 C16 C17 -120.2(10) . . . . ? C30 C13 C16 C17 154.9(8) . . . . ? C15 C13 C16 C17 -54.4(3) . . . . ? C14 C13 C16 C17 -176.6(2) . . . . ? C27 C13 C16 C17 -32.7(5) 2_666 . . . ? C13 C16 C17 C27 37.2(5) . . . 2_666 ? C13 C16 C17 C5 56.3(3) . . . 2_666 ? C13 C16 C17 C26 118.6(5) . . . 2_666 ? C19 N4 C18 Rh1 -74(10) . . . . ? C1 Rh1 C18 N4 -157(9) . . . . ? C12 Rh1 C18 N4 22(9) . . . . ? C7 Rh1 C18 N4 -146(8) . . . . ? C18 N4 C19 C34 -153.9(19) . . . . ? C18 N4 C19 C35 -27.1(18) . . . . ? C18 N4 C19 C33 93.3(19) . . . . ? C18 N4 C19 C23 31.4(18) . . . . ? C18 N4 C19 C20 153.3(16) . . . . ? C18 N4 C19 C21 -86.5(17) . . . . ? C24 C23 C19 N4 -61.8(3) . . . . ? C24 C23 C19 C34 127.5(16) . . . . ? C24 C23 C19 C35 35.5(6) . . . . ? C24 C23 C19 C33 -154.0(11) . . . . ? C24 C23 C19 C20 178.5(2) . . . . ? C24 C23 C19 C21 55.0(3) . . . . ? C22 C21 C19 N4 63.3(3) . . . . ? C22 C21 C19 C34 161.9(10) . . . . ? C22 C21 C19 C35 -34.2(6) . . . . ? C22 C21 C19 C33 -116(2) . . . . ? C22 C21 C19 C23 -53.5(3) . . . . ? C22 C21 C19 C20 -177.9(2) . . . . ? C19 C21 C22 C36 118.8(9) . . . . ? C19 C21 C22 C35 33.5(7) . . . . ? C19 C21 C22 C9 54.9(3) . . . 2_666 ? C19 C23 C24 C32 -117.8(7) . . . 2_666 ? C19 C23 C24 C35 -35.5(7) . . . . ? C19 C23 C24 C9 -58.0(3) . . . 2_666 ? C5 C6 C25 C2 -35.6(4) . . . . ? C15 C6 C25 C2 -118.3(7) 2_666 . . . ? C27 C6 C25 C2 -48.6(8) . . . . ? N1 C2 C25 C6 -67.3(7) . . . . ? C4 C2 C25 C6 -171.9(8) . . . . ? C26 C2 C25 C6 50.6(9) . . . . ? C28 C2 C25 C6 -179.1(7) . . . . ? C3 C2 C25 C6 108.3(7) . . . . ? C5 C2 C25 C6 35.3(4) . . . . ? N1 C2 C26 C17 68.0(6) . . . 2_666 ? C4 C2 C26 C17 -122.3(7) . . . 2_666 ? C28 C2 C26 C17 -174.3(7) . . . 2_666 ? C3 C2 C26 C17 165.3(9) . . . 2_666 ? C25 C2 C26 C17 -47.4(8) . . . 2_666 ? C5 C2 C26 C17 -32.7(4) . . . 2_666 ? C25 C6 C27 C17 54.1(9) . . . 2_666 ? C5 C6 C27 C17 40.4(5) . . . 2_666 ? C15 C6 C27 C17 -164.2(9) 2_666 . . 2_666 ? C25 C6 C27 C13 -174.1(6) . . . 2_666 ? C5 C6 C27 C13 172.3(8) . . . 2_666 ? C15 C6 C27 C13 -32.3(4) 2_666 . . 2_666 ? C21 C22 C36 C8 -126.8(7) . . . 2_666 ? C35 C22 C36 C8 -63.3(10) . . . 2_666 ? C9 C22 C36 C8 -39.6(5) 2_666 . . 2_666 ? N4 C19 C35 C24 64.0(7) . . . . ? C34 C19 C35 C24 -178.3(11) . . . . ? C33 C19 C35 C24 -46.1(14) . . . . ? C23 C19 C35 C24 -37.0(4) . . . . ? C20 C19 C35 C24 -116.7(8) . . . . ? C21 C19 C35 C24 165.1(10) . . . . ? N4 C19 C35 C22 -67.1(7) . . . . ? C34 C19 C35 C22 50.6(13) . . . . ? C33 C19 C35 C22 -177.2(12) . . . . ? C23 C19 C35 C22 -168.1(10) . . . . ? C20 C19 C35 C22 112.2(8) . . . . ? C21 C19 C35 C22 34.0(4) . . . . ? C32 C24 C35 C19 -179.0(7) 2_666 . . . ? C9 C24 C35 C19 -167.8(10) 2_666 . . . ? C23 C24 C35 C19 36.8(4) . . . . ? C32 C24 C35 C22 -46.8(12) 2_666 . . . ? C9 C24 C35 C22 -35.7(6) 2_666 . . . ? C23 C24 C35 C22 169.0(13) . . . . ? C36 C22 C35 C19 -168.7(8) . . . . ? C21 C22 C35 C19 -34.9(4) . . . . ? C9 C22 C35 C19 168.3(10) 2_666 . . . ? C36 C22 C35 C24 58.8(12) . . . . ? C21 C22 C35 C24 -167.5(12) . . . . ? C9 C22 C35 C24 35.7(6) 2_666 . . . ? N2 C8 C32 C24 -68.3(10) . . . 2_666 ? C31 C8 C32 C24 168.1(10) . . . 2_666 ? C11 C8 C32 C24 115.6(10) . . . 2_666 ? C9 C8 C32 C24 32.8(7) . . . 2_666 ? C10 C8 C32 C24 -166.5(13) . . . 2_666 ? C36 C8 C32 C24 46.8(12) 2_666 . . 2_666 ? N1S C1S C2S C1S 37(40) . . . 2_767 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.830 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.095 data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 248495' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Rh2(diprop)4)(BPh4)2 _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C68 H63 B2 N8 Rh2' _chemical_formula_weight 1219.70 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 9.1489(5) _cell_length_b 12.5958(6) _cell_length_c 13.6740(7) _cell_angle_alpha 70.101(2) _cell_angle_beta 76.012(2) _cell_angle_gamma 83.023(2) _cell_volume 1436.41(13) _cell_formula_units_Z 1 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.52 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 627 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type 'empirical SADABS 2.05' _exptl_absorpt_correction_T_min 0.9121 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details ? _exptl_special_details ; crystallization_solvent benzonitrile ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11477 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 22.52 _reflns_number_total 3755 _reflns_number_gt 2941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+8.2772P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model and ideal CH3 groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3755 _refine_ls_number_parameters 240 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.34085(7) 1.07481(5) 2.01747(4) 0.0266(2) Uani 1 1 d . . . N1 N 0.1736(7) 0.9305(5) 1.9374(5) 0.0356(15) Uani 1 1 d . . . N2 N 0.2589(7) 0.9084(5) 2.2484(5) 0.0344(15) Uani 1 1 d . . . N3 N 0.5325(7) 1.1992(5) 2.1023(5) 0.0366(16) Uani 1 1 d . . . N4 N 0.4493(7) 1.2265(5) 1.7825(5) 0.0303(14) Uani 1 1 d . . . C1 C 0.2320(8) 0.9870(6) 1.9678(5) 0.0292(17) Uani 1 1 d . . . C2 C 0.1198(9) 0.8543(7) 1.8958(7) 0.051(2) Uani 1 1 d . . . H2A H 0.1217 0.8921 1.8191 0.061 Uiso 1 1 calc R . . H2B H 0.0139 0.8370 1.9329 0.061 Uiso 1 1 calc R . . C3 C 0.2821(8) 0.9720(6) 2.1636(6) 0.0279(17) Uani 1 1 d . . . C4 C 0.2374(9) 0.8241(6) 2.3521(5) 0.042(2) Uani 1 1 d . . . H4A H 0.1282 0.8131 2.3812 0.050 Uiso 1 1 calc R . . H4B H 0.2767 0.8512 2.4005 0.050 Uiso 1 1 calc R . . C5 C 0.3163(9) 0.7123(6) 2.3490(6) 0.0389(19) Uani 1 1 d . . . H5A H 0.2803 0.6540 2.4184 0.047 Uiso 1 1 calc R . . H5B H 0.2858 0.6909 2.2937 0.047 Uiso 1 1 calc R . . C6 C 0.4581(9) 1.1580(6) 2.0692(5) 0.0310(18) Uani 1 1 d . . . C7 C 0.6270(10) 1.2469(7) 2.1468(7) 0.051(2) Uani 1 1 d . . . H7A H 0.6209 1.2006 2.2223 0.061 Uiso 1 1 calc R . . H7B H 0.5869 1.3241 2.1449 0.061 Uiso 1 1 calc R . . C8 C 0.7873(10) 1.2528(8) 2.0901(8) 0.061(3) Uani 1 1 d . . . H8A H 0.8362 1.3038 2.1127 0.073 Uiso 1 1 calc R . . H8B H 0.7904 1.2888 2.0131 0.073 Uiso 1 1 calc R . . C9 C 0.4046(8) 1.1739(6) 1.8701(6) 0.0303(17) Uani 1 1 d . . . C10 C 0.5137(9) 1.2901(6) 1.6734(5) 0.039(2) Uani 1 1 d . . . H10A H 0.4743 1.3694 1.6583 0.047 Uiso 1 1 calc R . . H10B H 0.4820 1.2583 1.6252 0.047 Uiso 1 1 calc R . . B1 B 0.2618(7) 1.2244(5) 1.4472(5) 0.016(3) Uani 0.50 1 d PD A 1 C11 C 0.1034(7) 1.2014(7) 1.4192(7) 0.021(3) Uiso 0.50 1 d PGD A 1 C12 C -0.0048(9) 1.2897(5) 1.4055(7) 0.030(3) Uiso 0.50 1 d PG A 1 H12A H 0.0145 1.3600 1.4103 0.036 Uiso 0.50 1 calc PR A 1 C13 C -0.1411(8) 1.2751(6) 1.3847(8) 0.053(5) Uiso 0.50 1 d PG A 1 H13A H -0.2151 1.3355 1.3754 0.063 Uiso 0.50 1 calc PR A 1 C14 C -0.1693(7) 1.1723(7) 1.3777(7) 0.012(3) Uiso 0.50 1 d PG A 1 H14A H -0.2625 1.1623 1.3635 0.015 Uiso 0.50 1 calc PR A 1 C15 C -0.0611(9) 1.0840(6) 1.3914(7) 0.025(3) Uiso 0.50 1 d PG A 1 H15A H -0.0803 1.0137 1.3866 0.030 Uiso 0.50 1 calc PR A 1 C16 C 0.0752(8) 1.0985(6) 1.4122(7) 0.032(3) Uiso 0.50 1 d PG A 1 H16A H 0.1492 1.0382 1.4215 0.039 Uiso 0.50 1 calc PR A 1 C17 C 0.3492(8) 1.3310(5) 1.3478(5) 0.017(3) Uiso 0.50 1 d PGD A 1 C18 C 0.4770(8) 1.3699(6) 1.3605(5) 0.017(3) Uiso 0.50 1 d PG A 1 H18A H 0.5125 1.3357 1.4245 0.021 Uiso 0.50 1 calc PR A 1 C19 C 0.5529(7) 1.4587(6) 1.2796(6) 0.021(3) Uiso 0.50 1 d PG A 1 H19A H 0.6403 1.4852 1.2883 0.025 Uiso 0.50 1 calc PR A 1 C20 C 0.5010(9) 1.5086(6) 1.1860(5) 0.026(3) Uiso 0.50 1 d PG A 1 H20A H 0.5529 1.5693 1.1308 0.031 Uiso 0.50 1 calc PR A 1 C21 C 0.3732(9) 1.4698(6) 1.1733(5) 0.030(3) Uiso 0.50 1 d PG A 1 H21A H 0.3377 1.5039 1.1094 0.036 Uiso 0.50 1 calc PR A 1 C22 C 0.2973(7) 1.3810(6) 1.2542(6) 0.022(3) Uiso 0.50 1 d PG A 1 H22A H 0.2099 1.3544 1.2455 0.027 Uiso 0.50 1 calc PR A 1 C23 C 0.1996(9) 1.2541(6) 1.5603(5) 0.015(3) Uiso 0.50 1 d PGD A 1 C24 C 0.1455(10) 1.1674(5) 1.6531(6) 0.027(3) Uiso 0.50 1 d PG A 1 H24A H 0.1558 1.0914 1.6532 0.032 Uiso 0.50 1 calc PR A 1 C25 C 0.0764(10) 1.1919(5) 1.7458(5) 0.024(3) Uiso 0.50 1 d PG A 1 H25A H 0.0394 1.1327 1.8092 0.028 Uiso 0.50 1 calc PR A 1 C26 C 0.0614(9) 1.3031(6) 1.7457(5) 0.026(3) Uiso 0.50 1 d PG A 1 H26A H 0.0141 1.3199 1.8090 0.031 Uiso 0.50 1 calc PR A 1 C27 C 0.1155(10) 1.3898(5) 1.6529(6) 0.027(3) Uiso 0.50 1 d PG A 1 H27A H 0.1052 1.4658 1.6528 0.032 Uiso 0.50 1 calc PR A 1 C28 C 0.1846(10) 1.3653(5) 1.5602(5) 0.044(4) Uiso 0.50 1 d PG A 1 H28A H 0.2216 1.4246 1.4968 0.053 Uiso 0.50 1 calc PR A 1 C29 C 0.3811(8) 1.1118(5) 1.4636(6) 0.020(3) Uiso 0.50 1 d PGD . 1 C30 C 0.4260(10) 1.0694(7) 1.3788(5) 0.033(4) Uiso 0.50 1 d PG . 1 H30A H 0.3863 1.1037 1.3158 0.039 Uiso 0.50 1 d PR . 1 C31 C 0.5283(11) 0.9775(7) 1.3854(6) 0.043(4) Uiso 0.50 1 d PG . 1 H31A H 0.5593 0.9483 1.3269 0.052 Uiso 0.50 1 d PR . 1 C32 C 0.5857(10) 0.9279(7) 1.4768(8) 0.046(5) Uiso 0.50 1 d PG . 1 H32A H 0.6564 0.8644 1.4813 0.055 Uiso 0.50 1 d PR . 1 C33 C 0.5408(11) 0.9702(8) 1.5615(6) 0.037(4) Uiso 0.50 1 d PG . 1 H33A H 0.5805 0.9359 1.6245 0.044 Uiso 0.50 1 d PR . 1 C34 C 0.4385(10) 1.0621(7) 1.5549(5) 0.013(3) Uiso 0.50 1 d PG . 1 H34A H 0.4075 1.0914 1.6134 0.015 Uiso 0.50 1 d PR . 1 B2 B -0.0812(8) 1.5319(6) 1.7835(6) 0.034(4) Uani 0.50 1 d PD B 2 C50 C -0.2644(7) 1.5320(8) 1.7880(6) 0.025(3) Uiso 0.50 1 d PGD B 2 C51 C -0.3611(9) 1.4711(8) 1.8804(5) 0.036(4) Uiso 0.50 1 d PG B 2 H51A H -0.3263 1.4389 1.9448 0.043 Uiso 0.50 1 calc PR B 2 C52 C -0.5087(8) 1.4573(8) 1.8785(6) 0.037(4) Uiso 0.50 1 d PG B 2 H52A H -0.5749 1.4157 1.9417 0.044 Uiso 0.50 1 calc PR B 2 C53 C -0.5597(7) 1.5045(9) 1.7843(7) 0.038(4) Uiso 0.50 1 d PG B 2 H53A H -0.6606 1.4950 1.7830 0.046 Uiso 0.50 1 calc PR B 2 C54 C -0.4630(9) 1.5654(8) 1.6919(6) 0.041(4) Uiso 0.50 1 d PG B 2 H54A H -0.4978 1.5976 1.6275 0.050 Uiso 0.50 1 calc PR B 2 C55 C -0.3153(8) 1.5792(7) 1.6938(5) 0.031(3) Uiso 0.50 1 d PG B 2 H55A H -0.2492 1.6208 1.6307 0.037 Uiso 0.50 1 calc PR B 2 C56 C -0.0117(12) 1.6574(6) 1.7128(9) 0.0558(19) Uiso 0.50 1 d PGD B 2 C57 C 0.1437(11) 1.6625(8) 1.6760(9) 0.0558(19) Uiso 0.50 1 d PG B 2 H57A H 0.2047 1.5948 1.6833 0.067 Uiso 0.50 1 calc PR B 2 C58 C 0.2098(9) 1.7667(10) 1.6286(9) 0.0558(19) Uiso 0.50 1 d PG B 2 H58A H 0.3159 1.7702 1.6034 0.067 Uiso 0.50 1 calc PR B 2 C59 C 0.1205(13) 1.8658(7) 1.6180(9) 0.0558(19) Uiso 0.50 1 d PG B 2 H59A H 0.1656 1.9370 1.5856 0.067 Uiso 0.50 1 calc PR B 2 C60 C -0.0349(12) 1.8607(7) 1.6548(9) 0.0558(19) Uiso 0.50 1 d PG B 2 H60A H -0.0959 1.9284 1.6475 0.067 Uiso 0.50 1 calc PR B 2 C61 C -0.1010(9) 1.7565(9) 1.7022(9) 0.0558(19) Uiso 0.50 1 d PG B 2 H61A H -0.2071 1.7530 1.7273 0.067 Uiso 0.50 1 calc PR B 2 C68 C -0.0052(14) 1.4293(9) 1.7343(10) 0.070(2) Uiso 0.50 1 d PGD B 2 C69 C -0.0307(14) 1.3202(11) 1.8042(8) 0.070(2) Uiso 0.50 1 d PG B 2 H69A H -0.0883 1.3087 1.8746 0.084 Uiso 0.50 1 calc PR B 2 C70 C 0.0280(15) 1.2279(8) 1.7712(9) 0.070(2) Uiso 0.50 1 d PG B 2 H70A H 0.0106 1.1534 1.8190 0.084 Uiso 0.50 1 calc PR B 2 C71 C 0.1123(14) 1.2447(8) 1.6683(10) 0.070(2) Uiso 0.50 1 d PG B 2 H71A H 0.1525 1.1816 1.6458 0.084 Uiso 0.50 1 calc PR B 2 C72 C 0.1379(14) 1.3538(10) 1.5984(8) 0.070(2) Uiso 0.50 1 d PG B 2 H72A H 0.1955 1.3652 1.5281 0.084 Uiso 0.50 1 calc PR B 2 C73 C 0.0791(15) 1.4461(7) 1.6314(9) 0.070(2) Uiso 0.50 1 d PG B 2 H73A H 0.0965 1.5206 1.5836 0.084 Uiso 0.50 1 calc PR B 2 C62 C -0.1077(9) 1.5752(7) 1.9592(6) 0.050(2) Uiso 1 1 d . . 2 H62A H -0.1833 1.6289 1.9333 0.060 Uiso 1 1 calc R . 2 C63 C -0.0267(9) 1.5127(7) 1.8959(6) 0.043(2) Uiso 1 1 d D B 2 C64 C 0.0820(9) 1.4381(7) 1.9400(7) 0.050(2) Uiso 1 1 d . . 2 H64A H 0.1423 1.3937 1.9001 0.060 Uiso 1 1 calc R . 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 0.0339(3) 0.0273(3) 0.0206(3) -0.0109(2) -0.0056(2) 0.0006(2) N1 0.039(4) 0.045(4) 0.027(3) -0.017(3) -0.009(3) 0.001(3) N2 0.042(4) 0.035(4) 0.026(4) -0.012(3) -0.004(3) -0.005(3) N3 0.050(4) 0.034(4) 0.034(4) -0.021(3) -0.012(3) 0.002(3) N4 0.039(4) 0.028(3) 0.027(4) -0.012(3) -0.007(3) -0.003(3) C1 0.031(4) 0.036(4) 0.020(4) -0.011(3) -0.003(3) 0.002(4) C2 0.048(5) 0.072(6) 0.052(5) -0.036(5) -0.022(4) -0.009(5) C3 0.036(4) 0.026(4) 0.028(4) -0.016(4) -0.009(4) 0.000(3) C4 0.049(5) 0.047(5) 0.020(4) -0.001(4) 0.000(4) -0.010(4) C5 0.056(5) 0.038(5) 0.020(4) -0.003(3) -0.005(4) -0.020(4) C6 0.044(5) 0.025(4) 0.024(4) -0.012(3) -0.005(4) 0.006(4) C7 0.071(6) 0.048(5) 0.058(6) -0.038(5) -0.030(5) 0.002(5) C8 0.063(6) 0.066(6) 0.076(7) -0.039(5) -0.022(5) -0.021(5) C9 0.040(5) 0.025(4) 0.030(5) -0.011(4) -0.011(4) -0.002(3) C10 0.071(6) 0.030(4) 0.014(4) 0.002(3) -0.015(4) -0.009(4) B1 0.013(7) 0.021(8) 0.017(8) -0.005(6) -0.011(6) -0.003(6) B2 0.030(10) 0.045(11) 0.017(9) 0.003(8) -0.001(7) -0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.945(8) . ? Rh1 C3 1.962(8) . ? Rh1 C9 1.964(8) . ? Rh1 C6 1.973(8) . ? N1 C1 1.169(9) . ? N1 C2 1.452(9) . ? N2 C3 1.149(8) . ? N2 C4 1.438(9) . ? N3 C6 1.154(9) . ? N3 C7 1.451(9) . ? N4 C9 1.153(8) . ? N4 C10 1.445(9) . ? C2 C8 1.485(12) 2_679 ? C4 C5 1.512(10) . ? C5 C10 1.509(10) 2_679 ? C7 C8 1.481(12) . ? C8 C2 1.485(12) 2_679 ? C10 C5 1.509(10) 2_679 ? B1 C23 1.666(5) . ? B1 C11 1.666(5) . ? B1 C29 1.667(5) . ? B1 C17 1.668(5) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C32 0.902(14) 2_678 ? C29 C33 1.279(12) 2_678 ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C33 0.902(10) 2_678 ? C30 C31 1.3900 . ? C30 C32 1.963(13) 2_678 ? C30 C34 2.032(14) 2_678 ? C31 C34 0.902(17) 2_678 ? C31 C33 1.168(12) 2_678 ? C31 C32 1.3900 . ? C32 C34 0.505(18) 2_678 ? C32 C29 0.902(10) 2_678 ? C32 C33 1.3900 . ? C32 C33 1.654(11) 2_678 ? C32 C30 1.96(2) 2_678 ? C33 C30 0.902(10) 2_678 ? C33 C31 1.168(19) 2_678 ? C33 C29 1.279(12) 2_678 ? C33 C34 1.3900 . ? C33 C32 1.654(14) 2_678 ? C33 C34 1.735(17) 2_678 ? C33 C33 1.887(10) 2_678 ? C34 C32 0.505(14) 2_678 ? C34 C31 0.902(14) 2_678 ? C34 C33 1.735(11) 2_678 ? C34 C30 2.032(16) 2_678 ? B2 C56 1.657(5) . ? B2 C63 1.660(5) . ? B2 C68 1.660(5) . ? B2 C50 1.662(5) . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C56 C57 1.3900 . ? C56 C61 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C60 C61 1.3900 . ? C68 C69 1.3900 . ? C68 C73 1.3900 . ? C69 C70 1.3900 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C62 C63 1.389(11) . ? C62 C64 1.406(11) 2_589 ? C63 C64 1.383(11) . ? C64 C62 1.406(11) 2_589 ? 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 C3 90.1(3) . . ? C1 Rh1 C9 89.4(3) . . ? C3 Rh1 C9 178.1(3) . . ? C1 Rh1 C6 177.4(3) . . ? C3 Rh1 C6 88.9(3) . . ? C9 Rh1 C6 91.4(3) . . ? C1 N1 C2 172.9(7) . . ? C3 N2 C4 176.3(7) . . ? C6 N3 C7 177.8(8) . . ? C9 N4 C10 176.8(7) . . ? N1 C1 Rh1 176.2(6) . . ? N1 C2 C8 112.0(7) . 2_679 ? N2 C3 Rh1 174.7(6) . . ? N2 C4 C5 112.1(6) . . ? C10 C5 C4 115.6(6) 2_679 . ? N3 C6 Rh1 174.9(6) . . ? N3 C7 C8 113.8(6) . . ? C7 C8 C2 118.1(8) . 2_679 ? N4 C9 Rh1 175.4(6) . . ? N4 C10 C5 112.3(6) . 2_679 ? C23 B1 C11 102.8(5) . . ? C23 B1 C29 111.1(5) . . ? C11 B1 C29 112.5(5) . . ? C23 B1 C17 113.1(5) . . ? C11 B1 C17 109.6(5) . . ? C29 B1 C17 107.9(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 B1 117.1(5) . . ? C16 C11 B1 122.9(5) . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 B1 118.2(5) . . ? C22 C17 B1 121.8(5) . . ? C19 C18 C17 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C24 C23 C28 120.0 . . ? C24 C23 B1 118.8(5) . . ? C28 C23 B1 120.7(5) . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C32 C29 C33 77.0(7) 2_678 2_678 ? C32 C29 C30 116.3(8) 2_678 . ? C33 C29 C30 39.2(4) 2_678 . ? C32 C29 C34 6.5(9) 2_678 . ? C33 C29 C34 81.0(5) 2_678 . ? C30 C29 C34 120.0 . . ? C32 C29 B1 126.9(10) 2_678 . ? C33 C29 B1 155.6(8) 2_678 . ? C30 C29 B1 116.7(6) . . ? C34 C29 B1 123.3(6) . . ? C33 C30 C31 56.5(8) 2_678 . ? C33 C30 C29 63.8(8) 2_678 . ? C31 C30 C29 120.0 . . ? C33 C30 C32 39.4(7) 2_678 2_678 ? C31 C30 C32 95.8(4) . 2_678 ? C29 C30 C32 24.3(4) . 2_678 ? C33 C30 C34 34.8(7) 2_678 2_678 ? C31 C30 C34 21.7(5) . 2_678 ? C29 C30 C34 98.4(5) . 2_678 ? C32 C30 C34 74.1(3) 2_678 2_678 ? C34 C31 C33 83.3(10) 2_678 2_678 ? C34 C31 C30 123.5(8) 2_678 . ? C33 C31 C30 40.1(5) 2_678 . ? C34 C31 C32 6.5(12) 2_678 . ? C33 C31 C32 80.1(5) 2_678 . ? C30 C31 C32 120.0 . . ? C34 C32 C29 162(3) 2_678 2_678 ? C34 C32 C31 12(2) 2_678 . ? C29 C32 C31 173.5(10) 2_678 . ? C34 C32 C33 125.9(13) 2_678 . ? C29 C32 C33 63.8(8) 2_678 . ? C31 C32 C33 120.0 . . ? C34 C32 C33 50.6(10) 2_678 2_678 ? C29 C32 C33 138.8(11) 2_678 2_678 ? C31 C32 C33 44.0(4) . 2_678 ? C33 C32 C33 76.1(4) . 2_678 ? C34 C32 C30 148(2) 2_678 2_678 ? C29 C32 C30 39.4(6) 2_678 2_678 ? C31 C32 C30 144.1(6) . 2_678 ? C33 C32 C30 24.3(6) . 2_678 ? C33 C32 C30 100.1(8) 2_678 2_678 ? C30 C33 C31 83.3(13) 2_678 2_678 ? C30 C33 C29 77.0(16) 2_678 2_678 ? C31 C33 C29 159.4(11) 2_678 2_678 ? C30 C33 C34 123.4(17) 2_678 . ? C31 C33 C34 40.1(8) 2_678 . ? C29 C33 C34 158.7(5) 2_678 . ? C30 C33 C32 116.3(17) 2_678 . ? C31 C33 C32 159.5(8) 2_678 . ? C29 C33 C32 39.2(5) 2_678 . ? C34 C33 C32 120.0 . . ? C30 C33 C32 138.8(18) 2_678 2_678 ? C31 C33 C32 55.9(6) 2_678 2_678 ? C29 C33 C32 142.4(8) 2_678 2_678 ? C34 C33 C32 16.3(4) . 2_678 ? C32 C33 C32 104.0(4) . 2_678 ? C30 C33 C34 129.1(16) 2_678 2_678 ? C31 C33 C34 145.9(9) 2_678 2_678 ? C29 C33 C34 52.3(4) 2_678 2_678 ? C34 C33 C34 106.6(4) . 2_678 ? C32 C33 C34 13.6(5) . 2_678 ? C32 C33 C34 90.5(5) 2_678 2_678 ? C30 C33 C33 170(2) 2_678 2_678 ? C31 C33 C33 101.4(8) 2_678 2_678 ? C29 C33 C33 97.1(6) 2_678 2_678 ? C34 C33 C33 61.8(4) . 2_678 ? C32 C33 C33 58.3(4) . 2_678 ? C32 C33 C33 45.6(2) 2_678 2_678 ? C34 C33 C33 44.9(3) 2_678 2_678 ? C32 C34 C31 162(3) 2_678 2_678 ? C32 C34 C33 113.1(14) 2_678 . ? C31 C34 C33 56.6(13) 2_678 . ? C32 C34 C29 11.8(17) 2_678 . ? C31 C34 C29 173.5(14) 2_678 . ? C33 C34 C29 120.0 . . ? C32 C34 C33 40.4(12) 2_678 2_678 ? C31 C34 C33 129.1(13) 2_678 2_678 ? C33 C34 C33 73.3(4) . 2_678 ? C29 C34 C33 46.7(4) . 2_678 ? C32 C34 C30 133.6(19) 2_678 2_678 ? C31 C34 C30 34.8(7) 2_678 2_678 ? C33 C34 C30 21.7(7) . 2_678 ? C29 C34 C30 141.5(7) . 2_678 ? C33 C34 C30 94.8(7) 2_678 2_678 ? C56 B2 C63 99.4(6) . . ? C56 B2 C68 114.0(7) . . ? C63 B2 C68 109.4(7) . . ? C56 B2 C50 111.6(6) . . ? C63 B2 C50 118.4(6) . . ? C68 B2 C50 104.5(7) . . ? C51 C50 C55 120.0 . . ? C51 C50 B2 120.6(6) . . ? C55 C50 B2 118.7(6) . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C50 120.0 . . ? C57 C56 C61 120.0 . . ? C57 C56 B2 117.7(7) . . ? C61 C56 B2 121.8(7) . . ? C56 C57 C58 120.0 . . ? C59 C58 C57 120.0 . . ? C58 C59 C60 120.0 . . ? C61 C60 C59 120.0 . . ? C60 C61 C56 120.0 . . ? C69 C68 C73 120.0 . . ? C69 C68 B2 115.2(8) . . ? C73 C68 B2 124.8(8) . . ? C70 C69 C68 120.0 . . ? C69 C70 C71 120.0 . . ? C70 C71 C72 120.0 . . ? C73 C72 C71 120.0 . . ? C72 C73 C68 120.0 . . ? C63 C62 C64 122.4(8) . 2_589 ? C64 C63 C62 114.3(7) . . ? C64 C63 B2 129.7(7) . . ? C62 C63 B2 115.9(7) . . ? C63 C64 C62 123.3(8) . 2_589 ? 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 C2 N1 C1 Rh1 -14(15) . . . . ? C3 Rh1 C1 N1 -86(10) . . . . ? C9 Rh1 C1 N1 92(10) . . . . ? C6 Rh1 C1 N1 -17(15) . . . . ? C1 N1 C2 C8 32(6) . . . 2_679 ? C4 N2 C3 Rh1 -27(17) . . . . ? C1 Rh1 C3 N2 105(7) . . . . ? C9 Rh1 C3 N2 29(14) . . . . ? C6 Rh1 C3 N2 -72(7) . . . . ? C3 N2 C4 C5 -14(12) . . . . ? N2 C4 C5 C10 70.1(8) . . . 2_679 ? C7 N3 C6 Rh1 -24(26) . . . . ? C1 Rh1 C6 N3 -12(13) . . . . ? C3 Rh1 C6 N3 57(7) . . . . ? C9 Rh1 C6 N3 -121(7) . . . . ? C6 N3 C7 C8 93(20) . . . . ? N3 C7 C8 C2 -72.5(10) . . . 2_679 ? C10 N4 C9 Rh1 -37(18) . . . . ? C1 Rh1 C9 N4 -79(8) . . . . ? C3 Rh1 C9 N4 -3(16) . . . . ? C6 Rh1 C9 N4 98(8) . . . . ? C9 N4 C10 C5 -9(12) . . . 2_679 ? C23 B1 C11 C12 59.6(6) . . . . ? C29 B1 C11 C12 179.1(5) . . . . ? C17 B1 C11 C12 -60.9(7) . . . . ? C23 B1 C11 C16 -118.7(6) . . . . ? C29 B1 C11 C16 0.9(8) . . . . ? C17 B1 C11 C16 120.8(6) . . . . ? C16 C11 C12 C13 0.0 . . . . ? B1 C11 C12 C13 -178.3(7) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? B1 C11 C16 C15 178.2(7) . . . . ? C23 B1 C17 C18 60.3(7) . . . . ? C11 B1 C17 C18 174.3(5) . . . . ? C29 B1 C17 C18 -63.0(6) . . . . ? C23 B1 C17 C22 -119.6(6) . . . . ? C11 B1 C17 C22 -5.6(7) . . . . ? C29 B1 C17 C22 117.1(6) . . . . ? C22 C17 C18 C19 0.0 . . . . ? B1 C17 C18 C19 -179.9(7) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C17 0.0 . . . . ? C18 C17 C22 C21 0.0 . . . . ? B1 C17 C22 C21 179.9(7) . . . . ? C11 B1 C23 C24 71.6(6) . . . . ? C29 B1 C23 C24 -48.8(7) . . . . ? C17 B1 C23 C24 -170.3(5) . . . . ? C11 B1 C23 C28 -100.6(6) . . . . ? C29 B1 C23 C28 139.0(5) . . . . ? C17 B1 C23 C28 17.5(7) . . . . ? C28 C23 C24 C25 0.0 . . . . ? B1 C23 C24 C25 -172.3(7) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C23 0.0 . . . . ? C24 C23 C28 C27 0.0 . . . . ? B1 C23 C28 C27 172.1(7) . . . . ? C23 B1 C29 C32 -3.1(17) . . . 2_678 ? C11 B1 C29 C32 -117.6(15) . . . 2_678 ? C17 B1 C29 C32 121.4(15) . . . 2_678 ? C23 B1 C29 C33 165(2) . . . 2_678 ? C11 B1 C29 C33 51(2) . . . 2_678 ? C17 B1 C29 C33 -70(2) . . . 2_678 ? C23 B1 C29 C30 172.0(5) . . . . ? C11 B1 C29 C30 57.4(6) . . . . ? C17 B1 C29 C30 -63.5(6) . . . . ? C23 B1 C29 C34 -9.8(8) . . . . ? C11 B1 C29 C34 -124.3(6) . . . . ? C17 B1 C29 C34 114.7(6) . . . . ? C32 C29 C30 C33 0.0(9) 2_678 . . 2_678 ? C34 C29 C30 C33 6.1(10) . . . 2_678 ? B1 C29 C30 C33 -175.6(14) . . . 2_678 ? C32 C29 C30 C31 -6.1(11) 2_678 . . . ? C33 C29 C30 C31 -6.1(10) 2_678 . . . ? C34 C29 C30 C31 0.0 . . . . ? B1 C29 C30 C31 178.3(6) . . . . ? C33 C29 C30 C32 0.0(9) 2_678 . . 2_678 ? C34 C29 C30 C32 6.1(11) . . . 2_678 ? B1 C29 C30 C32 -175.6(15) . . . 2_678 ? C32 C29 C30 C34 -3.6(11) 2_678 . . 2_678 ? C33 C29 C30 C34 -3.6(7) 2_678 . . 2_678 ? C34 C29 C30 C34 2.4(6) . . . 2_678 ? B1 C29 C30 C34 -179.2(7) . . . 2_678 ? C33 C30 C31 C34 0.0(11) 2_678 . . 2_678 ? C29 C30 C31 C34 6.5(16) . . . 2_678 ? C32 C30 C31 C34 4.0(15) 2_678 . . 2_678 ? C29 C30 C31 C33 6.5(11) . . . 2_678 ? C32 C30 C31 C33 4.0(9) 2_678 . . 2_678 ? C34 C30 C31 C33 0.0(11) 2_678 . . 2_678 ? C33 C30 C31 C32 -6.5(11) 2_678 . . . ? C29 C30 C31 C32 0.0 . . . . ? C32 C30 C31 C32 -2.5(5) 2_678 . . . ? C34 C30 C31 C32 -6.5(16) 2_678 . . . ? C33 C31 C32 C34 119(9) 2_678 . . 2_678 ? C30 C31 C32 C34 123(9) . . . 2_678 ? C34 C31 C32 C29 0(4) 2_678 . . 2_678 ? C33 C31 C32 C29 119(8) 2_678 . . 2_678 ? C30 C31 C32 C29 123(8) . . . 2_678 ? C34 C31 C32 C33 -123(9) 2_678 . . . ? C33 C31 C32 C33 -4.3(7) 2_678 . . . ? C30 C31 C32 C33 0.0 . . . . ? C34 C31 C32 C33 -119(9) 2_678 . . 2_678 ? C30 C31 C32 C33 4.3(7) . . . 2_678 ? C34 C31 C32 C30 -119(9) 2_678 . . 2_678 ? C33 C31 C32 C30 0.0(14) 2_678 . . 2_678 ? C30 C31 C32 C30 4.3(15) . . . 2_678 ? C34 C32 C33 C30 162(5) 2_678 . . 2_678 ? C29 C32 C33 C30 0.0(13) 2_678 . . 2_678 ? C31 C32 C33 C30 174(2) . . . 2_678 ? C33 C32 C33 C30 171(2) 2_678 . . 2_678 ? C34 C32 C33 C31 0(4) 2_678 . . 2_678 ? C29 C32 C33 C31 -162(4) 2_678 . . 2_678 ? C31 C32 C33 C31 12(3) . . . 2_678 ? C33 C32 C33 C31 9(3) 2_678 . . 2_678 ? C30 C32 C33 C31 -162(5) 2_678 . . 2_678 ? C34 C32 C33 C29 162(4) 2_678 . . 2_678 ? C31 C32 C33 C29 173.9(11) . . . 2_678 ? C33 C32 C33 C29 170.9(16) 2_678 . . 2_678 ? C30 C32 C33 C29 0.0(13) 2_678 . . 2_678 ? C34 C32 C33 C34 -12(3) 2_678 . . . ? C29 C32 C33 C34 -173.9(11) 2_678 . . . ? C31 C32 C33 C34 0.0 . . . . ? C33 C32 C33 C34 -3.1(5) 2_678 . . . ? C30 C32 C33 C34 -174(2) 2_678 . . . ? C34 C32 C33 C32 -9(3) 2_678 . . 2_678 ? C29 C32 C33 C32 -170.9(16) 2_678 . . 2_678 ? C31 C32 C33 C32 3.1(6) . . . 2_678 ? C33 C32 C33 C32 0.0(5) 2_678 . . 2_678 ? C30 C32 C33 C32 -171(2) 2_678 . . 2_678 ? C29 C32 C33 C34 -162(4) 2_678 . . 2_678 ? C31 C32 C33 C34 12(3) . . . 2_678 ? C33 C32 C33 C34 9(3) 2_678 . . 2_678 ? C30 C32 C33 C34 -162(5) 2_678 . . 2_678 ? C34 C32 C33 C33 -9(3) 2_678 . . 2_678 ? C29 C32 C33 C33 -170.9(16) 2_678 . . 2_678 ? C31 C32 C33 C33 3.1(5) . . . 2_678 ? C30 C32 C33 C33 -171(2) 2_678 . . 2_678 ? C30 C33 C34 C32 -163(4) 2_678 . . 2_678 ? C31 C33 C34 C32 -163(4) 2_678 . . 2_678 ? C29 C33 C34 C32 0.0(14) 2_678 . . 2_678 ? C32 C33 C34 C32 10.6(19) . . . 2_678 ? C34 C33 C34 C32 7.7(19) 2_678 . . 2_678 ? C33 C33 C34 C32 7.7(17) 2_678 . . 2_678 ? C30 C33 C34 C31 0.0(10) 2_678 . . 2_678 ? C29 C33 C34 C31 163(3) 2_678 . . 2_678 ? C32 C33 C34 C31 173.5(18) . . . 2_678 ? C32 C33 C34 C31 163(4) 2_678 . . 2_678 ? C34 C33 C34 C31 171(2) 2_678 . . 2_678 ? C33 C33 C34 C31 171(2) 2_678 . . 2_678 ? C30 C33 C34 C29 -173(2) 2_678 . . . ? C31 C33 C34 C29 -173.5(18) 2_678 . . . ? C29 C33 C34 C29 -10.6(19) 2_678 . . . ? C32 C33 C34 C29 0.0 . . . . ? C32 C33 C34 C29 -11(2) 2_678 . . . ? C34 C33 C34 C29 -3.0(7) 2_678 . . . ? C33 C33 C34 C29 -3.0(5) 2_678 . . . ? C30 C33 C34 C33 -171(2) 2_678 . . 2_678 ? C31 C33 C34 C33 -171(2) 2_678 . . 2_678 ? C29 C33 C34 C33 -7.7(16) 2_678 . . 2_678 ? C32 C33 C34 C33 3.0(5) . . . 2_678 ? C32 C33 C34 C33 -7.7(17) 2_678 . . 2_678 ? C34 C33 C34 C33 0.0(5) 2_678 . . 2_678 ? C31 C33 C34 C30 0.0(11) 2_678 . . 2_678 ? C29 C33 C34 C30 163(4) 2_678 . . 2_678 ? C32 C33 C34 C30 173(2) . . . 2_678 ? C32 C33 C34 C30 163(4) 2_678 . . 2_678 ? C34 C33 C34 C30 171(3) 2_678 . . 2_678 ? C33 C33 C34 C30 171(2) 2_678 . . 2_678 ? C33 C29 C34 C32 -53(7) 2_678 . . 2_678 ? C30 C29 C34 C32 -57(7) . . . 2_678 ? B1 C29 C34 C32 125(8) . . . 2_678 ? C32 C29 C34 C31 0(8) 2_678 . . 2_678 ? C33 C29 C34 C31 -53(12) 2_678 . . 2_678 ? C30 C29 C34 C31 -57(12) . . . 2_678 ? B1 C29 C34 C31 125(12) . . . 2_678 ? C32 C29 C34 C33 57(7) 2_678 . . . ? C33 C29 C34 C33 3.9(7) 2_678 . . . ? C30 C29 C34 C33 0.0 . . . . ? B1 C29 C34 C33 -178.2(7) . . . . ? C32 C29 C34 C33 53(7) 2_678 . . 2_678 ? C30 C29 C34 C33 -3.9(7) . . . 2_678 ? B1 C29 C34 C33 177.9(11) . . . 2_678 ? C32 C29 C34 C30 53(7) 2_678 . . 2_678 ? C33 C29 C34 C30 0.0(13) 2_678 . . 2_678 ? C30 C29 C34 C30 -3.9(14) . . . 2_678 ? B1 C29 C34 C30 177.9(13) . . . 2_678 ? C56 B2 C50 C51 -142.5(7) . . . . ? C63 B2 C50 C51 -28.1(9) . . . . ? C68 B2 C50 C51 93.9(8) . . . . ? C56 B2 C50 C55 47.4(9) . . . . ? C63 B2 C50 C55 161.7(6) . . . . ? C68 B2 C50 C55 -76.3(8) . . . . ? C55 C50 C51 C52 0.0 . . . . ? B2 C50 C51 C52 -170.0(8) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? B2 C50 C55 C54 170.2(8) . . . . ? C63 B2 C56 C57 72.7(8) . . . . ? C68 B2 C56 C57 -43.6(10) . . . . ? C50 B2 C56 C57 -161.6(6) . . . . ? C63 B2 C56 C61 -98.7(7) . . . . ? C68 B2 C56 C61 145.1(8) . . . . ? C50 B2 C56 C61 27.0(10) . . . . ? C61 C56 C57 C58 0.0 . . . . ? B2 C56 C57 C58 -171.5(9) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C56 0.0 . . . . ? C57 C56 C61 C60 0.0 . . . . ? B2 C56 C61 C60 171.2(10) . . . . ? C56 B2 C68 C69 163.9(7) . . . . ? C63 B2 C68 C69 53.6(9) . . . . ? C50 B2 C68 C69 -74.1(8) . . . . ? C56 B2 C68 C73 -16.0(11) . . . . ? C63 B2 C68 C73 -126.3(8) . . . . ? C50 B2 C68 C73 106.0(8) . . . . ? C73 C68 C69 C70 0.0 . . . . ? B2 C68 C69 C70 -179.9(10) . . . . ? C68 C69 C70 C71 0.0 . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C68 0.0 . . . . ? C69 C68 C73 C72 0.0 . . . . ? B2 C68 C73 C72 179.9(11) . . . . ? C64 C62 C63 C64 -0.9(13) 2_589 . . . ? C64 C62 C63 B2 175.2(7) 2_589 . . . ? C56 B2 C63 C64 -109.6(9) . . . . ? C68 B2 C63 C64 10.1(11) . . . . ? C50 B2 C63 C64 129.5(9) . . . . ? C56 B2 C63 C62 74.9(8) . . . . ? C68 B2 C63 C62 -165.4(8) . . . . ? C50 B2 C63 C62 -45.9(10) . . . . ? C62 C63 C64 C62 0.9(13) . . . 2_589 ? B2 C63 C64 C62 -174.6(7) . . . 2_589 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.897 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.108