# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email martin.albrecht@ucd.ie _publ_contact_author_name 'Martin Albrecht' loop_ _publ_author_name 'Anneke Kruger' 'Jonas Larsson' 'Helge Muller-Bunz' 'Olha Serada' 'Antonia Neels' 'Stuart Macgregor' 'Martin Albrecht' data_complex-3b _database_code_depnum_ccdc_archive 'CCDC 817392' #TrackingRef '- allComplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.50 H85 Cl F6 I3 N8 O0 P Rh2' _chemical_formula_weight 1739.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 26.7628(17) _cell_length_b 26.7351(18) _cell_length_c 20.3079(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14530.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17228 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 23.97 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6904 _exptl_absorpt_coefficient_mu 1.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57955 _diffrn_reflns_av_R_equivalents 0.1184 _diffrn_reflns_av_sigmaI/netI 0.1387 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.24 _reflns_number_total 12927 _reflns_number_gt 4389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12927 _refine_ls_number_parameters 386 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.2121 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.1977 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0567(8) -0.0346(6) 0.3109(7) 0.1075(15) Uani 1 1 d . . . C2 C 0.0661(7) -0.0156(6) 0.3719(7) 0.1075(15) Uani 1 1 d . . . H2A H 0.0493 0.0115 0.3924 0.129 Uiso 1 1 calc R . . C3 C 0.1185(8) -0.0807(6) 0.3574(7) 0.1075(15) Uani 1 1 d . . . C4 C 0.0902(7) -0.1023(6) 0.2430(6) 0.1075(15) Uani 1 1 d . . . H4A H 0.0976 -0.1381 0.2513 0.129 Uiso 1 1 calc R . . H4B H 0.1168 -0.0883 0.2146 0.129 Uiso 1 1 calc R . . C5 C 0.0368(8) -0.0961(6) 0.2091(7) 0.1075(15) Uani 1 1 d . . . H5 H 0.0413 -0.0965 0.1602 0.129 Uiso 1 1 calc R . . C6 C -0.0004(8) -0.1364(6) 0.2278(7) 0.1075(15) Uani 1 1 d . . . H6A H -0.0214 -0.1450 0.1893 0.129 Uiso 1 1 calc R . . H6B H 0.0175 -0.1669 0.2420 0.129 Uiso 1 1 calc R . . C7 C -0.0364(8) -0.0654(6) 0.2903(6) 0.1075(15) Uani 1 1 d . . . C8 C -0.0739(7) -0.0615(6) 0.3391(7) 0.1075(15) Uani 1 1 d . . . H8A H -0.0860 -0.0316 0.3589 0.129 Uiso 1 1 calc R . . C9 C -0.0668(8) -0.1429(6) 0.3170(7) 0.1075(15) Uani 1 1 d . . . C10 C 0.1249(9) -0.0396(7) 0.4648(8) 0.118(2) Uani 1 1 d . . . C11 C 0.1618(9) -0.0066(8) 0.4773(8) 0.118(2) Uani 1 1 d . . . C12 C 0.1810(8) -0.0031(7) 0.5423(8) 0.118(2) Uani 1 1 d . . . H12A H 0.2076 0.0192 0.5525 0.142 Uiso 1 1 calc R . . C13 C 0.1595(8) -0.0338(7) 0.5913(8) 0.118(2) Uani 1 1 d . . . C14 C 0.1242(8) -0.0651(7) 0.5762(8) 0.118(2) Uani 1 1 d . . . H14A H 0.1122 -0.0866 0.6100 0.142 Uiso 1 1 calc R . . C15 C 0.1024(8) -0.0693(7) 0.5138(8) 0.118(2) Uani 1 1 d . . . C16 C 0.1819(8) 0.0275(7) 0.4260(8) 0.118(2) Uani 1 1 d . . . H16A H 0.1973 0.0077 0.3908 0.177 Uiso 1 1 calc R . . H16B H 0.2070 0.0495 0.4457 0.177 Uiso 1 1 calc R . . H16C H 0.1546 0.0477 0.4078 0.177 Uiso 1 1 calc R . . C17 C 0.1818(8) -0.0298(7) 0.6611(8) 0.118(2) Uani 1 1 d . . . H17A H 0.1898 -0.0633 0.6776 0.177 Uiso 1 1 calc R . . H17B H 0.1574 -0.0139 0.6905 0.177 Uiso 1 1 calc R . . H17C H 0.2123 -0.0095 0.6597 0.177 Uiso 1 1 calc R . . C18 C 0.0618(8) -0.1056(7) 0.4991(8) 0.118(2) Uani 1 1 d . . . H18A H 0.0356 -0.0889 0.4737 0.177 Uiso 1 1 calc R . . H18B H 0.0478 -0.1181 0.5405 0.177 Uiso 1 1 calc R . . H18C H 0.0754 -0.1336 0.4736 0.177 Uiso 1 1 calc R . . C19 C 0.1555(7) -0.1206(6) 0.3669(6) 0.1075(15) Uani 1 1 d . . . H19A H 0.1389 -0.1502 0.3851 0.161 Uiso 1 1 calc R . . H19B H 0.1814 -0.1092 0.3975 0.161 Uiso 1 1 calc R . . H19C H 0.1708 -0.1291 0.3245 0.161 Uiso 1 1 calc R . . C20 C -0.1298(9) -0.1218(8) 0.3974(9) 0.134(3) Uani 1 1 d . . . C21 C -0.1188(9) -0.1336(8) 0.4646(9) 0.134(3) Uani 1 1 d . . . C22 C -0.1595(9) -0.1461(8) 0.5056(10) 0.134(3) Uani 1 1 d . . . H22A H -0.1532 -0.1554 0.5500 0.161 Uiso 1 1 calc R . . C23 C -0.2064(10) -0.1454(8) 0.4842(10) 0.134(3) Uani 1 1 d . . . C24 C -0.2166(9) -0.1389(7) 0.4207(9) 0.134(3) Uani 1 1 d . . . H24A H -0.2499 -0.1428 0.4051 0.161 Uiso 1 1 calc R . . C25 C -0.1784(10) -0.1262(8) 0.3768(9) 0.134(3) Uani 1 1 d . . . C26 C -0.0662(8) -0.1265(8) 0.4879(8) 0.134(3) Uani 1 1 d . . . H26A H -0.0432 -0.1438 0.4579 0.201 Uiso 1 1 calc R . . H26B H -0.0627 -0.1404 0.5323 0.201 Uiso 1 1 calc R . . H26C H -0.0582 -0.0907 0.4887 0.201 Uiso 1 1 calc R . . C27 C -0.2446(8) -0.1648(8) 0.5318(8) 0.134(3) Uani 1 1 d . . . H27A H -0.2781 -0.1583 0.5146 0.201 Uiso 1 1 calc R . . H27B H -0.2406 -0.1479 0.5743 0.201 Uiso 1 1 calc R . . H27C H -0.2399 -0.2009 0.5377 0.201 Uiso 1 1 calc R . . C28 C -0.1912(8) -0.1134(8) 0.3035(8) 0.134(3) Uani 1 1 d . . . H28A H -0.1603 -0.1074 0.2789 0.201 Uiso 1 1 calc R . . H28B H -0.2122 -0.0834 0.3020 0.201 Uiso 1 1 calc R . . H28C H -0.2093 -0.1415 0.2836 0.201 Uiso 1 1 calc R . . C29 C -0.0706(9) -0.1997(6) 0.3182(10) 0.143(8) Uani 1 1 d . . . H29A H -0.0404 -0.2143 0.2987 0.214 Uiso 1 1 calc R . . H29B H -0.0999 -0.2103 0.2928 0.214 Uiso 1 1 calc R . . H29C H -0.0740 -0.2112 0.3638 0.214 Uiso 1 1 calc R . . C30 C 0.0181(8) 0.1350(6) 0.1260(7) 0.1177(17) Uani 1 1 d . . . C31 C 0.0605(8) 0.1911(7) 0.0626(7) 0.1177(17) Uani 1 1 d . . . C32 C 0.0331(8) 0.1718(6) 0.1632(7) 0.1177(17) Uani 1 1 d . . . H32A H 0.0278 0.1740 0.2093 0.141 Uiso 1 1 calc R . . C33 C 0.0817(11) 0.2535(8) 0.1445(8) 0.130(3) Uani 1 1 d . . . C34 C 0.0557(10) 0.2963(8) 0.1528(8) 0.130(3) Uani 1 1 d . . . C35 C 0.0801(10) 0.3390(8) 0.1747(8) 0.130(3) Uani 1 1 d . . . H35A H 0.0613 0.3688 0.1809 0.156 Uiso 1 1 calc R . . C36 C 0.1289(11) 0.3396(8) 0.1873(8) 0.130(3) Uani 1 1 d . . . C37 C 0.1562(10) 0.2963(7) 0.1783(8) 0.130(3) Uani 1 1 d . . . H37A H 0.1910 0.2964 0.1875 0.156 Uiso 1 1 calc R . . C38 C 0.1340(11) 0.2532(8) 0.1562(8) 0.130(3) Uani 1 1 d . . . C39 C 0.1655(8) 0.2057(7) 0.1469(8) 0.130(3) Uani 1 1 d . . . H39A H 0.1767 0.1935 0.1899 0.196 Uiso 1 1 calc R . . H39B H 0.1947 0.2134 0.1195 0.196 Uiso 1 1 calc R . . H39C H 0.1453 0.1799 0.1253 0.196 Uiso 1 1 calc R . . C40 C 0.1552(9) 0.3866(7) 0.2118(8) 0.130(3) Uani 1 1 d . . . H40A H 0.1303 0.4104 0.2286 0.196 Uiso 1 1 calc R . . H40B H 0.1736 0.4020 0.1754 0.196 Uiso 1 1 calc R . . H40C H 0.1785 0.3778 0.2471 0.196 Uiso 1 1 calc R . . C41 C 0.0009(9) 0.2954(7) 0.1387(8) 0.130(3) Uani 1 1 d . . . H41A H -0.0047 0.2829 0.0940 0.196 Uiso 1 1 calc R . . H41B H -0.0126 0.3293 0.1426 0.196 Uiso 1 1 calc R . . H41C H -0.0158 0.2734 0.1704 0.196 Uiso 1 1 calc R . . C42 C 0.0816(8) 0.2153(6) 0.0036(6) 0.1177(17) Uani 1 1 d . . . H42A H 0.0897 0.2503 0.0137 0.177 Uiso 1 1 calc R . . H42B H 0.0572 0.2142 -0.0323 0.177 Uiso 1 1 calc R . . H42C H 0.1121 0.1977 -0.0099 0.177 Uiso 1 1 calc R . . C43 C 0.0275(8) 0.1133(6) 0.0080(7) 0.1177(17) Uani 1 1 d . . . H43A H 0.0602 0.1010 -0.0077 0.141 Uiso 1 1 calc R . . H43B H 0.0107 0.1307 -0.0289 0.141 Uiso 1 1 calc R . . C44 C -0.0041(8) 0.0701(6) 0.0311(7) 0.1177(17) Uani 1 1 d . . . H44 H 0.0129 0.0384 0.0176 0.141 Uiso 1 1 calc R . . C45 C -0.0554(8) 0.0709(7) -0.0005(7) 0.1177(17) Uani 1 1 d . . . H45A H -0.0538 0.0886 -0.0432 0.141 Uiso 1 1 calc R . . H45B H -0.0669 0.0363 -0.0087 0.141 Uiso 1 1 calc R . . C46 C -0.0758(8) 0.0971(6) 0.1101(7) 0.1177(17) Uani 1 1 d . . . C47 C -0.1171(8) 0.1211(6) 0.1382(7) 0.1177(17) Uani 1 1 d . A . H47A H -0.1204 0.1295 0.1834 0.141 Uiso 1 1 calc R . . C48 C -0.1354(9) 0.1130(7) 0.0330(7) 0.1177(17) Uani 1 1 d . A . C49 C -0.1624(8) 0.1144(6) -0.0342(6) 0.1177(17) Uani 1 1 d . . . H49A H -0.1583 0.1476 -0.0540 0.177 Uiso 1 1 calc R . . H49B H -0.1981 0.1076 -0.0277 0.177 Uiso 1 1 calc R . . H49C H -0.1480 0.0890 -0.0633 0.177 Uiso 1 1 calc R . . C50 C -0.2174(12) 0.1356(9) 0.1128(8) 0.134(6) Uani 0.50 1 d PD A 1 C50A C -0.1952(11) 0.1649(10) 0.0980(12) 0.133(5) Uani 0.50 1 d PD A 2 C51 C -0.2473(12) 0.0966(10) 0.1328(12) 0.134(6) Uani 0.50 1 d PD A 1 C51A C -0.2311(10) 0.1318(10) 0.1182(8) 0.133(5) Uani 0.50 1 d PD A 2 C52 C -0.2963(12) 0.1084(11) 0.1423(14) 0.134(6) Uani 0.50 1 d PD A 1 H52A H -0.3178 0.0825 0.1569 0.161 Uiso 0.50 1 calc PR A 1 C52A C -0.2716(12) 0.1622(10) 0.1369(18) 0.133(5) Uani 0.50 1 d PD A 2 H52B H -0.2964 0.1455 0.1621 0.159 Uiso 0.50 1 calc PR A 2 C53 C -0.3170(11) 0.1547(11) 0.1324(15) 0.134(6) Uani 0.50 1 d PD A 1 C53A C -0.2816(11) 0.2120(11) 0.1250(19) 0.133(5) Uani 0.50 1 d PD A 2 C54 C -0.2844(12) 0.1895(13) 0.1065(16) 0.134(6) Uani 0.50 1 d PD A 1 H54A H -0.2964 0.2227 0.1013 0.161 Uiso 0.50 1 calc PR A 1 C54A C -0.2391(10) 0.2349(12) 0.1006(18) 0.133(5) Uani 0.50 1 d PD A 2 H54B H -0.2436 0.2686 0.0872 0.159 Uiso 0.50 1 calc PR A 2 C55 C -0.2355(12) 0.1801(11) 0.0872(15) 0.134(6) Uani 0.50 1 d PD A 1 C55A C -0.1910(11) 0.2164(11) 0.0924(19) 0.133(5) Uani 0.50 1 d PD A 2 C56 C -0.2261(16) 0.0453(11) 0.1485(16) 0.134(6) Uani 0.50 1 d PD A 1 H56A H -0.2168 0.0439 0.1951 0.201 Uiso 0.50 1 calc PR A 1 H56B H -0.1965 0.0393 0.1213 0.201 Uiso 0.50 1 calc PR A 1 H56C H -0.2513 0.0197 0.1392 0.201 Uiso 0.50 1 calc PR A 1 C56A C -0.2309(16) 0.0784(10) 0.1379(19) 0.133(5) Uani 0.50 1 d PD A 2 H56D H -0.2249 0.0575 0.0991 0.199 Uiso 0.50 1 calc PR A 2 H56E H -0.2634 0.0698 0.1573 0.199 Uiso 0.50 1 calc PR A 2 H56F H -0.2045 0.0727 0.1704 0.199 Uiso 0.50 1 calc PR A 2 C57 C -0.3718(12) 0.1628(13) 0.1473(15) 0.134(6) Uani 0.50 1 d PD A 1 H57A H -0.3920 0.1426 0.1172 0.201 Uiso 0.50 1 calc PR A 1 H57B H -0.3801 0.1982 0.1415 0.201 Uiso 0.50 1 calc PR A 1 H57C H -0.3787 0.1529 0.1929 0.201 Uiso 0.50 1 calc PR A 1 C57A C -0.3309(12) 0.2373(14) 0.1344(17) 0.133(5) Uani 0.50 1 d PD A 2 H57D H -0.3307 0.2557 0.1761 0.199 Uiso 0.50 1 calc PR A 2 H57E H -0.3575 0.2121 0.1353 0.199 Uiso 0.50 1 calc PR A 2 H57F H -0.3368 0.2606 0.0980 0.199 Uiso 0.50 1 calc PR A 2 C58 C -0.2013(14) 0.2175(12) 0.0551(15) 0.134(6) Uani 0.50 1 d PD A 1 H58A H -0.1927 0.2437 0.0868 0.201 Uiso 0.50 1 calc PR A 1 H58B H -0.2182 0.2325 0.0171 0.201 Uiso 0.50 1 calc PR A 1 H58C H -0.1708 0.2006 0.0404 0.201 Uiso 0.50 1 calc PR A 1 C58A C -0.1480(12) 0.2447(12) 0.0632(18) 0.133(5) Uani 0.50 1 d PD A 2 H58D H -0.1165 0.2309 0.0798 0.199 Uiso 0.50 1 calc PR A 2 H58E H -0.1504 0.2800 0.0756 0.199 Uiso 0.50 1 calc PR A 2 H58F H -0.1489 0.2417 0.0151 0.199 Uiso 0.50 1 calc PR A 2 C59 C 0.1609(12) 0.0498(10) 0.0001(12) 0.069(7) Uiso 0.50 1 d P . . H59A H 0.1278 0.0401 0.0178 0.083 Uiso 0.50 1 calc PR . . H59B H 0.1571 0.0566 -0.0475 0.083 Uiso 0.50 1 calc PR . . Cl1 Cl 0.1978(8) 0.0070(6) 0.0102(7) 0.212(7) Uani 0.50 1 d P . . Cl2 Cl 0.1811(5) 0.1028(4) 0.0390(6) 0.143(4) Uani 0.50 1 d P . . F1 F -0.0467(14) 0.2929(10) -0.1354(14) 0.213(4) Uani 0.50 1 d PD B 1 F1A F -0.0276(11) 0.2904(10) -0.0707(15) 0.213(4) Uani 0.50 1 d PD B 2 F2 F -0.0273(12) 0.2691(11) -0.0394(14) 0.213(4) Uani 0.50 1 d PD B 1 F2A F -0.0512(16) 0.2242(11) -0.0249(14) 0.213(4) Uani 0.50 1 d PD B 2 F3 F -0.0635(15) 0.1969(10) -0.0450(16) 0.213(4) Uani 0.50 1 d PD B 1 F3A F -0.0800(15) 0.1907(10) -0.1125(15) 0.213(4) Uani 0.50 1 d PD B 2 F4 F -0.0872(16) 0.2121(11) -0.1488(15) 0.213(4) Uani 0.50 1 d PD B 1 F4A F -0.0555(15) 0.2567(11) -0.1741(14) 0.213(4) Uani 0.50 1 d PD B 2 F5 F -0.0029(9) 0.2201(5) -0.1160(7) 0.213(4) Uani 1 1 d . B . F6 F -0.1075(9) 0.2655(5) -0.0824(7) 0.213(4) Uani 1 1 d . B . I1 I -0.02926(5) 0.06745(4) 0.27050(4) 0.0933(4) Uani 1 1 d . . . I2 I -0.05859(5) -0.02598(4) 0.13351(4) 0.0998(4) Uani 1 1 d . . . I3 I 0.07881(5) 0.02195(5) 0.15639(5) 0.1089(5) Uani 1 1 d . . . N1 N 0.1059(6) -0.0444(5) 0.3990(5) 0.1075(15) Uani 1 1 d . . . N2 N 0.0871(6) -0.0753(5) 0.3036(5) 0.1075(15) Uani 1 1 d . . . N3 N -0.0897(6) -0.1102(5) 0.3523(5) 0.1075(15) Uani 1 1 d . . . N4 N -0.0323(6) -0.1180(5) 0.2820(5) 0.1075(15) Uani 1 1 d . . . N5 N 0.0345(7) 0.1476(5) 0.0626(6) 0.1177(17) Uani 1 1 d . . . N6 N 0.0584(7) 0.2080(5) 0.1247(5) 0.1177(17) Uani 1 1 d . . . N7 N -0.0901(7) 0.0961(5) 0.0426(6) 0.1177(17) Uani 1 1 d . . . N8 N -0.1532(7) 0.1308(5) 0.0893(5) 0.1177(17) Uani 1 1 d . . . P1 P -0.0549(4) 0.2437(2) -0.0986(3) 0.179(4) Uani 1 1 d . . . Rh1 Rh 0.00950(6) -0.02665(5) 0.23693(5) 0.0965(5) Uani 1 1 d . . . Rh2 Rh -0.01299(6) 0.06852(5) 0.13250(5) 0.0944(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C2 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C3 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C4 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C5 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C6 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C7 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C8 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C9 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C10 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C11 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C12 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C13 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C14 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C15 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C16 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C17 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C18 0.138(7) 0.123(6) 0.094(4) 0.003(4) -0.013(4) -0.001(4) C19 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) C20 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C21 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C22 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C23 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C24 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C25 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C26 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C27 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C28 0.141(9) 0.159(5) 0.102(5) -0.021(4) 0.008(5) 0.003(6) C29 0.18(3) 0.098(14) 0.152(17) -0.003(12) 0.058(15) -0.004(14) C30 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C31 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C32 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C33 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C34 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C35 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C36 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C37 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C38 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C39 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C40 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C41 0.201(10) 0.102(5) 0.088(4) 0.009(4) 0.019(5) -0.005(7) C42 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C43 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C44 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C45 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C46 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C47 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C48 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C49 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) C50 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C50A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C51 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C51A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C52 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C52A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C53 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C53A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C54 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C54A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C55 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C55A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C56 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C56A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C57 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C57A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) C58 0.190(19) 0.124(11) 0.089(8) -0.001(7) -0.048(10) 0.039(12) C58A 0.126(15) 0.143(12) 0.129(11) -0.010(10) 0.018(9) 0.061(11) Cl1 0.31(2) 0.163(11) 0.161(11) -0.034(9) 0.062(12) -0.035(13) Cl2 0.140(11) 0.122(8) 0.167(9) -0.027(7) 0.018(7) 0.014(7) F1 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F1A 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F2 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F2A 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F3 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F3A 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F4 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F4A 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F5 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) F6 0.361(12) 0.122(6) 0.155(7) 0.011(5) -0.018(7) 0.025(7) I1 0.1443(11) 0.0804(6) 0.0550(4) -0.0004(5) 0.0062(5) 0.0170(7) I2 0.1535(12) 0.0859(7) 0.0601(5) -0.0004(5) 0.0008(6) 0.0181(7) I3 0.1391(12) 0.1204(9) 0.0671(5) 0.0047(6) 0.0100(6) 0.0225(8) N1 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) N2 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) N3 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) N4 0.162(5) 0.093(3) 0.068(2) -0.001(2) 0.005(2) 0.038(3) N5 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) N6 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) N7 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) N8 0.187(6) 0.103(3) 0.064(2) 0.005(2) 0.011(3) 0.026(3) P1 0.343(14) 0.074(4) 0.120(5) 0.002(3) -0.049(7) 0.009(6) Rh1 0.1481(14) 0.0870(8) 0.0545(6) 0.0035(6) 0.0071(7) 0.0298(9) Rh2 0.1430(14) 0.0847(8) 0.0554(6) 0.0033(6) 0.0044(7) 0.0198(9) _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 C1 C2 1.362(19) . ? C1 N2 1.367(18) . ? C1 Rh1 1.974(17) . ? C2 N1 1.43(2) . ? C2 H2A 0.9500 . ? C3 N1 1.331(17) . ? C3 N2 1.39(2) . ? C3 C19 1.47(2) . ? C4 N2 1.428(16) . ? C4 C5 1.59(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.52(2) . ? C5 Rh1 2.075(15) . ? C5 H5 1.0000 . ? C6 N4 1.477(19) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.41(2) . ? C7 N4 1.420(18) . ? C7 Rh1 1.939(18) . ? C8 N3 1.39(2) . ? C8 H8A 0.9500 . ? C9 N3 1.286(18) . ? C9 N4 1.34(2) . ? C9 C29 1.52(2) . ? C10 C11 1.35(3) . ? C10 C15 1.41(2) . ? C10 N1 1.44(2) . ? C11 C12 1.42(2) . ? C11 C16 1.48(2) . ? C12 C13 1.41(2) . ? C12 H12A 0.9500 . ? C13 C14 1.30(2) . ? C13 C17 1.54(2) . ? C14 C15 1.40(2) . ? C14 H14A 0.9500 . ? C15 C18 1.49(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.37(3) . ? C20 C21 1.43(3) . ? C20 N3 1.44(2) . ? C21 C22 1.41(3) . ? C21 C26 1.50(3) . ? C22 C23 1.33(3) . ? C22 H22A 0.9500 . ? C23 C24 1.33(2) . ? C23 C27 1.50(3) . ? C24 C25 1.40(3) . ? C24 H24A 0.9500 . ? C25 C28 1.57(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.30(2) . ? C30 N5 1.402(18) . ? C30 Rh2 1.965(19) . ? C31 N6 1.342(17) . ? C31 N5 1.35(2) . ? C31 C42 1.47(2) . ? C32 N6 1.42(2) . ? C32 H32A 0.9500 . ? C33 C34 1.35(3) . ? C33 C38 1.42(3) . ? C33 N6 1.42(2) . ? C34 C35 1.39(3) . ? C34 C41 1.49(3) . ? C35 C36 1.33(3) . ? C35 H35A 0.9500 . ? C36 C37 1.38(3) . ? C36 C40 1.52(3) . ? C37 C38 1.37(3) . ? C37 H37A 0.9500 . ? C38 C39 1.54(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N5 1.450(19) . ? C43 C44 1.51(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.52(3) . ? C44 Rh2 2.073(14) . ? C44 H44 1.0000 . ? C45 N7 1.44(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.40(2) . ? C46 N7 1.424(18) . ? C46 Rh2 1.90(2) . ? C47 N8 1.41(2) . ? C47 H47A 0.9500 . ? C48 N7 1.31(2) . ? C48 N8 1.327(18) . ? C48 C49 1.54(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.378(18) . ? C50 C55 1.386(18) . ? C50 N8 1.79(3) . ? C50A C51A 1.369(18) . ? C50A C55A 1.389(18) . ? C50A N8 1.46(3) . ? C51 C52 1.361(18) . ? C51 C56 1.517(17) . ? C51A C52A 1.407(18) . ? C51A C56A 1.482(18) . ? C52 C53 1.371(18) . ? C52 H52A 0.9500 . ? C52A C53A 1.378(18) . ? C52A H52B 0.9500 . ? C53 C54 1.379(18) . ? C53 C57 1.513(18) . ? C53A C54A 1.383(18) . ? C53A C57A 1.495(18) . ? C54 C55 1.387(18) . ? C54 H54A 0.9500 . ? C54A C55A 1.390(18) . ? C54A H54B 0.9500 . ? C55 C58 1.505(18) . ? C55A C58A 1.498(18) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C57A H57D 0.9800 . ? C57A H57E 0.9800 . ? C57A H57F 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C59 Cl1 1.53(3) . ? C59 Cl2 1.71(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? F1 P1 1.53(3) . ? F1A P1 1.55(3) . ? F2 P1 1.57(3) . ? F2A P1 1.59(3) . ? F3 P1 1.67(3) . ? F3A P1 1.59(3) . ? F4 P1 1.58(4) . ? F4A P1 1.57(3) . ? F5 P1 1.57(2) . ? F6 P1 1.56(2) . ? I1 Rh1 2.8052(16) . ? I1 Rh2 2.8364(13) . ? I2 Rh1 2.7808(17) . ? I2 Rh2 2.8061(18) . ? I3 Rh1 2.7934(19) . ? I3 Rh2 2.797(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 106.7(14) . . ? C2 C1 Rh1 140.3(13) . . ? N2 C1 Rh1 112.5(10) . . ? C1 C2 N1 106.7(13) . . ? C1 C2 H2A 126.6 . . ? N1 C2 H2A 126.6 . . ? N1 C3 N2 105.7(14) . . ? N1 C3 C19 128.1(15) . . ? N2 C3 C19 126.1(13) . . ? N2 C4 C5 105.5(13) . . ? N2 C4 H4A 110.6 . . ? C5 C4 H4A 110.6 . . ? N2 C4 H4B 110.6 . . ? C5 C4 H4B 110.6 . . ? H4A C4 H4B 108.8 . . ? C6 C5 C4 114.0(13) . . ? C6 C5 Rh1 109.6(12) . . ? C4 C5 Rh1 106.9(10) . . ? C6 C5 H5 108.7 . . ? C4 C5 H5 108.7 . . ? Rh1 C5 H5 108.7 . . ? N4 C6 C5 109.3(13) . . ? N4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C8 C7 N4 102.2(15) . . ? C8 C7 Rh1 143.3(13) . . ? N4 C7 Rh1 114.4(11) . . ? N3 C8 C7 106.3(13) . . ? N3 C8 H8A 126.9 . . ? C7 C8 H8A 126.9 . . ? N3 C9 N4 106.6(16) . . ? N3 C9 C29 129.6(17) . . ? N4 C9 C29 123.4(15) . . ? C11 C10 C15 123.4(17) . . ? C11 C10 N1 119.5(17) . . ? C15 C10 N1 117.0(18) . . ? C10 C11 C12 118.8(18) . . ? C10 C11 C16 122.4(16) . . ? C12 C11 C16 118.7(19) . . ? C13 C12 C11 118.0(19) . . ? C13 C12 H12A 121.0 . . ? C11 C12 H12A 121.0 . . ? C14 C13 C12 120.3(17) . . ? C14 C13 C17 122.9(18) . . ? C12 C13 C17 116.7(18) . . ? C13 C14 C15 124.6(19) . . ? C13 C14 H14A 117.7 . . ? C15 C14 H14A 117.7 . . ? C14 C15 C10 115(2) . . ? C14 C15 C18 122.5(17) . . ? C10 C15 C18 122.6(16) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C3 C19 H19A 109.5 . . ? C3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 118(2) . . ? C25 C20 N3 122.0(19) . . ? C21 C20 N3 120(2) . . ? C22 C21 C20 117(2) . . ? C22 C21 C26 125(2) . . ? C20 C21 C26 118(2) . . ? C23 C22 C21 122(2) . . ? C23 C22 H22A 118.9 . . ? C21 C22 H22A 118.9 . . ? C22 C23 C24 121(2) . . ? C22 C23 C27 115(2) . . ? C24 C23 C27 122(2) . . ? C23 C24 C25 120(2) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C20 C25 C24 121(2) . . ? C20 C25 C28 119(2) . . ? C24 C25 C28 120(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C9 C29 H29A 109.5 . . ? C9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 N5 104.7(16) . . ? C32 C30 Rh2 140.6(12) . . ? N5 C30 Rh2 114.4(12) . . ? N6 C31 N5 105.5(15) . . ? N6 C31 C42 129.1(18) . . ? N5 C31 C42 125.1(14) . . ? C30 C32 N6 110.1(14) . . ? C30 C32 H32A 125.0 . . ? N6 C32 H32A 125.0 . . ? C34 C33 C38 119(2) . . ? C34 C33 N6 122(3) . . ? C38 C33 N6 118(2) . . ? C33 C34 C35 120(3) . . ? C33 C34 C41 118(2) . . ? C35 C34 C41 122(2) . . ? C36 C35 C34 122(2) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? C35 C36 C37 119(2) . . ? C35 C36 C40 122(2) . . ? C37 C36 C40 119(2) . . ? C38 C37 C36 121(3) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C37 C38 C33 119(2) . . ? C37 C38 C39 120(2) . . ? C33 C38 C39 122(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C31 C42 H42A 109.5 . . ? C31 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C31 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 C44 108.7(13) . . ? N5 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? N5 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? C43 C44 C45 111.4(14) . . ? C43 C44 Rh2 112.9(11) . . ? C45 C44 Rh2 108.4(12) . . ? C43 C44 H44 108.0 . . ? C45 C44 H44 108.0 . . ? Rh2 C44 H44 108.0 . . ? N7 C45 C44 109.5(14) . . ? N7 C45 H45A 109.8 . . ? C44 C45 H45A 109.8 . . ? N7 C45 H45B 109.8 . . ? C44 C45 H45B 109.8 . . ? H45A C45 H45B 108.2 . . ? C47 C46 N7 100.8(17) . . ? C47 C46 Rh2 141.8(12) . . ? N7 C46 Rh2 117.4(13) . . ? C46 C47 N8 109.9(14) . . ? C46 C47 H47A 125.1 . . ? N8 C47 H47A 125.1 . . ? N7 C48 N8 109.0(16) . . ? N7 C48 C49 125.1(15) . . ? N8 C48 C49 125.8(19) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C55 124(2) . . ? C51 C50 N8 125.6(19) . . ? C55 C50 N8 107(2) . . ? C51A C50A C55A 136(3) . . ? C51A C50A N8 100(2) . . ? C55A C50A N8 123(2) . . ? C52 C51 C50 115(3) . . ? C52 C51 C56 123(3) . . ? C50 C51 C56 122(2) . . ? C50A C51A C52A 104(2) . . ? C50A C51A C56A 135(2) . . ? C52A C51A C56A 119(2) . . ? C51 C52 C53 125(3) . . ? C51 C52 H52A 117.3 . . ? C53 C52 H52A 117.3 . . ? C53A C52A C51A 131(3) . . ? C53A C52A H52B 114.3 . . ? C51A C52A H52B 114.3 . . ? C52 C53 C54 114(3) . . ? C52 C53 C57 119(2) . . ? C54 C53 C57 126(3) . . ? C52A C53A C54A 109(3) . . ? C52A C53A C57A 126(3) . . ? C54A C53A C57A 125(2) . . ? C53 C54 C55 126(3) . . ? C53 C54 H54A 117.2 . . ? C55 C54 H54A 117.2 . . ? C53A C54A C55A 130(3) . . ? C53A C54A H54B 114.8 . . ? C55A C54A H54B 114.8 . . ? C50 C55 C54 112(3) . . ? C50 C55 C58 121(3) . . ? C54 C55 C58 125(2) . . ? C50A C55A C54A 105(2) . . ? C50A C55A C58A 127(2) . . ? C54A C55A C58A 125(3) . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C51A C56A H56D 109.5 . . ? C51A C56A H56E 109.5 . . ? H56D C56A H56E 109.5 . . ? C51A C56A H56F 109.5 . . ? H56D C56A H56F 109.5 . . ? H56E C56A H56F 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53A C57A H57D 109.5 . . ? C53A C57A H57E 109.5 . . ? H57D C57A H57E 109.5 . . ? C53A C57A H57F 109.5 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55A C58A H58D 109.5 . . ? C55A C58A H58E 109.5 . . ? H58D C58A H58E 109.5 . . ? C55A C58A H58F 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? Cl1 C59 Cl2 110.7(19) . . ? Cl1 C59 H59A 109.5 . . ? Cl2 C59 H59A 109.5 . . ? Cl1 C59 H59B 109.5 . . ? Cl2 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? Rh1 I1 Rh2 73.27(4) . . ? Rh1 I2 Rh2 74.11(5) . . ? Rh1 I3 Rh2 74.06(5) . . ? C3 N1 C2 109.8(13) . . ? C3 N1 C10 124.6(15) . . ? C2 N1 C10 125.2(13) . . ? C1 N2 C3 110.9(12) . . ? C1 N2 C4 122.1(13) . . ? C3 N2 C4 126.2(13) . . ? C9 N3 C8 112.6(16) . . ? C9 N3 C20 124.1(17) . . ? C8 N3 C20 123.2(14) . . ? C9 N4 C7 112.0(14) . . ? C9 N4 C6 128.8(14) . . ? C7 N4 C6 117.6(14) . . ? C31 N5 C30 111.6(14) . . ? C31 N5 C43 127.5(14) . . ? C30 N5 C43 120.5(15) . . ? C31 N6 C32 107.9(15) . . ? C31 N6 C33 122.4(16) . . ? C32 N6 C33 129.6(13) . . ? C48 N7 C46 112.8(15) . . ? C48 N7 C45 131.8(15) . . ? C46 N7 C45 114.8(16) . . ? C48 N8 C47 107.2(17) . . ? C48 N8 C50A 127.1(17) . . ? C47 N8 C50A 124.0(15) . . ? C48 N8 C50 126.9(16) . . ? C47 N8 C50 119.0(12) . . ? C50A N8 C50 35.1(14) . . ? F1 P1 F1A 54.5(14) . . ? F1 P1 F6 84.9(14) . . ? F1A P1 F6 92.7(10) . . ? F1 P1 F2 86.2(15) . . ? F1A P1 F2 31.7(12) . . ? F6 P1 F2 95.8(11) . . ? F1 P1 F5 96.2(15) . . ? F1A P1 F5 89.3(12) . . ? F6 P1 F5 178.0(10) . . ? F2 P1 F5 86.0(13) . . ? F1 P1 F4A 48.3(13) . . ? F1A P1 F4A 100.6(16) . . ? F6 P1 F4A 96.6(15) . . ? F2 P1 F4A 131.2(18) . . ? F5 P1 F4A 83.0(15) . . ? F1 P1 F4 102.9(16) . . ? F1A P1 F4 157.2(15) . . ? F6 P1 F4 80.9(16) . . ? F2 P1 F4 169.9(18) . . ? F5 P1 F4 97.2(15) . . ? F4A P1 F4 58.9(16) . . ? F1 P1 F2A 137.3(17) . . ? F1A P1 F2A 83.7(16) . . ? F6 P1 F2A 88.9(16) . . ? F2 P1 F2A 52.4(14) . . ? F5 P1 F2A 91.4(15) . . ? F4A P1 F2A 172.8(16) . . ? F4 P1 F2A 117.8(18) . . ? F1 P1 F3A 137.7(17) . . ? F1A P1 F3A 167.8(16) . . ? F6 P1 F3A 89.4(16) . . ? F2 P1 F3A 136.1(16) . . ? F5 P1 F3A 88.6(14) . . ? F4A P1 F3A 91.1(16) . . ? F4 P1 F3A 35.0(12) . . ? F2A P1 F3A 84.3(16) . . ? F1 P1 F3 168.6(16) . . ? F1A P1 F3 115.3(16) . . ? F6 P1 F3 91.0(15) . . ? F2 P1 F3 83.6(15) . . ? F5 P1 F3 88.2(14) . . ? F4A P1 F3 142.9(16) . . ? F4 P1 F3 86.9(16) . . ? F2A P1 F3 31.8(13) . . ? F3A P1 F3 52.6(14) . . ? C7 Rh1 C1 85.6(7) . . ? C7 Rh1 C5 84.1(7) . . ? C1 Rh1 C5 83.4(6) . . ? C7 Rh1 I2 90.6(5) . . ? C1 Rh1 I2 174.1(5) . . ? C5 Rh1 I2 91.8(5) . . ? C7 Rh1 I3 175.4(5) . . ? C1 Rh1 I3 94.1(5) . . ? C5 Rh1 I3 91.3(5) . . ? I2 Rh1 I3 89.43(5) . . ? C7 Rh1 I1 96.3(5) . . ? C1 Rh1 I1 98.5(4) . . ? C5 Rh1 I1 178.0(5) . . ? I2 Rh1 I1 86.30(5) . . ? I3 Rh1 I1 88.32(5) . . ? C46 Rh2 C30 89.7(8) . . ? C46 Rh2 C44 81.8(7) . . ? C30 Rh2 C44 82.3(7) . . ? C46 Rh2 I3 175.5(5) . . ? C30 Rh2 I3 92.4(6) . . ? C44 Rh2 I3 94.6(6) . . ? C46 Rh2 I2 88.8(6) . . ? C30 Rh2 I2 176.5(4) . . ? C44 Rh2 I2 94.3(5) . . ? I3 Rh2 I2 88.85(5) . . ? C46 Rh2 I1 96.0(4) . . ? C30 Rh2 I1 98.1(4) . . ? C44 Rh2 I1 177.7(6) . . ? I3 Rh2 I1 87.65(5) . . ? I2 Rh2 I1 85.23(4) . . ? 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 N2 C1 C2 N1 4(2) . . . . ? Rh1 C1 C2 N1 175.1(17) . . . . ? N2 C4 C5 C6 -89.7(15) . . . . ? N2 C4 C5 Rh1 31.6(15) . . . . ? C4 C5 C6 N4 96.4(15) . . . . ? Rh1 C5 C6 N4 -23.4(16) . . . . ? N4 C7 C8 N3 -2.8(18) . . . . ? Rh1 C7 C8 N3 -179.9(17) . . . . ? C15 C10 C11 C12 3(3) . . . . ? N1 C10 C11 C12 -178.5(17) . . . . ? C15 C10 C11 C16 -174.6(19) . . . . ? N1 C10 C11 C16 4(3) . . . . ? C10 C11 C12 C13 -1(3) . . . . ? C16 C11 C12 C13 176.5(18) . . . . ? C11 C12 C13 C14 2(3) . . . . ? C11 C12 C13 C17 179.1(17) . . . . ? C12 C13 C14 C15 -4(3) . . . . ? C17 C13 C14 C15 178.9(18) . . . . ? C13 C14 C15 C10 5(3) . . . . ? C13 C14 C15 C18 -180(2) . . . . ? C11 C10 C15 C14 -5(3) . . . . ? N1 C10 C15 C14 176.7(17) . . . . ? C11 C10 C15 C18 -180(2) . . . . ? N1 C10 C15 C18 2(3) . . . . ? C25 C20 C21 C22 -4(3) . . . . ? N3 C20 C21 C22 -178.1(18) . . . . ? C25 C20 C21 C26 -177(2) . . . . ? N3 C20 C21 C26 8(3) . . . . ? C20 C21 C22 C23 -2(3) . . . . ? C26 C21 C22 C23 171(2) . . . . ? C21 C22 C23 C24 8(4) . . . . ? C21 C22 C23 C27 173.9(19) . . . . ? C22 C23 C24 C25 -8(3) . . . . ? C27 C23 C24 C25 -173(2) . . . . ? C21 C20 C25 C24 4(3) . . . . ? N3 C20 C25 C24 178.1(18) . . . . ? C21 C20 C25 C28 180.0(18) . . . . ? N3 C20 C25 C28 -6(3) . . . . ? C23 C24 C25 C20 2(3) . . . . ? C23 C24 C25 C28 -174.1(19) . . . . ? N5 C30 C32 N6 1(2) . . . . ? Rh2 C30 C32 N6 173.2(19) . . . . ? C38 C33 C34 C35 -2(3) . . . . ? N6 C33 C34 C35 177.4(14) . . . . ? C38 C33 C34 C41 178.9(15) . . . . ? N6 C33 C34 C41 -2(3) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C41 C34 C35 C36 179.8(16) . . . . ? C34 C35 C36 C37 0(3) . . . . ? C34 C35 C36 C40 -179.6(14) . . . . ? C35 C36 C37 C38 0(3) . . . . ? C40 C36 C37 C38 -179.9(15) . . . . ? C36 C37 C38 C33 -2(3) . . . . ? C36 C37 C38 C39 -179.9(15) . . . . ? C34 C33 C38 C37 3(3) . . . . ? N6 C33 C38 C37 -177.0(13) . . . . ? C34 C33 C38 C39 -179.4(15) . . . . ? N6 C33 C38 C39 1(2) . . . . ? N5 C43 C44 C45 110.9(16) . . . . ? N5 C43 C44 Rh2 -11(2) . . . . ? C43 C44 C45 N7 -94.6(15) . . . . ? Rh2 C44 C45 N7 30.2(17) . . . . ? N7 C46 C47 N8 2(2) . . . . ? Rh2 C46 C47 N8 -177.5(17) . . . . ? C55 C50 C51 C52 -16(3) . . . . ? N8 C50 C51 C52 -174(2) . . . . ? C55 C50 C51 C56 168(3) . . . . ? N8 C50 C51 C56 11(3) . . . . ? C55A C50A C51A C52A 0(4) . . . . ? N8 C50A C51A C52A 172(2) . . . . ? C55A C50A C51A C56A -163(4) . . . . ? N8 C50A C51A C56A 9(4) . . . . ? C50 C51 C52 C53 1(4) . . . . ? C56 C51 C52 C53 176(3) . . . . ? C50A C51A C52A C53A 15(5) . . . . ? C56A C51A C52A C53A -179(4) . . . . ? C51 C52 C53 C54 5(5) . . . . ? C51 C52 C53 C57 -178(3) . . . . ? C51A C52A C53A C54A -12(6) . . . . ? C51A C52A C53A C57A 165(3) . . . . ? C52 C53 C54 C55 4(5) . . . . ? C57 C53 C54 C55 -173(3) . . . . ? C52A C53A C54A C55A -5(6) . . . . ? C57A C53A C54A C55A 177(4) . . . . ? C51 C50 C55 C54 23(4) . . . . ? N8 C50 C55 C54 -176(2) . . . . ? C51 C50 C55 C58 -169(2) . . . . ? N8 C50 C55 C58 -8(3) . . . . ? C53 C54 C55 C50 -17(5) . . . . ? C53 C54 C55 C58 176(3) . . . . ? C51A C50A C55A C54A -12(5) . . . . ? N8 C50A C55A C54A 177(3) . . . . ? C51A C50A C55A C58A -175(3) . . . . ? N8 C50A C55A C58A 14(6) . . . . ? C53A C54A C55A C50A 15(6) . . . . ? C53A C54A C55A C58A 178(4) . . . . ? N2 C3 N1 C2 0(2) . . . . ? C19 C3 N1 C2 -176.1(19) . . . . ? N2 C3 N1 C10 172.2(17) . . . . ? C19 C3 N1 C10 -4(3) . . . . ? C1 C2 N1 C3 -3(2) . . . . ? C1 C2 N1 C10 -174.7(17) . . . . ? C11 C10 N1 C3 100(2) . . . . ? C15 C10 N1 C3 -81(3) . . . . ? C11 C10 N1 C2 -89(3) . . . . ? C15 C10 N1 C2 90(2) . . . . ? C2 C1 N2 C3 -4(2) . . . . ? Rh1 C1 N2 C3 -178.1(12) . . . . ? C2 C1 N2 C4 -174.8(16) . . . . ? Rh1 C1 N2 C4 11(2) . . . . ? N1 C3 N2 C1 3(2) . . . . ? C19 C3 N2 C1 178.8(18) . . . . ? N1 C3 N2 C4 172.7(16) . . . . ? C19 C3 N2 C4 -11(3) . . . . ? C5 C4 N2 C1 -29(2) . . . . ? C5 C4 N2 C3 161.5(17) . . . . ? N4 C9 N3 C8 4(2) . . . . ? C29 C9 N3 C8 176.6(19) . . . . ? N4 C9 N3 C20 -179.9(17) . . . . ? C29 C9 N3 C20 -7(3) . . . . ? C7 C8 N3 C9 -1(2) . . . . ? C7 C8 N3 C20 -176.7(17) . . . . ? C25 C20 N3 C9 -84(3) . . . . ? C21 C20 N3 C9 90(2) . . . . ? C25 C20 N3 C8 91(2) . . . . ? C21 C20 N3 C8 -94(2) . . . . ? N3 C9 N4 C7 -6(2) . . . . ? C29 C9 N4 C7 -179.2(17) . . . . ? N3 C9 N4 C6 -171.3(15) . . . . ? C29 C9 N4 C6 16(3) . . . . ? C8 C7 N4 C9 5.6(19) . . . . ? Rh1 C7 N4 C9 -176.4(12) . . . . ? C8 C7 N4 C6 172.5(15) . . . . ? Rh1 C7 N4 C6 -9.5(19) . . . . ? C5 C6 N4 C9 -173.5(16) . . . . ? C5 C6 N4 C7 22(2) . . . . ? N6 C31 N5 C30 -4(2) . . . . ? C42 C31 N5 C30 -178.3(18) . . . . ? N6 C31 N5 C43 -176.9(16) . . . . ? C42 C31 N5 C43 8(3) . . . . ? C32 C30 N5 C31 2(2) . . . . ? Rh2 C30 N5 C31 -173.0(14) . . . . ? C32 C30 N5 C43 175.8(17) . . . . ? Rh2 C30 N5 C43 1(2) . . . . ? C44 C43 N5 C31 179.9(19) . . . . ? C44 C43 N5 C30 7(2) . . . . ? N5 C31 N6 C32 4(2) . . . . ? C42 C31 N6 C32 178(2) . . . . ? N5 C31 N6 C33 -179.9(19) . . . . ? C42 C31 N6 C33 -5(3) . . . . ? C30 C32 N6 C31 -3(2) . . . . ? C30 C32 N6 C33 -179(2) . . . . ? C34 C33 N6 C31 101(2) . . . . ? C38 C33 N6 C31 -79(2) . . . . ? C34 C33 N6 C32 -83(3) . . . . ? C38 C33 N6 C32 96(2) . . . . ? N8 C48 N7 C46 6(2) . . . . ? C49 C48 N7 C46 -177.1(16) . . . . ? N8 C48 N7 C45 176.3(17) . . . . ? C49 C48 N7 C45 -7(3) . . . . ? C47 C46 N7 C48 -5(2) . . . . ? Rh2 C46 N7 C48 175.0(14) . . . . ? C47 C46 N7 C45 -177.2(16) . . . . ? Rh2 C46 N7 C45 3(2) . . . . ? C44 C45 N7 C48 167.2(19) . . . . ? C44 C45 N7 C46 -22(2) . . . . ? N7 C48 N8 C47 -4(2) . . . . ? C49 C48 N8 C47 179.0(18) . . . . ? N7 C48 N8 C50A 162(2) . . . . ? C49 C48 N8 C50A -15(3) . . . . ? N7 C48 N8 C50 -154.0(17) . . . . ? C49 C48 N8 C50 29(3) . . . . ? C46 C47 N8 C48 1(2) . . . . ? C46 C47 N8 C50A -165.4(19) . . . . ? C46 C47 N8 C50 153.6(16) . . . . ? C51A C50A N8 C48 103(2) . . . . ? C55A C50A N8 C48 -83(3) . . . . ? C51A C50A N8 C47 -94(2) . . . . ? C55A C50A N8 C47 80(3) . . . . ? C51A C50A N8 C50 -0.5(4) . . . . ? C55A C50A N8 C50 173(4) . . . . ? C51 C50 N8 C48 76(2) . . . . ? C55 C50 N8 C48 -85(2) . . . . ? C51 C50 N8 C47 -71(2) . . . . ? C55 C50 N8 C47 128(2) . . . . ? C51 C50 N8 C50A -179.9(7) . . . . ? C55 C50 N8 C50A 19(2) . . . . ? C8 C7 Rh1 C1 89(2) . . . . ? N4 C7 Rh1 C1 -87.8(12) . . . . ? C8 C7 Rh1 C5 173(2) . . . . ? N4 C7 Rh1 C5 -4.0(12) . . . . ? C8 C7 Rh1 I2 -95(2) . . . . ? N4 C7 Rh1 I2 87.8(12) . . . . ? C8 C7 Rh1 I3 175(5) . . . . ? N4 C7 Rh1 I3 -2(7) . . . . ? C8 C7 Rh1 I1 -9(2) . . . . ? N4 C7 Rh1 I1 174.1(11) . . . . ? C2 C1 Rh1 C7 -78(2) . . . . ? N2 C1 Rh1 C7 92.7(14) . . . . ? C2 C1 Rh1 C5 -163(2) . . . . ? N2 C1 Rh1 C5 8.1(13) . . . . ? C2 C1 Rh1 I2 -127(4) . . . . ? N2 C1 Rh1 I2 44(6) . . . . ? C2 C1 Rh1 I3 107(2) . . . . ? N2 C1 Rh1 I3 -82.7(13) . . . . ? C2 C1 Rh1 I1 18(2) . . . . ? N2 C1 Rh1 I1 -171.7(12) . . . . ? C6 C5 Rh1 C7 15.6(11) . . . . ? C4 C5 Rh1 C7 -108.4(11) . . . . ? C6 C5 Rh1 C1 101.8(12) . . . . ? C4 C5 Rh1 C1 -22.2(11) . . . . ? C6 C5 Rh1 I2 -74.8(10) . . . . ? C4 C5 Rh1 I2 161.2(10) . . . . ? C6 C5 Rh1 I3 -164.2(10) . . . . ? C4 C5 Rh1 I3 71.7(10) . . . . ? C6 C5 Rh1 I1 -85(17) . . . . ? C4 C5 Rh1 I1 151(16) . . . . ? Rh2 I2 Rh1 C7 142.6(5) . . . . ? Rh2 I2 Rh1 C1 -169(5) . . . . ? Rh2 I2 Rh1 C5 -133.3(5) . . . . ? Rh2 I2 Rh1 I3 -42.01(4) . . . . ? Rh2 I2 Rh1 I1 46.35(4) . . . . ? Rh2 I3 Rh1 C7 132(6) . . . . ? Rh2 I3 Rh1 C1 -142.6(4) . . . . ? Rh2 I3 Rh1 C5 134.0(5) . . . . ? Rh2 I3 Rh1 I2 42.19(4) . . . . ? Rh2 I3 Rh1 I1 -44.12(4) . . . . ? Rh2 I1 Rh1 C7 -136.1(5) . . . . ? Rh2 I1 Rh1 C1 137.5(6) . . . . ? Rh2 I1 Rh1 C5 -35(17) . . . . ? Rh2 I1 Rh1 I2 -45.97(5) . . . . ? Rh2 I1 Rh1 I3 43.57(5) . . . . ? C47 C46 Rh2 C30 -86(2) . . . . ? N7 C46 Rh2 C30 94.5(14) . . . . ? C47 C46 Rh2 C44 -168(3) . . . . ? N7 C46 Rh2 C44 12.2(14) . . . . ? C47 C46 Rh2 I3 156(5) . . . . ? N7 C46 Rh2 I3 -23(8) . . . . ? C47 C46 Rh2 I2 97(2) . . . . ? N7 C46 Rh2 I2 -82.3(13) . . . . ? C47 C46 Rh2 I1 12(2) . . . . ? N7 C46 Rh2 I1 -167.4(13) . . . . ? C32 C30 Rh2 C46 100(3) . . . . ? N5 C30 Rh2 C46 -87.7(14) . . . . ? C32 C30 Rh2 C44 -178(3) . . . . ? N5 C30 Rh2 C44 -5.9(14) . . . . ? C32 C30 Rh2 I3 -84(3) . . . . ? N5 C30 Rh2 I3 88.4(14) . . . . ? C32 C30 Rh2 I2 165(8) . . . . ? N5 C30 Rh2 I2 -23(11) . . . . ? C32 C30 Rh2 I1 4(3) . . . . ? N5 C30 Rh2 I1 176.3(13) . . . . ? C43 C44 Rh2 C46 100.6(15) . . . . ? C45 C44 Rh2 C46 -23.3(12) . . . . ? C43 C44 Rh2 C30 9.8(15) . . . . ? C45 C44 Rh2 C30 -114.0(13) . . . . ? C43 C44 Rh2 I3 -82.0(14) . . . . ? C45 C44 Rh2 I3 154.1(11) . . . . ? C43 C44 Rh2 I2 -171.2(13) . . . . ? C45 C44 Rh2 I2 64.9(12) . . . . ? C43 C44 Rh2 I1 110(13) . . . . ? C45 C44 Rh2 I1 -13(14) . . . . ? Rh1 I3 Rh2 C46 -101(7) . . . . ? Rh1 I3 Rh2 C30 141.5(4) . . . . ? Rh1 I3 Rh2 C44 -136.0(5) . . . . ? Rh1 I3 Rh2 I2 -41.73(4) . . . . ? Rh1 I3 Rh2 I1 43.54(4) . . . . ? Rh1 I2 Rh2 C46 -141.9(4) . . . . ? Rh1 I2 Rh2 C30 153(10) . . . . ? Rh1 I2 Rh2 C44 136.5(6) . . . . ? Rh1 I2 Rh2 I3 41.95(4) . . . . ? Rh1 I2 Rh2 I1 -45.78(4) . . . . ? Rh1 I1 Rh2 C46 133.8(6) . . . . ? Rh1 I1 Rh2 C30 -135.6(6) . . . . ? Rh1 I1 Rh2 C44 124(13) . . . . ? Rh1 I1 Rh2 I3 -43.53(5) . . . . ? Rh1 I1 Rh2 I2 45.52(5) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.074 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.135 _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 579 A**3 RESPONSE: Pronounced disorder was found in co-crystallised solvent molecules. Therefore, the SQUEEZE option in PLATON was used to calculate the potential solvent accessible volume. Eight hexane molecules (8 x 50 electrons) per unit cell were included in all further calculations. Resulting from the disorder problems, the different rings and parts of the ligand have been refined having same thermal values. ; # end Validation Reply Form #===END data_complex-4 _database_code_depnum_ccdc_archive 'CCDC 817393' #TrackingRef '- allComplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 I2 N6 Rh' _chemical_formula_weight 725.24 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' I I -0.4742 1.8119 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.7813(9) _cell_length_b 11.0963(4) _cell_length_c 14.6937(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.152(4) _cell_angle_gamma 90.00 _cell_volume 2714.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44953 _cell_measurement_theta_min 1.735 _cell_measurement_theta_max 29.575 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 2.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3695 _exptl_absorpt_correction_T_max 0.5265 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 51616 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.28 _reflns_number_total 7338 _reflns_number_gt 5946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0504P)^2^+0.0240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7338 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.18076(17) 0.2103(2) 0.18099(19) 0.0321(5) Uani 1 1 d . . . C2 C 0.13311(17) 0.1384(2) 0.2243(2) 0.0356(6) Uani 1 1 d . . . H2 H 0.1494 0.0674 0.2576 0.053 Uiso 1 1 calc R . . C3 C 0.05610(19) 0.2868(3) 0.1605(2) 0.0396(6) Uani 1 1 d . . . C4 C 0.16623(19) 0.3966(2) 0.0902(2) 0.0396(6) Uani 1 1 d . . . H4A H 0.1786 0.4680 0.1298 0.059 Uiso 1 1 calc R . . H4B H 0.1275 0.4210 0.0370 0.059 Uiso 1 1 calc R . . C5 C 0.24334(18) 0.3484(2) 0.05722(19) 0.0338(6) Uani 1 1 d . . . H5 H 0.2828 0.4162 0.0595 0.051 Uiso 1 1 calc R . . C6 C 0.23172(19) 0.2990(2) -0.0406(2) 0.0375(6) Uani 1 1 d . . . H6A H 0.1837 0.3359 -0.0758 0.056 Uiso 1 1 calc R . . H6B H 0.2791 0.3183 -0.0719 0.056 Uiso 1 1 calc R . . C7 C 0.24893(17) 0.1118(2) 0.04352(19) 0.0317(5) Uani 1 1 d . . . C8 C 0.2003(2) -0.0231(3) -0.0633(2) 0.0416(7) Uani 1 1 d . . . H8 H 0.1853 -0.0978 -0.0920 0.062 Uiso 1 1 calc R . . C9 C 0.19258(19) 0.0865(3) -0.1023(2) 0.0394(6) Uani 1 1 d . . . H9 H 0.1713 0.1042 -0.1639 0.059 Uiso 1 1 calc R . . C10 C 0.2534(2) -0.1056(3) 0.0923(2) 0.0411(7) Uani 1 1 d . . . H10A H 0.2133 -0.1706 0.0785 0.062 Uiso 1 1 calc R . . H10B H 0.2493 -0.0763 0.1552 0.062 Uiso 1 1 calc R . . C11 C 0.3365(2) -0.1562(3) 0.0883(2) 0.0475(7) Uani 1 1 d . . . H11A H 0.3770 -0.0931 0.1072 0.071 Uiso 1 1 calc R . . H11B H 0.3421 -0.1796 0.0244 0.071 Uiso 1 1 calc R . . C12 C 0.3525(3) -0.2655(4) 0.1507(3) 0.0658(11) Uani 1 1 d . . . H12A H 0.3476 -0.2411 0.2146 0.099 Uiso 1 1 calc R . . H12B H 0.3108 -0.3271 0.1326 0.099 Uiso 1 1 calc R . . C13 C 0.4339(3) -0.3207(5) 0.1476(3) 0.0791(14) Uani 1 1 d . . . H13A H 0.4755 -0.2612 0.1676 0.119 Uiso 1 1 calc R . . H13B H 0.4390 -0.3461 0.0847 0.119 Uiso 1 1 calc R . . H13C H 0.4401 -0.3908 0.1884 0.119 Uiso 1 1 calc R . . C14 C -0.0143(2) 0.1366(3) 0.2502(3) 0.0538(9) Uani 1 1 d . . . H14A H -0.0136 0.0476 0.2459 0.081 Uiso 1 1 calc R . . H14B H -0.0642 0.1660 0.2140 0.081 Uiso 1 1 calc R . . C15 C -0.0135(3) 0.1739(5) 0.3501(4) 0.0824(16) Uani 1 1 d . . . H15A H 0.0390 0.1525 0.3847 0.124 Uiso 1 1 calc R . . H15B H -0.0558 0.1289 0.3772 0.124 Uiso 1 1 calc R . . C16 C -0.0282(3) 0.3108(5) 0.3596(4) 0.0830(14) Uani 1 1 d . . . H16A H 0.0115 0.3552 0.3279 0.124 Uiso 1 1 calc R . . H16B H -0.0823 0.3306 0.3283 0.124 Uiso 1 1 calc R . . C17 C -0.0220(4) 0.3531(7) 0.4569(4) 0.114(2) Uani 1 1 d . . . H17A H 0.0316 0.3350 0.4882 0.171 Uiso 1 1 calc R . . H17B H -0.0625 0.3118 0.4883 0.171 Uiso 1 1 calc R . . H17C H -0.0313 0.4403 0.4580 0.171 Uiso 1 1 calc R . . C18 C 0.3598(2) 0.4127(3) 0.2979(2) 0.0444(7) Uani 1 1 d . . . C19 C 0.3950(3) 0.4991(4) 0.3651(3) 0.0669(11) Uani 1 1 d . . . H19A H 0.3912 0.4683 0.4269 0.100 Uiso 1 1 calc R . . H19B H 0.3659 0.5757 0.3566 0.100 Uiso 1 1 calc R . . H19C H 0.4515 0.5119 0.3573 0.100 Uiso 1 1 calc R . . C20 C 0.36265(18) 0.0338(3) 0.3117(2) 0.0390(6) Uani 1 1 d . . . C21 C 0.3934(2) -0.0288(3) 0.3956(2) 0.0513(8) Uani 1 1 d . . . H21A H 0.4352 -0.0858 0.3828 0.077 Uiso 1 1 calc R . . H21B H 0.3495 -0.0726 0.4191 0.077 Uiso 1 1 calc R . . H21C H 0.4162 0.0299 0.4415 0.077 Uiso 1 1 calc R . . I1 I 0.436089(12) 0.229217(19) 0.075894(15) 0.04422(6) Uani 1 1 d . . . I2 I 0.168273(13) 0.868680(17) 0.399427(16) 0.04678(7) Uani 1 1 d . . . N1 N 0.13150(14) 0.3016(2) 0.14163(17) 0.0344(5) Uani 1 1 d . . . N2 N 0.05559(15) 0.1860(2) 0.21178(18) 0.0391(5) Uani 1 1 d . . . N3 N 0.22154(14) 0.1683(2) -0.03559(16) 0.0332(5) Uani 1 1 d . . . N4 N 0.23464(15) -0.0066(2) 0.02735(16) 0.0353(5) Uani 1 1 d . . . N5 N 0.33265(15) 0.3443(2) 0.24487(17) 0.0375(5) Uani 1 1 d . . . N6 N 0.33805(15) 0.0853(2) 0.24689(17) 0.0371(5) Uani 1 1 d . . . Rh1 Rh 0.291932(13) 0.215447(17) 0.146242(14) 0.02962(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0368(13) 0.0292(12) 0.0285(12) -0.0021(10) -0.0029(10) 0.0035(10) C2 0.0370(14) 0.0321(13) 0.0362(14) -0.0007(11) -0.0017(11) 0.0034(10) C3 0.0416(15) 0.0364(14) 0.0397(15) 0.0029(12) 0.0004(12) 0.0029(11) C4 0.0491(16) 0.0284(12) 0.0411(16) 0.0051(11) 0.0043(13) 0.0082(11) C5 0.0420(14) 0.0252(11) 0.0333(13) 0.0040(10) 0.0012(11) 0.0019(10) C6 0.0480(16) 0.0307(12) 0.0325(14) 0.0041(11) -0.0001(12) 0.0016(11) C7 0.0373(13) 0.0263(11) 0.0312(13) -0.0004(10) 0.0035(11) 0.0016(10) C8 0.0527(17) 0.0354(14) 0.0351(15) -0.0066(12) -0.0013(13) -0.0037(12) C9 0.0468(16) 0.0403(14) 0.0295(14) -0.0053(11) -0.0011(12) 0.0001(12) C10 0.0537(18) 0.0281(12) 0.0406(16) 0.0039(11) 0.0022(13) 0.0009(12) C11 0.059(2) 0.0404(16) 0.0431(17) 0.0052(13) 0.0046(15) 0.0112(14) C12 0.082(3) 0.062(2) 0.056(2) 0.0237(19) 0.022(2) 0.026(2) C13 0.094(4) 0.080(3) 0.066(3) 0.025(2) 0.020(2) 0.039(3) C14 0.0401(17) 0.0433(17) 0.078(3) 0.0077(17) 0.0086(17) -0.0045(13) C15 0.052(2) 0.116(4) 0.084(3) 0.049(3) 0.022(2) 0.001(2) C16 0.085(3) 0.094(4) 0.070(3) 0.017(3) 0.010(3) -0.007(3) C17 0.086(4) 0.189(7) 0.067(3) 0.007(4) 0.014(3) -0.004(4) C18 0.0499(17) 0.0475(17) 0.0359(15) 0.0008(13) 0.0054(13) -0.0114(14) C19 0.088(3) 0.066(2) 0.045(2) -0.0080(18) 0.0028(19) -0.037(2) C20 0.0353(14) 0.0387(14) 0.0421(16) 0.0031(12) 0.0011(12) 0.0031(11) C21 0.0448(17) 0.0565(19) 0.0494(19) 0.0147(16) -0.0069(14) 0.0087(15) I1 0.03592(10) 0.04786(12) 0.04906(13) 0.00373(9) 0.00599(8) 0.00213(8) I2 0.05097(12) 0.02965(10) 0.05524(13) 0.00529(8) -0.01108(9) -0.00630(8) N1 0.0367(12) 0.0304(10) 0.0350(12) 0.0008(9) -0.0002(10) 0.0056(9) N2 0.0345(12) 0.0370(12) 0.0450(14) 0.0023(11) 0.0023(11) 0.0005(10) N3 0.0403(12) 0.0297(10) 0.0282(11) -0.0002(9) -0.0015(9) 0.0017(9) N4 0.0466(13) 0.0254(10) 0.0333(12) -0.0007(9) 0.0023(10) 0.0004(9) N5 0.0415(13) 0.0360(12) 0.0337(12) -0.0014(10) -0.0003(10) -0.0037(10) N6 0.0367(12) 0.0374(12) 0.0356(12) 0.0033(10) -0.0018(10) 0.0053(10) Rh1 0.03297(11) 0.02678(10) 0.02783(10) 0.00043(7) -0.00127(8) 0.00134(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.344(4) . ? C1 N1 1.387(3) . ? C1 Rh1 1.995(3) . ? C2 N2 1.395(4) . ? C2 H2 0.9500 . ? C3 N1 1.339(4) . ? C3 N2 1.349(4) . ? C4 N1 1.461(4) . ? C4 C5 1.533(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(4) . ? C5 Rh1 2.071(3) . ? C5 H5 1.0000 . ? C6 N3 1.464(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N3 1.350(3) . ? C7 N4 1.351(3) . ? C7 Rh1 1.962(3) . ? C8 C9 1.344(4) . ? C8 N4 1.396(4) . ? C8 H8 0.9500 . ? C9 N3 1.379(4) . ? C9 H9 0.9500 . ? C10 N4 1.464(4) . ? C10 C11 1.512(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.524(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.503(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N2 1.469(4) . ? C14 C15 1.524(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.548(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N5 1.141(4) . ? C18 C19 1.449(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N6 1.144(4) . ? C20 C21 1.451(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? I1 Rh1 2.7508(3) . ? N5 Rh1 2.089(2) . ? N6 Rh1 2.142(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 105.8(2) . . ? C2 C1 Rh1 140.2(2) . . ? N1 C1 Rh1 113.6(2) . . ? C1 C2 N2 108.2(2) . . ? C1 C2 H2 125.9 . . ? N2 C2 H2 125.9 . . ? N1 C3 N2 106.8(3) . . ? N1 C4 C5 108.6(2) . . ? N1 C4 H4A 110.0 . . ? C5 C4 H4A 110.0 . . ? N1 C4 H4B 110.0 . . ? C5 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C6 C5 C4 114.1(2) . . ? C6 C5 Rh1 109.43(17) . . ? C4 C5 Rh1 109.29(18) . . ? C6 C5 H5 107.9 . . ? C4 C5 H5 107.9 . . ? Rh1 C5 H5 107.9 . . ? N3 C6 C5 108.1(2) . . ? N3 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? N3 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? N3 C7 N4 105.4(2) . . ? N3 C7 Rh1 116.31(18) . . ? N4 C7 Rh1 138.2(2) . . ? C9 C8 N4 107.1(2) . . ? C9 C8 H8 126.4 . . ? N4 C8 H8 126.4 . . ? C8 C9 N3 106.6(2) . . ? C8 C9 H9 126.7 . . ? N3 C9 H9 126.7 . . ? N4 C10 C11 112.2(3) . . ? N4 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N4 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.5(3) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 113.5(4) . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 111.0(3) . . ? N2 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N2 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.7(4) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 113.6(5) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C19 179.6(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 C21 178.4(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 N1 C1 110.7(2) . . ? C3 N1 C4 130.1(2) . . ? C1 N1 C4 119.2(2) . . ? C3 N2 C2 108.5(3) . . ? C3 N2 C14 125.8(3) . . ? C2 N2 C14 125.7(3) . . ? C7 N3 C9 111.0(2) . . ? C7 N3 C6 118.3(2) . . ? C9 N3 C6 130.5(2) . . ? C7 N4 C8 109.8(2) . . ? C7 N4 C10 126.6(2) . . ? C8 N4 C10 123.6(2) . . ? C18 N5 Rh1 175.6(3) . . ? C20 N6 Rh1 167.1(2) . . ? C7 Rh1 C1 85.07(11) . . ? C7 Rh1 C5 81.59(11) . . ? C1 Rh1 C5 82.81(11) . . ? C7 Rh1 N5 172.69(10) . . ? C1 Rh1 N5 94.45(10) . . ? C5 Rh1 N5 91.12(10) . . ? C7 Rh1 N6 101.68(10) . . ? C1 Rh1 N6 94.18(10) . . ? C5 Rh1 N6 175.39(11) . . ? N5 Rh1 N6 85.62(10) . . ? C7 Rh1 I1 89.99(8) . . ? C1 Rh1 I1 172.63(8) . . ? C5 Rh1 I1 91.07(8) . . ? N5 Rh1 I1 89.75(7) . . ? N6 Rh1 I1 92.17(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 N1 C1 C2 N2 -0.4(3) . . . . ? Rh1 C1 C2 N2 -171.6(2) . . . . ? N1 C4 C5 C6 95.6(3) . . . . ? N1 C4 C5 Rh1 -27.2(3) . . . . ? C4 C5 C6 N3 -96.3(3) . . . . ? Rh1 C5 C6 N3 26.5(3) . . . . ? N4 C8 C9 N3 -0.4(4) . . . . ? N4 C10 C11 C12 -175.4(3) . . . . ? C10 C11 C12 C13 178.8(4) . . . . ? N2 C14 C15 C16 68.3(4) . . . . ? C14 C15 C16 C17 -175.8(4) . . . . ? N2 C3 N1 C1 -0.2(3) . . . . ? N2 C3 N1 C4 -178.7(3) . . . . ? C2 C1 N1 C3 0.4(3) . . . . ? Rh1 C1 N1 C3 174.3(2) . . . . ? C2 C1 N1 C4 179.0(2) . . . . ? Rh1 C1 N1 C4 -7.1(3) . . . . ? C5 C4 N1 C3 -158.4(3) . . . . ? C5 C4 N1 C1 23.2(3) . . . . ? N1 C3 N2 C2 0.0(3) . . . . ? N1 C3 N2 C14 178.4(3) . . . . ? C1 C2 N2 C3 0.2(3) . . . . ? C1 C2 N2 C14 -178.2(3) . . . . ? C15 C14 N2 C3 -97.9(4) . . . . ? C15 C14 N2 C2 80.3(4) . . . . ? N4 C7 N3 C9 -2.0(3) . . . . ? Rh1 C7 N3 C9 -179.7(2) . . . . ? N4 C7 N3 C6 -177.6(3) . . . . ? Rh1 C7 N3 C6 4.7(3) . . . . ? C8 C9 N3 C7 1.5(4) . . . . ? C8 C9 N3 C6 176.4(3) . . . . ? C5 C6 N3 C7 -21.2(4) . . . . ? C5 C6 N3 C9 164.2(3) . . . . ? N3 C7 N4 C8 1.7(3) . . . . ? Rh1 C7 N4 C8 178.7(3) . . . . ? N3 C7 N4 C10 -179.8(3) . . . . ? Rh1 C7 N4 C10 -2.9(5) . . . . ? C9 C8 N4 C7 -0.9(4) . . . . ? C9 C8 N4 C10 -179.4(3) . . . . ? C11 C10 N4 C7 -89.9(4) . . . . ? C11 C10 N4 C8 88.4(4) . . . . ? C19 C18 N5 Rh1 -12(59) . . . . ? C21 C20 N6 Rh1 10(14) . . . . ? N3 C7 Rh1 C1 92.7(2) . . . . ? N4 C7 Rh1 C1 -83.9(3) . . . . ? N3 C7 Rh1 C5 9.3(2) . . . . ? N4 C7 Rh1 C5 -167.4(3) . . . . ? N3 C7 Rh1 N5 6.2(10) . . . . ? N4 C7 Rh1 N5 -170.5(7) . . . . ? N3 C7 Rh1 N6 -174.0(2) . . . . ? N4 C7 Rh1 N6 9.3(3) . . . . ? N3 C7 Rh1 I1 -81.8(2) . . . . ? N4 C7 Rh1 I1 101.5(3) . . . . ? C2 C1 Rh1 C7 80.8(3) . . . . ? N1 C1 Rh1 C7 -89.9(2) . . . . ? C2 C1 Rh1 C5 163.0(3) . . . . ? N1 C1 Rh1 C5 -7.81(19) . . . . ? C2 C1 Rh1 N5 -106.5(3) . . . . ? N1 C1 Rh1 N5 82.76(19) . . . . ? C2 C1 Rh1 N6 -20.5(3) . . . . ? N1 C1 Rh1 N6 168.68(19) . . . . ? C2 C1 Rh1 I1 128.9(5) . . . . ? N1 C1 Rh1 I1 -41.9(7) . . . . ? C6 C5 Rh1 C7 -20.0(2) . . . . ? C4 C5 Rh1 C7 105.7(2) . . . . ? C6 C5 Rh1 C1 -106.0(2) . . . . ? C4 C5 Rh1 C1 19.6(2) . . . . ? C6 C5 Rh1 N5 159.6(2) . . . . ? C4 C5 Rh1 N5 -74.7(2) . . . . ? C6 C5 Rh1 N6 -155.5(12) . . . . ? C4 C5 Rh1 N6 -29.8(14) . . . . ? C6 C5 Rh1 I1 69.9(2) . . . . ? C4 C5 Rh1 I1 -164.51(19) . . . . ? C18 N5 Rh1 C7 -110(3) . . . . ? C18 N5 Rh1 C1 164(3) . . . . ? C18 N5 Rh1 C5 -113(3) . . . . ? C18 N5 Rh1 N6 70(3) . . . . ? C18 N5 Rh1 I1 -22(3) . . . . ? C20 N6 Rh1 C7 -163.8(11) . . . . ? C20 N6 Rh1 C1 -78.0(11) . . . . ? C20 N6 Rh1 C5 -29(2) . . . . ? C20 N6 Rh1 N5 16.2(11) . . . . ? C20 N6 Rh1 I1 105.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.225 _refine_diff_density_min -1.631 _refine_diff_density_rms 0.104 #===END data_complex-5 _database_code_depnum_ccdc_archive 'CCDC 817394' #TrackingRef '- allComplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H31 Br2 N4 O2 Rh' _chemical_formula_weight 610.21 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.8107(11) _cell_length_b 12.0520(9) _cell_length_c 16.1426(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.827(12) _cell_angle_gamma 90.00 _cell_volume 2285.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44953 _cell_measurement_theta_min 1.735 _cell_measurement_theta_max 29.575 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 4.265 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2234 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.07 _reflns_number_total 2234 _reflns_number_gt 1560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2234 _refine_ls_number_parameters 190 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0431 _refine_ls_goodness_of_fit_ref 0.673 _refine_ls_restrained_S_all 0.672 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2378(9) 0.0939(7) 0.5039(6) 0.0217(8) Uani 1 1 d . . . C2 C 1.3050(7) 0.1802(7) 0.3947(5) 0.0217(8) Uani 1 1 d . . . H2A H 1.3319 0.2371 0.3610 0.026 Uiso 1 1 calc R . . C3 C 1.2859(7) 0.0756(7) 0.3727(5) 0.0217(8) Uani 1 1 d . . . H3A H 1.2992 0.0435 0.3208 0.026 Uiso 1 1 calc R . . C4 C 1.2169(7) -0.0967(6) 0.4357(5) 0.0236(12) Uani 1 1 d . . . H4A H 1.1905 -0.1193 0.3781 0.028 Uiso 1 1 calc R . . H4B H 1.1553 -0.1122 0.4713 0.028 Uiso 1 1 calc R . . C5 C 1.3227(8) -0.1618(7) 0.4669(5) 0.0236(12) Uani 1 1 d . . . H5A H 1.3830 -0.1470 0.4300 0.028 Uiso 1 1 calc R . . H5B H 1.3051 -0.2420 0.4637 0.028 Uiso 1 1 calc R . . C6 C 1.3672(8) -0.1323(7) 0.5561(5) 0.0236(12) Uani 1 1 d . . . H6A H 1.4358 -0.1771 0.5736 0.028 Uiso 1 1 calc R . . H6B H 1.3889 -0.0530 0.5593 0.028 Uiso 1 1 calc R . . C7 C 1.1921(7) -0.0836(6) 0.6265(5) 0.0198(7) Uani 1 1 d . . . C8 C 1.1654(6) -0.2550(7) 0.6802(5) 0.0198(7) Uani 1 1 d . . . H8A H 1.1320 -0.3144 0.7077 0.024 Uiso 1 1 calc R . . C9 C 1.2627(7) -0.2585(6) 0.6440(5) 0.0198(7) Uani 1 1 d . . . H9A H 1.3112 -0.3210 0.6410 0.024 Uiso 1 1 calc R . . C10 C 1.2777(7) 0.2997(6) 0.5143(5) 0.0209(18) Uani 1 1 d . . . H10A H 1.3488 0.3394 0.5050 0.025 Uiso 1 1 calc R . . H10B H 1.2765 0.2902 0.5751 0.025 Uiso 1 1 calc R . . C11 C 1.1777(7) 0.3694(7) 0.4815(5) 0.0226(19) Uani 1 1 d . . . H11A H 1.1068 0.3277 0.4876 0.027 Uiso 1 1 calc R . . H11B H 1.1816 0.3829 0.4213 0.027 Uiso 1 1 calc R . . C12 C 1.1725(9) 0.4807(7) 0.5259(7) 0.041(3) Uani 1 1 d . . . H12A H 1.1518 0.4678 0.5830 0.049 Uiso 1 1 calc R . . H12B H 1.2490 0.5152 0.5306 0.049 Uiso 1 1 calc R . . C13 C 1.0877(7) 0.5604(8) 0.4817(6) 0.041(2) Uani 1 1 d . . . H13A H 1.1121 0.5799 0.4273 0.061 Uiso 1 1 calc R . . H13B H 1.0835 0.6278 0.5153 0.061 Uiso 1 1 calc R . . H13C H 1.0125 0.5252 0.4739 0.061 Uiso 1 1 calc R . . C14 C 1.0105(7) -0.1196(7) 0.6944(5) 0.0202(19) Uani 1 1 d . . . H14A H 0.9526 -0.1677 0.6637 0.024 Uiso 1 1 calc R . . H14B H 0.9930 -0.0419 0.6777 0.024 Uiso 1 1 calc R . . C15 C 1.0008(7) -0.1312(7) 0.7866(5) 0.0238(19) Uani 1 1 d . . . H15A H 1.0515 -0.0768 0.8178 0.029 Uiso 1 1 calc R . . H15B H 1.0249 -0.2066 0.8053 0.029 Uiso 1 1 calc R . . C16 C 0.8774(7) -0.1111(7) 0.8043(6) 0.026(2) Uani 1 1 d . . . H16A H 0.8272 -0.1626 0.7697 0.031 Uiso 1 1 calc R . . H16B H 0.8702 -0.1289 0.8634 0.031 Uiso 1 1 calc R . . C17 C 0.8371(10) 0.0051(8) 0.7873(8) 0.055(3) Uani 1 1 d . . . H17A H 0.8888 0.0570 0.8189 0.083 Uiso 1 1 calc R . . H17B H 0.7603 0.0136 0.8043 0.083 Uiso 1 1 calc R . . H17C H 0.8360 0.0208 0.7277 0.083 Uiso 1 1 calc R . . C18 C 1.0976(7) 0.2155(7) 0.7097(6) 0.0260(15) Uani 1 1 d . . . C19 C 1.0519(8) 0.2971(7) 0.7686(6) 0.0260(15) Uani 1 1 d . . . H19A H 1.1151 0.3391 0.7974 0.039 Uiso 1 1 calc R . . H19B H 1.0116 0.2570 0.8095 0.039 Uiso 1 1 calc R . . H19C H 0.9993 0.3483 0.7371 0.039 Uiso 1 1 calc R . . N1 N 1.2788(6) 0.1913(6) 0.4755(4) 0.0217(8) Uani 1 1 d . . . N2 N 1.2434(6) 0.0210(6) 0.4380(4) 0.0217(8) Uani 1 1 d . . . N3 N 1.1233(5) -0.1489(5) 0.6698(4) 0.0198(7) Uani 1 1 d . . . N4 N 1.2794(5) -0.1540(5) 0.6119(4) 0.0198(7) Uani 1 1 d . . . O1 O 1.1008(5) 0.1131(5) 0.7280(4) 0.0219(14) Uani 1 1 d . . . O2 O 1.1313(4) 0.2483(5) 0.6422(3) 0.0224(12) Uani 1 1 d . . . Rh1 Rh 1.17566(10) 0.07819(7) 0.61255(8) 0.01472(15) Uani 1 1 d . . . Br1 Br 1.36589(6) 0.10117(7) 0.69158(5) 0.0244(3) Uani 1 1 d . . . Br2 Br 0.98863(5) 0.06603(8) 0.52924(4) 0.0228(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0249(19) 0.0287(19) 0.0119(17) 0.0029(16) 0.0036(14) 0.0001(16) C2 0.0249(19) 0.0287(19) 0.0119(17) 0.0029(16) 0.0036(14) 0.0001(16) C3 0.0249(19) 0.0287(19) 0.0119(17) 0.0029(16) 0.0036(14) 0.0001(16) C4 0.028(3) 0.019(3) 0.023(3) -0.003(2) 0.004(2) 0.003(2) C5 0.028(3) 0.019(3) 0.023(3) -0.003(2) 0.004(2) 0.003(2) C6 0.028(3) 0.019(3) 0.023(3) -0.003(2) 0.004(2) 0.003(2) C7 0.0229(19) 0.0167(15) 0.0194(19) 0.0002(14) 0.0005(14) -0.0001(14) C8 0.0229(19) 0.0167(15) 0.0194(19) 0.0002(14) 0.0005(14) -0.0001(14) C9 0.0229(19) 0.0167(15) 0.0194(19) 0.0002(14) 0.0005(14) -0.0001(14) C10 0.020(4) 0.021(4) 0.022(5) 0.002(4) 0.005(4) -0.007(4) C11 0.028(5) 0.018(4) 0.023(5) 0.001(4) 0.008(4) 0.002(4) C12 0.041(6) 0.021(5) 0.057(7) 0.001(5) -0.011(5) -0.002(4) C13 0.031(5) 0.041(6) 0.050(6) 0.015(5) 0.004(5) 0.006(5) C14 0.012(5) 0.025(4) 0.023(5) -0.002(4) 0.003(4) -0.003(3) C15 0.024(5) 0.028(4) 0.021(5) 0.004(4) 0.007(4) -0.002(4) C16 0.025(5) 0.028(5) 0.023(5) -0.002(4) 0.001(4) -0.003(4) C17 0.070(8) 0.025(5) 0.076(8) 0.008(6) 0.035(7) 0.022(5) C18 0.027(4) 0.024(3) 0.028(4) -0.010(3) 0.008(3) 0.002(3) C19 0.027(4) 0.024(3) 0.028(4) -0.010(3) 0.008(3) 0.002(3) N1 0.0249(19) 0.0287(19) 0.0119(17) 0.0029(16) 0.0036(14) 0.0001(16) N2 0.0249(19) 0.0287(19) 0.0119(17) 0.0029(16) 0.0036(14) 0.0001(16) N3 0.0229(19) 0.0167(15) 0.0194(19) 0.0002(14) 0.0005(14) -0.0001(14) N4 0.0229(19) 0.0167(15) 0.0194(19) 0.0002(14) 0.0005(14) -0.0001(14) O1 0.022(3) 0.025(3) 0.019(3) -0.003(3) 0.009(3) -0.003(3) O2 0.026(3) 0.026(3) 0.016(3) -0.001(3) 0.003(2) -0.004(3) Rh1 0.0160(3) 0.0162(3) 0.0122(3) -0.0005(3) 0.0023(3) -0.0004(3) Br1 0.0265(6) 0.0238(5) 0.0224(6) -0.0015(4) 0.0001(4) -0.0048(4) Br2 0.0176(6) 0.0283(5) 0.0226(6) 0.0014(4) 0.0021(5) 0.0009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.366(11) . ? C1 N2 1.386(11) . ? C1 Rh1 1.978(10) . ? C2 C3 1.323(11) . ? C2 N1 1.378(10) . ? C2 H2A 0.9500 . ? C3 N2 1.379(9) . ? C3 H3A 0.9500 . ? C4 N2 1.452(10) . ? C4 C5 1.517(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.465(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N3 1.372(10) . ? C7 N4 1.374(10) . ? C7 Rh1 1.970(8) . ? C8 C9 1.342(11) . ? C8 N3 1.376(10) . ? C8 H8A 0.9500 . ? C9 N4 1.384(10) . ? C9 H9A 0.9500 . ? C10 N1 1.450(10) . ? C10 C11 1.502(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.525(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.513(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N3 1.472(10) . ? C14 C15 1.511(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.533(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.495(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.262(10) . ? C18 O1 1.268(10) . ? C18 C19 1.505(11) . ? C18 Rh1 2.518(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O1 Rh1 2.183(6) . ? O2 Rh1 2.181(6) . ? Rh1 Br2 2.4710(15) . ? Rh1 Br1 2.4840(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 104.0(8) . . ? N1 C1 Rh1 123.7(7) . . ? N2 C1 Rh1 132.1(6) . . ? C3 C2 N1 107.4(7) . . ? C3 C2 H2A 126.3 . . ? N1 C2 H2A 126.3 . . ? C2 C3 N2 108.4(7) . . ? C2 C3 H3A 125.8 . . ? N2 C3 H3A 125.8 . . ? N2 C4 C5 109.2(7) . . ? N2 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C4 C5 C6 112.7(7) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C6 C5 110.0(7) . . ? N4 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N4 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 N4 103.1(6) . . ? N3 C7 Rh1 124.7(6) . . ? N4 C7 Rh1 131.2(6) . . ? C9 C8 N3 106.9(7) . . ? C9 C8 H8A 126.5 . . ? N3 C8 H8A 126.5 . . ? C8 C9 N4 107.2(7) . . ? C8 C9 H9A 126.4 . . ? N4 C9 H9A 126.4 . . ? N1 C10 C11 113.1(7) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 113.2(7) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 113.1(8) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 113.9(7) . . ? N3 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N3 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 109.7(7) . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 113.9(8) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 O1 120.1(7) . . ? O2 C18 C19 120.4(7) . . ? O1 C18 C19 119.5(8) . . ? O2 C18 Rh1 60.0(4) . . ? O1 C18 Rh1 60.1(4) . . ? C19 C18 Rh1 179.3(7) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C1 N1 C2 110.8(7) . . ? C1 N1 C10 127.7(7) . . ? C2 N1 C10 120.6(7) . . ? C3 N2 C1 109.5(7) . . ? C3 N2 C4 122.7(7) . . ? C1 N2 C4 127.7(7) . . ? C7 N3 C8 111.7(6) . . ? C7 N3 C14 126.8(6) . . ? C8 N3 C14 121.0(6) . . ? C7 N4 C9 111.1(6) . . ? C7 N4 C6 125.9(7) . . ? C9 N4 C6 122.0(7) . . ? C18 O1 Rh1 89.7(5) . . ? C18 O2 Rh1 89.9(5) . . ? C7 Rh1 C1 98.9(4) . . ? C7 Rh1 O2 158.2(3) . . ? C1 Rh1 O2 102.9(3) . . ? C7 Rh1 O1 97.9(3) . . ? C1 Rh1 O1 163.2(3) . . ? O2 Rh1 O1 60.3(2) . . ? C7 Rh1 Br2 94.4(2) . . ? C1 Rh1 Br2 85.1(3) . . ? O2 Rh1 Br2 87.35(14) . . ? O1 Rh1 Br2 93.37(18) . . ? C7 Rh1 Br1 88.7(2) . . ? C1 Rh1 Br1 92.7(3) . . ? O2 Rh1 Br1 90.42(14) . . ? O1 Rh1 Br1 87.92(18) . . ? Br2 Rh1 Br1 176.45(6) . . ? C7 Rh1 C18 128.1(3) . . ? C1 Rh1 C18 133.0(3) . . ? O2 Rh1 C18 30.1(2) . . ? O1 Rh1 C18 30.2(2) . . ? Br2 Rh1 C18 90.8(2) . . ? Br1 Rh1 C18 88.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 2.3(10) . . . . ? N2 C4 C5 C6 60.4(9) . . . . ? C4 C5 C6 N4 59.0(9) . . . . ? N3 C8 C9 N4 0.1(9) . . . . ? N1 C10 C11 C12 176.5(7) . . . . ? C10 C11 C12 C13 167.8(8) . . . . ? N3 C14 C15 C16 -173.9(7) . . . . ? C14 C15 C16 C17 -66.1(10) . . . . ? N2 C1 N1 C2 1.9(10) . . . . ? Rh1 C1 N1 C2 -173.6(7) . . . . ? N2 C1 N1 C10 170.8(7) . . . . ? Rh1 C1 N1 C10 -4.7(13) . . . . ? C3 C2 N1 C1 -2.7(10) . . . . ? C3 C2 N1 C10 -172.5(7) . . . . ? C11 C10 N1 C1 -95.2(10) . . . . ? C11 C10 N1 C2 72.8(9) . . . . ? C2 C3 N2 C1 -1.2(10) . . . . ? C2 C3 N2 C4 -177.7(7) . . . . ? N1 C1 N2 C3 -0.5(10) . . . . ? Rh1 C1 N2 C3 174.5(8) . . . . ? N1 C1 N2 C4 175.9(7) . . . . ? Rh1 C1 N2 C4 -9.1(15) . . . . ? C5 C4 N2 C3 87.8(9) . . . . ? C5 C4 N2 C1 -88.1(10) . . . . ? N4 C7 N3 C8 -0.9(8) . . . . ? Rh1 C7 N3 C8 -170.5(5) . . . . ? N4 C7 N3 C14 -173.2(7) . . . . ? Rh1 C7 N3 C14 17.1(10) . . . . ? C9 C8 N3 C7 0.5(9) . . . . ? C9 C8 N3 C14 173.4(7) . . . . ? C15 C14 N3 C7 -125.0(8) . . . . ? C15 C14 N3 C8 63.3(10) . . . . ? N3 C7 N4 C9 0.9(8) . . . . ? Rh1 C7 N4 C9 169.6(6) . . . . ? N3 C7 N4 C6 169.4(7) . . . . ? Rh1 C7 N4 C6 -22.0(12) . . . . ? C8 C9 N4 C7 -0.7(9) . . . . ? C8 C9 N4 C6 -169.6(7) . . . . ? C5 C6 N4 C7 -83.5(9) . . . . ? C5 C6 N4 C9 83.8(9) . . . . ? O2 C18 O1 Rh1 1.4(8) . . . . ? C19 C18 O1 Rh1 -179.3(7) . . . . ? O1 C18 O2 Rh1 -1.4(8) . . . . ? C19 C18 O2 Rh1 179.3(8) . . . . ? N3 C7 Rh1 C1 -151.0(7) . . . . ? N4 C7 Rh1 C1 42.5(8) . . . . ? N3 C7 Rh1 O2 28.5(11) . . . . ? N4 C7 Rh1 O2 -138.0(7) . . . . ? N3 C7 Rh1 O1 28.8(6) . . . . ? N4 C7 Rh1 O1 -137.8(7) . . . . ? N3 C7 Rh1 Br2 -65.3(6) . . . . ? N4 C7 Rh1 Br2 128.2(7) . . . . ? N3 C7 Rh1 Br1 116.5(6) . . . . ? N4 C7 Rh1 Br1 -50.0(7) . . . . ? N3 C7 Rh1 C18 29.2(8) . . . . ? N4 C7 Rh1 C18 -137.3(7) . . . . ? N1 C1 Rh1 C7 -159.2(8) . . . . ? N2 C1 Rh1 C7 26.6(10) . . . . ? N1 C1 Rh1 O2 21.0(9) . . . . ? N2 C1 Rh1 O2 -153.2(9) . . . . ? N1 C1 Rh1 O1 22(2) . . . . ? N2 C1 Rh1 O1 -152.5(9) . . . . ? N1 C1 Rh1 Br2 107.1(8) . . . . ? N2 C1 Rh1 Br2 -67.1(9) . . . . ? N1 C1 Rh1 Br1 -70.1(8) . . . . ? N2 C1 Rh1 Br1 115.7(9) . . . . ? N1 C1 Rh1 C18 20.6(11) . . . . ? N2 C1 Rh1 C18 -153.6(8) . . . . ? C18 O2 Rh1 C7 1.1(9) . . . . ? C18 O2 Rh1 C1 -179.4(6) . . . . ? C18 O2 Rh1 O1 0.8(5) . . . . ? C18 O2 Rh1 Br2 96.2(5) . . . . ? C18 O2 Rh1 Br1 -86.6(5) . . . . ? C18 O1 Rh1 C7 179.3(5) . . . . ? C18 O1 Rh1 C1 -1.6(18) . . . . ? C18 O1 Rh1 O2 -0.8(5) . . . . ? C18 O1 Rh1 Br2 -85.8(5) . . . . ? C18 O1 Rh1 Br1 90.9(5) . . . . ? O2 C18 Rh1 C7 -179.5(4) . . . . ? O1 C18 Rh1 C7 -0.9(7) . . . . ? C19 C18 Rh1 C7 56(58) . . . . ? O2 C18 Rh1 C1 0.7(8) . . . . ? O1 C18 Rh1 C1 179.4(7) . . . . ? C19 C18 Rh1 C1 -124(58) . . . . ? O1 C18 Rh1 O2 178.6(8) . . . . ? C19 C18 Rh1 O2 -125(58) . . . . ? O2 C18 Rh1 O1 -178.6(8) . . . . ? C19 C18 Rh1 O1 57(58) . . . . ? O2 C18 Rh1 Br2 -83.3(5) . . . . ? O1 C18 Rh1 Br2 95.3(5) . . . . ? C19 C18 Rh1 Br2 152(58) . . . . ? O2 C18 Rh1 Br1 93.2(5) . . . . ? O1 C18 Rh1 Br1 -88.2(5) . . . . ? C19 C18 Rh1 Br1 -31(58) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.604 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.135 # start Validation Reply Form _vrf_PLAT036_complex-5 ; PROBLEM: No s.u. Given for Flack Parameter ......... ? RESPONSE: The compound crystallizes as racemic twin. In SHELXL, a TWIN refinement has been performed. ; # end Validation Reply Form #===END data_complex-6 _database_code_depnum_ccdc_archive 'CCDC 817395' #TrackingRef '- allComplexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H30 I2 N5 Rh' _chemical_formula_sum 'C19 H30 I2 N5 Rh' _chemical_formula_weight 685.19 _chemical_absolute_configuration ad 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.6131(11) _cell_length_b 8.3587(11) _cell_length_c 10.6771(15) _cell_angle_alpha 68.734(3) _cell_angle_beta 73.159(3) _cell_angle_gamma 66.537(3) _cell_volume 572.37(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4612 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.33 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330 _exptl_absorpt_coefficient_mu 3.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5474 _exptl_absorpt_correction_T_max 0.9663 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) for selected reflections was 0.066 before and 0.033 after correction. The Ratio of minimum to maximum transmission is 0.566535. The \l/2 correction factor is 0.0015 ; _exptl_special_details ; DELU restraints were applied to all thermal displacement parameters. This was necessary because due to the small unit cell and the low symmetry only little data was available for absorption correction. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9954 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4798 _reflns_number_gt 4510 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+2.3755P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 4798 _refine_ls_number_parameters 247 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.37992(8) 0.70893(8) 0.54077(6) 0.00983(15) Uani 1 1 d U . . I1 I 0.43713(6) 0.70565(6) 0.78574(5) 0.01445(14) Uani 1 1 d U . . I2 I 0.49401(6) 1.00932(6) 0.39304(5) 0.01495(14) Uani 1 1 d U . . N1 N 0.3621(12) 0.6736(11) 0.2605(7) 0.0157(15) Uani 1 1 d U . . N2 N 0.1216(10) 0.8679(10) 0.3510(8) 0.0169(14) Uani 1 1 d U . . N3 N 0.0763(9) 0.5641(9) 0.6934(7) 0.0129(13) Uani 1 1 d U . . N4 N 0.3286(10) 0.3295(9) 0.6816(7) 0.0121(13) Uani 1 1 d U . . N5 N 0.6775(10) 0.5566(10) 0.4967(7) 0.0135(13) Uani 1 1 d U . . C1 C 0.2938(12) 0.7387(11) 0.3717(8) 0.0110(13) Uani 1 1 d U . . C2 C 0.2333(14) 0.7674(13) 0.1709(10) 0.0215(18) Uani 1 1 d U . . H2 H 0.2483 0.7497 0.0849 0.026 Uiso 1 1 calc R . . C3 C 0.0831(13) 0.8879(12) 0.2253(9) 0.0174(16) Uani 1 1 d U . . H3 H -0.0281 0.9711 0.1860 0.021 Uiso 1 1 calc R . . C4 C 0.0191(12) 0.9751(12) 0.4454(9) 0.0143(16) Uani 1 1 d U . . H4A H -0.1223 0.9987 0.4592 0.017 Uiso 1 1 calc R . . H4B H 0.0425 1.0933 0.4095 0.017 Uiso 1 1 calc R . . C5 C 0.0940(11) 0.8684(11) 0.5796(9) 0.0135(13) Uani 1 1 d U . . H5 H 0.0906 0.9579 0.6227 0.016 Uiso 1 1 calc R . . C6 C -0.0302(13) 0.7555(12) 0.6801(10) 0.0206(19) Uani 1 1 d U . . H6A H -0.0632 0.7788 0.7700 0.025 Uiso 1 1 calc R . . H6B H -0.1528 0.7904 0.6470 0.025 Uiso 1 1 calc R . . C7 C 0.2673(11) 0.5111(11) 0.6457(9) 0.0109(13) Uani 1 1 d U . . C8 C 0.0178(13) 0.4150(12) 0.7643(9) 0.0178(17) Uani 1 1 d U . . H8 H -0.1097 0.4160 0.8099 0.021 Uiso 1 1 calc R . . C9 C 0.1751(13) 0.2677(12) 0.7566(9) 0.0173(16) Uani 1 1 d U . . H9 H 0.1801 0.1445 0.7953 0.021 Uiso 1 1 calc R . . C10 C 0.5381(13) 0.5192(11) 0.2451(8) 0.0163(16) Uani 1 1 d U . . H10A H 0.5117 0.4422 0.2056 0.020 Uiso 1 1 calc R . . H10B H 0.5723 0.4448 0.3362 0.020 Uiso 1 1 calc R . . C11 C 0.7089(14) 0.5767(13) 0.1550(10) 0.0193(18) Uani 1 1 d U . . H11A H 0.7405 0.6487 0.1960 0.023 Uiso 1 1 calc R . . H11B H 0.6748 0.6542 0.0644 0.023 Uiso 1 1 calc R . . C12 C 0.8857(14) 0.4091(14) 0.1386(10) 0.023(2) Uani 1 1 d U . . H12A H 0.9075 0.3244 0.2300 0.028 Uiso 1 1 calc R . . H12B H 0.8580 0.3459 0.0878 0.028 Uiso 1 1 calc R . . C13 C 1.0685(15) 0.4557(15) 0.0643(10) 0.030(2) Uani 1 1 d U . . H13A H 1.0497 0.5355 -0.0277 0.044 Uiso 1 1 calc R . . H13B H 1.1772 0.3438 0.0581 0.044 Uiso 1 1 calc R . . H13C H 1.0970 0.5179 0.1142 0.044 Uiso 1 1 calc R . . C14 C 0.5306(12) 0.2113(11) 0.6550(9) 0.0126(15) Uani 1 1 d U . . H14A H 0.5902 0.2627 0.5608 0.015 Uiso 1 1 calc R . . H14B H 0.5310 0.0899 0.6617 0.015 Uiso 1 1 calc R . . C15 C 0.6514(12) 0.1903(11) 0.7522(9) 0.0138(16) Uani 1 1 d U . . H15A H 0.7894 0.1293 0.7186 0.017 Uiso 1 1 calc R . . H15B H 0.6391 0.3126 0.7524 0.017 Uiso 1 1 calc R . . C16 C 0.5980(14) 0.0848(16) 0.8946(10) 0.026(2) Uani 1 1 d U . . H16A H 0.6041 -0.0359 0.8950 0.032 Uiso 1 1 calc R . . H16B H 0.4626 0.1490 0.9312 0.032 Uiso 1 1 calc R . . C17 C 0.7345(16) 0.0593(17) 0.9877(11) 0.034(3) Uani 1 1 d U . . H17A H 0.8676 -0.0097 0.9545 0.051 Uiso 1 1 calc R . . H17B H 0.6923 -0.0071 1.0811 0.051 Uiso 1 1 calc R . . H17C H 0.7301 0.1786 0.9866 0.051 Uiso 1 1 calc R . . C18 C 0.8404(12) 0.4978(11) 0.4714(9) 0.0131(16) Uani 1 1 d U . . C19 C 1.0512(12) 0.4261(12) 0.4353(10) 0.0170(18) Uani 1 1 d U . . H19A H 1.0991 0.3016 0.4933 0.025 Uiso 1 1 calc R . . H19B H 1.1098 0.5025 0.4490 0.025 Uiso 1 1 calc R . . H19C H 1.0864 0.4261 0.3395 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0053(3) 0.0107(3) 0.0140(3) -0.0052(3) -0.0017(2) -0.0015(2) I1 0.0115(3) 0.0197(3) 0.0145(3) -0.0071(2) -0.0017(2) -0.0058(2) I2 0.0112(3) 0.0135(3) 0.0203(3) -0.0041(2) -0.0025(2) -0.0049(2) N1 0.023(3) 0.019(4) 0.004(3) -0.006(3) 0.002(3) -0.006(3) N2 0.014(3) 0.022(4) 0.018(3) -0.009(3) -0.007(3) -0.003(3) N3 0.005(3) 0.014(3) 0.016(4) -0.004(3) -0.001(3) 0.000(2) N4 0.012(3) 0.005(3) 0.016(4) -0.003(3) -0.006(3) 0.003(2) N5 0.010(2) 0.015(3) 0.016(3) -0.005(3) -0.002(2) -0.004(2) C1 0.011(3) 0.010(4) 0.013(3) -0.003(3) -0.001(2) -0.006(2) C2 0.025(4) 0.026(5) 0.019(4) -0.009(4) -0.009(3) -0.008(3) C3 0.023(4) 0.017(4) 0.015(4) -0.001(3) -0.007(3) -0.010(3) C4 0.006(3) 0.021(4) 0.018(4) -0.009(3) -0.003(3) -0.003(3) C5 0.008(3) 0.014(3) 0.017(3) -0.007(3) -0.002(2) -0.001(2) C6 0.009(3) 0.015(3) 0.029(5) -0.007(3) 0.006(3) 0.000(3) C7 0.006(3) 0.010(2) 0.015(4) -0.001(3) -0.004(3) 0.000(2) C8 0.014(3) 0.019(3) 0.020(5) -0.002(4) 0.000(3) -0.009(3) C9 0.020(3) 0.016(3) 0.019(5) 0.000(3) -0.008(3) -0.009(3) C10 0.027(4) 0.012(4) 0.007(4) -0.001(3) 0.000(3) -0.008(3) C11 0.024(4) 0.018(4) 0.015(5) -0.005(4) 0.001(3) -0.009(3) C12 0.023(4) 0.024(5) 0.022(5) -0.003(4) -0.007(4) -0.007(3) C13 0.024(4) 0.043(6) 0.024(5) -0.018(5) 0.007(4) -0.012(4) C14 0.015(3) 0.005(3) 0.020(4) -0.005(3) -0.006(3) -0.002(3) C15 0.014(4) 0.008(4) 0.015(4) -0.003(3) -0.006(3) 0.002(3) C16 0.011(4) 0.039(6) 0.016(4) 0.008(4) -0.004(4) -0.008(4) C17 0.034(6) 0.047(7) 0.021(5) 0.001(5) -0.011(4) -0.018(5) C18 0.011(3) 0.009(4) 0.021(5) -0.006(3) -0.004(3) -0.003(3) C19 0.011(3) 0.020(5) 0.026(5) -0.014(4) -0.002(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C7 1.988(8) . ? Rh1 C1 1.995(8) . ? Rh1 C5 2.063(8) . ? Rh1 N5 2.120(7) . ? Rh1 I2 2.7598(8) . ? Rh1 I1 2.7623(9) . ? N1 C1 1.365(11) . ? N1 C2 1.371(12) . ? N1 C10 1.462(12) . ? N2 C1 1.342(11) . ? N2 C3 1.393(11) . ? N2 C4 1.439(11) . ? N3 C7 1.338(10) . ? N3 C8 1.374(11) . ? N3 C6 1.451(11) . ? N4 C7 1.337(11) . ? N4 C9 1.382(11) . ? N4 C14 1.471(10) . ? N5 C18 1.127(11) . ? C2 C3 1.335(13) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.522(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(12) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.341(13) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.511(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.531(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.512(13) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.499(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.487(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.543(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.458(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C7 Rh1 C1 91.5(3) . . ? C7 Rh1 C5 81.7(3) . . ? C1 Rh1 C5 80.6(3) . . ? C7 Rh1 N5 101.0(3) . . ? C1 Rh1 N5 99.5(3) . . ? C5 Rh1 N5 177.2(3) . . ? C7 Rh1 I2 173.6(2) . . ? C1 Rh1 I2 85.9(2) . . ? C5 Rh1 I2 92.0(2) . . ? N5 Rh1 I2 85.26(19) . . ? C7 Rh1 I1 87.5(2) . . ? C1 Rh1 I1 170.4(2) . . ? C5 Rh1 I1 89.8(2) . . ? N5 Rh1 I1 89.99(19) . . ? I2 Rh1 I1 94.01(2) . . ? C1 N1 C2 109.3(8) . . ? C1 N1 C10 124.8(7) . . ? C2 N1 C10 125.7(8) . . ? C1 N2 C3 109.9(7) . . ? C1 N2 C4 119.6(7) . . ? C3 N2 C4 130.0(7) . . ? C7 N3 C8 110.0(7) . . ? C7 N3 C6 119.6(7) . . ? C8 N3 C6 129.9(7) . . ? C7 N4 C9 109.7(7) . . ? C7 N4 C14 125.7(7) . . ? C9 N4 C14 124.5(7) . . ? C18 N5 Rh1 170.1(7) . . ? N2 C1 N1 105.9(7) . . ? N2 C1 Rh1 114.6(6) . . ? N1 C1 Rh1 139.3(6) . . ? C3 C2 N1 108.2(8) . . ? C3 C2 H2 125.9 . . ? N1 C2 H2 125.9 . . ? C2 C3 N2 106.6(8) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 C5 107.6(7) . . ? N2 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? N2 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C4 C5 C6 113.1(7) . . ? C4 C5 Rh1 109.3(6) . . ? C6 C5 Rh1 111.4(6) . . ? C4 C5 H5 107.6 . . ? C6 C5 H5 107.6 . . ? Rh1 C5 H5 107.6 . . ? N3 C6 C5 109.4(7) . . ? N3 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N4 C7 N3 106.4(7) . . ? N4 C7 Rh1 137.5(6) . . ? N3 C7 Rh1 116.0(6) . . ? C9 C8 N3 106.9(8) . . ? C9 C8 H8 126.5 . . ? N3 C8 H8 126.5 . . ? C8 C9 N4 106.9(8) . . ? C8 C9 H9 126.5 . . ? N4 C9 H9 126.5 . . ? N1 C10 C11 112.8(7) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 110.1(7) . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C11 112.8(8) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 112.9(7) . . ? N4 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N4 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 114.3(8) . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C15 C16 C17 111.8(8) . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C19 178.4(10) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 C3 N2 C1 N1 -1.6(10) . . . . ? C4 N2 C1 N1 -174.5(7) . . . . ? C3 N2 C1 Rh1 175.0(6) . . . . ? C4 N2 C1 Rh1 2.1(10) . . . . ? C2 N1 C1 N2 1.8(10) . . . . ? C10 N1 C1 N2 -174.2(8) . . . . ? C2 N1 C1 Rh1 -173.5(7) . . . . ? C10 N1 C1 Rh1 10.5(15) . . . . ? C7 Rh1 C1 N2 94.3(6) . . . . ? C5 Rh1 C1 N2 13.0(6) . . . . ? N5 Rh1 C1 N2 -164.2(6) . . . . ? I2 Rh1 C1 N2 -79.8(6) . . . . ? C7 Rh1 C1 N1 -90.7(10) . . . . ? C5 Rh1 C1 N1 -172.1(10) . . . . ? N5 Rh1 C1 N1 10.7(10) . . . . ? I2 Rh1 C1 N1 95.2(9) . . . . ? C1 N1 C2 C3 -1.3(11) . . . . ? C10 N1 C2 C3 174.6(8) . . . . ? N1 C2 C3 N2 0.3(10) . . . . ? C1 N2 C3 C2 0.8(10) . . . . ? C4 N2 C3 C2 172.8(9) . . . . ? C1 N2 C4 C5 -21.9(11) . . . . ? C3 N2 C4 C5 166.8(8) . . . . ? N2 C4 C5 C6 -94.6(8) . . . . ? N2 C4 C5 Rh1 30.1(8) . . . . ? C7 Rh1 C5 C4 -116.7(6) . . . . ? C1 Rh1 C5 C4 -23.8(6) . . . . ? I2 Rh1 C5 C4 61.7(6) . . . . ? I1 Rh1 C5 C4 155.7(6) . . . . ? C7 Rh1 C5 C6 8.9(6) . . . . ? C1 Rh1 C5 C6 101.9(7) . . . . ? I2 Rh1 C5 C6 -172.6(6) . . . . ? I1 Rh1 C5 C6 -78.6(6) . . . . ? C7 N3 C6 C5 13.9(12) . . . . ? C8 N3 C6 C5 -174.9(8) . . . . ? C4 C5 C6 N3 109.5(9) . . . . ? Rh1 C5 C6 N3 -14.1(9) . . . . ? C9 N4 C7 N3 -1.9(10) . . . . ? C14 N4 C7 N3 -177.7(7) . . . . ? C9 N4 C7 Rh1 -179.5(7) . . . . ? C14 N4 C7 Rh1 4.7(14) . . . . ? C8 N3 C7 N4 2.2(10) . . . . ? C6 N3 C7 N4 175.0(8) . . . . ? C8 N3 C7 Rh1 -179.6(6) . . . . ? C6 N3 C7 Rh1 -6.8(11) . . . . ? C1 Rh1 C7 N4 95.4(9) . . . . ? C5 Rh1 C7 N4 175.7(10) . . . . ? N5 Rh1 C7 N4 -4.6(10) . . . . ? I1 Rh1 C7 N4 -94.1(9) . . . . ? C1 Rh1 C7 N3 -82.0(7) . . . . ? C5 Rh1 C7 N3 -1.7(6) . . . . ? N5 Rh1 C7 N3 178.0(6) . . . . ? I1 Rh1 C7 N3 88.5(6) . . . . ? C7 N3 C8 C9 -1.7(10) . . . . ? C6 N3 C8 C9 -173.6(9) . . . . ? N3 C8 C9 N4 0.5(10) . . . . ? C7 N4 C9 C8 0.9(10) . . . . ? C14 N4 C9 C8 176.8(8) . . . . ? C1 N1 C10 C11 -101.4(10) . . . . ? C2 N1 C10 C11 83.3(11) . . . . ? N1 C10 C11 C12 -177.8(7) . . . . ? C10 C11 C12 C13 -172.8(8) . . . . ? C7 N4 C14 C15 78.4(10) . . . . ? C9 N4 C14 C15 -96.9(9) . . . . ? N4 C14 C15 C16 68.9(10) . . . . ? C14 C15 C16 C17 176.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.168 _refine_diff_density_min -2.919 _refine_diff_density_rms 0.185