# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Douglas Stephan' _publ_contact_author_email stephan@uwindsor.ca loop_ _publ_author_name D.W.Stephan S.J.Geier data_RhNacNac(Ph2PPPh2) _database_code_depnum_ccdc_archive 'CCDC 658230' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C53 H61 N2 P2 Rh' _chemical_formula_weight 890.89 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8591(11) _cell_length_b 35.296(4) _cell_length_c 12.6312(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.769(2) _cell_angle_gamma 90.00 _cell_volume 4824.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.278556 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 46044 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8472 _reflns_number_gt 6281 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0687P)^2^+0.0997P] 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_number_reflns 8472 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.029 _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 0.36159(2) 0.139640(8) 0.25199(2) 0.05202(11) Uani 1 1 d . . . P1 P 0.37166(9) 0.07847(3) 0.29604(8) 0.0561(2) Uani 1 1 d . . . P2 P 0.36818(9) 0.11940(3) 0.42064(7) 0.0552(2) Uani 1 1 d . . . N1 N 0.3280(3) 0.14259(8) 0.0888(2) 0.0580(7) Uani 1 1 d . . . N2 N 0.3918(2) 0.19706(8) 0.2593(2) 0.0515(7) Uani 1 1 d . . . C1 C 0.2864(4) 0.10873(11) 0.0326(3) 0.0641(10) Uani 1 1 d . . . C2 C 0.3746(4) 0.08316(12) -0.0007(3) 0.0719(11) Uani 1 1 d . . . C3 C 0.3314(5) 0.05176(14) -0.0589(4) 0.0910(14) Uani 1 1 d . . . H3A H 0.3879 0.0347 -0.0834 0.109 Uiso 1 1 calc R . . C4 C 0.2068(6) 0.04529(15) -0.0811(4) 0.0991(16) Uani 1 1 d . . . H4A H 0.1797 0.0239 -0.1191 0.119 Uiso 1 1 calc R . . C5 C 0.1228(5) 0.07069(14) -0.0467(4) 0.0911(14) Uani 1 1 d . . . H5A H 0.0389 0.0661 -0.0621 0.109 Uiso 1 1 calc R . . C6 C 0.1589(4) 0.10272(12) 0.0096(3) 0.0755(11) Uani 1 1 d . . . C7 C 0.5108(4) 0.08950(14) 0.0231(4) 0.0825(12) Uani 1 1 d . . . H7A H 0.5213 0.1009 0.0941 0.099 Uiso 1 1 calc R . . C8 C 0.5873(5) 0.05327(16) 0.0283(4) 0.1148(19) Uani 1 1 d . . . H8A H 0.5531 0.0356 0.0757 0.172 Uiso 1 1 calc R . . H8B H 0.6710 0.0591 0.0537 0.172 Uiso 1 1 calc R . . H8C H 0.5861 0.0423 -0.0414 0.172 Uiso 1 1 calc R . . C9 C 0.5655(6) 0.1178(2) -0.0530(6) 0.145(3) Uani 1 1 d . . . H9A H 0.5172 0.1406 -0.0562 0.218 Uiso 1 1 calc R . . H9B H 0.5642 0.1068 -0.1226 0.218 Uiso 1 1 calc R . . H9C H 0.6491 0.1236 -0.0276 0.218 Uiso 1 1 calc R . . C10 C 0.0632(5) 0.12980(16) 0.0453(5) 0.1024(17) Uani 1 1 d . . . H10A H 0.1056 0.1527 0.0731 0.123 Uiso 1 1 calc R . . C11 C -0.0327(6) 0.14159(18) -0.0455(6) 0.138(2) Uani 1 1 d . . . H11A H 0.0088 0.1528 -0.1020 0.207 Uiso 1 1 calc R . . H11B H -0.0890 0.1596 -0.0194 0.207 Uiso 1 1 calc R . . H11C H -0.0778 0.1197 -0.0718 0.207 Uiso 1 1 calc R . . C12 C -0.0032(6) 0.1121(3) 0.1339(5) 0.165(3) Uani 1 1 d . . . H12A H 0.0562 0.1046 0.1907 0.247 Uiso 1 1 calc R . . H12B H -0.0482 0.0902 0.1073 0.247 Uiso 1 1 calc R . . H12C H -0.0595 0.1301 0.1599 0.247 Uiso 1 1 calc R . . C13 C 0.3026(5) 0.17274(13) -0.0894(3) 0.0896(14) Uani 1 1 d . . . H13A H 0.3091 0.1472 -0.1144 0.134 Uiso 1 1 calc R . . H13B H 0.3592 0.1886 -0.1235 0.134 Uiso 1 1 calc R . . H13C H 0.2198 0.1817 -0.1058 0.134 Uiso 1 1 calc R . . C14 C 0.3338(4) 0.17381(11) 0.0306(3) 0.0639(9) Uani 1 1 d . . . C15 C 0.3671(3) 0.20932(11) 0.0718(3) 0.0640(9) Uani 1 1 d . . . H15A H 0.3736 0.2283 0.0216 0.077 Uiso 1 1 calc R . . C16 C 0.3918(3) 0.22046(10) 0.1766(3) 0.0581(9) Uani 1 1 d . . . C17 C 0.4192(4) 0.26257(11) 0.1932(3) 0.0744(11) Uani 1 1 d . . . H17A H 0.3824 0.2712 0.2554 0.112 Uiso 1 1 calc R . . H17B H 0.3854 0.2766 0.1324 0.112 Uiso 1 1 calc R . . H17C H 0.5070 0.2664 0.2024 0.112 Uiso 1 1 calc R . . C18 C 0.4320(3) 0.21357(10) 0.3607(3) 0.0576(9) Uani 1 1 d . . . C19 C 0.3455(4) 0.22835(12) 0.4250(3) 0.0689(10) Uani 1 1 d . . . C20 C 0.3885(5) 0.24753(13) 0.5162(4) 0.0891(14) Uani 1 1 d . . . H20A H 0.3320 0.2578 0.5596 0.107 Uiso 1 1 calc R . . C21 C 0.5114(6) 0.25175(14) 0.5440(4) 0.0931(15) Uani 1 1 d . . . H21A H 0.5381 0.2656 0.6043 0.112 Uiso 1 1 calc R . . C22 C 0.5959(4) 0.23556(14) 0.4828(4) 0.0855(13) Uani 1 1 d . . . H22A H 0.6798 0.2381 0.5033 0.103 Uiso 1 1 calc R . . C23 C 0.5591(4) 0.21539(11) 0.3909(3) 0.0673(10) Uani 1 1 d . . . C24 C 0.2072(4) 0.22369(17) 0.3962(4) 0.1007(16) Uani 1 1 d . . . H24A H 0.1957 0.2029 0.3450 0.121 Uiso 1 1 calc R . . C25 C 0.1359(5) 0.21399(16) 0.4911(5) 0.1171(19) Uani 1 1 d . . . H25A H 0.0498 0.2114 0.4683 0.176 Uiso 1 1 calc R . . H25B H 0.1465 0.2339 0.5429 0.176 Uiso 1 1 calc R . . H25C H 0.1664 0.1906 0.5219 0.176 Uiso 1 1 calc R . . C26 C 0.1516(6) 0.2585(3) 0.3452(7) 0.189(4) Uani 1 1 d . . . H26A H 0.0647 0.2546 0.3282 0.283 Uiso 1 1 calc R . . H26B H 0.1905 0.2638 0.2812 0.283 Uiso 1 1 calc R . . H26C H 0.1639 0.2795 0.3931 0.283 Uiso 1 1 calc R . . C27 C 0.6528(4) 0.19626(16) 0.3263(4) 0.0904(14) Uani 1 1 d . . . H27A H 0.6074 0.1800 0.2737 0.109 Uiso 1 1 calc R . . C28 C 0.7436(5) 0.17187(16) 0.3911(5) 0.1151(19) Uani 1 1 d . . . H28A H 0.8001 0.1607 0.3456 0.173 Uiso 1 1 calc R . . H28B H 0.7001 0.1523 0.4252 0.173 Uiso 1 1 calc R . . H28C H 0.7887 0.1871 0.4441 0.173 Uiso 1 1 calc R . . C29 C 0.7277(7) 0.2236(2) 0.2672(6) 0.180(4) Uani 1 1 d . . . H29A H 0.7851 0.2098 0.2280 0.270 Uiso 1 1 calc R . . H29B H 0.7722 0.2402 0.3168 0.270 Uiso 1 1 calc R . . H29C H 0.6737 0.2382 0.2190 0.270 Uiso 1 1 calc R . . C30 C 0.5170(4) 0.05213(11) 0.3029(3) 0.0643(9) Uani 1 1 d . . . C31 C 0.6258(4) 0.07241(14) 0.2973(3) 0.0792(12) Uani 1 1 d . . . H31A H 0.6227 0.0985 0.2868 0.095 Uiso 1 1 calc R . . C32 C 0.7376(5) 0.05430(19) 0.3070(4) 0.0991(16) Uani 1 1 d . . . H32A H 0.8101 0.0682 0.3050 0.119 Uiso 1 1 calc R . . C33 C 0.7436(6) 0.0155(2) 0.3198(4) 0.114(2) Uani 1 1 d . . . H33A H 0.8197 0.0032 0.3265 0.137 Uiso 1 1 calc R . . C34 C 0.6373(6) -0.00480(16) 0.3226(4) 0.1034(17) Uani 1 1 d . . . H34A H 0.6408 -0.0310 0.3297 0.124 Uiso 1 1 calc R . . C35 C 0.5243(5) 0.01338(13) 0.3149(4) 0.0829(12) Uani 1 1 d . . . H35A H 0.4523 -0.0007 0.3179 0.100 Uiso 1 1 calc R . . C36 C 0.2554(3) 0.04116(10) 0.2973(3) 0.0611(9) Uani 1 1 d . . . C37 C 0.2064(5) 0.02798(14) 0.2017(4) 0.1014(17) Uani 1 1 d . . . H37A H 0.2322 0.0384 0.1396 0.122 Uiso 1 1 calc R . . C38 C 0.1192(6) -0.00045(16) 0.1954(5) 0.123(2) Uani 1 1 d . . . H38A H 0.0876 -0.0093 0.1292 0.148 Uiso 1 1 calc R . . C39 C 0.0794(5) -0.01562(14) 0.2845(6) 0.1040(18) Uani 1 1 d . . . H39A H 0.0201 -0.0347 0.2800 0.125 Uiso 1 1 calc R . . C40 C 0.1265(5) -0.00280(13) 0.3808(5) 0.0932(15) Uani 1 1 d . . . H40A H 0.0989 -0.0130 0.4424 0.112 Uiso 1 1 calc R . . C41 C 0.2162(4) 0.02567(12) 0.3878(4) 0.0804(12) Uani 1 1 d . . . H41A H 0.2491 0.0341 0.4539 0.096 Uiso 1 1 calc R . . C42 C 0.4936(3) 0.11687(11) 0.5255(3) 0.0598(9) Uani 1 1 d . . . C43 C 0.5236(4) 0.14964(13) 0.5818(3) 0.0813(12) Uani 1 1 d . . . H43A H 0.4801 0.1719 0.5653 0.098 Uiso 1 1 calc R . . C44 C 0.6174(5) 0.14962(17) 0.6623(4) 0.1001(16) Uani 1 1 d . . . H44A H 0.6376 0.1719 0.6992 0.120 Uiso 1 1 calc R . . C45 C 0.6811(4) 0.1171(2) 0.6882(4) 0.0995(17) Uani 1 1 d . . . H45A H 0.7446 0.1172 0.7424 0.119 Uiso 1 1 calc R . . C46 C 0.6513(4) 0.08443(17) 0.6348(4) 0.0958(15) Uani 1 1 d . . . H46A H 0.6942 0.0623 0.6530 0.115 Uiso 1 1 calc R . . C47 C 0.5576(4) 0.08402(14) 0.5535(3) 0.0791(12) Uani 1 1 d . . . H47A H 0.5376 0.0616 0.5176 0.095 Uiso 1 1 calc R . . C48 C 0.2315(3) 0.11460(10) 0.4951(3) 0.0620(9) Uani 1 1 d . . . C49 C 0.1152(4) 0.11596(13) 0.4405(4) 0.0767(11) Uani 1 1 d . . . H49A H 0.1077 0.1196 0.3673 0.092 Uiso 1 1 calc R . . C50 C 0.0106(4) 0.11197(15) 0.4945(5) 0.0978(15) Uani 1 1 d . . . H50A H -0.0668 0.1120 0.4571 0.117 Uiso 1 1 calc R . . C51 C 0.0197(5) 0.10794(16) 0.6016(5) 0.1089(18) Uani 1 1 d . . . H51A H -0.0515 0.1057 0.6374 0.131 Uiso 1 1 calc R . . C52 C 0.1329(5) 0.10721(15) 0.6571(4) 0.0986(15) Uani 1 1 d . . . H52A H 0.1389 0.1048 0.7307 0.118 Uiso 1 1 calc R . . C53 C 0.2378(4) 0.11003(12) 0.6043(3) 0.0758(11) Uani 1 1 d . . . H53A H 0.3147 0.1089 0.6426 0.091 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 0.05573(17) 0.05222(17) 0.04801(16) -0.00063(12) 0.00368(11) -0.00273(13) P1 0.0606(6) 0.0527(5) 0.0551(5) -0.0017(4) 0.0046(4) -0.0037(4) P2 0.0592(5) 0.0562(5) 0.0504(5) 0.0001(4) 0.0049(4) -0.0025(4) N1 0.0626(18) 0.0644(19) 0.0470(16) -0.0026(14) 0.0043(13) -0.0019(15) N2 0.0546(16) 0.0460(15) 0.0542(17) 0.0000(13) 0.0056(13) -0.0013(12) C1 0.082(3) 0.063(2) 0.047(2) -0.0027(17) 0.0040(18) -0.003(2) C2 0.093(3) 0.069(3) 0.053(2) -0.0086(19) 0.006(2) 0.005(2) C3 0.120(4) 0.081(3) 0.072(3) -0.016(2) 0.009(3) 0.014(3) C4 0.136(5) 0.081(3) 0.077(3) -0.020(3) -0.012(3) -0.015(3) C5 0.096(3) 0.095(4) 0.078(3) -0.014(3) -0.013(3) -0.012(3) C6 0.079(3) 0.079(3) 0.066(3) -0.017(2) -0.005(2) -0.004(2) C7 0.086(3) 0.094(3) 0.069(3) -0.006(2) 0.017(2) 0.015(3) C8 0.113(4) 0.129(5) 0.101(4) -0.033(3) 0.005(3) 0.036(4) C9 0.102(4) 0.178(7) 0.164(6) 0.049(5) 0.060(4) 0.013(4) C10 0.075(3) 0.114(4) 0.116(4) -0.042(3) -0.006(3) -0.004(3) C11 0.106(4) 0.141(6) 0.162(7) 0.001(5) -0.020(4) 0.025(4) C12 0.121(5) 0.271(11) 0.103(5) -0.020(6) 0.018(4) 0.052(6) C13 0.120(4) 0.095(3) 0.052(2) 0.007(2) -0.004(2) -0.003(3) C14 0.065(2) 0.073(3) 0.053(2) 0.0028(19) 0.0032(17) 0.0020(19) C15 0.071(2) 0.064(2) 0.057(2) 0.0124(18) 0.0058(18) 0.0001(19) C16 0.0525(19) 0.056(2) 0.066(2) 0.0045(18) 0.0023(17) 0.0021(16) C17 0.083(3) 0.061(2) 0.079(3) 0.009(2) 0.007(2) -0.005(2) C18 0.069(2) 0.0480(19) 0.056(2) -0.0005(16) 0.0058(17) -0.0063(16) C19 0.078(3) 0.069(2) 0.060(2) -0.0126(19) 0.009(2) -0.003(2) C20 0.105(4) 0.088(3) 0.076(3) -0.020(3) 0.016(3) 0.001(3) C21 0.124(4) 0.081(3) 0.073(3) -0.022(2) 0.002(3) -0.014(3) C22 0.083(3) 0.088(3) 0.082(3) -0.001(3) -0.015(2) -0.025(2) C23 0.067(2) 0.069(2) 0.065(2) 0.0002(19) -0.0034(19) -0.0104(19) C24 0.083(3) 0.135(5) 0.086(3) -0.038(3) 0.016(3) 0.013(3) C25 0.110(4) 0.097(4) 0.149(5) 0.002(4) 0.037(4) 0.001(3) C26 0.092(4) 0.269(10) 0.206(9) 0.137(8) 0.024(5) 0.035(5) C27 0.061(3) 0.121(4) 0.088(3) -0.021(3) -0.007(2) 0.000(3) C28 0.091(4) 0.115(4) 0.143(5) 0.025(4) 0.031(3) 0.014(3) C29 0.170(7) 0.215(8) 0.170(7) 0.106(6) 0.100(6) 0.080(6) C30 0.070(2) 0.067(2) 0.056(2) -0.0043(18) 0.0071(18) 0.0018(19) C31 0.071(3) 0.093(3) 0.074(3) -0.011(2) 0.008(2) 0.003(2) C32 0.068(3) 0.141(5) 0.089(4) -0.019(3) 0.009(2) 0.006(3) C33 0.089(4) 0.162(6) 0.089(4) -0.012(4) 0.003(3) 0.053(4) C34 0.112(4) 0.093(4) 0.106(4) 0.001(3) 0.015(3) 0.041(3) C35 0.095(3) 0.072(3) 0.083(3) -0.003(2) 0.013(2) 0.014(2) C36 0.061(2) 0.053(2) 0.069(2) 0.0025(18) 0.0052(18) -0.0030(17) C37 0.126(4) 0.092(3) 0.083(3) 0.011(3) -0.013(3) -0.042(3) C38 0.148(5) 0.096(4) 0.117(5) 0.013(3) -0.040(4) -0.054(4) C39 0.075(3) 0.073(3) 0.162(6) 0.009(4) -0.008(3) -0.017(2) C40 0.093(3) 0.074(3) 0.118(4) 0.013(3) 0.043(3) -0.008(3) C41 0.094(3) 0.067(3) 0.082(3) 0.003(2) 0.016(2) -0.010(2) C42 0.060(2) 0.070(2) 0.049(2) 0.0042(18) 0.0046(16) -0.0052(18) C43 0.101(3) 0.079(3) 0.062(3) 0.003(2) -0.003(2) -0.015(2) C44 0.109(4) 0.119(4) 0.069(3) -0.006(3) -0.009(3) -0.036(3) C45 0.066(3) 0.169(6) 0.061(3) 0.005(3) -0.007(2) -0.010(3) C46 0.080(3) 0.130(4) 0.076(3) 0.004(3) -0.005(2) 0.028(3) C47 0.082(3) 0.090(3) 0.064(3) -0.004(2) -0.002(2) 0.007(2) C48 0.065(2) 0.055(2) 0.067(2) 0.0028(18) 0.0113(18) 0.0033(17) C49 0.066(3) 0.086(3) 0.078(3) 0.002(2) 0.007(2) 0.005(2) C50 0.061(3) 0.109(4) 0.123(4) 0.003(3) 0.008(3) 0.003(3) C51 0.088(4) 0.120(5) 0.125(5) 0.017(4) 0.047(4) 0.000(3) C52 0.095(4) 0.120(4) 0.086(3) 0.014(3) 0.034(3) -0.002(3) C53 0.076(3) 0.086(3) 0.066(3) 0.009(2) 0.016(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 2.054(3) . ? Rh1 N1 2.065(3) . ? Rh1 P1 2.2300(10) . ? Rh1 P2 2.2424(10) . ? P1 C36 1.825(4) . ? P1 C30 1.828(4) . ? P1 P2 2.1390(14) . ? P2 C42 1.821(4) . ? P2 C48 1.830(4) . ? N1 C14 1.329(5) . ? N1 C1 1.444(5) . ? N2 C16 1.331(4) . ? N2 C18 1.441(4) . ? C1 C2 1.406(5) . ? C1 C6 1.407(6) . ? C2 C3 1.390(6) . ? C2 C7 1.501(6) . ? C3 C4 1.378(7) . ? C4 C5 1.375(7) . ? C5 C6 1.376(6) . ? C6 C10 1.508(6) . ? C7 C8 1.524(6) . ? C7 C9 1.539(7) . ? C10 C12 1.517(9) . ? C10 C11 1.541(8) . ? C13 C14 1.526(5) . ? C14 C15 1.393(5) . ? C15 C16 1.385(5) . ? C16 C17 1.527(5) . ? C18 C19 1.393(5) . ? C18 C23 1.403(5) . ? C19 C20 1.384(6) . ? C19 C24 1.524(6) . ? C20 C21 1.359(7) . ? C21 C22 1.373(7) . ? C22 C23 1.393(6) . ? C23 C27 1.515(6) . ? C24 C26 1.491(8) . ? C24 C25 1.518(7) . ? C27 C29 1.499(8) . ? C27 C28 1.500(7) . ? C30 C35 1.378(6) . ? C30 C31 1.389(6) . ? C31 C32 1.368(6) . ? C32 C33 1.381(8) . ? C33 C34 1.360(8) . ? C34 C35 1.381(7) . ? C36 C37 1.360(6) . ? C36 C41 1.367(5) . ? C37 C38 1.377(7) . ? C38 C39 1.350(8) . ? C39 C40 1.357(7) . ? C40 C41 1.397(6) . ? C42 C47 1.383(6) . ? C42 C43 1.383(6) . ? C43 C44 1.379(6) . ? C44 C45 1.367(8) . ? C45 C46 1.360(7) . ? C46 C47 1.384(6) . ? C48 C53 1.386(5) . ? C48 C49 1.389(5) . ? C49 C50 1.380(6) . ? C50 C51 1.356(7) . ? C51 C52 1.364(7) . ? C52 C53 1.371(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 N1 90.52(11) . . ? N2 Rh1 P1 160.02(8) . . ? N1 Rh1 P1 107.38(9) . . ? N2 Rh1 P2 106.23(8) . . ? N1 Rh1 P2 162.38(9) . . ? P1 Rh1 P2 57.14(4) . . ? C36 P1 C30 103.15(18) . . ? C36 P1 P2 115.24(13) . . ? C30 P1 P2 112.14(13) . . ? C36 P1 Rh1 132.94(13) . . ? C30 P1 Rh1 121.91(13) . . ? P2 P1 Rh1 61.72(4) . . ? C42 P2 C48 102.22(17) . . ? C42 P2 P1 116.35(13) . . ? C48 P2 P1 112.35(13) . . ? C42 P2 Rh1 132.00(12) . . ? C48 P2 Rh1 123.67(13) . . ? P1 P2 Rh1 61.14(4) . . ? C14 N1 C1 116.2(3) . . ? C14 N1 Rh1 125.5(3) . . ? C1 N1 Rh1 118.1(2) . . ? C16 N2 C18 115.3(3) . . ? C16 N2 Rh1 126.0(2) . . ? C18 N2 Rh1 118.3(2) . . ? C2 C1 C6 121.7(4) . . ? C2 C1 N1 119.1(4) . . ? C6 C1 N1 119.3(3) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 C7 120.6(4) . . ? C1 C2 C7 121.9(4) . . ? C4 C3 C2 121.5(5) . . ? C5 C4 C3 119.6(5) . . ? C4 C5 C6 122.1(5) . . ? C5 C6 C1 117.7(4) . . ? C5 C6 C10 120.1(4) . . ? C1 C6 C10 122.3(4) . . ? C2 C7 C8 114.1(4) . . ? C2 C7 C9 113.3(4) . . ? C8 C7 C9 109.5(4) . . ? C6 C10 C12 109.9(5) . . ? C6 C10 C11 112.9(5) . . ? C12 C10 C11 109.2(5) . . ? N1 C14 C15 124.2(3) . . ? N1 C14 C13 120.8(4) . . ? C15 C14 C13 115.0(4) . . ? C16 C15 C14 129.5(4) . . ? N2 C16 C15 124.1(3) . . ? N2 C16 C17 120.6(3) . . ? C15 C16 C17 115.3(3) . . ? C19 C18 C23 121.4(4) . . ? C19 C18 N2 120.0(3) . . ? C23 C18 N2 118.6(3) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C24 120.6(4) . . ? C18 C19 C24 121.3(4) . . ? C21 C20 C19 121.7(5) . . ? C20 C21 C22 119.8(4) . . ? C21 C22 C23 121.5(4) . . ? C22 C23 C18 117.3(4) . . ? C22 C23 C27 121.2(4) . . ? C18 C23 C27 121.6(3) . . ? C26 C24 C25 108.2(5) . . ? C26 C24 C19 111.7(5) . . ? C25 C24 C19 113.2(4) . . ? C29 C27 C28 106.4(4) . . ? C29 C27 C23 113.4(5) . . ? C28 C27 C23 113.7(4) . . ? C35 C30 C31 118.4(4) . . ? C35 C30 P1 123.5(3) . . ? C31 C30 P1 118.1(3) . . ? C32 C31 C30 120.5(5) . . ? C31 C32 C33 120.4(5) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 120.3(5) . . ? C30 C35 C34 120.8(5) . . ? C37 C36 C41 118.6(4) . . ? C37 C36 P1 117.3(3) . . ? C41 C36 P1 124.1(3) . . ? C36 C37 C38 121.2(5) . . ? C39 C38 C37 120.5(5) . . ? C38 C39 C40 119.5(5) . . ? C39 C40 C41 120.3(5) . . ? C36 C41 C40 120.0(5) . . ? C47 C42 C43 118.6(4) . . ? C47 C42 P2 123.8(3) . . ? C43 C42 P2 117.6(3) . . ? C44 C43 C42 120.5(5) . . ? C45 C44 C43 120.3(5) . . ? C46 C45 C44 119.9(5) . . ? C45 C46 C47 120.4(5) . . ? C42 C47 C46 120.3(4) . . ? C53 C48 C49 117.8(4) . . ? C53 C48 P2 123.2(3) . . ? C49 C48 P2 119.0(3) . . ? C50 C49 C48 120.2(4) . . ? C51 C50 C49 120.7(5) . . ? C50 C51 C52 120.1(5) . . ? C51 C52 C53 120.0(5) . . ? C52 C53 C48 121.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.647 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.072 #===end data_RhNacNac(Et2PPEt2) _database_code_depnum_ccdc_archive 'CCDC 658231' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C37 H61 N2 P2 Rh' _chemical_formula_weight 698.73 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.566(3) _cell_length_b 11.676(4) _cell_length_c 17.636(6) _cell_angle_alpha 102.412(4) _cell_angle_beta 93.045(4) _cell_angle_gamma 114.125(4) _cell_volume 1914.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.158795 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 18475 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6726 _reflns_number_gt 6106 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1137P)^2^+0.1449P] 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_number_reflns 6726 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.013 _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 0.06574(2) 0.277892(18) -0.271033(12) 0.06049(12) Uani 1 1 d . . . P1 P -0.02460(8) 0.41981(8) -0.22896(5) 0.0715(2) Uani 1 1 d . . . P2 P -0.15441(9) 0.21786(9) -0.24861(6) 0.0793(2) Uani 1 1 d . . . N1 N 0.2670(2) 0.3810(2) -0.29148(13) 0.0577(5) Uani 1 1 d . . . N2 N 0.0972(2) 0.1115(2) -0.28887(14) 0.0616(5) Uani 1 1 d . . . C1 C 0.3165(3) 0.5195(3) -0.27876(16) 0.0620(6) Uani 1 1 d . . . C2 C 0.3702(3) 0.6000(3) -0.20141(18) 0.0697(7) Uani 1 1 d . . . C3 C 0.4165(4) 0.7335(3) -0.1917(2) 0.0857(9) Uani 1 1 d . . . H3A H 0.4521 0.7888 -0.1414 0.103 Uiso 1 1 calc R . . C4 C 0.4114(4) 0.7858(3) -0.2532(3) 0.0918(10) Uani 1 1 d . . . H4A H 0.4440 0.8753 -0.2446 0.110 Uiso 1 1 calc R . . C5 C 0.3583(4) 0.7064(3) -0.3277(2) 0.0842(9) Uani 1 1 d . . . H5A H 0.3547 0.7429 -0.3693 0.101 Uiso 1 1 calc R . . C6 C 0.3092(3) 0.5713(3) -0.34262(18) 0.0690(7) Uani 1 1 d . . . C7 C 0.3755(4) 0.5420(4) -0.13307(19) 0.0849(9) Uani 1 1 d . . . H7A H 0.2864 0.4645 -0.1409 0.102 Uiso 1 1 calc R . . C8 C 0.3868(5) 0.6330(5) -0.0524(2) 0.1199(16) Uani 1 1 d . . . H8A H 0.3916 0.5917 -0.0115 0.180 Uiso 1 1 calc R . . H8B H 0.3058 0.6508 -0.0518 0.180 Uiso 1 1 calc R . . H8C H 0.4700 0.7130 -0.0439 0.180 Uiso 1 1 calc R . . C9 C 0.4919(5) 0.4970(5) -0.1301(3) 0.1049(12) Uani 1 1 d . . . H9A H 0.4832 0.4386 -0.1797 0.157 Uiso 1 1 calc R . . H9B H 0.4842 0.4531 -0.0892 0.157 Uiso 1 1 calc R . . H9C H 0.5816 0.5709 -0.1196 0.157 Uiso 1 1 calc R . . C10 C 0.2459(4) 0.4842(3) -0.42479(19) 0.0795(8) Uani 1 1 d . . . H10A H 0.2593 0.4051 -0.4279 0.095 Uiso 1 1 calc R . . C11 C 0.0878(5) 0.4437(5) -0.4382(3) 0.1158(15) Uani 1 1 d . . . H11A H 0.0467 0.4058 -0.3971 0.174 Uiso 1 1 calc R . . H11B H 0.0465 0.3812 -0.4881 0.174 Uiso 1 1 calc R . . H11C H 0.0710 0.5186 -0.4376 0.174 Uiso 1 1 calc R . . C12 C 0.3162(8) 0.5441(5) -0.4889(3) 0.150(2) Uani 1 1 d . . . H12A H 0.2732 0.4836 -0.5393 0.225 Uiso 1 1 calc R . . H12B H 0.4143 0.5642 -0.4804 0.225 Uiso 1 1 calc R . . H12C H 0.3055 0.6223 -0.4873 0.225 Uiso 1 1 calc R . . C13 C 0.4928(3) 0.4160(3) -0.3377(2) 0.0799(8) Uani 1 1 d . . . H13A H 0.4794 0.4292 -0.3889 0.120 Uiso 1 1 calc R . . H13B H 0.5545 0.3743 -0.3373 0.120 Uiso 1 1 calc R . . H13C H 0.5335 0.4984 -0.2992 0.120 Uiso 1 1 calc R . . C14 C 0.3518(3) 0.3305(3) -0.31841(17) 0.0640(6) Uani 1 1 d . . . C15 C 0.3237(3) 0.1998(3) -0.32866(18) 0.0675(7) Uani 1 1 d . . . H15A H 0.3901 0.1757 -0.3506 0.081 Uiso 1 1 calc R . . C16 C 0.2107(3) 0.1006(3) -0.31069(17) 0.0661(6) Uani 1 1 d . . . C17 C 0.2270(4) -0.0244(3) -0.3145(2) 0.0870(9) Uani 1 1 d . . . H17A H 0.2952 -0.0103 -0.2711 0.131 Uiso 1 1 calc R . . H17B H 0.2578 -0.0494 -0.3630 0.131 Uiso 1 1 calc R . . H17C H 0.1384 -0.0923 -0.3117 0.131 Uiso 1 1 calc R . . C18 C -0.0035(3) 0.0077(3) -0.26282(18) 0.0662(6) Uani 1 1 d . . . C19 C -0.1287(3) -0.0815(3) -0.3134(2) 0.0736(7) Uani 1 1 d . . . C20 C -0.2274(4) -0.1741(3) -0.2833(3) 0.0913(10) Uani 1 1 d . . . H20A H -0.3109 -0.2341 -0.3157 0.110 Uiso 1 1 calc R . . C21 C -0.2054(4) -0.1799(4) -0.2066(3) 0.0946(11) Uani 1 1 d . . . H21A H -0.2745 -0.2418 -0.1877 0.114 Uiso 1 1 calc R . . C22 C -0.0828(4) -0.0953(4) -0.1590(2) 0.0888(10) Uani 1 1 d . . . H22A H -0.0684 -0.1012 -0.1077 0.107 Uiso 1 1 calc R . . C23 C 0.0223(3) 0.0006(3) -0.18504(19) 0.0741(7) Uani 1 1 d . . . C24 C -0.1530(4) -0.0760(3) -0.3983(2) 0.0862(9) Uani 1 1 d . . . H24A H -0.1215 0.0155 -0.3980 0.103 Uiso 1 1 calc R . . C25 C -0.3091(5) -0.1490(5) -0.4365(3) 0.1189(15) Uani 1 1 d . . . H25A H -0.3180 -0.1423 -0.4896 0.178 Uiso 1 1 calc R . . H25B H -0.3628 -0.1112 -0.4072 0.178 Uiso 1 1 calc R . . H25C H -0.3436 -0.2389 -0.4364 0.178 Uiso 1 1 calc R . . C26 C -0.0697(5) -0.1299(5) -0.4511(3) 0.1165(14) Uani 1 1 d . . . H26A H -0.0912 -0.1267 -0.5040 0.175 Uiso 1 1 calc R . . H26B H -0.0945 -0.2183 -0.4501 0.175 Uiso 1 1 calc R . . H26C H 0.0289 -0.0786 -0.4326 0.175 Uiso 1 1 calc R . . C27 C 0.1578(4) 0.0941(4) -0.1302(2) 0.0885(9) Uani 1 1 d . . . H27A H 0.2250 0.1387 -0.1622 0.106 Uiso 1 1 calc R . . C28 C 0.1357(6) 0.1977(5) -0.0702(3) 0.1149(14) Uani 1 1 d . . . H28A H 0.0949 0.2406 -0.0973 0.172 Uiso 1 1 calc R . . H28B H 0.2244 0.2602 -0.0395 0.172 Uiso 1 1 calc R . . H28C H 0.0738 0.1572 -0.0362 0.172 Uiso 1 1 calc R . . C29 C 0.2219(6) 0.0222(6) -0.0893(3) 0.1275(16) Uani 1 1 d . . . H29A H 0.2334 -0.0429 -0.1281 0.191 Uiso 1 1 calc R . . H29B H 0.1607 -0.0185 -0.0551 0.191 Uiso 1 1 calc R . . H29C H 0.3117 0.0830 -0.0591 0.191 Uiso 1 1 calc R . . C30 C -0.0970(4) 0.5068(4) -0.2802(3) 0.0884(10) Uani 1 1 d . . . H30A H -0.1260 0.4608 -0.3355 0.106 Uiso 1 1 calc R . . H30B H -0.1795 0.5070 -0.2588 0.106 Uiso 1 1 calc R . . C31 C 0.0091(5) 0.6472(4) -0.2724(3) 0.1075(13) Uani 1 1 d . . . H31A H -0.0339 0.6890 -0.2990 0.161 Uiso 1 1 calc R . . H31B H 0.0893 0.6474 -0.2956 0.161 Uiso 1 1 calc R . . H31C H 0.0382 0.6931 -0.2178 0.161 Uiso 1 1 calc R . . C32 C 0.0121(5) 0.5120(5) -0.1268(3) 0.1023(12) Uani 1 1 d . . . H32A H 0.0322 0.4619 -0.0946 0.123 Uiso 1 1 calc R . . H32B H 0.0971 0.5913 -0.1201 0.123 Uiso 1 1 calc R . . C33 C -0.1004(6) 0.5492(6) -0.0941(3) 0.1336(18) Uani 1 1 d . . . H33A H -0.0663 0.6001 -0.0406 0.200 Uiso 1 1 calc R . . H33B H -0.1834 0.4719 -0.0961 0.200 Uiso 1 1 calc R . . H33C H -0.1221 0.5991 -0.1250 0.200 Uiso 1 1 calc R . . C34 C -0.2240(5) 0.1628(5) -0.1642(3) 0.1123(14) Uani 1 1 d . . . H34A H -0.2403 0.0727 -0.1730 0.135 Uiso 1 1 calc R . . H34B H -0.1514 0.2121 -0.1186 0.135 Uiso 1 1 calc R . . C35 C -0.3591(6) 0.1719(6) -0.1430(4) 0.161(3) Uani 1 1 d . . . H35A H -0.3856 0.1358 -0.0992 0.242 Uiso 1 1 calc R . . H35B H -0.4329 0.1243 -0.1873 0.242 Uiso 1 1 calc R . . H35C H -0.3433 0.2613 -0.1294 0.242 Uiso 1 1 calc R . . C36 C -0.3134(4) 0.1533(4) -0.3215(3) 0.1130(15) Uani 1 1 d . . . H36A H -0.3636 0.0608 -0.3267 0.136 Uiso 1 1 calc R . . H36B H -0.3734 0.1934 -0.3015 0.136 Uiso 1 1 calc R . . C37 C -0.2899(6) 0.1736(5) -0.4030(4) 0.1312(19) Uani 1 1 d . . . H37A H -0.3788 0.1364 -0.4368 0.197 Uiso 1 1 calc R . . H37B H -0.2329 0.1323 -0.4243 0.197 Uiso 1 1 calc R . . H37C H -0.2433 0.2650 -0.3993 0.197 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 0.05408(16) 0.05537(16) 0.07571(18) 0.01992(11) 0.01341(11) 0.02537(11) P1 0.0634(4) 0.0641(4) 0.0925(5) 0.0190(4) 0.0164(4) 0.0332(4) P2 0.0615(4) 0.0697(5) 0.1114(6) 0.0271(4) 0.0236(4) 0.0300(4) N1 0.0531(11) 0.0579(12) 0.0635(11) 0.0202(9) 0.0123(9) 0.0228(9) N2 0.0612(12) 0.0520(11) 0.0735(13) 0.0163(9) 0.0137(10) 0.0261(10) C1 0.0529(13) 0.0601(14) 0.0759(16) 0.0228(12) 0.0134(11) 0.0241(11) C2 0.0563(15) 0.0683(16) 0.0775(17) 0.0128(13) 0.0061(12) 0.0235(13) C3 0.0749(19) 0.0665(18) 0.099(2) 0.0030(16) 0.0017(16) 0.0248(15) C4 0.082(2) 0.0551(17) 0.135(3) 0.0234(19) 0.017(2) 0.0276(16) C5 0.078(2) 0.074(2) 0.113(3) 0.0423(19) 0.0224(18) 0.0353(16) C6 0.0648(16) 0.0682(16) 0.0819(17) 0.0302(14) 0.0170(13) 0.0305(13) C7 0.077(2) 0.090(2) 0.0729(18) 0.0153(16) 0.0001(15) 0.0259(17) C8 0.116(3) 0.147(4) 0.077(2) 0.006(2) -0.004(2) 0.051(3) C9 0.112(3) 0.124(3) 0.091(2) 0.037(2) 0.000(2) 0.060(3) C10 0.093(2) 0.084(2) 0.0737(17) 0.0301(15) 0.0164(15) 0.0451(17) C11 0.119(3) 0.146(4) 0.091(2) 0.006(2) -0.015(2) 0.081(3) C12 0.221(7) 0.125(4) 0.094(3) 0.055(3) 0.056(4) 0.049(4) C13 0.0610(16) 0.0809(19) 0.106(2) 0.0367(17) 0.0285(16) 0.0311(15) C14 0.0572(14) 0.0650(15) 0.0711(15) 0.0244(12) 0.0113(12) 0.0242(12) C15 0.0622(15) 0.0720(17) 0.0799(17) 0.0233(13) 0.0201(13) 0.0374(13) C16 0.0697(16) 0.0583(14) 0.0727(15) 0.0160(12) 0.0144(13) 0.0299(13) C17 0.090(2) 0.0708(19) 0.119(3) 0.0328(18) 0.033(2) 0.0465(17) C18 0.0660(16) 0.0547(14) 0.0827(17) 0.0194(12) 0.0210(13) 0.0287(12) C19 0.0664(17) 0.0576(15) 0.095(2) 0.0176(14) 0.0157(14) 0.0253(13) C20 0.074(2) 0.0698(19) 0.123(3) 0.0260(19) 0.0201(19) 0.0230(16) C21 0.086(2) 0.077(2) 0.128(3) 0.047(2) 0.042(2) 0.0291(19) C22 0.097(3) 0.084(2) 0.098(2) 0.0381(18) 0.036(2) 0.042(2) C23 0.0790(19) 0.0691(17) 0.0850(18) 0.0271(14) 0.0221(15) 0.0377(15) C24 0.082(2) 0.0669(18) 0.092(2) 0.0097(16) 0.0027(17) 0.0219(16) C25 0.101(3) 0.101(3) 0.124(3) 0.015(3) -0.018(3) 0.024(2) C26 0.120(3) 0.114(3) 0.096(3) 0.007(2) 0.015(2) 0.042(3) C27 0.091(2) 0.092(2) 0.084(2) 0.0278(17) 0.0135(17) 0.0390(19) C28 0.131(4) 0.113(3) 0.090(3) 0.015(2) 0.007(2) 0.049(3) C29 0.117(4) 0.142(4) 0.134(4) 0.048(3) -0.004(3) 0.063(3) C30 0.077(2) 0.083(2) 0.121(3) 0.031(2) 0.0173(19) 0.0472(18) C31 0.101(3) 0.081(2) 0.164(4) 0.046(3) 0.040(3) 0.052(2) C32 0.102(3) 0.106(3) 0.099(3) 0.005(2) 0.016(2) 0.055(2) C33 0.147(4) 0.141(4) 0.127(4) 0.013(3) 0.052(3) 0.084(4) C34 0.110(3) 0.105(3) 0.146(4) 0.052(3) 0.059(3) 0.056(3) C35 0.128(4) 0.122(4) 0.208(6) 0.011(4) 0.097(4) 0.035(3) C36 0.066(2) 0.092(3) 0.165(4) 0.013(3) 0.003(2) 0.0304(19) C37 0.115(4) 0.110(3) 0.149(5) 0.018(3) -0.035(3) 0.044(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 N2 2.064(2) . ? Rh1 N1 2.068(2) . ? Rh1 P2 2.2231(11) . ? Rh1 P1 2.2465(10) . ? P1 C32 1.819(4) . ? P1 C30 1.840(4) . ? P1 P2 2.1250(14) . ? P2 C34 1.819(5) . ? P2 C36 1.834(4) . ? N1 C14 1.317(4) . ? N1 C1 1.441(3) . ? N2 C16 1.325(4) . ? N2 C18 1.431(4) . ? C1 C6 1.401(4) . ? C1 C2 1.413(4) . ? C2 C3 1.397(5) . ? C2 C7 1.513(5) . ? C3 C4 1.363(6) . ? C4 C5 1.369(6) . ? C5 C6 1.402(4) . ? C6 C10 1.513(5) . ? C7 C9 1.524(6) . ? C7 C8 1.548(5) . ? C10 C12 1.524(5) . ? C10 C11 1.527(6) . ? C13 C14 1.522(4) . ? C14 C15 1.398(4) . ? C15 C16 1.391(4) . ? C16 C17 1.527(4) . ? C18 C19 1.407(4) . ? C18 C23 1.411(4) . ? C19 C20 1.387(5) . ? C19 C24 1.524(5) . ? C20 C21 1.381(6) . ? C21 C22 1.357(6) . ? C22 C23 1.399(5) . ? C23 C27 1.515(5) . ? C24 C26 1.525(6) . ? C24 C25 1.545(5) . ? C27 C28 1.532(6) . ? C27 C29 1.536(6) . ? C30 C31 1.532(5) . ? C32 C33 1.523(6) . ? C34 C35 1.533(7) . ? C36 C37 1.523(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 N1 90.30(9) . . ? N2 Rh1 P2 105.36(7) . . ? N1 Rh1 P2 164.24(7) . . ? N2 Rh1 P1 160.10(7) . . ? N1 Rh1 P1 108.03(7) . . ? P2 Rh1 P1 56.77(4) . . ? C32 P1 C30 103.0(2) . . ? C32 P1 P2 114.21(18) . . ? C30 P1 P2 115.15(13) . . ? C32 P1 Rh1 122.09(15) . . ? C30 P1 Rh1 132.61(15) . . ? P2 P1 Rh1 61.06(4) . . ? C34 P2 C36 102.4(3) . . ? C34 P2 P1 116.75(18) . . ? C36 P2 P1 115.11(17) . . ? C34 P2 Rh1 126.51(18) . . ? C36 P2 Rh1 127.41(19) . . ? P1 P2 Rh1 62.17(3) . . ? C14 N1 C1 117.0(2) . . ? C14 N1 Rh1 125.62(19) . . ? C1 N1 Rh1 117.34(16) . . ? C16 N2 C18 118.3(2) . . ? C16 N2 Rh1 125.64(19) . . ? C18 N2 Rh1 115.24(17) . . ? C6 C1 C2 121.4(3) . . ? C6 C1 N1 119.7(2) . . ? C2 C1 N1 118.8(2) . . ? C3 C2 C1 116.9(3) . . ? C3 C2 C7 122.4(3) . . ? C1 C2 C7 120.6(3) . . ? C4 C3 C2 122.5(3) . . ? C3 C4 C5 119.9(3) . . ? C4 C5 C6 121.4(3) . . ? C1 C6 C5 117.9(3) . . ? C1 C6 C10 121.2(3) . . ? C5 C6 C10 120.9(3) . . ? C2 C7 C9 113.1(3) . . ? C2 C7 C8 113.4(3) . . ? C9 C7 C8 109.6(3) . . ? C6 C10 C12 113.4(3) . . ? C6 C10 C11 109.7(3) . . ? C12 C10 C11 111.5(4) . . ? N1 C14 C15 124.0(3) . . ? N1 C14 C13 120.4(3) . . ? C15 C14 C13 115.5(3) . . ? C16 C15 C14 129.3(3) . . ? N2 C16 C15 124.1(3) . . ? N2 C16 C17 120.5(3) . . ? C15 C16 C17 115.3(3) . . ? C19 C18 C23 121.2(3) . . ? C19 C18 N2 119.9(3) . . ? C23 C18 N2 118.9(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C24 121.8(3) . . ? C18 C19 C24 120.6(3) . . ? C21 C20 C19 122.0(4) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C23 121.6(4) . . ? C22 C23 C18 117.8(3) . . ? C22 C23 C27 120.3(3) . . ? C18 C23 C27 121.9(3) . . ? C19 C24 C26 113.0(3) . . ? C19 C24 C25 113.1(3) . . ? C26 C24 C25 107.7(3) . . ? C23 C27 C28 111.2(3) . . ? C23 C27 C29 111.6(3) . . ? C28 C27 C29 111.2(4) . . ? C31 C30 P1 112.5(3) . . ? C33 C32 P1 118.0(4) . . ? C35 C34 P2 118.7(4) . . ? C37 C36 P2 115.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.202 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.093 #===end