# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2313 data_12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 B2 F4 N6 O2 P Rh' _chemical_formula_weight 850.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6364(12) _cell_length_b 10.507(2) _cell_length_c 20.417(4) _cell_angle_alpha 75.132(9) _cell_angle_beta 87.82(2) _cell_angle_gamma 86.555(17) _cell_volume 1993.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20537 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0979 _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 -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.60 _reflns_number_total 9047 _reflns_number_gt 6140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0528P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9047 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.003 _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 2.07783(3) 1.26110(3) 0.285458(14) 0.02227(10) Uani 1 1 d . . . P1 P 2.02674(10) 1.37363(9) 0.17808(4) 0.0215(2) Uani 1 1 d . . . O1 O 2.3692(3) 1.2495(3) 0.23400(16) 0.0514(9) Uani 1 1 d . . . B1 B 1.9843(5) 1.3281(4) 0.4278(2) 0.0249(9) Uani 1 1 d . . . H1 H 1.947(4) 1.346(4) 0.476(2) 0.050 Uiso 1 1 d . . . N2 N 1.9792(3) 1.5573(3) 0.34766(15) 0.0252(7) Uani 1 1 d . . . H99 H 1.904(5) 1.549(5) 0.337(2) 0.050 Uiso 1 1 d . . . N1 N 2.0576(3) 1.4545(3) 0.38522(14) 0.0241(7) Uani 1 1 d . . . N3 N 2.0863(3) 1.2084(3) 0.43752(14) 0.0256(7) Uani 1 1 d . . . N4 N 2.1386(3) 1.1627(3) 0.38354(14) 0.0240(7) Uani 1 1 d . . . N5 N 1.8577(3) 1.3082(3) 0.38816(14) 0.0214(7) Uani 1 1 d . . . N6 N 1.8773(3) 1.2597(3) 0.33044(13) 0.0207(7) Uani 1 1 d . . . C1 C 1.8464(4) 1.4207(3) 0.15383(17) 0.0223(8) Uani 1 1 d . . . C2 C 1.7623(4) 1.4831(4) 0.19497(19) 0.0295(9) Uani 1 1 d . . . H2 H 1.7995 1.5006 0.2340 0.035 Uiso 1 1 calc R . . C3 C 1.6259(4) 1.5192(4) 0.1787(2) 0.0364(10) Uani 1 1 d . . . H3 H 1.5697 1.5617 0.2069 0.044 Uiso 1 1 calc R . . C4 C 1.5693(4) 1.4951(4) 0.1226(2) 0.0370(10) Uani 1 1 d . . . H4 H 1.4743 1.5191 0.1127 0.044 Uiso 1 1 calc R . . C5 C 1.6514(4) 1.4358(4) 0.0808(2) 0.0346(10) Uani 1 1 d . . . H5 H 1.6136 1.4211 0.0412 0.041 Uiso 1 1 calc R . . C6 C 1.7890(4) 1.3977(4) 0.09647(18) 0.0281(9) Uani 1 1 d . . . H6 H 1.8445 1.3555 0.0679 0.034 Uiso 1 1 calc R . . C7 C 2.0909(4) 1.2807(4) 0.11734(17) 0.0246(8) Uani 1 1 d . . . C8 C 2.0428(5) 1.1562(4) 0.1255(2) 0.0433(11) Uani 1 1 d . . . H8 H 1.9786 1.1232 0.1614 0.052 Uiso 1 1 calc R . . C9 C 2.0868(5) 1.0787(5) 0.0823(2) 0.0473(12) Uani 1 1 d . . . H9 H 2.0519 0.9936 0.0886 0.057 Uiso 1 1 calc R . . C10 C 2.1795(5) 1.1240(5) 0.0310(2) 0.0473(13) Uani 1 1 d . . . H10 H 2.2101 1.0708 0.0015 0.057 Uiso 1 1 calc R . . C11 C 2.2280(5) 1.2465(5) 0.0223(2) 0.0472(13) Uani 1 1 d . . . H11 H 2.2927 1.2784 -0.0136 0.057 Uiso 1 1 calc R . . C12 C 2.1844(5) 1.3256(4) 0.0650(2) 0.0382(10) Uani 1 1 d . . . H12 H 2.2192 1.4109 0.0581 0.046 Uiso 1 1 calc R . . C13 C 2.1096(4) 1.5306(4) 0.14978(17) 0.0240(8) Uani 1 1 d . . . C14 C 2.2058(4) 1.5669(4) 0.18985(18) 0.0270(9) Uani 1 1 d . . . H14 H 2.2257 1.5110 0.2334 0.032 Uiso 1 1 calc R . . C15 C 2.2728(4) 1.6832(4) 0.1672(2) 0.0326(9) Uani 1 1 d . . . H15 H 2.3367 1.7080 0.1954 0.039 Uiso 1 1 calc R . . C16 C 2.2464(4) 1.7632(4) 0.1033(2) 0.0337(10) Uani 1 1 d . . . H16 H 2.2952 1.8414 0.0867 0.040 Uiso 1 1 calc R . . C17 C 2.1491(5) 1.7298(4) 0.0634(2) 0.0359(10) Uani 1 1 d . . . H17 H 2.1304 1.7858 0.0198 0.043 Uiso 1 1 calc R . . C18 C 2.0795(4) 1.6162(4) 0.08656(19) 0.0313(9) Uani 1 1 d . . . H18 H 2.0105 1.5954 0.0595 0.038 Uiso 1 1 calc R . . C19 C 2.0552(4) 1.6624(4) 0.32369(18) 0.0271(9) Uani 1 1 d . . . C20 C 2.1863(4) 1.6263(4) 0.34844(19) 0.0298(9) Uani 1 1 d . . . H20 H 2.2635 1.6807 0.3409 0.036 Uiso 1 1 calc R . . C21 C 2.1860(4) 1.4971(4) 0.38621(18) 0.0268(8) Uani 1 1 d . . . C22 C 1.9965(4) 1.7848(4) 0.2779(2) 0.0374(10) Uani 1 1 d . . . H22A H 2.0541 1.8583 0.2785 0.056 Uiso 1 1 calc R . . H22B H 1.9016 1.8035 0.2932 0.056 Uiso 1 1 calc R . . H22C H 1.9949 1.7740 0.2317 0.056 Uiso 1 1 calc R . . C23 C 2.3042(4) 1.4134(4) 0.4223(2) 0.0400(11) Uani 1 1 d . . . H23A H 2.3862 1.4661 0.4179 0.060 Uiso 1 1 calc R . . H23B H 2.3253 1.3388 0.4023 0.060 Uiso 1 1 calc R . . H23C H 2.2788 1.3804 0.4704 0.060 Uiso 1 1 calc R . . C24 C 2.2237(4) 1.0576(4) 0.40831(19) 0.0317(9) Uani 1 1 d . . . C25 C 2.2253(5) 1.0341(4) 0.4787(2) 0.0379(11) Uani 1 1 d . . . H25 H 2.2769 0.9655 0.5091 0.045 Uiso 1 1 calc R . . C26 C 2.1386(4) 1.1287(4) 0.49534(18) 0.0316(9) Uani 1 1 d . . . C27 C 2.2988(5) 0.9808(4) 0.3640(2) 0.0436(11) Uani 1 1 d . . . H27A H 2.3847 1.0234 0.3457 0.065 Uiso 1 1 calc R . . H27B H 2.2393 0.9781 0.3266 0.065 Uiso 1 1 calc R . . H27C H 2.3215 0.8908 0.3908 0.065 Uiso 1 1 calc R . . C28 C 2.1024(5) 1.1476(5) 0.5646(2) 0.0462(12) Uani 1 1 d . . . H28A H 2.1485 1.0767 0.5990 0.069 Uiso 1 1 calc R . . H28B H 2.0014 1.1455 0.5723 0.069 Uiso 1 1 calc R . . H28C H 2.1336 1.2329 0.5678 0.069 Uiso 1 1 calc R . . C29 C 1.7237(4) 1.2931(4) 0.41038(17) 0.0245(8) Uani 1 1 d . . . C30 C 1.6569(4) 1.2363(4) 0.36775(18) 0.0272(9) Uani 1 1 d . . . H30 H 1.5620 1.2152 0.3705 0.033 Uiso 1 1 calc R . . C31 C 1.7567(4) 1.2157(4) 0.31938(18) 0.0244(8) Uani 1 1 d . . . C32 C 1.6680(4) 1.3354(4) 0.47151(18) 0.0331(10) Uani 1 1 d . . . H32A H 1.5759 1.3005 0.4842 0.050 Uiso 1 1 calc R . . H32B H 1.6604 1.4319 0.4611 0.050 Uiso 1 1 calc R . . H32C H 1.7311 1.3013 0.5093 0.050 Uiso 1 1 calc R . . C33 C 1.7374(4) 1.1491(4) 0.26381(19) 0.0340(10) Uani 1 1 d . . . H33A H 1.6918 1.0662 0.2824 0.051 Uiso 1 1 calc R . . H33B H 1.8283 1.1307 0.2440 0.051 Uiso 1 1 calc R . . H33C H 1.6796 1.2070 0.2287 0.051 Uiso 1 1 calc R . . C34 C 2.2561(4) 1.2537(4) 0.25292(18) 0.0304(9) Uani 1 1 d . . . O7 O 1.2795(4) 1.9486(4) 0.9154(2) 0.0769(12) Uani 1 1 d . . . C70 C 1.4218(7) 1.9050(6) 0.9166(4) 0.103(3) Uani 1 1 d . . . H70A H 1.4316 1.8126 0.9131 0.124 Uiso 1 1 calc R . . H70B H 1.4638 1.9097 0.9593 0.124 Uiso 1 1 calc R . . C71 C 1.4916(7) 1.9939(8) 0.8574(4) 0.093(2) Uani 1 1 d . . . H71A H 1.5897 2.0051 0.8665 0.111 Uiso 1 1 calc R . . H71B H 1.4873 1.9622 0.8159 0.111 Uiso 1 1 calc R . . C72 C 1.4041(7) 2.1166(7) 0.8529(3) 0.089(2) Uani 1 1 d . . . H72A H 1.4281 2.1609 0.8880 0.107 Uiso 1 1 calc R . . H72B H 1.4134 2.1788 0.8076 0.107 Uiso 1 1 calc R . . C73 C 1.2639(6) 2.0669(6) 0.8647(3) 0.0688(17) Uani 1 1 d . . . H73A H 1.1989 2.1306 0.8800 0.083 Uiso 1 1 calc R . . H73B H 1.2282 2.0508 0.8229 0.083 Uiso 1 1 calc R . . B2 B 1.5983(5) 1.7043(5) 0.3392(2) 0.0324(11) Uani 1 1 d . . . F20 F 1.5585(4) 1.6701(3) 0.40584(13) 0.0765(10) Uani 1 1 d . . . F21 F 1.4890(3) 1.7024(3) 0.29887(14) 0.0591(8) Uani 1 1 d . . . F22 F 1.6539(3) 1.8261(3) 0.32250(14) 0.0578(8) Uani 1 1 d . . . F23 F 1.7011(3) 1.6117(3) 0.32735(14) 0.0538(7) 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 Rh1 0.02073(17) 0.02478(17) 0.02002(15) -0.00423(11) 0.00142(11) 0.00134(11) P1 0.0223(5) 0.0226(5) 0.0197(5) -0.0061(4) 0.0013(4) 0.0010(4) O1 0.0300(18) 0.057(2) 0.057(2) 0.0000(16) 0.0143(16) 0.0079(16) B1 0.026(2) 0.026(2) 0.023(2) -0.0058(18) -0.0008(18) 0.0002(19) N2 0.0203(17) 0.0278(18) 0.0275(17) -0.0073(14) -0.0005(14) -0.0001(15) N1 0.0223(17) 0.0249(17) 0.0252(16) -0.0075(13) -0.0013(13) 0.0043(13) N3 0.0276(18) 0.0263(17) 0.0204(16) -0.0026(13) -0.0009(13) 0.0027(14) N4 0.0275(18) 0.0221(17) 0.0216(15) -0.0045(13) -0.0032(13) 0.0013(14) N5 0.0225(17) 0.0227(16) 0.0182(14) -0.0049(12) 0.0024(12) 0.0008(13) N6 0.0237(17) 0.0234(16) 0.0152(14) -0.0054(12) 0.0023(12) -0.0023(13) C1 0.022(2) 0.0188(19) 0.0243(18) -0.0022(15) 0.0005(15) 0.0005(15) C2 0.030(2) 0.033(2) 0.026(2) -0.0114(17) 0.0009(17) 0.0044(18) C3 0.030(2) 0.042(3) 0.037(2) -0.0126(19) 0.0027(19) 0.009(2) C4 0.022(2) 0.045(3) 0.040(2) -0.005(2) -0.0014(18) 0.0041(19) C5 0.032(2) 0.040(3) 0.033(2) -0.0096(19) -0.0067(18) -0.0014(19) C6 0.028(2) 0.035(2) 0.0221(19) -0.0104(16) 0.0007(16) 0.0006(18) C7 0.024(2) 0.026(2) 0.0224(19) -0.0064(16) -0.0012(15) 0.0042(16) C8 0.046(3) 0.033(2) 0.056(3) -0.023(2) 0.020(2) -0.006(2) C9 0.046(3) 0.037(3) 0.066(3) -0.029(2) 0.010(2) 0.002(2) C10 0.062(3) 0.050(3) 0.034(2) -0.023(2) 0.001(2) 0.019(3) C11 0.069(3) 0.041(3) 0.028(2) -0.008(2) 0.021(2) 0.010(2) C12 0.050(3) 0.029(2) 0.032(2) -0.0059(18) 0.012(2) 0.005(2) C13 0.024(2) 0.025(2) 0.0231(18) -0.0072(15) 0.0029(15) 0.0019(16) C14 0.027(2) 0.028(2) 0.0255(19) -0.0075(16) 0.0031(16) 0.0008(17) C15 0.029(2) 0.031(2) 0.039(2) -0.0118(19) -0.0035(18) -0.0003(18) C16 0.032(2) 0.024(2) 0.042(2) -0.0048(18) 0.0085(19) -0.0023(18) C17 0.044(3) 0.026(2) 0.033(2) -0.0005(18) 0.0000(19) -0.002(2) C18 0.037(2) 0.028(2) 0.030(2) -0.0086(17) -0.0087(18) -0.0003(18) C19 0.026(2) 0.028(2) 0.028(2) -0.0080(16) 0.0062(16) -0.0011(17) C20 0.024(2) 0.029(2) 0.039(2) -0.0135(18) 0.0048(17) -0.0067(17) C21 0.023(2) 0.031(2) 0.029(2) -0.0134(17) 0.0004(16) -0.0010(17) C22 0.034(2) 0.033(2) 0.041(2) -0.0013(19) 0.0052(19) 0.0005(19) C23 0.029(2) 0.044(3) 0.049(3) -0.015(2) -0.008(2) 0.000(2) C24 0.033(2) 0.026(2) 0.034(2) -0.0034(17) -0.0070(18) 0.0048(18) C25 0.048(3) 0.029(2) 0.030(2) 0.0022(18) -0.012(2) 0.010(2) C26 0.036(2) 0.032(2) 0.025(2) -0.0025(17) -0.0084(17) 0.0024(19) C27 0.054(3) 0.031(2) 0.043(3) -0.008(2) -0.002(2) 0.015(2) C28 0.053(3) 0.058(3) 0.026(2) -0.008(2) -0.004(2) 0.005(2) C29 0.024(2) 0.024(2) 0.0211(18) 0.0016(15) 0.0016(15) 0.0036(16) C30 0.019(2) 0.032(2) 0.027(2) -0.0018(17) 0.0028(16) -0.0038(17) C31 0.027(2) 0.023(2) 0.0228(18) -0.0035(15) -0.0024(16) -0.0024(16) C32 0.031(2) 0.041(2) 0.026(2) -0.0058(18) 0.0063(17) 0.0022(19) C33 0.036(2) 0.037(2) 0.033(2) -0.0126(18) 0.0020(18) -0.013(2) C34 0.032(2) 0.031(2) 0.024(2) -0.0004(16) -0.0004(17) 0.0055(18) O7 0.074(3) 0.057(3) 0.095(3) -0.013(2) 0.026(2) -0.012(2) C70 0.077(5) 0.050(4) 0.166(7) -0.002(4) 0.016(5) 0.005(4) C71 0.050(4) 0.151(7) 0.110(5) -0.089(5) 0.023(4) -0.036(4) C72 0.089(5) 0.097(6) 0.067(4) 0.004(4) 0.014(4) -0.025(5) C73 0.071(4) 0.089(5) 0.052(3) -0.031(3) -0.006(3) 0.008(4) B2 0.032(3) 0.032(3) 0.032(3) -0.007(2) 0.009(2) 0.000(2) F20 0.113(3) 0.073(2) 0.0366(16) -0.0069(14) 0.0278(16) -0.0006(19) F21 0.0251(14) 0.084(2) 0.0667(18) -0.0160(16) -0.0052(13) -0.0031(14) F22 0.0606(19) 0.0404(16) 0.0711(19) -0.0101(14) 0.0034(15) -0.0138(14) F23 0.0310(15) 0.0593(18) 0.0743(19) -0.0265(15) -0.0028(13) 0.0135(13) _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 C34 1.823(4) . ? Rh1 N4 2.092(3) . ? Rh1 N6 2.107(3) . ? Rh1 P1 2.2646(10) . ? Rh1 B1 3.245(4) . ? Rh1 N2 3.713(3) . ? P1 C13 1.823(4) . ? P1 C1 1.829(4) . ? P1 C7 1.834(4) . ? O1 C34 1.144(5) . ? B1 N3 1.525(5) . ? B1 N5 1.543(5) . ? B1 N1 1.579(5) . ? N2 C19 1.337(5) . ? N2 N1 1.359(4) . ? N1 C21 1.343(5) . ? N3 C26 1.355(4) . ? N3 N4 1.378(4) . ? N4 C24 1.336(5) . ? N5 C29 1.357(5) . ? N5 N6 1.402(4) . ? N6 C31 1.324(5) . ? C1 C6 1.396(5) . ? C1 C2 1.400(5) . ? C2 C3 1.375(5) . ? C3 C4 1.374(6) . ? C4 C5 1.381(6) . ? C5 C6 1.387(5) . ? C7 C12 1.377(5) . ? C7 C8 1.380(5) . ? C8 C9 1.386(6) . ? C9 C10 1.359(6) . ? C10 C11 1.362(6) . ? C11 C12 1.389(6) . ? C13 C14 1.391(5) . ? C13 C18 1.400(5) . ? C14 C15 1.380(5) . ? C15 C16 1.383(5) . ? C16 C17 1.381(6) . ? C17 C18 1.371(5) . ? C19 C20 1.373(5) . ? C19 C22 1.478(5) . ? C20 C21 1.378(5) . ? C21 C23 1.492(5) . ? C24 C25 1.395(5) . ? C24 C27 1.499(6) . ? C25 C26 1.361(6) . ? C26 C28 1.504(5) . ? C29 C30 1.373(5) . ? C29 C32 1.499(5) . ? C30 C31 1.400(5) . ? C31 C33 1.500(5) . ? O7 C73 1.404(7) . ? O7 C70 1.419(7) . ? C70 C71 1.490(9) . ? C71 C72 1.482(9) . ? C72 C73 1.467(8) . ? B2 F20 1.362(5) . ? B2 F21 1.366(5) . ? B2 F22 1.372(5) . ? B2 F23 1.405(5) . ? 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 C34 Rh1 N4 91.52(14) . . ? C34 Rh1 N6 175.42(14) . . ? N4 Rh1 N6 83.95(12) . . ? C34 Rh1 P1 85.08(12) . . ? N4 Rh1 P1 176.02(9) . . ? N6 Rh1 P1 99.48(8) . . ? C34 Rh1 B1 125.35(15) . . ? N4 Rh1 B1 51.43(11) . . ? N6 Rh1 B1 51.79(11) . . ? P1 Rh1 B1 129.49(8) . . ? C34 Rh1 N2 114.83(14) . . ? N4 Rh1 N2 88.85(10) . . ? N6 Rh1 N2 65.87(10) . . ? P1 Rh1 N2 90.72(6) . . ? B1 Rh1 N2 42.14(9) . . ? C13 P1 C1 102.00(17) . . ? C13 P1 C7 104.15(17) . . ? C1 P1 C7 103.54(16) . . ? C13 P1 Rh1 113.90(12) . . ? C1 P1 Rh1 120.68(12) . . ? C7 P1 Rh1 110.83(12) . . ? N3 B1 N5 110.0(3) . . ? N3 B1 N1 109.4(3) . . ? N5 B1 N1 108.0(3) . . ? N3 B1 Rh1 67.59(18) . . ? N5 B1 Rh1 68.29(18) . . ? N1 B1 Rh1 74.94(19) . . ? C19 N2 N1 111.0(3) . . ? C19 N2 Rh1 116.5(2) . . ? N1 N2 Rh1 58.52(18) . . ? C21 N1 N2 106.7(3) . . ? C21 N1 B1 132.6(3) . . ? N2 N1 B1 119.4(3) . . ? C26 N3 N4 108.5(3) . . ? C26 N3 B1 129.7(3) . . ? N4 N3 B1 121.8(3) . . ? C24 N4 N3 107.5(3) . . ? C24 N4 Rh1 133.3(3) . . ? N3 N4 Rh1 119.2(2) . . ? C29 N5 N6 108.7(3) . . ? C29 N5 B1 128.2(3) . . ? N6 N5 B1 120.1(3) . . ? C31 N6 N5 106.7(3) . . ? C31 N6 Rh1 134.9(2) . . ? N5 N6 Rh1 118.3(2) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 P1 123.3(3) . . ? C2 C1 P1 118.1(3) . . ? C3 C2 C1 119.9(4) . . ? C4 C3 C2 121.4(4) . . ? C3 C4 C5 119.5(4) . . ? C4 C5 C6 120.0(4) . . ? C5 C6 C1 120.6(4) . . ? C12 C7 C8 118.1(4) . . ? C12 C7 P1 124.6(3) . . ? C8 C7 P1 117.3(3) . . ? C7 C8 C9 121.2(4) . . ? C10 C9 C8 120.2(4) . . ? C9 C10 C11 119.3(4) . . ? C10 C11 C12 121.1(4) . . ? C7 C12 C11 120.1(4) . . ? C14 C13 C18 118.5(4) . . ? C14 C13 P1 120.9(3) . . ? C18 C13 P1 120.6(3) . . ? C15 C14 C13 120.8(3) . . ? C14 C15 C16 119.7(4) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 120.3(4) . . ? C17 C18 C13 120.4(4) . . ? N2 C19 C20 106.1(3) . . ? N2 C19 C22 121.8(4) . . ? C20 C19 C22 132.1(4) . . ? C19 C20 C21 108.0(4) . . ? N1 C21 C20 108.2(3) . . ? N1 C21 C23 123.7(4) . . ? C20 C21 C23 128.1(4) . . ? N4 C24 C25 108.9(4) . . ? N4 C24 C27 122.5(3) . . ? C25 C24 C27 128.5(4) . . ? C26 C25 C24 106.6(3) . . ? N3 C26 C25 108.4(3) . . ? N3 C26 C28 123.3(4) . . ? C25 C26 C28 128.2(4) . . ? N5 C29 C30 108.2(3) . . ? N5 C29 C32 122.4(3) . . ? C30 C29 C32 129.4(3) . . ? C29 C30 C31 106.2(3) . . ? N6 C31 C30 110.2(3) . . ? N6 C31 C33 122.8(3) . . ? C30 C31 C33 126.9(4) . . ? O1 C34 Rh1 178.3(4) . . ? C73 O7 C70 108.1(5) . . ? O7 C70 C71 106.8(6) . . ? C72 C71 C70 99.6(5) . . ? C73 C72 C71 102.1(6) . . ? O7 C73 C72 104.8(5) . . ? F20 B2 F21 110.7(4) . . ? F20 B2 F22 110.6(4) . . ? F21 B2 F22 110.7(4) . . ? F20 B2 F23 108.9(4) . . ? F21 B2 F23 107.6(4) . . ? F22 B2 F23 108.1(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 Rh1 B1 N1 N2 94.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.561 _refine_diff_density_min -1.508 _refine_diff_density_rms 0.101 data_2+ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H39 B Cl2 F6 N6 O P2 Rh' _chemical_formula_weight 920.28 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _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 10.6665(19) _cell_length_b 15.090(2) _cell_length_c 25.261(4) _cell_angle_alpha 90.00(13) _cell_angle_beta 90.78(14) _cell_angle_gamma 90.00(14) _cell_volume 4065.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1868 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19030 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7130 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SAINT (Siemens, 1995b)' _computing_publication_material 'SAINT (Siemens, 1995b)' _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^)+(0.0222P)^2^+4.6822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7130 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.006 _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 0.889050(19) 0.212555(14) 0.882197(8) 0.02370(7) Uani 1 1 d . . . P1 P 0.90166(7) 0.36107(5) 0.85799(3) 0.02584(16) Uani 1 1 d . . . P2 P 1.07480(8) 0.26367(5) 0.57987(3) 0.03634(19) Uani 1 1 d . . . N2 N 0.9797(2) 0.15342(16) 0.81173(9) 0.0291(5) Uani 1 1 d . . . N1 N 1.0847(2) 0.10399(16) 0.82333(9) 0.0299(5) Uani 1 1 d . . . N3 N 0.9991(2) 0.03660(15) 0.90649(9) 0.0270(5) Uani 1 1 d . . . N4 N 0.8886(2) 0.08229(15) 0.91042(9) 0.0259(5) Uani 1 1 d . . . N5 N 1.1484(2) 0.16321(15) 0.91370(9) 0.0266(5) Uani 1 1 d . . . N6 N 1.0538(2) 0.21997(15) 0.92799(8) 0.0247(5) Uani 1 1 d . . . O1 O 0.6283(2) 0.20145(19) 0.83526(11) 0.0617(7) Uani 1 1 d . . . B1 B 1.1159(3) 0.0796(2) 0.88095(13) 0.0283(7) Uani 1 1 d . . . H1A H 1.192(3) 0.0338(18) 0.8815(10) 0.025(7) Uiso 1 1 d . . . C1 C 1.0613(3) 0.40384(19) 0.86586(11) 0.0284(6) Uani 1 1 d . . . C2 C 1.1610(3) 0.3519(2) 0.84849(11) 0.0341(7) Uani 1 1 d . . . H2 H 1.1452 0.2967 0.8316 0.041 Uiso 1 1 calc R . . C3 C 1.2838(3) 0.3815(2) 0.85602(12) 0.0410(8) Uani 1 1 d . . . H3 H 1.3518 0.3463 0.8442 0.049 Uiso 1 1 calc R . . C4 C 1.3072(3) 0.4621(2) 0.88071(13) 0.0454(8) Uani 1 1 d . . . H4 H 1.3911 0.4816 0.8862 0.054 Uiso 1 1 calc R . . C5 C 1.2089(3) 0.5137(2) 0.89719(13) 0.0427(8) Uani 1 1 d . . . H5 H 1.2250 0.5694 0.9135 0.051 Uiso 1 1 calc R . . C6 C 1.0866(3) 0.4849(2) 0.89012(12) 0.0356(7) Uani 1 1 d . . . H6 H 1.0193 0.5207 0.9019 0.043 Uiso 1 1 calc R . . C7 C 0.7989(2) 0.43002(18) 0.89725(11) 0.0271(6) Uani 1 1 d . . . C8 C 0.7369(3) 0.3950(2) 0.94085(11) 0.0323(7) Uani 1 1 d . . . H8 H 0.7461 0.3340 0.9494 0.039 Uiso 1 1 calc R . . C9 C 0.6620(3) 0.4487(2) 0.97169(12) 0.0381(7) Uani 1 1 d . . . H9 H 0.6210 0.4247 1.0016 0.046 Uiso 1 1 calc R . . C10 C 0.6470(3) 0.5371(2) 0.95882(13) 0.0413(8) Uani 1 1 d . . . H10 H 0.5967 0.5740 0.9804 0.050 Uiso 1 1 calc R . . C11 C 0.7046(3) 0.5724(2) 0.91483(12) 0.0383(7) Uani 1 1 d . . . H11 H 0.6924 0.6329 0.9057 0.046 Uiso 1 1 calc R . . C12 C 0.7800(3) 0.51914(19) 0.88419(12) 0.0322(7) Uani 1 1 d . . . H12 H 0.8194 0.5433 0.8539 0.039 Uiso 1 1 calc R . . C13 C 0.8560(3) 0.39040(19) 0.79055(11) 0.0316(6) Uani 1 1 d . . . C14 C 0.7285(3) 0.4006(2) 0.77803(13) 0.0422(8) Uani 1 1 d . . . H14 H 0.6675 0.3940 0.8048 0.051 Uiso 1 1 calc R . . C15 C 0.6909(4) 0.4205(2) 0.72654(15) 0.0559(10) Uani 1 1 d . . . H15 H 0.6045 0.4284 0.7182 0.067 Uiso 1 1 calc R . . C16 C 0.7798(4) 0.4287(3) 0.68754(15) 0.0629(11) Uani 1 1 d . . . H16 H 0.7538 0.4409 0.6522 0.075 Uiso 1 1 calc R . . C17 C 0.9051(4) 0.4195(3) 0.69935(13) 0.0570(10) Uani 1 1 d . . . H17 H 0.9653 0.4261 0.6723 0.068 Uiso 1 1 calc R . . C18 C 0.9438(3) 0.4006(2) 0.75089(12) 0.0417(8) Uani 1 1 d . . . H18 H 1.0307 0.3947 0.7590 0.050 Uiso 1 1 calc R . . C19 C 0.9610(3) 0.1484(2) 0.75914(11) 0.0332(7) Uani 1 1 d . . . C20 C 1.0562(3) 0.0983(2) 0.73708(12) 0.0427(8) Uani 1 1 d . . . H20 H 1.0667 0.0857 0.7006 0.051 Uiso 1 1 calc R . . C21 C 1.1318(3) 0.0705(2) 0.77794(12) 0.0391(7) Uani 1 1 d . . . C22 C 0.8486(3) 0.1855(2) 0.73076(12) 0.0444(8) Uani 1 1 d . . . H22A H 0.7859 0.1386 0.7257 0.067 Uiso 1 1 calc R . . H22B H 0.8735 0.2085 0.6962 0.067 Uiso 1 1 calc R . . H22C H 0.8126 0.2335 0.7518 0.067 Uiso 1 1 calc R . . C23 C 1.2485(3) 0.0152(3) 0.77704(14) 0.0605(11) Uani 1 1 d . . . H23A H 1.2350 -0.0396 0.7970 0.091 Uiso 1 1 calc R . . H23B H 1.3181 0.0484 0.7932 0.091 Uiso 1 1 calc R . . H23C H 1.2689 0.0007 0.7403 0.091 Uiso 1 1 calc R . . C24 C 0.8067(3) 0.03039(19) 0.93554(10) 0.0289(6) Uani 1 1 d . . . C25 C 0.8650(3) -0.0492(2) 0.94786(11) 0.0342(7) Uani 1 1 d . . . H25 H 0.8286 -0.0982 0.9656 0.041 Uiso 1 1 calc R . . C26 C 0.9855(3) -0.04386(18) 0.92960(11) 0.0305(6) Uani 1 1 d . . . C27 C 0.6751(3) 0.0591(2) 0.94522(13) 0.0419(8) Uani 1 1 d . . . H27A H 0.6372 0.0198 0.9714 0.063 Uiso 1 1 calc R . . H27B H 0.6267 0.0562 0.9120 0.063 Uiso 1 1 calc R . . H27C H 0.6751 0.1200 0.9586 0.063 Uiso 1 1 calc R . . C28 C 1.0891(3) -0.1100(2) 0.93291(14) 0.0465(8) Uani 1 1 d . . . H28A H 1.0588 -0.1641 0.9500 0.070 Uiso 1 1 calc R . . H28B H 1.1590 -0.0854 0.9538 0.070 Uiso 1 1 calc R . . H28C H 1.1177 -0.1241 0.8972 0.070 Uiso 1 1 calc R . . C29 C 1.2525(3) 0.1815(2) 0.94303(11) 0.0307(6) Uani 1 1 d . . . C30 C 1.2241(3) 0.2497(2) 0.97676(11) 0.0308(6) Uani 1 1 d . . . H30 H 1.2791 0.2763 1.0020 0.037 Uiso 1 1 calc R . . C31 C 1.0995(3) 0.27256(18) 0.96698(10) 0.0274(6) Uani 1 1 d . . . C32 C 1.3723(3) 0.1318(2) 0.93679(14) 0.0456(8) Uani 1 1 d . . . H32A H 1.4344 0.1535 0.9627 0.068 Uiso 1 1 calc R . . H32B H 1.4038 0.1408 0.9009 0.068 Uiso 1 1 calc R . . H32C H 1.3574 0.0685 0.9427 0.068 Uiso 1 1 calc R . . C33 C 1.0220(3) 0.3385(2) 0.99586(11) 0.0343(7) Uani 1 1 d . . . H33A H 1.0076 0.3904 0.9733 0.052 Uiso 1 1 calc R . . H33B H 1.0660 0.3565 1.0284 0.052 Uiso 1 1 calc R . . H33C H 0.9413 0.3117 1.0048 0.052 Uiso 1 1 calc R . . C34 C 0.7271(3) 0.2062(2) 0.85221(12) 0.0368(7) Uani 1 1 d . . . F1 F 0.93433(19) 0.27957(15) 0.59796(9) 0.0636(6) Uani 1 1 d . . . F2 F 1.1262(2) 0.29462(19) 0.63576(9) 0.0806(8) Uani 1 1 d . . . F3 F 1.0678(2) 0.16316(14) 0.59988(9) 0.0647(6) Uani 1 1 d . . . F4 F 1.0233(2) 0.23110(15) 0.52351(8) 0.0663(6) Uani 1 1 d . . . F5 F 1.0816(2) 0.36242(14) 0.55933(10) 0.0724(7) Uani 1 1 d . . . F6 F 1.21460(19) 0.24462(15) 0.56124(10) 0.0681(6) Uani 1 1 d . . . C62A C 1.3778(5) 0.2054(3) 0.68505(18) 0.0798(14) Uani 0.231(10) 1 d P A 1 H62A H 1.3328 0.1481 0.6865 0.096 Uiso 0.231(10) 1 calc PR A 1 H62B H 1.3490 0.2375 0.6529 0.096 Uiso 0.231(10) 1 calc PR A 1 Cl1A Cl 1.3435(17) 0.2681(7) 0.7414(6) 0.085(3) Uani 0.231(10) 1 d P A 1 Cl2A Cl 1.5285(17) 0.188(2) 0.6820(14) 0.341(16) Uani 0.231(10) 1 d P A 1 C62B C 1.3778(5) 0.2054(3) 0.68505(18) 0.0798(14) Uani 0.769(10) 1 d P A 2 H62C H 1.3160 0.2292 0.6591 0.096 Uiso 0.769(10) 1 calc PR A 2 H62D H 1.3573 0.1423 0.6914 0.096 Uiso 0.769(10) 1 calc PR A 2 Cl1B Cl 1.3673(7) 0.2625(4) 0.7427(3) 0.174(3) Uani 0.769(10) 1 d P A 2 Cl2B Cl 1.5289(3) 0.21331(18) 0.65890(11) 0.0838(10) Uani 0.769(10) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02162(11) 0.02270(11) 0.02666(11) -0.00002(9) -0.00345(8) 0.00366(9) P1 0.0270(4) 0.0234(4) 0.0271(4) 0.0011(3) -0.0021(3) 0.0036(3) P2 0.0330(4) 0.0354(5) 0.0405(5) 0.0034(3) -0.0041(3) -0.0050(3) N2 0.0287(13) 0.0314(13) 0.0269(12) -0.0017(10) -0.0029(9) 0.0024(10) N1 0.0279(13) 0.0329(14) 0.0290(12) -0.0047(10) 0.0000(10) 0.0052(10) N3 0.0263(12) 0.0263(13) 0.0283(12) -0.0019(10) -0.0039(9) 0.0057(10) N4 0.0244(12) 0.0256(12) 0.0276(12) -0.0010(10) -0.0012(9) 0.0053(10) N5 0.0233(12) 0.0285(13) 0.0278(12) -0.0005(10) -0.0025(9) 0.0052(10) N6 0.0252(12) 0.0249(12) 0.0240(11) -0.0006(9) -0.0023(9) 0.0033(10) O1 0.0329(13) 0.0755(19) 0.0762(18) 0.0198(15) -0.0237(12) -0.0058(13) B1 0.0254(16) 0.0268(17) 0.0326(17) -0.0042(13) -0.0016(13) 0.0081(14) C1 0.0301(15) 0.0292(15) 0.0257(14) 0.0048(12) -0.0024(11) -0.0008(12) C2 0.0334(16) 0.0381(17) 0.0309(15) 0.0047(13) 0.0021(12) -0.0028(13) C3 0.0326(17) 0.052(2) 0.0383(18) 0.0086(15) 0.0041(13) -0.0001(15) C4 0.0355(18) 0.059(2) 0.0412(19) 0.0131(16) -0.0066(14) -0.0150(16) C5 0.048(2) 0.0394(19) 0.0409(18) 0.0026(15) -0.0106(15) -0.0101(16) C6 0.0385(17) 0.0342(17) 0.0339(16) 0.0038(13) -0.0054(13) 0.0005(14) C7 0.0237(14) 0.0264(15) 0.0310(15) -0.0012(12) -0.0028(11) 0.0046(11) C8 0.0283(15) 0.0314(16) 0.0369(16) 0.0038(13) -0.0029(12) 0.0025(12) C9 0.0299(16) 0.045(2) 0.0393(17) -0.0003(14) 0.0066(13) 0.0022(14) C10 0.0315(17) 0.044(2) 0.0490(19) -0.0097(15) 0.0048(14) 0.0080(14) C11 0.0363(17) 0.0302(17) 0.0482(19) -0.0027(14) -0.0055(14) 0.0081(14) C12 0.0307(16) 0.0291(16) 0.0366(16) 0.0018(13) -0.0011(12) 0.0023(12) C13 0.0392(17) 0.0258(15) 0.0295(15) 0.0017(12) -0.0070(12) 0.0018(13) C14 0.0453(19) 0.0400(19) 0.0409(18) 0.0010(14) -0.0104(14) 0.0107(15) C15 0.062(2) 0.051(2) 0.054(2) 0.0003(18) -0.0282(19) 0.0116(19) C16 0.093(3) 0.058(3) 0.037(2) 0.0092(18) -0.023(2) -0.002(2) C17 0.080(3) 0.060(2) 0.0309(18) 0.0099(17) -0.0039(18) -0.007(2) C18 0.051(2) 0.0404(19) 0.0336(17) 0.0031(14) -0.0037(14) -0.0056(15) C19 0.0416(17) 0.0308(16) 0.0269(15) -0.0016(12) -0.0057(12) -0.0034(13) C20 0.052(2) 0.051(2) 0.0248(16) -0.0097(14) 0.0021(14) 0.0036(16) C21 0.0395(18) 0.0416(19) 0.0364(17) -0.0097(14) 0.0072(14) 0.0038(14) C22 0.059(2) 0.0429(19) 0.0310(17) -0.0047(14) -0.0165(15) 0.0043(16) C23 0.054(2) 0.080(3) 0.047(2) -0.017(2) 0.0092(17) 0.027(2) C24 0.0320(15) 0.0308(16) 0.0239(14) -0.0020(12) -0.0006(11) -0.0007(12) C25 0.0430(18) 0.0275(16) 0.0322(16) 0.0063(12) -0.0021(13) -0.0026(13) C26 0.0403(17) 0.0225(15) 0.0284(15) -0.0008(12) -0.0078(12) 0.0030(12) C27 0.0327(17) 0.047(2) 0.0460(19) 0.0041(15) 0.0068(14) 0.0005(15) C28 0.052(2) 0.0323(18) 0.055(2) 0.0048(15) -0.0087(16) 0.0127(15) C29 0.0222(14) 0.0389(17) 0.0309(15) 0.0043(13) -0.0039(11) 0.0005(12) C30 0.0301(15) 0.0341(15) 0.0281(15) -0.0013(12) -0.0092(12) -0.0013(13) C31 0.0317(15) 0.0286(16) 0.0219(13) 0.0014(11) -0.0017(11) 0.0000(12) C32 0.0244(16) 0.059(2) 0.054(2) -0.0067(17) -0.0089(14) 0.0065(15) C33 0.0395(17) 0.0335(17) 0.0299(15) -0.0037(13) -0.0062(12) 0.0052(13) C34 0.0354(17) 0.0331(17) 0.0419(17) 0.0046(14) -0.0057(13) 0.0038(14) F1 0.0391(11) 0.0637(14) 0.0883(16) -0.0053(12) 0.0086(10) 0.0023(10) F2 0.0756(16) 0.106(2) 0.0599(14) -0.0271(14) -0.0284(12) 0.0113(15) F3 0.0567(13) 0.0476(13) 0.0896(16) 0.0288(12) -0.0015(11) 0.0009(10) F4 0.0807(16) 0.0617(15) 0.0558(13) -0.0132(11) -0.0264(11) 0.0131(12) F5 0.0903(17) 0.0345(12) 0.0925(17) 0.0125(11) 0.0109(13) -0.0086(11) F6 0.0387(12) 0.0631(14) 0.1028(18) -0.0144(13) 0.0170(11) -0.0112(10) C62A 0.091(3) 0.078(3) 0.070(3) -0.022(2) -0.020(2) 0.007(3) Cl1A 0.110(7) 0.069(5) 0.077(6) -0.044(4) 0.012(5) 0.018(4) Cl2A 0.159(12) 0.39(2) 0.47(3) -0.35(2) -0.226(16) 0.207(15) C62B 0.091(3) 0.078(3) 0.070(3) -0.022(2) -0.020(2) 0.007(3) Cl1B 0.143(4) 0.247(6) 0.133(4) -0.114(4) 0.004(3) -0.023(3) Cl2B 0.0794(16) 0.0753(14) 0.0962(16) -0.0162(13) -0.0146(12) 0.0249(11) _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 C34 1.879(4) . ? Rh1 N4 2.091(3) . ? Rh1 N6 2.093(3) . ? Rh1 N2 2.224(4) . ? Rh1 P1 2.3275(16) . ? Rh1 B1 3.143(5) . ? P1 C7 1.815(4) . ? P1 C13 1.820(3) . ? P1 C1 1.829(3) . ? P2 F2 1.578(3) . ? P2 F5 1.580(2) . ? P2 F1 1.591(2) . ? P2 F6 1.596(3) . ? P2 F4 1.596(3) . ? P2 F3 1.601(2) . ? N2 C19 1.343(4) . ? N2 N1 1.374(4) . ? N1 C21 1.356(4) . ? N1 B1 1.533(4) . ? N3 C26 1.356(4) . ? N3 N4 1.371(3) . ? N3 B1 1.553(4) . ? N4 C24 1.339(4) . ? N5 C29 1.355(4) . ? N5 N6 1.376(3) . ? N5 B1 1.545(4) . ? N6 C31 1.351(4) . ? O1 C34 1.134(4) . ? C1 C6 1.393(4) . ? C1 C2 1.397(4) . ? C2 C3 1.395(4) . ? C3 C4 1.388(5) . ? C4 C5 1.376(5) . ? C5 C6 1.385(4) . ? C7 C8 1.397(4) . ? C7 C12 1.399(4) . ? C8 C9 1.385(5) . ? C9 C10 1.383(5) . ? C10 C11 1.384(5) . ? C11 C12 1.382(5) . ? C13 C18 1.390(5) . ? C13 C14 1.401(4) . ? C14 C15 1.388(5) . ? C15 C16 1.382(6) . ? C16 C17 1.372(6) . ? C17 C18 1.390(5) . ? C19 C20 1.389(5) . ? C19 C22 1.497(5) . ? C20 C21 1.367(5) . ? C21 C23 1.499(5) . ? C24 C25 1.387(4) . ? C24 C27 1.492(4) . ? C25 C26 1.373(4) . ? C26 C28 1.491(4) . ? C29 C30 1.372(4) . ? C29 C32 1.492(4) . ? C30 C31 1.391(4) . ? C31 C33 1.491(4) . ? C62A Cl2A 1.632(16) . ? C62A Cl1A 1.753(12) . ? 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 C34 Rh1 N4 94.74(18) . . ? C34 Rh1 N6 170.23(11) . . ? N4 Rh1 N6 82.40(16) . . ? C34 Rh1 N2 93.66(15) . . ? N4 Rh1 N2 84.19(13) . . ? N6 Rh1 N2 95.34(12) . . ? C34 Rh1 P1 89.98(17) . . ? N4 Rh1 P1 174.38(6) . . ? N6 Rh1 P1 92.44(15) . . ? N2 Rh1 P1 98.56(13) . . ? C34 Rh1 B1 131.81(13) . . ? N4 Rh1 B1 53.78(12) . . ? N6 Rh1 B1 53.07(12) . . ? N2 Rh1 B1 52.62(13) . . ? P1 Rh1 B1 124.37(11) . . ? C7 P1 C13 102.48(16) . . ? C7 P1 C1 107.83(16) . . ? C13 P1 C1 104.64(19) . . ? C7 P1 Rh1 111.77(14) . . ? C13 P1 Rh1 117.66(15) . . ? C1 P1 Rh1 111.61(16) . . ? F2 P2 F5 89.87(19) . . ? F2 P2 F1 90.87(18) . . ? F5 P2 F1 89.99(19) . . ? F2 P2 F6 90.16(18) . . ? F5 P2 F6 91.47(19) . . ? F1 P2 F6 178.22(13) . . ? F2 P2 F4 179.28(14) . . ? F5 P2 F4 90.82(17) . . ? F1 P2 F4 89.35(17) . . ? F6 P2 F4 89.61(17) . . ? F2 P2 F3 90.87(18) . . ? F5 P2 F3 179.23(14) . . ? F1 P2 F3 90.22(18) . . ? F6 P2 F3 88.31(18) . . ? F4 P2 F3 88.44(17) . . ? C19 N2 N1 106.9(3) . . ? C19 N2 Rh1 139.0(2) . . ? N1 N2 Rh1 114.14(19) . . ? C21 N1 N2 109.4(3) . . ? C21 N1 B1 129.5(3) . . ? N2 N1 B1 119.9(2) . . ? C26 N3 N4 108.8(2) . . ? C26 N3 B1 130.1(3) . . ? N4 N3 B1 121.0(2) . . ? C24 N4 N3 107.9(2) . . ? C24 N4 Rh1 135.7(2) . . ? N3 N4 Rh1 116.2(2) . . ? C29 N5 N6 109.2(2) . . ? C29 N5 B1 129.5(3) . . ? N6 N5 B1 119.2(2) . . ? C31 N6 N5 107.3(2) . . ? C31 N6 Rh1 136.6(2) . . ? N5 N6 Rh1 115.79(18) . . ? N1 B1 N5 110.9(3) . . ? N1 B1 N3 109.3(3) . . ? N5 B1 N3 107.1(2) . . ? N1 B1 Rh1 72.52(19) . . ? N5 B1 Rh1 68.97(16) . . ? N3 B1 Rh1 68.95(15) . . ? C6 C1 C2 119.1(3) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 P1 118.7(2) . . ? C3 C2 C1 119.7(3) . . ? C4 C3 C2 120.3(3) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 120.2(3) . . ? C5 C6 C1 120.6(3) . . ? C8 C7 C12 118.8(3) . . ? C8 C7 P1 120.7(2) . . ? C12 C7 P1 120.6(2) . . ? C9 C8 C7 120.4(3) . . ? C10 C9 C8 119.9(3) . . ? C11 C10 C9 120.6(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C7 120.7(3) . . ? C18 C13 C14 119.2(3) . . ? C18 C13 P1 121.8(2) . . ? C14 C13 P1 119.0(3) . . ? C15 C14 C13 120.1(4) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 120.8(3) . . ? C16 C17 C18 120.0(4) . . ? C13 C18 C17 120.2(3) . . ? N2 C19 C20 109.2(3) . . ? N2 C19 C22 124.0(3) . . ? C20 C19 C22 126.6(3) . . ? C21 C20 C19 106.9(3) . . ? N1 C21 C20 107.6(3) . . ? N1 C21 C23 122.5(3) . . ? C20 C21 C23 129.9(3) . . ? N4 C24 C25 108.7(3) . . ? N4 C24 C27 121.9(3) . . ? C25 C24 C27 129.4(3) . . ? C26 C25 C24 107.0(3) . . ? N3 C26 C25 107.7(3) . . ? N3 C26 C28 122.7(3) . . ? C25 C26 C28 129.6(3) . . ? N5 C29 C30 107.8(3) . . ? N5 C29 C32 122.4(3) . . ? C30 C29 C32 129.8(3) . . ? C29 C30 C31 107.1(3) . . ? N6 C31 C30 108.6(3) . . ? N6 C31 C33 123.5(3) . . ? C30 C31 C33 127.8(3) . . ? O1 C34 Rh1 178.3(3) . . ? Cl2A C62A Cl1A 110.1(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 -7.5(2) . . . . ? N3 B1 N1 N2 51.9(3) . . . . ? N5 B1 N1 N2 -66.0(3) . . . . ? B1 N1 N2 C19 -167.0(2) . . . . ? H1A B1 N1 N2 171.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.411 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.060 data_4+ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 B Cl2 F6 N9 O1.50 P2 Rh' _chemical_formula_weight 843.24 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 24.390(10) _cell_length_b 13.330(4) _cell_length_c 22.563(10) _cell_angle_alpha 90.00(3) _cell_angle_beta 90.00(6) _cell_angle_gamma 90.00(3) _cell_volume 7336(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.527951 _exptl_absorpt_correction_T_max 0.927971 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33447 _diffrn_reflns_av_R_equivalents 0.3432 _diffrn_reflns_av_sigmaI/netI 0.3419 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 24.00 _reflns_number_total 9746 _reflns_number_gt 3938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.1656P)^2^+95.2565P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(14) _refine_ls_number_reflns 9746 _refine_ls_number_parameters 863 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2888 _refine_ls_R_factor_gt 0.1447 _refine_ls_wR_factor_ref 0.3938 _refine_ls_wR_factor_gt 0.2981 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 2.322 _refine_ls_shift/su_mean 0.066 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 0.82193(9) -0.09078(18) -0.40553(13) 0.0243(7) Uani 1 1 d . . . Rh2 Rh 1.19150(12) -0.4160(2) 0.27503(13) 0.0323(9) Uani 1 1 d . . . P1 P 0.7439(3) -0.1854(6) -0.4281(5) 0.031(3) Uani 1 1 d . . . P3 P 1.0364(4) 0.3791(8) -0.4843(6) 0.050(3) Uani 1 1 d . . . P4 P 1.0947(4) 0.1079(9) -0.1517(6) 0.047(3) Uani 1 1 d . . . P11 P 1.1134(4) -0.3267(7) 0.2984(5) 0.035(3) Uani 1 1 d . . . O1 O 0.7540(10) 0.0831(19) -0.391(2) 0.092(15) Uani 1 1 d . . . O2 O 1.1213(10) -0.6065(15) 0.2615(14) 0.045(9) Uani 1 1 d . . . O3 O 1.0587(6) 0.0849(13) -0.4066(15) 0.036(7) Uani 1 1 d . . . N9 N 0.7300(10) -0.164(3) -0.4961(15) 0.043(10) Uani 1 1 d . . . N3 N 0.9172(12) -0.2167(19) -0.3754(16) 0.040(10) Uani 1 1 d . . . N6 N 0.8928(11) 0.0014(17) -0.3967(16) 0.033(8) Uani 1 1 d . . . N5 N 0.9313(12) -0.039(2) -0.3559(17) 0.048(10) Uani 1 1 d . . . N2 N 0.8271(10) -0.1128(18) -0.3066(16) 0.026(8) Uani 1 1 d . . . N1 N 0.8768(12) -0.133(2) -0.2878(18) 0.033(10) Uani 1 1 d . . . N16 N 1.2636(13) -0.496(4) 0.266(2) 0.074(17) Uani 1 1 d . . . N15 N 1.3041(12) -0.4721(17) 0.2299(14) 0.030(9) Uani 1 1 d . . . N14 N 1.2470(10) -0.2984(19) 0.2908(14) 0.019(7) Uani 1 1 d . . . N13 N 1.2887(10) -0.286(2) 0.2446(13) 0.026(8) Uani 1 1 d . . . N12 N 1.1957(15) -0.398(2) 0.1774(17) 0.047(10) Uani 1 1 d . . . N11 N 1.2482(13) -0.367(2) 0.1562(12) 0.029(8) Uani 1 1 d . . . N19 N 1.1030(16) -0.350(2) 0.3690(17) 0.058(12) Uani 1 1 d . . . N18 N 1.1233(12) -0.202(2) 0.2834(17) 0.050(11) Uani 1 1 d . . . N17 N 1.0490(13) -0.354(3) 0.2650(17) 0.073(14) Uani 1 1 d . . . N4 N 0.8764(12) -0.213(2) -0.4198(13) 0.029(8) Uani 1 1 d . . . N8 N 0.7526(11) -0.3052(16) -0.4166(15) 0.037(9) Uani 1 1 d . . . N7 N 0.6853(8) -0.1642(16) -0.3977(15) 0.027(7) Uani 1 1 d . . . B1 B 0.911(4) -0.134(4) -0.299(7) 0.32(10) Uani 1 1 d . . . H1 H 0.9385 -0.1490 -0.2682 0.385 Uiso 1 1 calc R . . B2 B 1.2956(17) -0.363(2) 0.1975(16) 0.019(9) Uani 1 1 d . . . H2 H 1.3287 -0.3467 0.1747 0.023 Uiso 1 1 calc R . . C1 C 0.8519(12) -0.299(2) -0.5139(19) 0.037(12) Uani 1 1 d . . . H1A H 0.8177 -0.2644 -0.5093 0.056 Uiso 1 1 calc R . . H1B H 0.8452 -0.3697 -0.5184 0.056 Uiso 1 1 calc R . . H1C H 0.8706 -0.2743 -0.5484 0.056 Uiso 1 1 calc R . . C2 C 0.8879(16) -0.281(3) -0.4586(17) 0.038(11) Uani 1 1 d . . . C3 C 0.9347(12) -0.340(2) -0.4398(14) 0.014(9) Uani 1 1 d . . . H3 H 0.9505 -0.3961 -0.4574 0.017 Uiso 1 1 calc R . . C4 C 0.9494(17) -0.291(3) -0.3895(15) 0.042(11) Uani 1 1 d . . . C5 C 0.9972(17) -0.334(2) -0.358(2) 0.061(16) Uani 1 1 d . . . H5A H 1.0074 -0.3967 -0.3755 0.091 Uiso 1 1 calc R . . H5B H 0.9875 -0.3454 -0.3168 0.091 Uiso 1 1 calc R . . H5C H 1.0274 -0.2882 -0.3595 0.091 Uiso 1 1 calc R . . C6 C 0.8782(14) 0.131(2) -0.464(2) 0.056(16) Uani 1 1 d . . . H6A H 0.8772 0.0898 -0.4989 0.084 Uiso 1 1 calc R . . H6B H 0.8919 0.1963 -0.4742 0.084 Uiso 1 1 calc R . . H6C H 0.8419 0.1371 -0.4480 0.084 Uiso 1 1 calc R . . C7 C 0.9114(12) 0.089(2) -0.4233(15) 0.024(10) Uani 1 1 d . . . C8 C 0.9624(11) 0.113(2) -0.400(2) 0.039(11) Uani 1 1 d . . . H8 H 0.9839 0.1681 -0.4104 0.047 Uiso 1 1 calc R . . C9 C 0.9756(14) 0.036(3) -0.3568(18) 0.034(10) Uani 1 1 d . . . C10 C 1.0206(15) 0.022(2) -0.313(2) 0.053(14) Uani 1 1 d . . . H10A H 1.0445 0.0794 -0.3142 0.080 Uiso 1 1 calc R . . H10B H 1.0410 -0.0371 -0.3229 0.080 Uiso 1 1 calc R . . H10C H 1.0053 0.0155 -0.2742 0.080 Uiso 1 1 calc R . . C11 C 0.7360(17) -0.067(3) -0.2691(18) 0.061(17) Uani 1 1 d . . . H11D H 0.7344 0.0049 -0.2742 0.092 Uiso 1 1 calc R . . H11E H 0.7158 -0.0850 -0.2342 0.092 Uiso 1 1 calc R . . H11F H 0.7201 -0.0988 -0.3030 0.092 Uiso 1 1 calc R . . C12 C 0.7936(17) -0.098(3) -0.2627(17) 0.032(10) Uani 1 1 d . . . C13 C 0.826(2) -0.123(3) -0.209(2) 0.08(2) Uani 1 1 d . . . H13 H 0.8096 -0.1237 -0.1722 0.101 Uiso 1 1 calc R . . C14 C 0.876(4) -0.143(3) -0.2154(18) 0.14(4) Uani 1 1 d . . . C15 C 0.9279(16) -0.169(3) -0.181(3) 0.09(2) Uani 1 1 d . . . H15A H 0.9186 -0.2034 -0.1455 0.135 Uiso 1 1 calc R . . H15B H 0.9474 -0.1083 -0.1720 0.135 Uiso 1 1 calc R . . H15C H 0.9507 -0.2112 -0.2055 0.135 Uiso 1 1 calc R . . C16 C 0.6781(13) -0.197(3) -0.5348(18) 0.055(13) Uani 1 1 d . . . H16A H 0.6656 -0.1405 -0.5576 0.082 Uiso 1 1 calc R . . H16B H 0.6492 -0.2192 -0.5091 0.082 Uiso 1 1 calc R . . H16C H 0.6883 -0.2504 -0.5611 0.082 Uiso 1 1 calc R . . C17 C 0.7724(15) -0.089(4) -0.529(2) 0.068(17) Uani 1 1 d . . . H17A H 0.7769 -0.1087 -0.5693 0.101 Uiso 1 1 calc R . . H17B H 0.8072 -0.0909 -0.5089 0.101 Uiso 1 1 calc R . . H17C H 0.7582 -0.0216 -0.5273 0.101 Uiso 1 1 calc R . . C18 C 0.6564(14) -0.068(3) -0.411(3) 0.058(14) Uani 1 1 d . . . H18A H 0.6208 -0.0823 -0.4271 0.087 Uiso 1 1 calc R . . H18B H 0.6773 -0.0304 -0.4394 0.087 Uiso 1 1 calc R . . H18C H 0.6526 -0.0298 -0.3753 0.087 Uiso 1 1 calc R . . C19 C 0.6531(12) -0.228(2) -0.3573(18) 0.026(10) Uani 1 1 d . . . H19A H 0.6444 -0.1910 -0.3221 0.040 Uiso 1 1 calc R . . H19B H 0.6741 -0.2864 -0.3470 0.040 Uiso 1 1 calc R . . H19C H 0.6198 -0.2483 -0.3766 0.040 Uiso 1 1 calc R . . C20 C 0.7847(16) -0.341(3) -0.3604(15) 0.038(10) Uani 1 1 d . . . H20A H 0.7602 -0.3755 -0.3342 0.057 Uiso 1 1 calc R . . H20B H 0.7998 -0.2834 -0.3403 0.057 Uiso 1 1 calc R . . H20C H 0.8139 -0.3848 -0.3721 0.057 Uiso 1 1 calc R . . C21 C 0.719(2) -0.383(3) -0.441(2) 0.11(2) Uani 1 1 d . . . H21A H 0.7346 -0.4062 -0.4779 0.159 Uiso 1 1 calc R . . H21B H 0.6827 -0.3567 -0.4492 0.159 Uiso 1 1 calc R . . H21C H 0.7160 -0.4376 -0.4140 0.159 Uiso 1 1 calc R . . C23 C 0.7796(11) 0.016(2) -0.404(2) 0.049(14) Uani 1 1 d . . . C101 C 1.3978(16) -0.513(3) 0.190(2) 0.058(14) Uani 1 1 d . . . H10J H 1.3993 -0.4437 0.1787 0.086 Uiso 1 1 calc R . . H10K H 1.3953 -0.5541 0.1550 0.086 Uiso 1 1 calc R . . H10L H 1.4304 -0.5304 0.2115 0.086 Uiso 1 1 calc R . . C102 C 1.3476(13) -0.531(3) 0.2291(18) 0.036(11) Uani 1 1 d . . . C103 C 1.336(2) -0.610(2) 0.264(2) 0.064(15) Uani 1 1 d . . . H103 H 1.3553 -0.6679 0.2741 0.076 Uiso 1 1 calc R . . C104 C 1.2784(15) -0.569(4) 0.283(3) 0.09(2) Uani 1 1 d . . . C105 C 1.245(2) -0.639(3) 0.345(2) 0.073(15) Uani 1 1 d . . . H10G H 1.2177 -0.6832 0.3288 0.109 Uiso 1 1 calc R . . H10H H 1.2285 -0.5926 0.3716 0.109 Uiso 1 1 calc R . . H10I H 1.2723 -0.6779 0.3654 0.109 Uiso 1 1 calc R . . C106 C 1.3663(14) -0.170(3) 0.223(2) 0.052(14) Uani 1 1 d . . . H10D H 1.3989 -0.1584 0.2463 0.078 Uiso 1 1 calc R . . H10E H 1.3561 -0.1093 0.2033 0.078 Uiso 1 1 calc R . . H10F H 1.3731 -0.2218 0.1949 0.078 Uiso 1 1 calc R . . C107 C 1.3228(12) -0.200(2) 0.2619(16) 0.021(8) Uani 1 1 d . . . C108 C 1.3016(14) -0.167(2) 0.314(2) 0.046(13) Uani 1 1 d . . . H108 H 1.3153 -0.1149 0.3365 0.056 Uiso 1 1 calc R . . C109 C 1.2559(13) -0.225(3) 0.327(3) 0.07(2) Uani 1 1 d . . . C110 C 1.2235(17) -0.212(2) 0.3825(18) 0.039(11) Uani 1 1 d . . . H11A H 1.2347 -0.1516 0.4021 0.059 Uiso 1 1 calc R . . H11B H 1.2296 -0.2684 0.4082 0.059 Uiso 1 1 calc R . . H11C H 1.1852 -0.2080 0.3730 0.059 Uiso 1 1 calc R . . C111 C 1.291(2) -0.321(2) 0.0615(19) 0.058(14) Uani 1 1 d . . . H11V H 1.3197 -0.3703 0.0605 0.087 Uiso 1 1 calc R . . H11W H 1.3055 -0.2590 0.0769 0.087 Uiso 1 1 calc R . . H11$ H 1.2774 -0.3101 0.0221 0.087 Uiso 1 1 calc R . . C112 C 1.2438(14) -0.358(3) 0.1019(19) 0.035(10) Uani 1 1 d . . . C113 C 1.1919(15) -0.367(3) 0.0747(17) 0.032(11) Uani 1 1 d . . . H113 H 1.1798 -0.3588 0.0359 0.039 Uiso 1 1 calc R . . C114 C 1.1649(18) -0.395(3) 0.128(3) 0.08(2) Uani 1 1 d . . . C115 C 1.1030(18) -0.422(3) 0.131(3) 0.079(17) Uani 1 1 d . . . H11S H 1.0898 -0.4120 0.1706 0.119 Uiso 1 1 calc R . . H11T H 1.0982 -0.4914 0.1201 0.119 Uiso 1 1 calc R . . H11U H 1.0828 -0.3805 0.1041 0.119 Uiso 1 1 calc R . . C116 C 1.0952(18) -0.134(5) 0.319(3) 0.13(3) Uani 1 1 d . . . H11P H 1.1076 -0.0676 0.3107 0.196 Uiso 1 1 calc R . . H11Q H 1.1018 -0.1499 0.3599 0.196 Uiso 1 1 calc R . . H11R H 1.0566 -0.1391 0.3109 0.196 Uiso 1 1 calc R . . C117 C 1.1523(16) -0.170(3) 0.234(3) 0.08(2) Uani 1 1 d . . . H11G H 1.1788 -0.1203 0.2459 0.126 Uiso 1 1 calc R . . H11H H 1.1274 -0.1408 0.2059 0.126 Uiso 1 1 calc R . . H11I H 1.1709 -0.2257 0.2163 0.126 Uiso 1 1 calc R . . C118 C 1.1363(17) -0.404(3) 0.4092(19) 0.048(12) Uani 1 1 d . . . H11M H 1.1173 -0.4635 0.4218 0.072 Uiso 1 1 calc R . . H11N H 1.1442 -0.3630 0.4431 0.072 Uiso 1 1 calc R . . H11O H 1.1699 -0.4226 0.3901 0.072 Uiso 1 1 calc R . . C119 C 1.0498(14) -0.327(3) 0.400(3) 0.073(19) Uani 1 1 d . . . H11J H 1.0473 -0.3660 0.4358 0.110 Uiso 1 1 calc R . . H11K H 1.0196 -0.3429 0.3746 0.110 Uiso 1 1 calc R . . H11L H 1.0486 -0.2568 0.4100 0.110 Uiso 1 1 calc R . . C120 C 1.0236(16) -0.290(4) 0.220(3) 0.14(3) Uani 1 1 d . . . H12D H 1.0115 -0.3309 0.1872 0.216 Uiso 1 1 calc R . . H12E H 1.0500 -0.2422 0.2059 0.216 Uiso 1 1 calc R . . H12F H 0.9929 -0.2557 0.2367 0.216 Uiso 1 1 calc R . . C121 C 1.0232(12) -0.445(2) 0.2831(18) 0.024(9) Uani 1 1 d . . . H12A H 1.0172 -0.4869 0.2491 0.036 Uiso 1 1 calc R . . H12B H 0.9886 -0.4295 0.3013 0.036 Uiso 1 1 calc R . . H12C H 1.0462 -0.4791 0.3110 0.036 Uiso 1 1 calc R . . C122 C 1.1455(19) -0.539(3) 0.2603(17) 0.051(13) Uani 1 1 d . . . C201 C 1.027(2) 0.015(8) -0.524(2) 0.21(6) Uani 1 1 d . . . H20F H 1.0316 0.0692 -0.4955 0.252 Uiso 1 1 calc R . . H20G H 0.9990 0.0328 -0.5523 0.252 Uiso 1 1 calc R . . C202 C 1.011(2) -0.096(4) -0.4884(18) 0.09(2) Uani 1 1 d . . . H20D H 1.0042 -0.1472 -0.5179 0.107 Uiso 1 1 calc R . . H20E H 0.9785 -0.0870 -0.4650 0.107 Uiso 1 1 calc R . . C203 C 1.120(3) -0.397(4) -0.120(4) 0.22(6) Uani 1 1 d . . . H20H H 1.1003 -0.4591 -0.1253 0.262 Uiso 1 1 calc R . . H20I H 1.0985 -0.3568 -0.0927 0.262 Uiso 1 1 calc R . . C204 C 1.1185(16) -0.354(3) -0.167(8) 0.6(2) Uani 1 1 d D . . H20J H 1.1343 -0.3949 -0.1980 0.771 Uiso 1 1 calc R . . H20K H 1.1380 -0.2907 -0.1651 0.771 Uiso 1 1 calc R . . Cl1 Cl 1.0880(11) -0.016(2) -0.5577(10) 0.226(15) Uani 1 1 d . . . Cl2 Cl 1.0682(8) -0.1381(13) -0.4395(9) 0.137(8) Uani 1 1 d . . . Cl3 Cl 1.1836(6) -0.4325(11) -0.0766(6) 0.092(5) Uani 1 1 d . . . Cl4 Cl 1.0484(6) -0.3346(11) -0.1791(9) 0.104(6) Uani 1 1 d D . . F1 F 1.0210(11) 0.408(5) -0.415(3) 0.29(4) Uani 1 1 d . . . F2 F 1.0611(15) 0.294(4) -0.453(3) 0.29(4) Uani 1 1 d . . . F3 F 1.0960(11) 0.426(3) -0.4776(16) 0.127(14) Uani 1 1 d . . . F4 F 0.9777(15) 0.335(4) -0.4899(18) 0.152(18) Uani 1 1 d . . . F5 F 1.0552(19) 0.364(4) -0.5448(16) 0.19(2) Uani 1 1 d . . . F6 F 1.0176(18) 0.484(2) -0.500(2) 0.156(19) Uani 1 1 d . . . F7 F 1.0351(11) 0.058(4) -0.1582(19) 0.154(18) Uani 1 1 d . . . F8 F 1.0968(18) 0.117(6) -0.2146(14) 0.30(4) Uani 1 1 d . . . F9 F 1.1503(10) 0.165(3) -0.1483(14) 0.100(12) Uani 1 1 d . . . F10 F 1.0932(19) 0.097(5) -0.0834(19) 0.21(3) Uani 1 1 d . . . F11 F 1.065(3) 0.204(3) -0.138(4) 0.29(4) Uani 1 1 d . . . F12 F 1.127(3) 0.021(3) -0.144(6) 0.46(8) 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 Rh1 0.0110(11) 0.0134(13) 0.049(2) 0.0075(18) 0.0011(15) 0.0004(11) Rh2 0.0278(16) 0.0178(16) 0.051(2) 0.0017(19) -0.0015(18) -0.0035(14) P1 0.011(5) 0.006(4) 0.077(9) 0.017(5) -0.004(5) 0.000(3) P3 0.028(6) 0.042(7) 0.079(11) 0.016(6) 0.010(6) 0.013(5) P4 0.025(6) 0.065(9) 0.051(9) -0.003(6) -0.002(5) 0.016(5) P11 0.032(6) 0.023(6) 0.050(8) 0.008(5) -0.001(5) -0.003(4) O1 0.031(14) 0.030(16) 0.21(5) 0.02(2) 0.00(2) 0.008(14) O2 0.043(15) 0.000(12) 0.09(3) -0.026(13) 0.004(15) -0.022(11) O3 0.000(9) 0.000(9) 0.11(2) 0.007(15) -0.024(16) -0.011(8) N9 0.000(14) 0.09(3) 0.04(2) -0.025(19) -0.029(15) 0.002(15) N3 0.040(19) 0.000(15) 0.08(3) -0.012(15) -0.006(19) 0.027(13) N6 0.036(17) 0.000(13) 0.06(3) 0.015(16) 0.016(19) 0.001(12) N5 0.024(18) 0.036(19) 0.08(3) -0.027(19) -0.023(19) 0.015(15) N2 0.008(14) 0.003(14) 0.07(3) 0.004(14) 0.034(15) 0.009(11) N1 0.000(16) 0.005(16) 0.09(3) 0.003(16) -0.013(18) 0.005(13) N16 0.004(18) 0.15(4) 0.06(3) 0.07(3) 0.018(19) 0.05(2) N15 0.05(2) 0.000(13) 0.04(2) -0.007(13) -0.059(18) -0.010(13) N14 0.011(14) 0.000(14) 0.04(2) 0.023(13) 0.015(13) -0.004(11) N13 0.000(14) 0.045(19) 0.03(2) -0.004(15) -0.007(14) 0.022(13) N12 0.07(3) 0.007(16) 0.07(3) -0.018(16) 0.01(2) 0.026(17) N11 0.06(2) 0.032(17) 0.000(17) -0.016(13) -0.041(15) 0.029(16) N19 0.10(3) 0.000(16) 0.08(3) -0.011(17) -0.03(2) -0.015(17) N18 0.040(19) 0.024(17) 0.09(3) -0.001(18) 0.07(2) 0.020(14) N17 0.04(2) 0.10(3) 0.08(3) -0.02(2) 0.03(2) -0.10(2) N4 0.033(18) 0.032(18) 0.02(2) 0.009(15) 0.034(15) -0.007(13) N8 0.037(16) 0.000(12) 0.07(3) 0.008(15) 0.030(18) -0.014(11) N7 0.000(12) 0.018(13) 0.06(2) 0.001(15) -0.018(15) -0.014(10) B1 0.21(9) 0.00(3) 0.8(3) 0.06(7) -0.44(14) -0.04(4) B2 0.05(3) 0.000(17) 0.00(2) -0.006(14) -0.009(19) -0.002(16) C1 0.000(17) 0.02(2) 0.09(4) -0.01(2) -0.026(19) 0.018(14) C2 0.06(3) 0.03(2) 0.02(2) -0.015(18) 0.04(2) -0.04(2) C3 0.02(2) 0.008(17) 0.01(2) 0.032(14) 0.014(15) 0.042(15) C4 0.07(3) 0.05(3) 0.00(2) 0.024(18) -0.02(2) 0.02(2) C5 0.07(3) 0.00(2) 0.11(4) 0.03(2) -0.04(3) 0.008(19) C6 0.04(2) 0.000(17) 0.13(4) -0.03(2) -0.07(3) 0.003(15) C7 0.021(19) 0.006(16) 0.04(3) 0.006(17) 0.038(17) -0.010(14) C8 0.000(15) 0.04(2) 0.08(3) 0.00(3) 0.04(2) 0.006(14) C9 0.03(2) 0.04(2) 0.04(3) -0.04(2) 0.00(2) 0.003(17) C10 0.05(3) 0.000(18) 0.11(4) -0.05(2) -0.03(3) 0.011(16) C11 0.07(3) 0.08(3) 0.03(3) -0.06(2) 0.06(2) -0.06(3) C12 0.05(3) 0.03(2) 0.02(2) -0.010(19) -0.03(2) 0.02(2) C13 0.17(5) 0.02(2) 0.07(5) -0.03(2) 0.12(4) -0.05(3) C14 0.39(10) 0.03(3) 0.00(2) -0.02(2) 0.17(5) -0.04(4) C15 0.03(3) 0.03(3) 0.21(7) -0.01(3) -0.07(4) -0.002(19) C16 0.000(18) 0.11(4) 0.05(3) 0.00(3) 0.03(2) 0.00(2) C17 0.01(2) 0.10(4) 0.09(4) 0.08(3) -0.01(2) -0.01(2) C18 0.03(2) 0.06(3) 0.09(4) 0.01(3) 0.02(3) 0.027(18) C19 0.007(17) 0.000(16) 0.07(3) 0.013(17) 0.007(18) 0.020(13) C20 0.06(3) 0.05(2) 0.01(2) 0.037(18) -0.008(19) 0.00(2) C21 0.20(6) 0.01(2) 0.11(5) 0.04(2) -0.10(4) -0.09(3) C23 0.000(14) 0.000(15) 0.15(4) 0.03(2) 0.04(2) 0.025(12) C101 0.04(3) 0.06(3) 0.07(4) 0.05(3) 0.00(3) 0.03(2) C102 0.017(19) 0.03(2) 0.06(3) 0.02(2) 0.011(19) 0.030(17) C103 0.12(4) 0.000(18) 0.07(4) 0.020(19) 0.00(3) 0.00(2) C104 0.00(2) 0.11(4) 0.15(6) -0.13(4) 0.05(3) -0.05(2) C105 0.07(3) 0.12(4) 0.03(3) 0.00(3) -0.06(2) 0.03(3) C106 0.03(2) 0.03(2) 0.10(4) -0.02(2) 0.04(2) -0.033(17) C107 0.018(17) 0.000(14) 0.05(3) -0.015(14) 0.003(17) 0.014(13) C108 0.03(2) 0.000(17) 0.11(4) -0.02(2) -0.01(2) 0.000(15) C109 0.000(18) 0.03(2) 0.19(6) 0.08(3) 0.06(3) -0.006(17) C110 0.07(3) 0.001(17) 0.05(3) -0.008(17) 0.02(2) 0.015(17) C111 0.12(4) 0.000(18) 0.05(3) 0.019(17) 0.02(3) 0.00(2) C112 0.04(2) 0.04(2) 0.02(3) -0.02(2) -0.03(2) 0.009(17) C113 0.04(2) 0.05(3) 0.00(2) 0.027(18) 0.004(18) 0.019(19) C114 0.05(3) 0.04(3) 0.15(6) -0.01(3) -0.13(4) 0.01(2) C115 0.09(4) 0.02(2) 0.13(5) 0.00(3) 0.00(3) 0.01(2) C116 0.04(3) 0.22(7) 0.13(6) -0.14(5) 0.06(3) -0.05(4) C117 0.03(2) 0.000(19) 0.22(7) 0.00(3) 0.00(3) 0.011(17) C118 0.06(3) 0.03(2) 0.06(3) 0.01(2) 0.04(2) -0.01(2) C119 0.01(2) 0.02(2) 0.19(6) -0.02(3) 0.05(3) 0.026(17) C120 0.01(3) 0.12(5) 0.30(9) 0.13(6) -0.05(4) 0.04(3) C121 0.000(15) 0.03(2) 0.05(3) 0.009(19) -0.013(18) 0.005(13) C122 0.08(3) 0.05(3) 0.02(3) -0.03(2) -0.04(2) 0.03(3) C201 0.03(3) 0.60(18) 0.00(3) 0.03(6) 0.00(2) 0.08(6) C202 0.12(4) 0.15(5) 0.00(2) -0.02(3) -0.02(3) 0.08(4) C203 0.29(10) 0.05(4) 0.32(11) 0.12(5) -0.19(9) -0.17(6) C204 0.7(2) 0.07(6) 1.2(4) 0.31(13) -0.7(3) -0.30(11) Cl1 0.26(3) 0.31(3) 0.112(18) -0.02(2) 0.021(19) -0.21(3) Cl2 0.129(14) 0.126(14) 0.154(19) 0.073(13) 0.051(12) 0.057(11) Cl3 0.116(12) 0.091(11) 0.070(10) -0.010(8) -0.012(9) -0.024(9) Cl4 0.081(10) 0.089(11) 0.140(16) -0.008(10) -0.043(10) -0.033(8) F1 0.034(17) 0.58(10) 0.27(6) -0.31(7) 0.05(3) -0.10(4) F2 0.11(3) 0.38(7) 0.38(7) 0.38(7) 0.09(4) 0.11(4) F3 0.036(17) 0.23(4) 0.12(3) 0.04(3) 0.021(17) -0.01(2) F4 0.11(3) 0.24(5) 0.11(3) 0.09(3) 0.00(2) -0.04(3) F5 0.22(4) 0.29(6) 0.06(3) -0.09(3) 0.09(3) -0.12(4) F6 0.22(5) 0.033(18) 0.21(5) 0.01(2) 0.11(4) 0.03(2) F7 0.024(16) 0.28(5) 0.16(4) -0.02(3) 0.00(2) -0.05(2) F8 0.17(4) 0.71(12) 0.019(19) -0.09(4) 0.03(2) -0.30(6) F9 0.047(17) 0.16(3) 0.09(2) 0.01(2) -0.045(16) -0.068(18) F10 0.18(4) 0.34(7) 0.12(4) 0.06(4) -0.07(3) -0.23(5) F11 0.29(7) 0.11(4) 0.48(12) 0.00(5) 0.14(7) 0.10(4) F12 0.26(7) 0.05(3) 1.1(3) -0.04(6) 0.21(11) 0.09(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C23 1.76(2) . ? Rh1 N4 2.13(3) . ? Rh1 N6 2.13(3) . ? Rh1 N2 2.26(4) . ? Rh1 P1 2.339(9) . ? Rh1 B1 3.30(7) . ? Rh2 C122 2.01(5) . ? Rh2 N16 2.07(3) . ? Rh2 N14 2.10(3) . ? Rh2 N12 2.22(4) . ? Rh2 P11 2.306(11) . ? Rh2 B2 3.17(4) . ? P1 N9 1.60(3) . ? P1 N7 1.61(3) . ? P1 N8 1.63(2) . ? P3 F5 1.45(3) . ? P3 F2 1.47(3) . ? P3 F6 1.51(3) . ? P3 F4 1.55(4) . ? P3 F3 1.59(3) . ? P3 F1 1.66(5) . ? P4 F12 1.42(5) . ? P4 F8 1.43(4) . ? P4 F11 1.51(4) . ? P4 F10 1.55(4) . ? P4 F9 1.56(2) . ? P4 F7 1.61(3) . ? P11 N19 1.64(4) . ? P11 N18 1.71(3) . ? P11 N17 1.78(3) . ? O1 C23 1.12(4) . ? O2 C122 1.08(5) . ? N9 C16 1.60(5) . ? N9 C17 1.62(5) . ? N3 C4 1.31(4) . ? N3 N4 1.41(4) . ? N3 B1 2.05(15) . ? N6 C7 1.38(4) . ? N6 N5 1.42(4) . ? N5 C9 1.47(4) . ? N5 B1 1.87(13) . ? N2 C12 1.30(5) . ? N2 N1 1.31(4) . ? N1 B1 0.88(13) . ? N1 C14 1.64(6) . ? N16 C104 1.11(6) . ? N16 N15 1.33(4) . ? N15 C102 1.32(4) . ? N15 B2 1.65(4) . ? N15 C104 1.88(7) . ? N14 C109 1.29(6) . ? N14 N13 1.47(4) . ? N13 C107 1.47(4) . ? N13 B2 1.49(4) . ? N12 C114 1.35(5) . ? N12 N11 1.43(4) . ? N11 C112 1.24(5) . ? N11 B2 1.49(4) . ? N19 C118 1.42(5) . ? N19 C119 1.51(5) . ? N18 C116 1.39(5) . ? N18 C117 1.39(6) . ? N17 C121 1.42(4) . ? N17 C120 1.47(6) . ? N4 C2 1.30(4) . ? N8 C21 1.44(4) . ? N8 C20 1.56(4) . ? N7 C19 1.47(4) . ? N7 C18 1.49(4) . ? C1 C2 1.54(5) . ? C2 C3 1.45(5) . ? C3 C4 1.35(5) . ? C4 C5 1.49(5) . ? C6 C7 1.35(5) . ? C7 C8 1.39(5) . ? C8 C9 1.45(5) . ? C9 C10 1.49(5) . ? C11 C12 1.47(5) . ? C12 C13 1.47(7) . ? C13 C14 1.25(9) . ? C14 C15 1.53(9) . ? C101 C102 1.53(5) . ? C102 C103 1.35(5) . ? C103 C104 1.56(6) . ? C104 C105 1.85(8) . ? C106 C107 1.43(4) . ? C107 C108 1.35(5) . ? C108 C109 1.39(4) . ? C109 C110 1.49(6) . ? C111 C112 1.55(5) . ? C112 C113 1.41(5) . ? C113 C114 1.42(6) . ? C114 C115 1.55(6) . ? C201 C202 1.71(10) . ? C201 Cl1 1.73(5) . ? C202 Cl2 1.86(4) . ? C203 C204 1.21(16) . ? C203 Cl3 1.88(7) . ? C204 Cl4 1.75(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 C23 Rh1 N4 171.6(17) . . ? C23 Rh1 N6 90.4(12) . . ? N4 Rh1 N6 87.1(10) . . ? C23 Rh1 N2 96.9(19) . . ? N4 Rh1 N2 90.9(10) . . ? N6 Rh1 N2 86.4(12) . . ? C23 Rh1 P1 87.9(11) . . ? N4 Rh1 P1 93.6(8) . . ? N6 Rh1 P1 172.6(10) . . ? N2 Rh1 P1 100.9(7) . . ? C23 Rh1 B1 121(3) . . ? N4 Rh1 B1 64(2) . . ? N6 Rh1 B1 59.8(19) . . ? N2 Rh1 B1 39(3) . . ? P1 Rh1 B1 127.0(16) . . ? C122 Rh2 N16 92.1(18) . . ? C122 Rh2 N14 173.7(13) . . ? N16 Rh2 N14 81.7(16) . . ? C122 Rh2 N12 87.3(15) . . ? N16 Rh2 N12 85.7(14) . . ? N14 Rh2 N12 93.2(12) . . ? C122 Rh2 P11 89.9(12) . . ? N16 Rh2 P11 172.2(13) . . ? N14 Rh2 P11 96.2(7) . . ? N12 Rh2 P11 102.0(9) . . ? C122 Rh2 B2 122.7(13) . . ? N16 Rh2 B2 51.8(13) . . ? N14 Rh2 B2 53.8(10) . . ? N12 Rh2 B2 52.4(11) . . ? P11 Rh2 B2 132.3(7) . . ? N9 P1 N7 100.9(16) . . ? N9 P1 N8 110.6(18) . . ? N7 P1 N8 102.7(13) . . ? N9 P1 Rh1 106.7(12) . . ? N7 P1 Rh1 122.3(10) . . ? N8 P1 Rh1 112.8(11) . . ? F5 P3 F2 102(3) . . ? F5 P3 F6 90(3) . . ? F2 P3 F6 163(4) . . ? F5 P3 F4 99(2) . . ? F2 P3 F4 97(2) . . ? F6 P3 F4 93(2) . . ? F5 P3 F3 82(2) . . ? F2 P3 F3 83(2) . . ? F6 P3 F3 86(2) . . ? F4 P3 F3 179(3) . . ? F5 P3 F1 173(2) . . ? F2 P3 F1 79(4) . . ? F6 P3 F1 87(3) . . ? F4 P3 F1 88(2) . . ? F3 P3 F1 91.5(18) . . ? F12 P4 F8 100(5) . . ? F12 P4 F11 161(6) . . ? F8 P4 F11 98(4) . . ? F12 P4 F10 80(5) . . ? F8 P4 F10 179(4) . . ? F11 P4 F10 82(4) . . ? F12 P4 F9 85(3) . . ? F8 P4 F9 88.5(18) . . ? F11 P4 F9 90(3) . . ? F10 P4 F9 91.0(16) . . ? F12 P4 F7 100(3) . . ? F8 P4 F7 89(2) . . ? F11 P4 F7 86(3) . . ? F10 P4 F7 92(2) . . ? F9 P4 F7 175(2) . . ? N19 P11 N18 113.3(17) . . ? N19 P11 N17 103.5(18) . . ? N18 P11 N17 104.0(19) . . ? N19 P11 Rh2 104.6(14) . . ? N18 P11 Rh2 109.9(9) . . ? N17 P11 Rh2 121.6(14) . . ? C16 N9 P1 130(3) . . ? C16 N9 C17 115(3) . . ? P1 N9 C17 114(2) . . ? C4 N3 N4 106(3) . . ? C4 N3 B1 131(3) . . ? N4 N3 B1 122(2) . . ? C7 N6 N5 112(3) . . ? C7 N6 Rh1 135(3) . . ? N5 N6 Rh1 112(2) . . ? N6 N5 C9 103(3) . . ? N6 N5 B1 122(3) . . ? C9 N5 B1 132(3) . . ? C12 N2 N1 112(4) . . ? C12 N2 Rh1 134(2) . . ? N1 N2 Rh1 113(2) . . ? B1 N1 N2 143(10) . . ? B1 N1 C14 108(10) . . ? N2 N1 C14 109(4) . . ? C104 N16 N15 101(4) . . ? C104 N16 Rh2 134(4) . . ? N15 N16 Rh2 124(3) . . ? C102 N15 N16 118(3) . . ? C102 N15 B2 129(3) . . ? N16 N15 B2 113(3) . . ? C102 N15 C104 82(2) . . ? N16 N15 C104 35.4(18) . . ? B2 N15 C104 149(3) . . ? C109 N14 N13 104(2) . . ? C109 N14 Rh2 141(2) . . ? N13 N14 Rh2 114(2) . . ? N14 N13 C107 107(3) . . ? N14 N13 B2 121(3) . . ? C107 N13 B2 132(3) . . ? C114 N12 N11 102(4) . . ? C114 N12 Rh2 143(4) . . ? N11 N12 Rh2 114(2) . . ? C112 N11 N12 106(3) . . ? C112 N11 B2 133(4) . . ? N12 N11 B2 120(3) . . ? C118 N19 C119 107(4) . . ? C118 N19 P11 129(3) . . ? C119 N19 P11 123(3) . . ? C116 N18 C117 121(4) . . ? C116 N18 P11 117(3) . . ? C117 N18 P11 122(2) . . ? C121 N17 C120 120(3) . . ? C121 N17 P11 117(3) . . ? C120 N17 P11 123(3) . . ? C2 N4 N3 108(3) . . ? C2 N4 Rh1 141(3) . . ? N3 N4 Rh1 111(2) . . ? C21 N8 C20 113(3) . . ? C21 N8 P1 125(3) . . ? C20 N8 P1 119(2) . . ? C19 N7 C18 112(3) . . ? C19 N7 P1 129.4(19) . . ? C18 N7 P1 119(2) . . ? N1 B1 N5 116(6) . . ? N1 B1 N3 109(7) . . ? N5 B1 N3 77(6) . . ? N1 B1 Rh1 65(7) . . ? N5 B1 Rh1 63(2) . . ? N3 B1 Rh1 62(2) . . ? N13 B2 N11 113(3) . . ? N13 B2 N15 108(3) . . ? N11 B2 N15 110(2) . . ? N13 B2 Rh2 71(2) . . ? N11 B2 Rh2 73(2) . . ? N15 B2 Rh2 69.9(18) . . ? N4 C2 C3 111(4) . . ? N4 C2 C1 122(4) . . ? C3 C2 C1 127(3) . . ? C4 C3 C2 101(3) . . ? N3 C4 C3 114(3) . . ? N3 C4 C5 130(4) . . ? C3 C4 C5 115(4) . . ? C6 C7 N6 117(3) . . ? C6 C7 C8 134(3) . . ? N6 C7 C8 109(3) . . ? C7 C8 C9 107(3) . . ? C8 C9 N5 109(3) . . ? C8 C9 C10 134(3) . . ? N5 C9 C10 117(4) . . ? N2 C12 C13 105(3) . . ? N2 C12 C11 125(3) . . ? C13 C12 C11 131(4) . . ? C14 C13 C12 119(5) . . ? C13 C14 C15 144(5) . . ? C13 C14 N1 96(6) . . ? C15 C14 N1 120(5) . . ? O1 C23 Rh1 166(5) . . ? N15 C102 C103 107(3) . . ? N15 C102 C101 124(3) . . ? C103 C102 C101 129(3) . . ? C102 C103 C104 95(4) . . ? N16 C104 C103 120(5) . . ? N16 C104 C105 124(4) . . ? C103 C104 C105 115(5) . . ? N16 C104 N15 44(3) . . ? C103 C104 N15 76(2) . . ? C105 C104 N15 166(3) . . ? C108 C107 C106 136(3) . . ? C108 C107 N13 105(3) . . ? C106 C107 N13 119(3) . . ? C107 C108 C109 108(4) . . ? N14 C109 C108 115(4) . . ? N14 C109 C110 122(3) . . ? C108 C109 C110 123(5) . . ? N11 C112 C113 120(4) . . ? N11 C112 C111 123(4) . . ? C113 C112 C111 116(4) . . ? C112 C113 C114 94(3) . . ? N12 C114 C113 117(4) . . ? N12 C114 C115 120(6) . . ? C113 C114 C115 123(4) . . ? O2 C122 Rh2 169(4) . . ? C202 C201 Cl1 101(5) . . ? C201 C202 Cl2 112(4) . . ? C204 C203 Cl3 127(6) . . ? C203 C204 Cl4 104(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 -7(8) . . . . ? Rh2 B2 N11 N12 -5(2) . . . . ? N3 B1 N1 N2 -52(9) . . . . ? N13 B2 N11 N12 -65(4) . . . . ? N5 B1 N1 N2 32(15) . . . . ? N15 B2 N11 N12 55(4) . . . . ? B1 N1 N2 C14 -167(11) . . . . ? B2 N11 N12 C114 -178(3) . . . . ? H1 B1 N1 N2 174.4 . . . . ? H2 B2 N11 N12 174.4 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.125 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.209 data_8+[BF4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H60 B2 Cl6 F4 N6 P2 Rh' _chemical_formula_weight 1304.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 10.6624(15) _cell_length_b 17.463(2) _cell_length_c 17.664(4) _cell_angle_alpha 93.214(12) _cell_angle_beta 103.270(11) _cell_angle_gamma 107.329(12) _cell_volume 3028.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 154 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1334 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.796182 _exptl_absorpt_correction_T_max 0.894390 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25610 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.1448 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10566 _reflns_number_gt 6213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0597P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10566 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.007 _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 0.56628(5) 0.78738(3) 0.73796(3) 0.02126(15) Uani 1 1 d . . . P1 P 0.41830(16) 0.65745(10) 0.67918(10) 0.0253(4) Uani 1 1 d . . . P2 P 0.46301(16) 0.80839(10) 0.83801(10) 0.0249(4) Uani 1 1 d . . . N1 N 0.5640(5) 0.9403(3) 0.6616(3) 0.0261(12) Uani 1 1 d . . . N2 N 0.4715(5) 0.8680(3) 0.6679(3) 0.0245(12) Uani 1 1 d . . . N3 N 0.7345(5) 0.8756(3) 0.6357(3) 0.0254(12) Uani 1 1 d . . . N4 N 0.6887(5) 0.7965(3) 0.6530(3) 0.0243(12) Uani 1 1 d . . . N5 N 0.7792(5) 0.9512(3) 0.7671(3) 0.0269(12) Uani 1 1 d . . . N6 N 0.7424(5) 0.8810(3) 0.8007(3) 0.0249(12) Uani 1 1 d . . . C1 C 0.7232(7) 0.6646(4) 0.6082(4) 0.0338(17) Uani 1 1 d . . . H1A H 0.6460 0.6380 0.6290 0.051 Uiso 1 1 calc R . . H1B H 0.8065 0.6586 0.6410 0.051 Uiso 1 1 calc R . . H1C H 0.7074 0.6394 0.5543 0.051 Uiso 1 1 calc R . . C2 C 0.7382(6) 0.7520(4) 0.6083(4) 0.0260(15) Uani 1 1 d . . . C3 C 0.8128(6) 0.8016(4) 0.5641(4) 0.0311(16) Uani 1 1 d . . . H3A H 0.8586 0.7858 0.5289 0.037 Uiso 1 1 calc R . . C4 C 0.8071(6) 0.8775(4) 0.5816(4) 0.0291(15) Uani 1 1 d . . . C5 C 0.8752(8) 0.9542(4) 0.5517(4) 0.047(2) Uani 1 1 d . . . H5A H 0.8068 0.9789 0.5279 0.071 Uiso 1 1 calc R . . H5B H 0.9200 0.9415 0.5124 0.071 Uiso 1 1 calc R . . H5C H 0.9430 0.9922 0.5955 0.071 Uiso 1 1 calc R . . C6 C 0.5670(8) 1.0683(4) 0.6031(5) 0.052(2) Uani 1 1 d . . . H6A H 0.5005 1.0957 0.5833 0.078 Uiso 1 1 calc R . . H6B H 0.6142 1.0615 0.5629 0.078 Uiso 1 1 calc R . . H6C H 0.6333 1.1009 0.6505 0.078 Uiso 1 1 calc R . . C7 C 0.4949(7) 0.9865(4) 0.6224(4) 0.0299(16) Uani 1 1 d . . . C8 C 0.3600(7) 0.9447(4) 0.6041(4) 0.0330(16) Uani 1 1 d . . . H8A H 0.2879 0.9628 0.5779 0.040 Uiso 1 1 calc R . . C9 C 0.3478(6) 0.8708(4) 0.6311(4) 0.0261(15) Uani 1 1 d . . . C10 C 0.2206(6) 0.8005(4) 0.6190(4) 0.0300(16) Uani 1 1 d . . . H10A H 0.2362 0.7626 0.6562 0.045 Uiso 1 1 calc R . . H10B H 0.1951 0.7729 0.5653 0.045 Uiso 1 1 calc R . . H10C H 0.1471 0.8199 0.6277 0.045 Uiso 1 1 calc R . . C11 C 0.8333(7) 0.8267(4) 0.9213(4) 0.0359(17) Uani 1 1 d . . . H11A H 0.8212 0.7760 0.8895 0.054 Uiso 1 1 calc R . . H11B H 0.7582 0.8194 0.9463 0.054 Uiso 1 1 calc R . . H11C H 0.9196 0.8420 0.9618 0.054 Uiso 1 1 calc R . . C12 C 0.8345(6) 0.8921(4) 0.8699(4) 0.0320(16) Uani 1 1 d . . . C13 C 0.9276(6) 0.9687(4) 0.8819(4) 0.0331(17) Uani 1 1 d . . . H13A H 1.0025 0.9923 0.9263 0.040 Uiso 1 1 calc R . . C14 C 0.8900(7) 1.0042(4) 0.8165(4) 0.0348(17) Uani 1 1 d . . . C15 C 0.9527(8) 1.0878(4) 0.7971(4) 0.052(2) Uani 1 1 d . . . H15A H 0.8817 1.1128 0.7804 0.078 Uiso 1 1 calc R . . H15B H 0.9966 1.0839 0.7546 0.078 Uiso 1 1 calc R . . H15C H 1.0206 1.1210 0.8437 0.078 Uiso 1 1 calc R . . C16 C 0.3993(6) 0.6427(3) 0.5735(4) 0.0243(14) Uani 1 1 d . . . C17 C 0.4084(6) 0.7087(4) 0.5312(4) 0.0287(15) Uani 1 1 d . . . H17A H 0.4264 0.7611 0.5581 0.034 Uiso 1 1 calc R . . C18 C 0.3915(7) 0.6989(4) 0.4512(4) 0.0381(17) Uani 1 1 d . . . H18A H 0.3964 0.7444 0.4234 0.046 Uiso 1 1 calc R . . C19 C 0.3675(7) 0.6238(4) 0.4109(4) 0.0394(18) Uani 1 1 d . . . H19A H 0.3553 0.6175 0.3556 0.047 Uiso 1 1 calc R . . C20 C 0.3611(7) 0.5577(4) 0.4511(4) 0.0374(18) Uani 1 1 d . . . H20A H 0.3479 0.5064 0.4237 0.045 Uiso 1 1 calc R . . C21 C 0.3738(6) 0.5657(4) 0.5308(4) 0.0335(17) Uani 1 1 d . . . H21A H 0.3654 0.5194 0.5575 0.040 Uiso 1 1 calc R . . C22 C 0.5010(6) 0.5855(4) 0.7213(4) 0.0262(15) Uani 1 1 d . . . C23 C 0.4322(8) 0.5023(4) 0.7127(4) 0.0409(18) Uani 1 1 d . . . H23A H 0.3396 0.4817 0.6837 0.049 Uiso 1 1 calc R . . C24 C 0.4969(9) 0.4495(5) 0.7458(5) 0.054(2) Uani 1 1 d . . . H24A H 0.4497 0.3931 0.7390 0.065 Uiso 1 1 calc R . . C25 C 0.6318(10) 0.4802(5) 0.7891(5) 0.054(2) Uani 1 1 d . . . H25A H 0.6762 0.4445 0.8127 0.065 Uiso 1 1 calc R . . C26 C 0.7017(8) 0.5616(5) 0.7984(4) 0.053(2) Uani 1 1 d . . . H26A H 0.7941 0.5819 0.8277 0.063 Uiso 1 1 calc R . . C27 C 0.6362(7) 0.6134(4) 0.7647(4) 0.0357(17) Uani 1 1 d . . . H27A H 0.6847 0.6697 0.7713 0.043 Uiso 1 1 calc R . . C28 C 0.2442(6) 0.6083(4) 0.6853(4) 0.0296(16) Uani 1 1 d . . . C29 C 0.1331(6) 0.5973(4) 0.6214(4) 0.0343(17) Uani 1 1 d . . . H29A H 0.1472 0.6172 0.5740 0.041 Uiso 1 1 calc R . . C30 C 0.0009(7) 0.5572(4) 0.6265(4) 0.0389(18) Uani 1 1 d . . . H30A H -0.0743 0.5501 0.5826 0.047 Uiso 1 1 calc R . . C31 C -0.0205(7) 0.5278(4) 0.6950(5) 0.0403(19) Uani 1 1 d . . . H31A H -0.1104 0.5013 0.6985 0.048 Uiso 1 1 calc R . . C32 C 0.0872(7) 0.5368(4) 0.7576(4) 0.0392(18) Uani 1 1 d . . . H32A H 0.0721 0.5159 0.8044 0.047 Uiso 1 1 calc R . . C33 C 0.2195(7) 0.5765(4) 0.7535(4) 0.0319(16) Uani 1 1 d . . . H33A H 0.2938 0.5820 0.7974 0.038 Uiso 1 1 calc R . . C34 C 0.2908(6) 0.8176(4) 0.8099(4) 0.0266(15) Uani 1 1 d . . . C35 C 0.1768(6) 0.7523(4) 0.8057(4) 0.0332(16) Uani 1 1 d . . . H35A H 0.1878 0.7021 0.8183 0.040 Uiso 1 1 calc R . . C36 C 0.0470(7) 0.7580(5) 0.7837(4) 0.0404(18) Uani 1 1 d . . . H36A H -0.0299 0.7119 0.7802 0.048 Uiso 1 1 calc R . . C37 C 0.0304(7) 0.8312(5) 0.7668(4) 0.0425(19) Uani 1 1 d . . . H37A H -0.0584 0.8357 0.7518 0.051 Uiso 1 1 calc R . . C38 C 0.1416(7) 0.8973(4) 0.7716(4) 0.0392(18) Uani 1 1 d . . . H38A H 0.1297 0.9476 0.7603 0.047 Uiso 1 1 calc R . . C39 C 0.2720(6) 0.8914(4) 0.7930(4) 0.0299(16) Uani 1 1 d . . . H39A H 0.3486 0.9376 0.7963 0.036 Uiso 1 1 calc R . . C40 C 0.4464(6) 0.7343(4) 0.9078(4) 0.0309(16) Uani 1 1 d . . . C41 C 0.3701(7) 0.7353(4) 0.9629(4) 0.0405(18) Uani 1 1 d . . . H41A H 0.3264 0.7752 0.9650 0.049 Uiso 1 1 calc R . . C42 C 0.3593(8) 0.6775(5) 1.0142(4) 0.051(2) Uani 1 1 d . . . H42A H 0.3055 0.6770 1.0503 0.061 Uiso 1 1 calc R . . C43 C 0.4257(8) 0.6210(5) 1.0131(5) 0.057(2) Uani 1 1 d . . . H43A H 0.4197 0.5825 1.0491 0.068 Uiso 1 1 calc R . . C44 C 0.5004(7) 0.6211(4) 0.9599(4) 0.0449(19) Uani 1 1 d . . . H44A H 0.5450 0.5815 0.9585 0.054 Uiso 1 1 calc R . . C45 C 0.5127(7) 0.6775(4) 0.9077(4) 0.0334(16) Uani 1 1 d . . . H45A H 0.5667 0.6770 0.8719 0.040 Uiso 1 1 calc R . . C46 C 0.5608(6) 0.9051(4) 0.8998(4) 0.0302(16) Uani 1 1 d . . . C47 C 0.6089(7) 0.9102(5) 0.9812(4) 0.0411(18) Uani 1 1 d . . . H47A H 0.5899 0.8622 1.0053 0.049 Uiso 1 1 calc R . . C48 C 0.6835(7) 0.9835(5) 1.0274(5) 0.055(2) Uani 1 1 d . . . H48A H 0.7137 0.9857 1.0826 0.066 Uiso 1 1 calc R . . C49 C 0.7139(8) 1.0531(5) 0.9932(6) 0.057(2) Uani 1 1 d . . . H49A H 0.7664 1.1032 1.0250 0.068 Uiso 1 1 calc R . . C50 C 0.6685(7) 1.0511(4) 0.9124(5) 0.047(2) Uani 1 1 d . . . H50A H 0.6888 1.0996 0.8893 0.056 Uiso 1 1 calc R . . C51 C 0.5927(6) 0.9768(4) 0.8654(4) 0.0337(17) Uani 1 1 d . . . H51A H 0.5628 0.9750 0.8102 0.040 Uiso 1 1 calc R . . C101 C 0.1320(14) 0.3406(10) 0.9359(10) 0.151(6) Uani 1 1 d . B . C102 C 0.1011(15) 0.4086(11) 0.9652(9) 0.154(6) Uani 1 1 d . . . C103 C 0.4215(14) 1.1737(11) 0.8126(8) 0.157(7) Uani 1 1 d . . . C104 C 0.4055(11) 1.1473(8) 0.7354(7) 0.111(4) Uani 1 1 d . C . C105 C 0.0188(9) 0.3319(5) 0.6410(5) 0.060(2) Uani 1 1 d . . . H10F H 0.0618 0.3730 0.6881 0.072 Uiso 1 1 calc R . . H10G H -0.0783 0.3281 0.6240 0.072 Uiso 1 1 calc R . . C106 C 0.0277(10) 0.2530(5) 0.6626(5) 0.071(3) Uani 1 1 d . . . H10D H -0.0100 0.2411 0.7085 0.085 Uiso 1 1 calc R . . H10E H 0.1245 0.2557 0.6779 0.085 Uiso 1 1 calc R . . B1 B 0.7144(7) 0.9487(4) 0.6801(5) 0.0296(18) Uani 1 1 d . . . H1 H 0.7639 0.9996 0.6620 0.036 Uiso 1 1 calc R . . B2 B -0.2234(11) 0.2861(7) 0.7932(7) 0.062(3) Uani 1 1 d . . . F1 F -0.235(3) 0.2400(16) 0.7360(16) 0.353(17) Uani 0.755(9) 1 d P A . F1' F -0.265(2) 0.2378(12) 0.7166(13) 0.034(5) Uiso 0.245(9) 1 d P A 2 F2 F -0.3373(11) 0.3087(5) 0.7879(8) 0.149(5) Uani 0.755(9) 1 d P A . F2' F -0.320(3) 0.2765(15) 0.7258(16) 0.080(8) Uiso 0.245(9) 1 d P A 2 F3 F -0.1242(9) 0.3535(5) 0.7905(6) 0.132(4) Uani 0.755(9) 1 d P A . F3' F -0.1962(19) 0.3548(10) 0.8403(10) 0.039(5) Uiso 0.245(9) 1 d P A 2 F4 F -0.2212(8) 0.2386(4) 0.8472(4) 0.096(3) Uani 0.755(9) 1 d P A . F4' F -0.078(2) 0.2835(15) 0.8037(14) 0.090(9) Uiso 0.245(9) 1 d P A 2 Cl1 Cl -0.0025(3) 0.3366(4) 1.0322(2) 0.109(3) Uani 0.792(11) 1 d P B 1 Cl1' Cl -0.0121(18) 0.4029(14) 1.0397(10) 0.115(8) Uiso 0.208(11) 1 d P B 2 Cl2 Cl 0.2436(3) 0.40567(19) 0.87239(18) 0.1028(10) Uani 1 1 d . . . Cl3 Cl 0.2416(4) 1.1133(3) 0.6668(2) 0.107(2) Uani 0.781(10) 1 d P C 1 Cl3' Cl 0.326(2) 1.1785(13) 0.6550(11) 0.126(8) Uiso 0.219(10) 1 d P C 2 Cl4 Cl 0.3154(3) 1.2242(3) 0.8398(2) 0.101(2) Uani 0.756(8) 1 d P D 1 Cl4' Cl 0.310(2) 1.1354(14) 0.8332(13) 0.189(10) Uiso 0.244(8) 1 d P C 2 Cl5 Cl 0.0975(3) 0.36458(13) 0.56537(14) 0.0761(7) Uani 1 1 d . . . Cl6 Cl -0.0626(2) 0.17326(12) 0.58383(13) 0.0681(7) 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 Rh1 0.0186(3) 0.0236(3) 0.0223(3) 0.0006(2) 0.0062(2) 0.0077(2) P1 0.0228(10) 0.0252(9) 0.0277(10) 0.0023(8) 0.0074(8) 0.0071(8) P2 0.0205(9) 0.0312(10) 0.0238(10) -0.0027(8) 0.0074(8) 0.0094(8) N1 0.032(3) 0.022(3) 0.028(3) 0.006(2) 0.011(3) 0.011(3) N2 0.030(3) 0.022(3) 0.025(3) 0.001(2) 0.009(3) 0.013(3) N3 0.030(3) 0.022(3) 0.026(3) 0.005(2) 0.012(3) 0.007(2) N4 0.025(3) 0.024(3) 0.028(3) 0.008(2) 0.011(2) 0.009(2) N5 0.022(3) 0.028(3) 0.031(3) -0.002(3) 0.014(3) 0.004(3) N6 0.020(3) 0.029(3) 0.026(3) 0.001(2) 0.006(3) 0.008(2) C1 0.034(4) 0.031(4) 0.040(4) -0.003(3) 0.012(3) 0.014(3) C2 0.025(4) 0.022(3) 0.030(4) -0.005(3) 0.009(3) 0.006(3) C3 0.033(4) 0.035(4) 0.030(4) 0.002(3) 0.017(3) 0.012(3) C4 0.030(4) 0.031(4) 0.023(4) 0.002(3) 0.012(3) 0.002(3) C5 0.061(5) 0.037(4) 0.048(5) 0.007(4) 0.039(4) 0.004(4) C6 0.057(5) 0.034(4) 0.075(6) 0.023(4) 0.029(5) 0.017(4) C7 0.041(4) 0.025(4) 0.031(4) 0.008(3) 0.010(3) 0.020(3) C8 0.035(4) 0.039(4) 0.029(4) 0.008(3) 0.004(3) 0.021(4) C9 0.027(4) 0.030(4) 0.021(4) -0.003(3) 0.002(3) 0.012(3) C10 0.022(4) 0.037(4) 0.028(4) 0.001(3) 0.002(3) 0.009(3) C11 0.028(4) 0.047(4) 0.029(4) -0.002(3) 0.000(3) 0.014(3) C12 0.019(4) 0.048(5) 0.030(4) -0.004(3) 0.008(3) 0.013(3) C13 0.015(3) 0.043(4) 0.029(4) -0.014(3) 0.000(3) 0.000(3) C14 0.024(4) 0.028(4) 0.048(5) -0.010(3) 0.015(4) 0.000(3) C15 0.047(5) 0.043(5) 0.049(5) -0.008(4) 0.009(4) -0.004(4) C16 0.018(3) 0.020(3) 0.033(4) -0.001(3) 0.007(3) 0.004(3) C17 0.029(4) 0.028(4) 0.028(4) -0.004(3) 0.009(3) 0.009(3) C18 0.048(5) 0.032(4) 0.034(5) 0.002(3) 0.013(4) 0.010(4) C19 0.038(4) 0.050(5) 0.030(4) -0.003(4) 0.008(3) 0.016(4) C20 0.048(5) 0.027(4) 0.037(5) -0.007(3) 0.013(4) 0.013(4) C21 0.028(4) 0.029(4) 0.040(5) -0.002(3) 0.007(3) 0.005(3) C22 0.025(4) 0.028(4) 0.027(4) 0.002(3) 0.011(3) 0.008(3) C23 0.051(5) 0.040(4) 0.041(5) 0.012(4) 0.021(4) 0.022(4) C24 0.083(7) 0.043(5) 0.058(6) 0.018(4) 0.040(5) 0.034(5) C25 0.088(7) 0.062(6) 0.047(5) 0.030(5) 0.036(5) 0.057(6) C26 0.055(5) 0.073(6) 0.039(5) 0.008(4) 0.009(4) 0.037(5) C27 0.041(4) 0.044(4) 0.033(4) 0.007(3) 0.015(4) 0.025(4) C28 0.027(4) 0.023(4) 0.040(4) 0.001(3) 0.011(3) 0.009(3) C29 0.022(4) 0.033(4) 0.046(5) 0.007(3) 0.009(3) 0.005(3) C30 0.025(4) 0.040(4) 0.050(5) 0.004(4) 0.006(4) 0.010(3) C31 0.030(4) 0.034(4) 0.061(6) 0.005(4) 0.024(4) 0.008(3) C32 0.042(5) 0.041(4) 0.041(5) 0.008(4) 0.022(4) 0.013(4) C33 0.028(4) 0.032(4) 0.029(4) 0.000(3) 0.006(3) 0.001(3) C34 0.021(4) 0.033(4) 0.026(4) -0.006(3) 0.007(3) 0.010(3) C35 0.025(4) 0.035(4) 0.041(5) -0.001(3) 0.011(3) 0.011(3) C36 0.018(4) 0.055(5) 0.041(5) 0.000(4) 0.008(3) 0.003(4) C37 0.026(4) 0.071(6) 0.034(4) -0.008(4) 0.001(3) 0.027(4) C38 0.034(4) 0.046(5) 0.041(5) -0.013(4) 0.007(4) 0.023(4) C39 0.019(4) 0.040(4) 0.027(4) -0.003(3) 0.003(3) 0.008(3) C40 0.028(4) 0.041(4) 0.022(4) 0.003(3) 0.010(3) 0.006(3) C41 0.034(4) 0.061(5) 0.034(5) 0.007(4) 0.020(4) 0.018(4) C42 0.043(5) 0.073(6) 0.038(5) 0.016(4) 0.022(4) 0.009(4) C43 0.050(5) 0.078(6) 0.047(6) 0.031(5) 0.014(4) 0.022(5) C44 0.047(5) 0.051(5) 0.040(5) 0.016(4) 0.009(4) 0.020(4) C45 0.031(4) 0.042(4) 0.025(4) 0.002(3) 0.008(3) 0.009(3) C46 0.021(4) 0.038(4) 0.035(4) -0.007(3) 0.013(3) 0.012(3) C47 0.030(4) 0.056(5) 0.037(5) -0.007(4) 0.011(4) 0.015(4) C48 0.031(5) 0.076(6) 0.044(5) -0.031(5) 0.006(4) 0.006(4) C49 0.036(5) 0.052(6) 0.073(7) -0.026(5) 0.016(5) 0.007(4) C50 0.032(4) 0.038(5) 0.074(6) -0.001(4) 0.018(4) 0.013(4) C51 0.020(4) 0.035(4) 0.046(5) -0.013(3) 0.010(3) 0.011(3) C101 0.087(10) 0.169(16) 0.175(17) 0.064(13) -0.008(10) 0.031(11) C102 0.112(12) 0.193(18) 0.118(13) 0.006(12) -0.001(10) 0.016(12) C103 0.090(10) 0.31(2) 0.089(11) -0.013(12) 0.013(8) 0.103(13) C104 0.074(8) 0.154(11) 0.087(9) -0.050(8) 0.007(7) 0.032(8) C105 0.085(7) 0.046(5) 0.054(6) 0.003(4) 0.033(5) 0.017(5) C106 0.109(8) 0.045(5) 0.059(6) 0.005(4) 0.030(6) 0.019(5) B1 0.026(4) 0.022(4) 0.043(5) 0.013(4) 0.016(4) 0.002(3) B2 0.050(7) 0.061(7) 0.073(9) -0.017(7) 0.029(6) 0.009(6) F1 0.42(4) 0.38(3) 0.31(3) -0.11(2) 0.12(3) 0.20(3) F2 0.153(10) 0.102(7) 0.261(14) 0.068(8) 0.132(10) 0.078(7) F3 0.091(7) 0.094(7) 0.155(10) 0.037(6) 0.004(6) -0.033(5) F4 0.155(8) 0.085(5) 0.081(6) 0.058(5) 0.044(5) 0.068(5) Cl1 0.058(2) 0.180(6) 0.079(3) 0.051(3) 0.0131(19) 0.023(3) Cl2 0.0746(19) 0.139(3) 0.107(2) 0.068(2) 0.0285(17) 0.0385(18) Cl3 0.084(3) 0.131(5) 0.094(3) -0.050(3) -0.005(2) 0.050(3) Cl4 0.063(2) 0.137(4) 0.091(3) -0.046(2) -0.0065(19) 0.046(2) Cl5 0.100(2) 0.0508(13) 0.0674(17) 0.0094(12) 0.0341(15) -0.0010(13) Cl6 0.0879(18) 0.0393(12) 0.0656(16) 0.0019(11) 0.0215(13) 0.0031(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N6 2.108(5) . ? Rh1 N4 2.187(5) . ? Rh1 N2 2.236(5) . ? Rh1 P2 2.3521(17) . ? Rh1 P1 2.3593(18) . ? Rh1 B1 3.145(7) . ? P1 C16 1.826(6) . ? P1 C28 1.830(6) . ? P1 C22 1.837(6) . ? P2 C46 1.831(7) . ? P2 C40 1.836(6) . ? P2 C34 1.847(6) . ? N1 C7 1.362(7) . ? N1 N2 1.381(6) . ? N1 B1 1.521(8) . ? N2 C9 1.346(7) . ? N3 C4 1.356(7) . ? N3 N4 1.398(6) . ? N3 B1 1.556(8) . ? N4 C2 1.368(7) . ? N5 C14 1.341(8) . ? N5 N6 1.381(6) . ? N5 B1 1.526(9) . ? N6 C12 1.343(8) . ? C1 C2 1.488(8) . ? C2 C3 1.394(8) . ? C3 C4 1.367(8) . ? C4 C5 1.508(8) . ? C6 C7 1.506(9) . ? C7 C8 1.357(9) . ? C8 C9 1.382(8) . ? C9 C10 1.496(8) . ? C11 C12 1.498(9) . ? C12 C13 1.379(9) . ? C13 C14 1.377(9) . ? C14 C15 1.508(9) . ? C16 C17 1.401(8) . ? C16 C21 1.422(8) . ? C17 C18 1.378(9) . ? C18 C19 1.380(9) . ? C19 C20 1.382(9) . ? C20 C21 1.378(9) . ? C22 C27 1.391(9) . ? C22 C23 1.400(9) . ? C23 C24 1.387(9) . ? C24 C25 1.389(11) . ? C25 C26 1.373(11) . ? C26 C27 1.382(9) . ? C28 C29 1.393(9) . ? C28 C33 1.400(8) . ? C29 C30 1.402(8) . ? C30 C31 1.381(9) . ? C31 C32 1.362(9) . ? C32 C33 1.396(9) . ? C34 C35 1.382(8) . ? C34 C39 1.399(8) . ? C35 C36 1.383(8) . ? C36 C37 1.383(9) . ? C37 C38 1.368(9) . ? C38 C39 1.391(8) . ? C40 C45 1.379(8) . ? C40 C41 1.406(8) . ? C41 C42 1.392(9) . ? C42 C43 1.376(10) . ? C43 C44 1.365(10) . ? C44 C45 1.384(9) . ? C46 C47 1.401(9) . ? C46 C51 1.407(9) . ? C47 C48 1.384(10) . ? C48 C49 1.372(11) . ? C49 C50 1.392(11) . ? C50 C51 1.404(9) . ? C101 C102 1.424(19) . ? C101 Cl2 1.979(16) . ? C102 Cl1' 1.97(2) . ? C102 Cl1 2.034(17) . ? C103 Cl4' 1.32(2) . ? C103 C104 1.369(15) . ? C103 Cl4 1.757(13) . ? C104 Cl3' 1.69(2) . ? C104 Cl3 1.791(12) . ? C104 Cl4' 2.19(3) . ? C105 C106 1.475(10) . ? C105 Cl5 1.770(8) . ? C106 Cl6 1.780(8) . ? B2 F1 1.22(2) . ? B2 F4 1.299(13) . ? B2 F3' 1.335(19) . ? B2 F3 1.340(13) . ? B2 F2' 1.35(3) . ? B2 F2 1.369(13) . ? B2 F1' 1.45(3) . ? B2 F4' 1.53(3) . ? F1 F2' 1.24(4) . ? F1 F4' 1.74(3) . ? F1' F2' 1.05(3) . ? F2 F2' 1.28(3) . ? F2 F3' 1.524(18) . ? F3 F3' 1.297(17) . ? F3 F4' 1.46(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 N6 Rh1 N4 80.43(19) . . ? N6 Rh1 N2 95.43(19) . . ? N4 Rh1 N2 85.15(17) . . ? N6 Rh1 P2 88.21(14) . . ? N4 Rh1 P2 167.15(13) . . ? N2 Rh1 P2 90.01(13) . . ? N6 Rh1 P1 161.01(13) . . ? N4 Rh1 P1 93.55(14) . . ? N2 Rh1 P1 102.03(14) . . ? P2 Rh1 P1 99.11(6) . . ? N6 Rh1 B1 52.3(2) . . ? N4 Rh1 B1 54.75(18) . . ? N2 Rh1 B1 52.25(19) . . ? P2 Rh1 B1 113.23(14) . . ? P1 Rh1 B1 136.60(15) . . ? C16 P1 C28 101.7(3) . . ? C16 P1 C22 106.6(3) . . ? C28 P1 C22 100.4(3) . . ? C16 P1 Rh1 111.9(2) . . ? C28 P1 Rh1 128.2(2) . . ? C22 P1 Rh1 106.0(2) . . ? C46 P2 C40 104.2(3) . . ? C46 P2 C34 101.9(3) . . ? C40 P2 C34 102.7(3) . . ? C46 P2 Rh1 110.4(2) . . ? C40 P2 Rh1 117.3(2) . . ? C34 P2 Rh1 118.4(2) . . ? C7 N1 N2 108.7(5) . . ? C7 N1 B1 130.3(5) . . ? N2 N1 B1 119.4(5) . . ? C9 N2 N1 106.4(5) . . ? C9 N2 Rh1 139.9(4) . . ? N1 N2 Rh1 113.6(4) . . ? C4 N3 N4 109.4(5) . . ? C4 N3 B1 127.4(5) . . ? N4 N3 B1 122.8(5) . . ? C2 N4 N3 105.3(5) . . ? C2 N4 Rh1 142.9(4) . . ? N3 N4 Rh1 111.8(3) . . ? C14 N5 N6 108.7(5) . . ? C14 N5 B1 131.4(6) . . ? N6 N5 B1 118.2(5) . . ? C12 N6 N5 106.9(5) . . ? C12 N6 Rh1 135.7(4) . . ? N5 N6 Rh1 117.4(4) . . ? N4 C2 C3 110.1(5) . . ? N4 C2 C1 126.5(6) . . ? C3 C2 C1 123.4(5) . . ? C4 C3 C2 106.3(5) . . ? N3 C4 C3 108.9(5) . . ? N3 C4 C5 123.2(6) . . ? C3 C4 C5 127.8(6) . . ? C8 C7 N1 108.4(5) . . ? C8 C7 C6 129.6(6) . . ? N1 C7 C6 122.0(6) . . ? C7 C8 C9 106.7(5) . . ? N2 C9 C8 109.8(6) . . ? N2 C9 C10 122.9(5) . . ? C8 C9 C10 127.2(6) . . ? N6 C12 C13 109.7(6) . . ? N6 C12 C11 122.4(6) . . ? C13 C12 C11 127.8(6) . . ? C14 C13 C12 106.0(6) . . ? N5 C14 C13 108.7(6) . . ? N5 C14 C15 121.3(7) . . ? C13 C14 C15 130.0(7) . . ? C17 C16 C21 117.4(6) . . ? C17 C16 P1 119.8(5) . . ? C21 C16 P1 122.8(5) . . ? C18 C17 C16 121.0(6) . . ? C17 C18 C19 120.7(6) . . ? C18 C19 C20 119.8(7) . . ? C21 C20 C19 120.4(6) . . ? C20 C21 C16 120.6(6) . . ? C27 C22 C23 117.7(6) . . ? C27 C22 P1 119.8(5) . . ? C23 C22 P1 122.4(5) . . ? C24 C23 C22 121.1(7) . . ? C23 C24 C25 119.1(7) . . ? C26 C25 C24 120.9(7) . . ? C25 C26 C27 119.3(8) . . ? C26 C27 C22 121.7(7) . . ? C29 C28 C33 118.0(6) . . ? C29 C28 P1 121.3(5) . . ? C33 C28 P1 120.5(5) . . ? C28 C29 C30 120.5(7) . . ? C31 C30 C29 120.2(7) . . ? C32 C31 C30 120.0(7) . . ? C31 C32 C33 120.5(7) . . ? C32 C33 C28 120.8(6) . . ? C35 C34 C39 117.9(6) . . ? C35 C34 P2 121.1(5) . . ? C39 C34 P2 121.0(5) . . ? C34 C35 C36 121.8(6) . . ? C37 C36 C35 119.4(7) . . ? C38 C37 C36 120.0(6) . . ? C37 C38 C39 120.5(7) . . ? C38 C39 C34 120.3(6) . . ? C45 C40 C41 119.1(6) . . ? C45 C40 P2 119.5(5) . . ? C41 C40 P2 121.4(5) . . ? C42 C41 C40 119.5(7) . . ? C43 C42 C41 120.7(7) . . ? C44 C43 C42 119.3(7) . . ? C43 C44 C45 121.5(7) . . ? C40 C45 C44 120.0(6) . . ? C47 C46 C51 118.1(6) . . ? C47 C46 P2 121.9(5) . . ? C51 C46 P2 120.0(5) . . ? C48 C47 C46 121.5(7) . . ? C49 C48 C47 119.9(8) . . ? C48 C49 C50 120.7(8) . . ? C49 C50 C51 119.5(7) . . ? C50 C51 C46 120.3(7) . . ? C102 C101 Cl2 92.4(11) . . ? C101 C102 Cl1' 123.3(16) . . ? C101 C102 Cl1 88.7(12) . . ? Cl1' C102 Cl1 34.7(7) . . ? Cl4' C103 C104 108.7(17) . . ? Cl4' C103 Cl4 57.6(11) . . ? C104 C103 Cl4 120.9(10) . . ? C103 C104 Cl3' 128.1(12) . . ? C103 C104 Cl3 121.6(9) . . ? Cl3' C104 Cl3 43.3(8) . . ? C103 C104 Cl4' 34.9(9) . . ? Cl3' C104 Cl4' 116.7(10) . . ? Cl3 C104 Cl4' 90.4(8) . . ? C106 C105 Cl5 113.6(6) . . ? C105 C106 Cl6 111.8(6) . . ? N1 B1 N5 113.8(5) . . ? N1 B1 N3 109.8(5) . . ? N5 B1 N3 106.9(5) . . ? N1 B1 Rh1 72.8(3) . . ? N5 B1 Rh1 70.6(3) . . ? N3 B1 Rh1 70.3(3) . . ? F1 B2 F4 100.7(17) . . ? F1 B2 F3' 161(2) . . ? F4 B2 F3' 97.4(12) . . ? F1 B2 F3 105.1(17) . . ? F4 B2 F3 126.7(12) . . ? F3' B2 F3 58.0(9) . . ? F1 B2 F2' 57.8(17) . . ? F4 B2 F2' 128.4(14) . . ? F3' B2 F2' 114.4(18) . . ? F3 B2 F2' 104.8(14) . . ? F1 B2 F2 111.8(18) . . ? F4 B2 F2 106.5(9) . . ? F3' B2 F2 68.6(9) . . ? F3 B2 F2 105.8(10) . . ? F2' B2 F2 56.2(14) . . ? F1 B2 F1' 13.9(19) . . ? F4 B2 F1' 109.1(11) . . ? F3' B2 F1' 153.1(15) . . ? F3 B2 F1' 106.8(12) . . ? F2' B2 F1' 43.8(14) . . ? F2 B2 F1' 98.3(12) . . ? F1 B2 F4' 77.6(17) . . ? F4 B2 F4' 81.2(12) . . ? F3' B2 F4' 98.9(14) . . ? F3 B2 F4' 60.6(10) . . ? F2' B2 F4' 128.3(18) . . ? F2 B2 F4' 165.8(14) . . ? F1' B2 F4' 90.1(13) . . ? B2 F1 F2' 66.5(16) . . ? B2 F1 F4' 59.3(15) . . ? F2' F1 F4' 120(2) . . ? F2' F1' B2 62.8(19) . . ? F2' F2 B2 61.1(13) . . ? F2' F2 F3' 106.9(15) . . ? B2 F2 F3' 54.6(8) . . ? F1' F2' F1 18(2) . . ? F1' F2' F2 133(3) . . ? F1 F2' F2 116(3) . . ? F1' F2' B2 73.4(19) . . ? F1 F2' B2 55.7(16) . . ? F2 F2' B2 62.7(15) . . ? F3' F3 B2 60.8(9) . . ? F3' F3 F4' 104.6(13) . . ? B2 F3 F4' 66.2(11) . . ? F3 F3' B2 61.2(9) . . ? F3 F3' F2 99.6(12) . . ? B2 F3' F2 56.8(9) . . ? F3 F4' B2 53.3(10) . . ? F3 F4' F1 78.4(15) . . ? B2 F4' F1 43.1(10) . . ? C103 Cl4' C104 36.4(10) . . ? 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 Rh1 B1 N1 N2 -11.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.914 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.104 data_8+[PF6] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H64 B Cl6 F6 N6 P3 Rh' _chemical_formula_weight 1366.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.630(3) _cell_length_b 17.590(4) _cell_length_c 17.957(3) _cell_angle_alpha 95.33(2) _cell_angle_beta 102.693(19) _cell_angle_gamma 107.102(16) _cell_volume 3085.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 101 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.453220 _exptl_absorpt_correction_T_max 0.949899 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20832 _diffrn_reflns_av_R_equivalents 0.1605 _diffrn_reflns_av_sigmaI/netI 0.3232 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10676 _reflns_number_gt 4212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0564P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10676 _refine_ls_number_parameters 743 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.2341 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2058 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.56564(9) 0.79310(5) 0.73333(5) 0.0226(3) Uani 1 1 d . . . P1 P 0.4620(3) 0.81556(17) 0.83159(17) 0.0268(8) Uani 1 1 d . . . P2 P 0.4211(3) 0.66200(16) 0.67623(16) 0.0240(7) Uani 1 1 d . . . N1 N 0.5587(9) 0.9422(5) 0.6594(5) 0.026(2) Uani 1 1 d . . . N2 N 0.4683(8) 0.8688(5) 0.6656(5) 0.027(2) Uani 1 1 d . . . N5 N 0.7318(9) 0.8793(5) 0.6325(5) 0.027(2) Uani 1 1 d . . . N6 N 0.6873(8) 0.8009(5) 0.6496(5) 0.023(2) Uani 1 1 d . . . N3 N 0.7754(9) 0.9564(5) 0.7629(5) 0.030(2) Uani 1 1 d . . . N4 N 0.7398(9) 0.8887(5) 0.7951(5) 0.031(2) Uani 1 1 d . . . C1 C 0.5569(12) 1.0655(6) 0.6014(7) 0.043(3) Uani 1 1 d . . . H1A H 0.6248 1.0980 0.6466 0.064 Uiso 1 1 calc R . . H1B H 0.4908 1.0919 0.5851 0.064 Uiso 1 1 calc R . . H1C H 0.5994 1.0582 0.5605 0.064 Uiso 1 1 calc R . . C2 C 0.4886(12) 0.9860(7) 0.6197(6) 0.030(3) Uani 1 1 d . . . C3 C 0.3541(12) 0.9416(6) 0.6013(6) 0.030(3) Uani 1 1 d . . . H3 H 0.2820 0.9569 0.5753 0.036 Uiso 1 1 calc R . . C4 C 0.3440(11) 0.8693(6) 0.6285(6) 0.026(3) Uani 1 1 d . . . C5 C 0.2184(10) 0.7985(6) 0.6172(6) 0.029(3) Uani 1 1 d . . . H5A H 0.1942 0.7692 0.5655 0.044 Uiso 1 1 calc R . . H5B H 0.1451 0.8170 0.6250 0.044 Uiso 1 1 calc R . . H5C H 0.2353 0.7639 0.6538 0.044 Uiso 1 1 calc R . . C6 C 0.8667(12) 0.9557(6) 0.5506(7) 0.047(4) Uani 1 1 d . . . H6A H 0.8009 0.9825 0.5348 0.071 Uiso 1 1 calc R . . H6B H 0.8986 0.9411 0.5070 0.071 Uiso 1 1 calc R . . H6C H 0.9422 0.9913 0.5907 0.071 Uiso 1 1 calc R . . C7 C 0.8022(10) 0.8817(6) 0.5802(6) 0.029(3) Uani 1 1 d . . . C8 C 0.8138(11) 0.8056(7) 0.5616(7) 0.035(3) Uani 1 1 d . . . H8 H 0.8608 0.7904 0.5280 0.042 Uiso 1 1 calc R . . C9 C 0.7385(10) 0.7574(6) 0.6049(6) 0.023(3) Uani 1 1 d . . . C10 C 0.7251(11) 0.6706(6) 0.6043(7) 0.035(3) Uani 1 1 d . . . H10A H 0.8047 0.6662 0.6387 0.052 Uiso 1 1 calc R . . H10B H 0.7160 0.6454 0.5527 0.052 Uiso 1 1 calc R . . H10C H 0.6459 0.6442 0.6210 0.052 Uiso 1 1 calc R . . C11 C 0.9454(12) 1.0935(6) 0.7944(7) 0.050(4) Uani 1 1 d . . . H11A H 1.0066 1.1283 0.8407 0.076 Uiso 1 1 calc R . . H11B H 0.8740 1.1152 0.7750 0.076 Uiso 1 1 calc R . . H11C H 0.9945 1.0899 0.7560 0.076 Uiso 1 1 calc R . . C12 C 0.8854(11) 1.0119(6) 0.8121(7) 0.032(3) Uani 1 1 d . . . C13 C 0.9252(11) 0.9785(7) 0.8747(7) 0.037(3) Uani 1 1 d . . . H13 H 1.0002 1.0024 0.9169 0.045 Uiso 1 1 calc R . . C14 C 0.8324(11) 0.9022(7) 0.8634(7) 0.031(3) Uani 1 1 d . . . C15 C 0.8348(11) 0.8392(7) 0.9126(6) 0.044(3) Uani 1 1 d . . . H15A H 0.7482 0.8196 0.9243 0.067 Uiso 1 1 calc R . . H15B H 0.9052 0.8617 0.9598 0.067 Uiso 1 1 calc R . . H15C H 0.8525 0.7954 0.8854 0.067 Uiso 1 1 calc R . . C16 C 0.2913(10) 0.8237(6) 0.8038(6) 0.023(3) Uani 1 1 d . . . C17 C 0.1782(11) 0.7588(7) 0.7981(6) 0.033(3) Uani 1 1 d . . . H17 H 0.1889 0.7100 0.8085 0.040 Uiso 1 1 calc R . . C18 C 0.0496(11) 0.7643(7) 0.7774(7) 0.045(3) Uani 1 1 d . . . H18 H -0.0248 0.7191 0.7744 0.054 Uiso 1 1 calc R . . C19 C 0.0273(11) 0.8353(8) 0.7610(7) 0.045(4) Uani 1 1 d . . . H19 H -0.0604 0.8380 0.7453 0.054 Uiso 1 1 calc R . . C20 C 0.1408(12) 0.9018(7) 0.7689(6) 0.041(3) Uani 1 1 d . . . H20 H 0.1286 0.9508 0.7604 0.050 Uiso 1 1 calc R . . C21 C 0.2713(11) 0.8981(7) 0.7889(6) 0.032(3) Uani 1 1 d . . . H21 H 0.3456 0.9436 0.7927 0.038 Uiso 1 1 calc R . . C22 C 0.4452(11) 0.7452(6) 0.8979(6) 0.032(3) Uani 1 1 d . . . C23 C 0.5123(10) 0.6880(7) 0.9002(6) 0.032(3) Uani 1 1 d . . . H23 H 0.5668 0.6864 0.8665 0.039 Uiso 1 1 calc R . . C24 C 0.5004(12) 0.6341(7) 0.9506(7) 0.046(3) Uani 1 1 d . . . H24 H 0.5451 0.5959 0.9498 0.055 Uiso 1 1 calc R . . C25 C 0.4243(13) 0.6358(8) 1.0016(8) 0.059(4) Uani 1 1 d . . . H25 H 0.4182 0.5994 1.0360 0.071 Uiso 1 1 calc R . . C26 C 0.3564(14) 0.6906(10) 1.0028(8) 0.069(5) Uani 1 1 d . . . H26 H 0.3035 0.6911 1.0377 0.082 Uiso 1 1 calc R . . C27 C 0.3663(12) 0.7462(8) 0.9515(7) 0.048(4) Uani 1 1 d . . . H27 H 0.3208 0.7838 0.9528 0.057 Uiso 1 1 calc R . . C28 C 0.5594(11) 0.9124(7) 0.8946(7) 0.032(3) Uani 1 1 d . . . C29 C 0.6074(11) 0.9171(7) 0.9727(7) 0.039(3) Uani 1 1 d . . . H29 H 0.5881 0.8702 0.9941 0.047 Uiso 1 1 calc R . . C30 C 0.6846(13) 0.9904(9) 1.0209(9) 0.064(4) Uani 1 1 d . . . H30 H 0.7135 0.9926 1.0741 0.076 Uiso 1 1 calc R . . C31 C 0.7172(12) 1.0587(9) 0.9892(9) 0.062(5) Uani 1 1 d . . . H31 H 0.7725 1.1072 1.0209 0.075 Uiso 1 1 calc R . . C32 C 0.6700(11) 1.0576(7) 0.9112(8) 0.047(4) Uani 1 1 d . . . H32 H 0.6888 1.1049 0.8904 0.056 Uiso 1 1 calc R . . C33 C 0.5927(10) 0.9830(7) 0.8636(7) 0.036(3) Uani 1 1 d . . . H33 H 0.5632 0.9808 0.8105 0.043 Uiso 1 1 calc R . . C34 C 0.4022(10) 0.6422(6) 0.5735(6) 0.024(3) Uani 1 1 d . . . C35 C 0.4123(10) 0.7045(6) 0.5297(6) 0.032(3) Uani 1 1 d . . . H35 H 0.4309 0.7567 0.5552 0.039 Uiso 1 1 calc R . . C36 C 0.3963(11) 0.6928(6) 0.4524(6) 0.035(3) Uani 1 1 d . . . H36 H 0.3999 0.7356 0.4253 0.042 Uiso 1 1 calc R . . C37 C 0.3742(12) 0.6158(7) 0.4137(7) 0.042(3) Uani 1 1 d . . . H37 H 0.3657 0.6070 0.3606 0.050 Uiso 1 1 calc R . . C38 C 0.3651(11) 0.5524(6) 0.4546(6) 0.032(3) Uani 1 1 d . . . H38 H 0.3497 0.5009 0.4288 0.039 Uiso 1 1 calc R . . C39 C 0.3784(10) 0.5647(6) 0.5318(6) 0.030(3) Uani 1 1 d . . . H39 H 0.3717 0.5212 0.5582 0.036 Uiso 1 1 calc R . . C40 C 0.2474(10) 0.6114(6) 0.6819(6) 0.026(3) Uani 1 1 d . . . C41 C 0.2223(11) 0.5827(6) 0.7488(7) 0.032(3) Uani 1 1 d . . . H41 H 0.2948 0.5908 0.7918 0.039 Uiso 1 1 calc R . . C42 C 0.0903(12) 0.5421(7) 0.7521(7) 0.042(3) Uani 1 1 d . . . H42 H 0.0757 0.5221 0.7967 0.051 Uiso 1 1 calc R . . C43 C -0.0190(12) 0.5314(7) 0.6896(7) 0.042(3) Uani 1 1 d . . . H43 H -0.1075 0.5048 0.6917 0.051 Uiso 1 1 calc R . . C44 C 0.0059(11) 0.5608(7) 0.6241(7) 0.038(3) Uani 1 1 d . . . H44 H -0.0669 0.5538 0.5815 0.046 Uiso 1 1 calc R . . C45 C 0.1369(11) 0.6007(6) 0.6202(7) 0.032(3) Uani 1 1 d . . . H45 H 0.1506 0.6205 0.5754 0.038 Uiso 1 1 calc R . . C46 C 0.5075(10) 0.5936(6) 0.7185(5) 0.021(3) Uani 1 1 d . . . C47 C 0.4423(11) 0.5133(6) 0.7123(6) 0.032(3) Uani 1 1 d . . . H47 H 0.3519 0.4907 0.6837 0.039 Uiso 1 1 calc R . . C48 C 0.5103(13) 0.4651(7) 0.7485(7) 0.043(3) Uani 1 1 d . . . H48 H 0.4654 0.4102 0.7439 0.052 Uiso 1 1 calc R . . C49 C 0.6442(13) 0.4982(8) 0.7914(7) 0.046(3) Uani 1 1 d . . . H49 H 0.6894 0.4662 0.8168 0.055 Uiso 1 1 calc R . . C50 C 0.7094(13) 0.5788(7) 0.7958(7) 0.043(3) Uani 1 1 d . . . H50 H 0.8004 0.6017 0.8232 0.052 Uiso 1 1 calc R . . C51 C 0.6395(11) 0.6264(6) 0.7595(6) 0.028(3) Uani 1 1 d . . . H51 H 0.6839 0.6813 0.7633 0.033 Uiso 1 1 calc R . . C61 C 0.9639(16) 0.7443(8) 0.3434(7) 0.075(5) Uani 1 1 d . . . H61A H 0.8699 0.7435 0.3311 0.090 Uiso 1 1 calc R . . H61B H 0.9973 0.7541 0.2979 0.090 Uiso 1 1 calc R . . C62 C 0.9681(14) 0.6647(7) 0.3607(7) 0.058(4) Uani 1 1 d . . . H62A H 1.0624 0.6660 0.3736 0.069 Uiso 1 1 calc R . . H62B H 0.9200 0.6247 0.3144 0.069 Uiso 1 1 calc R . . C63 C 0.8527(19) 0.5908(16) 0.0423(12) 0.28(2) Uani 1 1 d D C . H63A H 0.9341 0.5793 0.0672 0.330 Uiso 1 1 calc R . . H63B H 0.8071 0.5510 -0.0044 0.330 Uiso 1 1 calc R . . C64 C 0.8900(19) 0.6641(17) 0.0222(13) 0.249(19) Uani 1 1 d D . . H64A H 0.9265 0.7030 0.0699 0.299 Uiso 1 1 calc R A 1 H64B H 0.8072 0.6728 -0.0050 0.299 Uiso 1 1 calc R A 1 C65 C 0.6104(14) 0.8527(11) 0.2659(9) 0.122(7) Uani 1 1 d D D . H65A H 0.5579 0.8092 0.2873 0.147 Uiso 1 1 calc R . . H65B H 0.5677 0.8945 0.2660 0.147 Uiso 1 1 calc R . . C66 C 0.599(2) 0.8234(12) 0.1899(11) 0.151(9) Uiso 1 1 d D . . H66A H 0.6214 0.8700 0.1644 0.181 Uiso 1 1 calc R B 1 H66B H 0.5033 0.7940 0.1668 0.181 Uiso 1 1 calc R B 1 B1 B 0.7101(13) 0.9506(7) 0.6775(7) 0.029(3) Uani 1 1 d . . . H1 H 0.7579 1.0000 0.6606 0.035 Uiso 1 1 calc R . . P3 P 0.2209(4) 0.6992(2) 0.2107(2) 0.0426(9) Uani 1 1 d . . . F1 F 0.1657(8) 0.6269(4) 0.2520(4) 0.074(2) Uani 1 1 d . . . F2 F 0.3656(7) 0.6888(4) 0.2317(6) 0.101(3) Uani 1 1 d . . . F3 F 0.2777(10) 0.7713(5) 0.1707(6) 0.125(4) Uani 1 1 d . . . F4 F 0.0761(7) 0.7102(5) 0.1901(5) 0.081(3) Uani 1 1 d . . . F5 F 0.1840(9) 0.6371(5) 0.1346(4) 0.091(3) Uani 1 1 d . . . F6 F 0.2566(9) 0.7588(5) 0.2891(5) 0.097(3) Uani 1 1 d . . . Cl1 Cl 1.0609(4) 0.82437(19) 0.4200(2) 0.0663(11) Uani 1 1 d . . . Cl2 Cl 0.8978(4) 0.6343(2) 0.4359(2) 0.0736(12) Uani 1 1 d . . . Cl3 Cl 0.7382(5) 0.5790(3) 0.1082(3) 0.135(2) Uani 1 1 d D . . Cl4 Cl 1.0028(13) 0.6891(7) -0.0322(9) 0.074(6) Uani 0.41(2) 1 d PD C 1 Cl4' Cl 0.9920(17) 0.639(3) -0.0399(9) 0.50(3) Uani 0.59(2) 1 d PD C 2 Cl5 Cl 0.7692(5) 0.8913(3) 0.3268(3) 0.1120(18) Uani 1 1 d D . . Cl6 Cl 0.6880(7) 0.7630(6) 0.1635(6) 0.102(5) Uani 0.555(13) 1 d PD D 1 Cl6' Cl 0.7038(13) 0.8502(12) 0.1381(7) 0.173(10) Uani 0.445(13) 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0188(5) 0.0193(5) 0.0277(6) -0.0019(4) 0.0057(4) 0.0051(4) P1 0.0233(17) 0.0283(18) 0.0282(18) -0.0025(14) 0.0071(14) 0.0096(15) P2 0.0223(16) 0.0218(17) 0.0266(18) 0.0017(13) 0.0084(13) 0.0044(14) N1 0.037(6) 0.013(5) 0.026(5) -0.001(4) 0.012(4) 0.003(5) N2 0.011(5) 0.033(6) 0.037(6) 0.002(4) 0.015(4) 0.002(4) N5 0.030(6) 0.018(5) 0.030(6) 0.002(4) 0.016(5) -0.001(5) N6 0.023(5) 0.014(5) 0.033(6) 0.006(4) 0.013(4) 0.005(4) N3 0.027(6) 0.019(5) 0.039(6) -0.009(5) 0.013(5) -0.001(5) N4 0.027(6) 0.030(6) 0.027(6) -0.014(5) 0.003(5) 0.003(5) C1 0.053(8) 0.027(7) 0.049(8) 0.014(6) 0.015(7) 0.011(7) C2 0.040(8) 0.026(7) 0.024(7) 0.001(5) 0.016(6) 0.007(6) C3 0.047(8) 0.021(7) 0.023(7) 0.003(5) 0.005(6) 0.013(6) C4 0.032(7) 0.015(6) 0.029(7) -0.010(5) 0.009(5) 0.007(6) C5 0.025(6) 0.030(7) 0.038(7) 0.002(5) 0.014(5) 0.013(6) C6 0.058(9) 0.028(7) 0.053(9) 0.013(6) 0.034(7) -0.007(7) C7 0.020(6) 0.025(7) 0.035(7) -0.006(6) 0.007(5) -0.002(6) C8 0.028(7) 0.035(7) 0.050(8) 0.008(6) 0.028(6) 0.011(6) C9 0.022(6) 0.017(6) 0.026(7) -0.006(5) 0.002(5) 0.007(5) C10 0.027(7) 0.027(7) 0.055(8) 0.009(6) 0.024(6) 0.004(6) C11 0.041(8) 0.016(7) 0.075(10) -0.003(7) 0.007(7) -0.011(6) C12 0.021(7) 0.020(7) 0.049(8) -0.013(6) 0.011(6) 0.006(6) C13 0.013(6) 0.035(8) 0.052(9) -0.010(6) -0.006(6) 0.005(6) C14 0.021(6) 0.037(8) 0.036(8) -0.004(6) 0.009(6) 0.012(6) C15 0.038(8) 0.052(9) 0.037(8) -0.013(7) 0.008(6) 0.012(7) C16 0.023(6) 0.024(6) 0.021(6) -0.001(5) 0.008(5) 0.009(6) C17 0.024(7) 0.027(7) 0.056(8) 0.009(6) 0.013(6) 0.014(6) C18 0.021(7) 0.044(8) 0.062(9) -0.015(7) 0.008(6) 0.010(7) C19 0.014(7) 0.060(9) 0.053(9) -0.020(7) 0.010(6) 0.006(7) C20 0.042(8) 0.037(8) 0.038(8) -0.014(6) -0.007(6) 0.020(7) C21 0.020(6) 0.041(8) 0.037(7) -0.003(6) 0.015(5) 0.011(6) C22 0.027(7) 0.028(7) 0.036(8) -0.005(6) 0.000(6) 0.013(6) C23 0.022(6) 0.045(8) 0.018(7) -0.005(6) -0.002(5) -0.001(6) C24 0.043(8) 0.050(9) 0.051(9) 0.023(7) 0.018(7) 0.017(7) C25 0.039(9) 0.070(11) 0.065(11) 0.036(9) 0.007(8) 0.010(8) C26 0.052(10) 0.111(14) 0.046(10) 0.027(9) 0.018(8) 0.023(10) C27 0.046(8) 0.074(10) 0.035(8) 0.007(7) 0.014(7) 0.037(8) C28 0.027(7) 0.036(8) 0.032(7) -0.011(6) 0.008(6) 0.014(6) C29 0.035(7) 0.042(8) 0.034(8) -0.018(6) 0.007(6) 0.009(6) C30 0.040(9) 0.069(11) 0.061(11) -0.039(9) 0.009(8) 0.006(9) C31 0.016(7) 0.059(11) 0.084(12) -0.048(9) 0.010(8) -0.011(8) C32 0.027(7) 0.021(7) 0.081(11) -0.015(7) 0.016(7) -0.003(6) C33 0.017(6) 0.044(8) 0.042(8) -0.005(7) 0.011(6) 0.006(6) C34 0.020(6) 0.020(6) 0.032(7) 0.006(5) 0.014(5) 0.002(5) C35 0.027(7) 0.029(7) 0.028(7) -0.015(6) -0.005(5) 0.006(6) C36 0.037(7) 0.033(7) 0.028(7) 0.000(6) -0.002(6) 0.011(6) C37 0.051(8) 0.041(8) 0.026(7) -0.005(6) 0.008(6) 0.008(7) C38 0.039(7) 0.023(7) 0.027(7) -0.013(6) 0.004(6) 0.007(6) C39 0.031(7) 0.017(6) 0.035(7) -0.009(5) 0.001(5) 0.008(5) C40 0.027(6) 0.017(6) 0.036(7) 0.004(5) 0.018(6) 0.004(5) C41 0.024(7) 0.024(7) 0.046(8) 0.006(6) 0.011(6) 0.002(6) C42 0.050(9) 0.040(8) 0.045(8) 0.016(7) 0.035(7) 0.007(7) C43 0.031(8) 0.032(8) 0.058(9) 0.003(7) 0.011(7) 0.003(6) C44 0.020(7) 0.036(8) 0.046(8) 0.003(6) -0.003(6) 0.000(6) C45 0.029(7) 0.019(6) 0.048(8) 0.014(6) 0.004(6) 0.009(6) C46 0.017(6) 0.022(6) 0.015(6) -0.007(5) 0.002(5) -0.005(5) C47 0.018(6) 0.026(7) 0.046(8) 0.001(6) 0.001(6) 0.002(6) C48 0.057(9) 0.024(7) 0.057(9) 0.004(6) 0.028(7) 0.015(7) C49 0.048(9) 0.060(10) 0.045(9) 0.014(7) 0.016(7) 0.037(8) C50 0.045(8) 0.037(8) 0.048(8) 0.010(7) 0.013(7) 0.013(7) C51 0.033(7) 0.023(6) 0.032(7) 0.008(5) 0.021(6) 0.007(6) C61 0.112(13) 0.095(12) 0.042(9) 0.021(9) 0.034(9) 0.056(11) C62 0.068(10) 0.045(9) 0.061(10) 0.011(7) 0.035(8) 0.006(8) C63 0.089(17) 0.40(5) 0.15(2) 0.14(3) -0.063(16) -0.16(2) C64 0.049(16) 0.46(6) 0.20(3) 0.14(3) -0.021(17) 0.03(3) C65 0.093(14) 0.151(18) 0.076(13) -0.058(12) 0.022(11) -0.006(13) B1 0.029(8) 0.021(7) 0.038(9) -0.001(6) 0.009(6) 0.011(7) P3 0.048(2) 0.038(2) 0.045(2) 0.0117(18) 0.0173(18) 0.0118(19) F1 0.082(6) 0.070(6) 0.084(6) 0.038(5) 0.045(5) 0.018(5) F2 0.047(5) 0.046(5) 0.211(11) 0.031(6) 0.033(6) 0.013(4) F3 0.154(9) 0.102(7) 0.195(11) 0.108(8) 0.118(9) 0.076(7) F4 0.054(5) 0.084(6) 0.104(7) -0.001(5) 0.005(5) 0.036(5) F5 0.132(8) 0.096(7) 0.055(6) -0.004(5) 0.022(5) 0.058(6) F6 0.107(7) 0.075(6) 0.076(6) -0.030(5) -0.007(5) 0.016(6) Cl1 0.084(3) 0.038(2) 0.069(3) 0.0048(19) 0.024(2) 0.007(2) Cl2 0.085(3) 0.047(2) 0.082(3) 0.010(2) 0.041(2) -0.003(2) Cl3 0.077(3) 0.156(5) 0.150(5) 0.087(4) 0.001(3) 0.008(4) Cl4 0.043(7) 0.063(9) 0.108(11) 0.055(6) 0.012(7) 0.001(5) Cl4' 0.101(12) 1.05(7) 0.134(15) 0.21(3) -0.049(10) -0.09(3) Cl5 0.091(3) 0.121(4) 0.114(4) -0.027(3) 0.008(3) 0.049(3) Cl6 0.056(5) 0.104(9) 0.110(8) -0.054(6) 0.008(5) 0.004(5) Cl6' 0.113(10) 0.22(2) 0.098(10) 0.074(10) -0.026(8) -0.048(11) _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 N4 2.099(9) . ? Rh1 N6 2.177(8) . ? Rh1 N2 2.210(9) . ? Rh1 P1 2.337(3) . ? Rh1 P2 2.348(3) . ? Rh1 B1 3.119(14) . ? P1 C22 1.794(12) . ? P1 C16 1.825(10) . ? P1 C28 1.829(11) . ? P2 C34 1.801(10) . ? P2 C40 1.829(11) . ? P2 C46 1.839(11) . ? N1 C2 1.365(12) . ? N1 N2 1.396(10) . ? N1 B1 1.529(14) . ? N2 C4 1.346(12) . ? N5 C7 1.319(12) . ? N5 N6 1.407(10) . ? N5 B1 1.530(14) . ? N6 C9 1.360(12) . ? N3 C12 1.347(12) . ? N3 N4 1.362(11) . ? N3 B1 1.519(14) . ? N4 C14 1.344(13) . ? C1 C2 1.479(13) . ? C2 C3 1.361(14) . ? C3 C4 1.387(13) . ? C4 C5 1.493(13) . ? C6 C7 1.488(14) . ? C7 C8 1.397(14) . ? C8 C9 1.400(14) . ? C9 C10 1.491(12) . ? C11 C12 1.486(14) . ? C12 C13 1.360(14) . ? C13 C14 1.378(14) . ? C14 C15 1.483(14) . ? C16 C17 1.370(13) . ? C16 C21 1.425(13) . ? C17 C18 1.370(14) . ? C18 C19 1.383(15) . ? C19 C20 1.381(14) . ? C20 C21 1.377(14) . ? C22 C23 1.393(14) . ? C22 C27 1.411(14) . ? C23 C24 1.369(14) . ? C24 C25 1.352(16) . ? C25 C26 1.365(18) . ? C26 C27 1.401(16) . ? C28 C29 1.368(14) . ? C28 C33 1.391(14) . ? C29 C30 1.393(15) . ? C30 C31 1.364(18) . ? C31 C32 1.377(18) . ? C32 C33 1.405(14) . ? C34 C35 1.400(13) . ? C34 C39 1.416(13) . ? C35 C36 1.350(14) . ? C36 C37 1.393(14) . ? C37 C38 1.382(14) . ? C38 C39 1.353(13) . ? C40 C45 1.380(13) . ? C40 C41 1.393(14) . ? C41 C42 1.392(14) . ? C42 C43 1.380(15) . ? C43 C44 1.375(15) . ? C44 C45 1.383(14) . ? C46 C51 1.354(13) . ? C46 C47 1.360(13) . ? C47 C48 1.386(14) . ? C48 C49 1.380(15) . ? C49 C50 1.369(15) . ? C50 C51 1.391(14) . ? C61 C62 1.474(15) . ? C61 Cl1 1.761(14) . ? C62 Cl2 1.735(12) . ? C63 C64 1.341(18) . ? C63 Cl3 1.858(17) . ? C64 Cl4 1.694(18) . ? C64 Cl4' 1.826(19) . ? C65 C66 1.380(15) . ? C65 Cl5 1.698(13) . ? C66 Cl6' 1.599(15) . ? C66 Cl6 1.715(15) . ? P3 F3 1.549(8) . ? P3 F1 1.563(7) . ? P3 F5 1.564(8) . ? P3 F2 1.570(8) . ? P3 F4 1.576(8) . ? P3 F6 1.576(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 N4 Rh1 N6 80.4(3) . . ? N4 Rh1 N2 95.5(3) . . ? N6 Rh1 N2 85.1(3) . . ? N4 Rh1 P1 88.3(3) . . ? N6 Rh1 P1 167.2(2) . . ? N2 Rh1 P1 90.0(2) . . ? N4 Rh1 P2 160.8(3) . . ? N6 Rh1 P2 93.9(2) . . ? N2 Rh1 P2 102.4(2) . . ? P1 Rh1 P2 98.72(11) . . ? N4 Rh1 B1 52.1(3) . . ? N6 Rh1 B1 54.4(3) . . ? N2 Rh1 B1 52.7(3) . . ? P1 Rh1 B1 113.5(2) . . ? P2 Rh1 B1 137.1(2) . . ? C22 P1 C16 102.7(5) . . ? C22 P1 C28 103.4(5) . . ? C16 P1 C28 102.2(5) . . ? C22 P1 Rh1 117.6(4) . . ? C16 P1 Rh1 118.1(3) . . ? C28 P1 Rh1 110.7(4) . . ? C34 P2 C40 101.3(5) . . ? C34 P2 C46 106.1(5) . . ? C40 P2 C46 100.3(5) . . ? C34 P2 Rh1 112.4(3) . . ? C40 P2 Rh1 128.7(3) . . ? C46 P2 Rh1 105.8(3) . . ? C2 N1 N2 109.8(8) . . ? C2 N1 B1 130.6(10) . . ? N2 N1 B1 117.4(8) . . ? C4 N2 N1 105.4(8) . . ? C4 N2 Rh1 140.3(8) . . ? N1 N2 Rh1 114.2(6) . . ? C7 N5 N6 110.8(8) . . ? C7 N5 B1 127.4(10) . . ? N6 N5 B1 121.5(9) . . ? C9 N6 N5 104.0(8) . . ? C9 N6 Rh1 143.7(7) . . ? N5 N6 Rh1 112.2(6) . . ? C12 N3 N4 109.3(10) . . ? C12 N3 B1 131.5(10) . . ? N4 N3 B1 117.7(9) . . ? C14 N4 N3 106.6(9) . . ? C14 N4 Rh1 135.5(8) . . ? N3 N4 Rh1 117.9(7) . . ? C3 C2 N1 107.2(10) . . ? C3 C2 C1 130.2(11) . . ? N1 C2 C1 122.6(10) . . ? C2 C3 C4 107.5(11) . . ? N2 C4 C3 110.1(10) . . ? N2 C4 C5 122.3(9) . . ? C3 C4 C5 127.5(10) . . ? N5 C7 C8 109.3(10) . . ? N5 C7 C6 124.7(10) . . ? C8 C7 C6 125.9(11) . . ? C7 C8 C9 104.2(10) . . ? N6 C9 C8 111.5(9) . . ? N6 C9 C10 125.4(10) . . ? C8 C9 C10 123.0(9) . . ? N3 C12 C13 108.1(10) . . ? N3 C12 C11 122.0(11) . . ? C13 C12 C11 129.9(10) . . ? C12 C13 C14 106.4(10) . . ? N4 C14 C13 109.4(11) . . ? N4 C14 C15 122.6(11) . . ? C13 C14 C15 127.8(11) . . ? C17 C16 C21 117.8(10) . . ? C17 C16 P1 121.0(8) . . ? C21 C16 P1 121.2(8) . . ? C18 C17 C16 121.4(11) . . ? C17 C18 C19 121.9(12) . . ? C20 C19 C18 117.2(11) . . ? C21 C20 C19 122.3(11) . . ? C20 C21 C16 119.4(11) . . ? C23 C22 C27 116.6(11) . . ? C23 C22 P1 121.5(9) . . ? C27 C22 P1 121.9(9) . . ? C24 C23 C22 122.1(12) . . ? C25 C24 C23 120.5(13) . . ? C24 C25 C26 120.6(14) . . ? C25 C26 C27 120.0(14) . . ? C26 C27 C22 120.3(12) . . ? C29 C28 C33 118.1(11) . . ? C29 C28 P1 121.3(10) . . ? C33 C28 P1 120.5(9) . . ? C28 C29 C30 121.8(13) . . ? C31 C30 C29 119.2(14) . . ? C30 C31 C32 121.4(13) . . ? C31 C32 C33 118.3(13) . . ? C28 C33 C32 121.1(12) . . ? C35 C34 C39 115.6(10) . . ? C35 C34 P2 120.9(8) . . ? C39 C34 P2 123.5(8) . . ? C36 C35 C34 123.3(10) . . ? C35 C36 C37 119.2(11) . . ? C38 C37 C36 119.5(11) . . ? C39 C38 C37 120.6(10) . . ? C38 C39 C34 121.6(10) . . ? C45 C40 C41 117.8(10) . . ? C45 C40 P2 121.0(8) . . ? C41 C40 P2 121.1(9) . . ? C42 C41 C40 121.0(11) . . ? C43 C42 C41 120.4(11) . . ? C44 C43 C42 118.5(11) . . ? C43 C44 C45 121.4(11) . . ? C40 C45 C44 120.8(11) . . ? C51 C46 C47 120.0(10) . . ? C51 C46 P2 117.6(8) . . ? C47 C46 P2 122.4(8) . . ? C46 C47 C48 120.0(10) . . ? C49 C48 C47 120.4(11) . . ? C50 C49 C48 118.8(12) . . ? C49 C50 C51 120.1(11) . . ? C46 C51 C50 120.6(11) . . ? C62 C61 Cl1 113.5(10) . . ? C61 C62 Cl2 114.6(9) . . ? C64 C63 Cl3 114.6(18) . . ? C63 C64 Cl4 121.9(18) . . ? C63 C64 Cl4' 94.9(17) . . ? Cl4 C64 Cl4' 27.5(16) . . ? C66 C65 Cl5 117.8(14) . . ? C65 C66 Cl6' 129.5(19) . . ? C65 C66 Cl6 123.3(16) . . ? Cl6' C66 Cl6 58.1(8) . . ? N3 B1 N1 113.7(9) . . ? N3 B1 N5 108.2(9) . . ? N1 B1 N5 110.7(9) . . ? N3 B1 Rh1 70.9(6) . . ? N1 B1 Rh1 73.5(6) . . ? N5 B1 Rh1 71.5(6) . . ? F3 P3 F1 179.1(6) . . ? F3 P3 F5 92.3(6) . . ? F1 P3 F5 88.3(5) . . ? F3 P3 F2 89.5(5) . . ? F1 P3 F2 89.8(5) . . ? F5 P3 F2 88.6(5) . . ? F3 P3 F4 90.4(5) . . ? F1 P3 F4 90.3(5) . . ? F5 P3 F4 91.9(5) . . ? F2 P3 F4 179.5(5) . . ? F3 P3 F6 90.1(5) . . ? F1 P3 F6 89.4(5) . . ? F5 P3 F6 177.7(5) . . ? F2 P3 F6 91.2(5) . . ? F4 P3 F6 88.4(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 Rh1 B1 N1 N2 -11.8(7) . . . . ? N3 B1 N1 N2 -71.6(11) . . . . ? N5 B1 N1 N2 50.5(12) . . . . ? B1 N1 N2 C4 -164.6(9) . . . . ? H1 B1 N1 N2 168.6 . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.877 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.131 data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H55 B N6 O P Rh' _chemical_formula_weight 708.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 12.567(4) _cell_length_b 22.521(8) _cell_length_c 12.931(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.714(19) _cell_angle_gamma 90.00 _cell_volume 3570.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 75 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34555 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8155 _reflns_number_gt 5034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0792P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8155 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.09478(3) 0.618614(18) 0.18384(3) 0.02066(13) Uani 1 1 d . . . P1 P 0.05593(10) 0.66657(6) 0.32747(10) 0.0197(3) Uani 1 1 d . . . O1 O -0.0289(4) 0.7157(2) 0.0568(3) 0.0564(14) Uani 1 1 d . . . N2 N 0.4016(4) 0.6684(2) 0.2506(4) 0.0292(11) Uani 1 1 d . . . N1 N 0.3418(3) 0.64637(19) 0.1555(3) 0.0225(9) Uani 1 1 d . . . N3 N 0.2371(3) 0.56142(18) 0.0514(3) 0.0207(9) Uani 1 1 d . . . N4 N 0.1304(3) 0.57774(18) 0.0488(3) 0.0193(9) Uani 1 1 d . . . N5 N 0.3043(3) 0.55088(18) 0.2479(3) 0.0217(9) Uani 1 1 d . . . N6 N 0.1993(3) 0.54995(18) 0.2637(3) 0.0203(9) Uani 1 1 d . . . B1 B 0.3311(5) 0.5785(3) 0.1460(5) 0.0219(13) Uani 1 1 d . . . H1 H 0.400(5) 0.557(3) 0.126(5) 0.050 Uiso 1 1 d . . . C1 C 0.1347(4) 0.6375(2) 0.4562(4) 0.0243(12) Uani 1 1 d . . . C2 C 0.2564(4) 0.6539(2) 0.4754(4) 0.0296(13) Uani 1 1 d . . . H2A H 0.2839 0.6456 0.4108 0.035 Uiso 1 1 calc R . . H2B H 0.2658 0.6969 0.4913 0.035 Uiso 1 1 calc R . . C3 C 0.3212(5) 0.6181(3) 0.5678(5) 0.0381(14) Uani 1 1 d . . . H3A H 0.3987 0.6302 0.5813 0.046 Uiso 1 1 calc R . . H3B H 0.3172 0.5755 0.5485 0.046 Uiso 1 1 calc R . . C4 C 0.2790(5) 0.6265(3) 0.6688(5) 0.0412(16) Uani 1 1 d . . . H4A H 0.3194 0.5999 0.7248 0.049 Uiso 1 1 calc R . . H4B H 0.2923 0.6679 0.6938 0.049 Uiso 1 1 calc R . . C5 C 0.1583(5) 0.6131(3) 0.6496(4) 0.0360(14) Uani 1 1 d . . . H5A H 0.1322 0.6220 0.7148 0.043 Uiso 1 1 calc R . . H5B H 0.1464 0.5702 0.6341 0.043 Uiso 1 1 calc R . . C6 C 0.0917(5) 0.6493(3) 0.5572(4) 0.0282(12) Uani 1 1 d . . . H6A H 0.0978 0.6921 0.5747 0.034 Uiso 1 1 calc R . . H6B H 0.0138 0.6379 0.5449 0.034 Uiso 1 1 calc R . . C7 C -0.0899(4) 0.6615(2) 0.3372(4) 0.0219(11) Uani 1 1 d . . . C8 C -0.1250(4) 0.5969(2) 0.3473(5) 0.0322(13) Uani 1 1 d . . . H8A H -0.1164 0.5745 0.2838 0.039 Uiso 1 1 calc R . . H8B H -0.0765 0.5787 0.4099 0.039 Uiso 1 1 calc R . . C9 C -0.2432(5) 0.5918(3) 0.3586(7) 0.052(2) Uani 1 1 d . . . H9A H -0.2506 0.6103 0.4261 0.063 Uiso 1 1 calc R . . H9B H -0.2633 0.5494 0.3605 0.063 Uiso 1 1 calc R . . C10 C -0.3206(5) 0.6226(3) 0.2658(6) 0.0512(19) Uani 1 1 d . . . H10A H -0.3201 0.6008 0.1993 0.061 Uiso 1 1 calc R . . H10B H -0.3959 0.6215 0.2775 0.061 Uiso 1 1 calc R . . C11 C -0.2880(4) 0.6853(2) 0.2546(5) 0.0348(14) Uani 1 1 d . . . H11A H -0.2963 0.7081 0.3178 0.042 Uiso 1 1 calc R . . H11B H -0.3370 0.7032 0.1917 0.042 Uiso 1 1 calc R . . C12 C -0.1690(4) 0.6899(3) 0.2424(5) 0.0357(14) Uani 1 1 d . . . H12A H -0.1619 0.6696 0.1763 0.043 Uiso 1 1 calc R . . H12B H -0.1496 0.7322 0.2367 0.043 Uiso 1 1 calc R . . C13 C 0.0758(4) 0.7485(2) 0.3230(4) 0.0240(11) Uani 1 1 d . . . C14 C 0.0650(4) 0.7829(2) 0.4232(4) 0.0287(12) Uani 1 1 d . . . H14A H -0.0045 0.7721 0.4424 0.034 Uiso 1 1 calc R . . H14B H 0.1255 0.7718 0.4830 0.034 Uiso 1 1 calc R . . C15 C 0.0677(5) 0.8499(3) 0.4046(5) 0.0367(14) Uani 1 1 d . . . H15A H 0.0032 0.8616 0.3494 0.044 Uiso 1 1 calc R . . H15B H 0.0641 0.8711 0.4708 0.044 Uiso 1 1 calc R . . C16 C 0.1714(5) 0.8678(3) 0.3695(5) 0.0412(16) Uani 1 1 d . . . H16A H 0.1689 0.9109 0.3536 0.049 Uiso 1 1 calc R . . H16B H 0.2354 0.8604 0.4281 0.049 Uiso 1 1 calc R . . C17 C 0.1842(5) 0.8336(3) 0.2726(5) 0.0389(15) Uani 1 1 d . . . H17A H 0.2544 0.8446 0.2548 0.047 Uiso 1 1 calc R . . H17B H 0.1248 0.8448 0.2118 0.047 Uiso 1 1 calc R . . C18 C 0.1815(4) 0.7664(2) 0.2895(5) 0.0303(13) Uani 1 1 d . . . H18A H 0.2453 0.7543 0.3451 0.036 Uiso 1 1 calc R . . H18B H 0.1857 0.7457 0.2230 0.036 Uiso 1 1 calc R . . C19 C 0.4232(4) 0.7247(2) 0.2321(4) 0.0263(12) Uani 1 1 d . . . C20 C 0.3788(5) 0.7400(2) 0.1274(4) 0.0299(13) Uani 1 1 d . . . H20 H 0.3826 0.7776 0.0950 0.036 Uiso 1 1 calc R . . C21 C 0.3283(4) 0.6897(2) 0.0800(4) 0.0259(12) Uani 1 1 d . . . C22 C 0.4859(5) 0.7626(3) 0.3195(5) 0.0410(16) Uani 1 1 d . . . H22A H 0.4358 0.7897 0.3444 0.061 Uiso 1 1 calc R . . H22B H 0.5406 0.7857 0.2932 0.061 Uiso 1 1 calc R . . H22C H 0.5225 0.7373 0.3783 0.061 Uiso 1 1 calc R . . C23 C 0.2725(5) 0.6808(3) -0.0351(4) 0.0373(15) Uani 1 1 d . . . H23A H 0.2734 0.7181 -0.0738 0.056 Uiso 1 1 calc R . . H23B H 0.1968 0.6684 -0.0398 0.056 Uiso 1 1 calc R . . H23C H 0.3110 0.6501 -0.0661 0.056 Uiso 1 1 calc R . . C24 C 0.0701(4) 0.5606(2) -0.0451(4) 0.0232(11) Uani 1 1 d . . . C25 C 0.1368(5) 0.5342(2) -0.1037(4) 0.0294(13) Uani 1 1 d . . . H25 H 0.1148 0.5185 -0.1733 0.035 Uiso 1 1 calc R . . C26 C 0.2420(4) 0.5350(2) -0.0416(4) 0.0258(12) Uani 1 1 d . . . C27 C -0.0497(4) 0.5714(2) -0.0754(4) 0.0315(13) Uani 1 1 d . . . H27A H -0.0851 0.5387 -0.1200 0.047 Uiso 1 1 calc R . . H27B H -0.0637 0.6088 -0.1148 0.047 Uiso 1 1 calc R . . H27C H -0.0791 0.5739 -0.0113 0.047 Uiso 1 1 calc R . . C28 C 0.3468(5) 0.5134(3) -0.0670(5) 0.0375(15) Uani 1 1 d . . . H28A H 0.3329 0.5007 -0.1413 0.056 Uiso 1 1 calc R . . H28B H 0.3750 0.4798 -0.0209 0.056 Uiso 1 1 calc R . . H28C H 0.4005 0.5456 -0.0555 0.056 Uiso 1 1 calc R . . C29 C 0.3645(4) 0.5095(2) 0.3126(4) 0.0276(12) Uani 1 1 d . . . C30 C 0.2991(4) 0.4818(2) 0.3683(4) 0.0278(12) Uani 1 1 d . . . H30 H 0.3195 0.4514 0.4198 0.033 Uiso 1 1 calc R . . C31 C 0.1959(4) 0.5070(2) 0.3347(4) 0.0220(11) Uani 1 1 d . . . C32 C 0.4831(5) 0.5004(3) 0.3175(5) 0.0440(17) Uani 1 1 d . . . H32A H 0.5068 0.5271 0.2673 0.066 Uiso 1 1 calc R . . H32B H 0.4956 0.4591 0.2991 0.066 Uiso 1 1 calc R . . H32C H 0.5247 0.5088 0.3894 0.066 Uiso 1 1 calc R . . C33 C 0.0924(4) 0.4885(2) 0.3640(5) 0.0304(13) Uani 1 1 d . . . H33A H 0.1013 0.4907 0.4411 0.046 Uiso 1 1 calc R . . H33B H 0.0748 0.4476 0.3403 0.046 Uiso 1 1 calc R . . H33C H 0.0331 0.5149 0.3298 0.046 Uiso 1 1 calc R . . C34 C 0.0174(5) 0.6771(3) 0.1076(4) 0.0315(13) 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 Rh1 0.0173(2) 0.0225(2) 0.0215(2) 0.00266(19) 0.00277(14) 0.00392(18) P1 0.0154(6) 0.0218(7) 0.0218(7) 0.0021(5) 0.0036(5) 0.0025(5) O1 0.075(4) 0.056(3) 0.037(3) 0.018(2) 0.010(2) 0.043(3) N2 0.021(2) 0.034(3) 0.030(3) -0.005(2) 0.000(2) 0.002(2) N1 0.020(2) 0.023(2) 0.024(2) -0.0011(19) 0.0035(18) -0.0030(18) N3 0.017(2) 0.021(2) 0.024(2) 0.0021(18) 0.0024(18) 0.0024(17) N4 0.014(2) 0.021(2) 0.023(2) 0.0066(17) 0.0028(17) 0.0003(16) N5 0.016(2) 0.018(2) 0.030(2) 0.0051(18) 0.0027(18) 0.0022(16) N6 0.013(2) 0.024(2) 0.023(2) 0.0029(18) 0.0024(17) 0.0014(16) B1 0.018(3) 0.023(3) 0.024(3) 0.001(2) 0.004(2) 0.002(2) C1 0.021(3) 0.029(3) 0.022(3) 0.002(2) 0.002(2) 0.005(2) C2 0.019(3) 0.033(3) 0.033(3) 0.001(2) -0.003(2) 0.002(2) C3 0.028(3) 0.034(3) 0.044(3) 0.002(3) -0.010(3) 0.004(3) C4 0.043(4) 0.038(4) 0.033(3) 0.003(3) -0.014(3) 0.000(3) C5 0.049(4) 0.031(3) 0.024(3) 0.004(3) 0.000(3) -0.001(3) C6 0.027(3) 0.032(3) 0.026(3) 0.000(2) 0.007(2) 0.001(2) C7 0.014(2) 0.021(3) 0.029(3) 0.003(2) 0.001(2) 0.002(2) C8 0.019(3) 0.028(3) 0.049(4) 0.008(3) 0.006(3) -0.001(2) C9 0.023(3) 0.035(4) 0.097(6) 0.018(4) 0.009(4) -0.007(3) C10 0.021(3) 0.036(4) 0.088(5) -0.003(4) -0.007(3) -0.003(3) C11 0.019(3) 0.032(3) 0.049(4) 0.001(3) -0.001(3) 0.003(2) C12 0.016(3) 0.041(4) 0.048(4) 0.009(3) 0.003(3) 0.003(2) C13 0.017(3) 0.022(3) 0.036(3) -0.001(2) 0.010(2) 0.000(2) C14 0.022(3) 0.024(3) 0.039(3) -0.002(2) 0.006(2) -0.001(2) C15 0.034(3) 0.027(3) 0.048(4) -0.001(3) 0.008(3) 0.000(3) C16 0.035(4) 0.029(3) 0.056(4) 0.005(3) 0.004(3) -0.004(3) C17 0.029(3) 0.034(3) 0.053(4) 0.011(3) 0.008(3) -0.005(3) C18 0.025(3) 0.029(3) 0.040(3) 0.005(3) 0.014(3) 0.003(2) C19 0.017(3) 0.028(3) 0.035(3) -0.005(2) 0.009(2) 0.000(2) C20 0.030(3) 0.025(3) 0.038(3) 0.000(2) 0.014(3) -0.004(2) C21 0.026(3) 0.021(3) 0.032(3) 0.003(2) 0.011(2) -0.002(2) C22 0.027(3) 0.041(4) 0.056(4) -0.015(3) 0.012(3) -0.006(3) C23 0.041(4) 0.035(3) 0.031(3) 0.010(3) -0.003(3) -0.011(3) C24 0.029(3) 0.018(3) 0.021(3) 0.004(2) 0.001(2) -0.003(2) C25 0.042(3) 0.024(3) 0.021(3) 0.000(2) 0.005(2) -0.004(2) C26 0.030(3) 0.021(3) 0.029(3) -0.001(2) 0.013(2) -0.002(2) C27 0.026(3) 0.031(3) 0.033(3) 0.002(3) -0.003(2) -0.002(2) C28 0.042(4) 0.033(3) 0.040(4) -0.002(3) 0.017(3) 0.004(3) C29 0.025(3) 0.024(3) 0.031(3) 0.006(2) 0.001(2) 0.004(2) C30 0.027(3) 0.022(3) 0.032(3) 0.006(2) 0.002(2) 0.004(2) C31 0.022(3) 0.018(3) 0.024(3) 0.000(2) 0.002(2) 0.000(2) C32 0.022(3) 0.048(4) 0.055(4) 0.026(3) -0.004(3) 0.004(3) C33 0.029(3) 0.021(3) 0.042(3) 0.003(2) 0.009(3) -0.002(2) C34 0.034(3) 0.044(4) 0.020(3) 0.001(2) 0.013(2) 0.012(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 C34 1.797(6) . ? Rh1 N4 2.108(4) . ? Rh1 N6 2.142(4) . ? Rh1 P1 2.2920(14) . ? Rh1 B1 3.243(6) . ? Rh1 N2 3.925(5) . ? P1 C1 1.858(5) . ? P1 C13 1.864(5) . ? P1 C7 1.868(5) . ? O1 C34 1.166(7) . ? N2 C19 1.330(7) . ? N2 N1 1.385(6) . ? N1 C21 1.365(7) . ? N1 B1 1.537(7) . ? N3 C26 1.355(7) . ? N3 N4 1.383(5) . ? N3 B1 1.551(7) . ? N4 C24 1.339(6) . ? N5 C29 1.364(6) . ? N5 N6 1.379(6) . ? N5 B1 1.560(7) . ? N6 C31 1.341(6) . ? C1 C2 1.540(7) . ? C1 C6 1.542(7) . ? C2 C3 1.521(7) . ? C3 C4 1.525(9) . ? C4 C5 1.513(9) . ? C5 C6 1.534(7) . ? C7 C8 1.534(7) . ? C7 C12 1.537(7) . ? C8 C9 1.529(8) . ? C9 C10 1.534(9) . ? C10 C11 1.487(8) . ? C11 C12 1.541(8) . ? C13 C18 1.539(7) . ? C13 C14 1.542(7) . ? C14 C15 1.528(8) . ? C15 C16 1.526(9) . ? C16 C17 1.510(9) . ? C17 C18 1.531(8) . ? C19 C20 1.390(8) . ? C19 C22 1.495(7) . ? C20 C21 1.375(7) . ? C21 C23 1.513(8) . ? C24 C25 1.382(8) . ? C24 C27 1.490(7) . ? C25 C26 1.388(8) . ? C26 C28 1.507(8) . ? C29 C30 1.359(8) . ? C29 C32 1.491(8) . ? C30 C31 1.395(7) . ? C31 C33 1.492(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 Rh1 N4 93.1(2) . . ? C34 Rh1 N6 173.8(2) . . ? N4 Rh1 N6 82.21(15) . . ? C34 Rh1 P1 85.01(17) . . ? N4 Rh1 P1 177.77(11) . . ? N6 Rh1 P1 99.61(12) . . ? C34 Rh1 B1 121.6(2) . . ? N4 Rh1 B1 52.03(15) . . ? N6 Rh1 B1 52.16(15) . . ? P1 Rh1 B1 128.23(11) . . ? C34 Rh1 N2 107.3(2) . . ? N4 Rh1 N2 85.95(13) . . ? N6 Rh1 N2 68.37(13) . . ? P1 Rh1 N2 93.51(8) . . ? B1 Rh1 N2 39.16(12) . . ? C1 P1 C13 109.1(2) . . ? C1 P1 C7 104.8(2) . . ? C13 P1 C7 101.7(2) . . ? C1 P1 Rh1 113.17(18) . . ? C13 P1 Rh1 112.78(18) . . ? C7 P1 Rh1 114.41(17) . . ? C19 N2 N1 105.9(4) . . ? C19 N2 Rh1 117.6(3) . . ? N1 N2 Rh1 52.2(2) . . ? C21 N1 N2 109.7(4) . . ? C21 N1 B1 131.3(4) . . ? N2 N1 B1 116.6(4) . . ? C26 N3 N4 109.1(4) . . ? C26 N3 B1 129.3(4) . . ? N4 N3 B1 121.3(4) . . ? C24 N4 N3 107.4(4) . . ? C24 N4 Rh1 134.1(3) . . ? N3 N4 Rh1 118.5(3) . . ? C29 N5 N6 108.6(4) . . ? C29 N5 B1 126.6(4) . . ? N6 N5 B1 121.5(4) . . ? C31 N6 N5 106.8(4) . . ? C31 N6 Rh1 137.9(3) . . ? N5 N6 Rh1 115.0(3) . . ? N1 B1 N3 110.3(4) . . ? N1 B1 N5 111.1(4) . . ? N3 B1 N5 107.4(4) . . ? N1 B1 Rh1 77.2(3) . . ? N3 B1 Rh1 67.9(3) . . ? N5 B1 Rh1 66.9(3) . . ? C2 C1 C6 110.0(4) . . ? C2 C1 P1 112.0(4) . . ? C6 C1 P1 118.8(4) . . ? C3 C2 C1 109.9(5) . . ? C2 C3 C4 112.3(5) . . ? C5 C4 C3 111.1(5) . . ? C4 C5 C6 112.1(5) . . ? C5 C6 C1 109.6(5) . . ? C8 C7 C12 108.3(4) . . ? C8 C7 P1 111.6(3) . . ? C12 C7 P1 113.1(4) . . ? C9 C8 C7 112.5(5) . . ? C8 C9 C10 110.7(6) . . ? C11 C10 C9 111.4(5) . . ? C10 C11 C12 111.6(5) . . ? C7 C12 C11 111.3(5) . . ? C18 C13 C14 110.2(4) . . ? C18 C13 P1 113.5(4) . . ? C14 C13 P1 115.8(4) . . ? C15 C14 C13 110.8(5) . . ? C16 C15 C14 111.0(5) . . ? C17 C16 C15 111.4(5) . . ? C16 C17 C18 112.1(5) . . ? C17 C18 C13 110.4(5) . . ? N2 C19 C20 111.0(5) . . ? N2 C19 C22 120.2(5) . . ? C20 C19 C22 128.8(5) . . ? C21 C20 C19 106.0(5) . . ? N1 C21 C20 107.4(5) . . ? N1 C21 C23 124.5(5) . . ? C20 C21 C23 128.1(5) . . ? N4 C24 C25 109.3(5) . . ? N4 C24 C27 121.9(5) . . ? C25 C24 C27 128.8(5) . . ? C24 C25 C26 107.0(5) . . ? N3 C26 C25 107.2(5) . . ? N3 C26 C28 123.3(5) . . ? C25 C26 C28 129.5(5) . . ? C30 C29 N5 108.6(5) . . ? C30 C29 C32 129.0(5) . . ? N5 C29 C32 122.4(5) . . ? C29 C30 C31 106.1(5) . . ? N6 C31 C30 109.8(5) . . ? N6 C31 C33 122.5(4) . . ? C30 C31 C33 127.6(5) . . ? O1 C34 Rh1 177.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 103.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.648 _refine_diff_density_min -1.677 _refine_diff_density_rms 0.132 data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 B N9 O P Rh' _chemical_formula_weight 591.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.287(3) _cell_length_b 10.529(3) _cell_length_c 16.589(4) _cell_angle_alpha 72.499(19) _cell_angle_beta 77.36(2) _cell_angle_gamma 69.48(3) _cell_volume 1437.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.611298 _exptl_absorpt_correction_T_max 0.927970 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12462 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5032 _reflns_number_gt 3439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0715P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5032 _refine_ls_number_parameters 373 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.52284(5) 0.89788(4) 0.74081(3) 0.03605(18) Uani 1 1 d . A . P1 P 0.3390(2) 1.04906(15) 0.80932(12) 0.0594(6) Uani 1 1 d D . . O1 O 0.737(7) 0.836(7) 0.863(7) 0.069(18) Uani 0.50(15) 1 d P A 1 O1' O 0.683(10) 0.814(2) 0.898(4) 0.059(11) Uani 0.50(15) 1 d P A 2 N1 N 0.4429(5) 0.6172(4) 0.7660(3) 0.0290(10) Uani 1 1 d . A . N2 N 0.2846(6) 0.6448(5) 0.7812(3) 0.0484(14) Uani 1 1 d . . . N3 N 0.6789(5) 0.6525(4) 0.6609(3) 0.0317(11) Uani 1 1 d . A . N4 N 0.7081(5) 0.7572(4) 0.6818(3) 0.0358(11) Uani 1 1 d . . . N5 N 0.4115(5) 0.7917(5) 0.6241(3) 0.0310(10) Uani 1 1 d . A . N6 N 0.4100(5) 0.9147(4) 0.6381(3) 0.0315(11) Uani 1 1 d . . . N7 N 0.3708(11) 1.1943(7) 0.8080(7) 0.132(4) Uani 1 1 d . B . N8 N 0.3595(14) 0.9959(10) 0.9063(6) 0.035(3) Uani 0.466(13) 1 d PD B 1 N8' N 0.2887(13) 0.9695(9) 0.9205(5) 0.032(3) Uiso 0.534(13) 1 d PD B 2 N9 N 0.1631(6) 1.1172(5) 0.7758(3) 0.0504(14) Uani 1 1 d . B . C1 C 0.6338(9) 0.8604(7) 0.8271(5) 0.073(3) Uani 1 1 d . . . C6 C 0.102(2) 0.621(2) 0.9208(16) 0.061(7) Uani 0.45(4) 1 d P B 1 H6C H 0.0426 0.7187 0.8984 0.091 Uiso 0.45(4) 1 calc PR B 1 H6B H 0.1247 0.6098 0.9781 0.091 Uiso 0.45(4) 1 calc PR B 1 H6A H 0.0421 0.5597 0.9235 0.091 Uiso 0.45(4) 1 calc PR B 1 C6' C 0.074(2) 0.579(2) 0.8853(16) 0.067(7) Uani 0.55(4) 1 d P B 2 H6F H 0.0079 0.6590 0.9082 0.100 Uiso 0.55(4) 1 calc PR B 2 H6E H 0.0693 0.4919 0.9277 0.100 Uiso 0.55(4) 1 calc PR B 2 H6D H 0.0362 0.5827 0.8334 0.100 Uiso 0.55(4) 1 calc PR B 2 C7 C 0.2535(8) 0.5834(7) 0.8626(5) 0.078(3) Uani 1 1 d . B . C8 C 0.3879(8) 0.5136(6) 0.9005(4) 0.068(2) Uani 1 1 d . . . H8A H 0.3962 0.4611 0.9579 0.081 Uiso 1 1 calc R B . C9 C 0.5069(7) 0.5362(5) 0.8379(3) 0.0362(14) Uani 1 1 d . A . C10 C 0.6772(7) 0.4844(6) 0.8439(4) 0.0464(16) Uani 1 1 d . . . H10C H 0.7175 0.5642 0.8285 0.070 Uiso 1 1 calc R B . H10B H 0.7304 0.4238 0.8048 0.070 Uiso 1 1 calc R . . H10A H 0.6953 0.4314 0.9024 0.070 Uiso 1 1 calc R . . C11 C 0.8201(8) 0.4455(7) 0.6004(4) 0.0582(19) Uani 1 1 d . B . H11F H 0.7152 0.4396 0.6061 0.087 Uiso 0.50 1 calc PR . . H11E H 0.8843 0.3596 0.6348 0.087 Uiso 0.50 1 calc PR . . H11D H 0.8654 0.4569 0.5404 0.087 Uiso 0.50 1 calc PR . . H11C H 0.9281 0.3978 0.5815 0.087 Uiso 0.50 1 calc PR . . H11B H 0.7590 0.4778 0.5528 0.087 Uiso 0.50 1 calc PR . . H11A H 0.7778 0.3805 0.6472 0.087 Uiso 0.50 1 calc PR . . C12 C 0.8132(6) 0.5670(6) 0.6302(3) 0.0381(14) Uani 1 1 d . . . C13 C 0.9312(7) 0.6160(7) 0.6307(4) 0.0506(18) Uani 1 1 d . B . H13A H 1.0382 0.5768 0.6128 0.061 Uiso 1 1 calc R . . C14 C 0.8635(7) 0.7350(7) 0.6628(4) 0.0510(18) Uani 1 1 d . B . C15 C 0.9361(8) 0.8335(7) 0.6752(5) 0.082(3) Uani 1 1 d . . . H15C H 0.8555 0.9087 0.6972 0.123 Uiso 1 1 calc R B . H15B H 0.9888 0.8736 0.6205 0.123 Uiso 1 1 calc R . . H15A H 1.0115 0.7825 0.7159 0.123 Uiso 1 1 calc R . . C16 C 0.3156(8) 0.7120(9) 0.5248(4) 0.077(3) Uani 1 1 d . B . H16C H 0.2853 0.6413 0.5729 0.115 Uiso 1 1 calc R . . H16B H 0.4139 0.6676 0.4935 0.115 Uiso 1 1 calc R . . H16A H 0.2351 0.7547 0.4867 0.115 Uiso 1 1 calc R . . C17 C 0.3344(6) 0.8206(8) 0.5569(4) 0.0506(18) Uani 1 1 d . . . C18 C 0.2835(7) 0.9638(9) 0.5279(4) 0.061(2) Uani 1 1 d . B . H18A H 0.2249 1.0152 0.4818 0.073 Uiso 1 1 calc R . . C19 C 0.3332(6) 1.0186(7) 0.5780(4) 0.0471(17) Uani 1 1 d . B . C20 C 0.3129(8) 1.1697(7) 0.5717(4) 0.067(2) Uani 1 1 d . . . H20C H 0.3976 1.1754 0.5955 0.101 Uiso 1 1 calc R B . H20B H 0.2136 1.2101 0.6038 0.101 Uiso 1 1 calc R . . H20A H 0.3143 1.2218 0.5118 0.101 Uiso 1 1 calc R . . C21 C 0.3669(14) 1.3039(9) 0.7288(8) 0.148(5) Uani 1 1 d . . . H21C H 0.2839 1.3104 0.6986 0.222 Uiso 1 1 calc R B . H21B H 0.4665 1.2811 0.6928 0.222 Uiso 1 1 calc R . . H21A H 0.3475 1.3936 0.7420 0.222 Uiso 1 1 calc R . . C22 C 0.477(2) 1.1662(13) 0.8751(12) 0.087(7) Uani 0.62(2) 1 d P B 1 H22C H 0.4616 1.0884 0.9228 0.130 Uiso 0.62(2) 1 calc PR B 1 H22B H 0.4518 1.2502 0.8959 0.130 Uiso 0.62(2) 1 calc PR B 1 H22A H 0.5856 1.1420 0.8492 0.130 Uiso 0.62(2) 1 calc PR B 1 C22' C 0.552(2) 1.1913(19) 0.8009(19) 0.060(9) Uani 0.38(2) 1 d P B 2 H22F H 0.5990 1.1234 0.8505 0.090 Uiso 0.38(2) 1 calc PR B 2 H22E H 0.5543 1.2844 0.7994 0.090 Uiso 0.38(2) 1 calc PR B 2 H22D H 0.6109 1.1644 0.7487 0.090 Uiso 0.38(2) 1 calc PR B 2 C23 C 0.2881(18) 1.0918(14) 0.9613(9) 0.058(5) Uiso 0.466(13) 1 d PD B 1 H23C H 0.3387 1.0562 1.0131 0.087 Uiso 0.466(13) 1 calc PR B 1 H23B H 0.1777 1.1000 0.9765 0.087 Uiso 0.466(13) 1 calc PR B 1 H23A H 0.2998 1.1840 0.9312 0.087 Uiso 0.466(13) 1 calc PR B 1 C23' C 0.1812(14) 1.0476(12) 0.9823(7) 0.050(4) Uiso 0.534(13) 1 d PD B 2 H23F H 0.0766 1.0425 0.9855 0.075 Uiso 0.534(13) 1 calc PR B 2 H23E H 0.1795 1.1457 0.9635 0.075 Uiso 0.534(13) 1 calc PR B 2 H23D H 0.2165 1.0062 1.0386 0.075 Uiso 0.534(13) 1 calc PR B 2 C24 C 0.3565(17) 0.8517(13) 0.9446(8) 0.040(4) Uani 0.466(13) 1 d PD B 1 H24A H 0.4202 0.8095 0.9914 0.060 Uiso 0.466(13) 1 calc PR B 1 H24B H 0.3978 0.7974 0.9014 0.060 Uiso 0.466(13) 1 calc PR B 1 H24C H 0.2496 0.8518 0.9666 0.060 Uiso 0.466(13) 1 calc PR B 1 C24' C 0.2910(17) 0.8223(12) 0.9475(8) 0.045(4) Uiso 0.534(13) 1 d PD B 2 H24D H 0.3329 0.7779 1.0020 0.067 Uiso 0.534(13) 1 calc PR B 2 H24E H 0.3564 0.7732 0.9043 0.067 Uiso 0.534(13) 1 calc PR B 2 H24F H 0.1853 0.8178 0.9540 0.067 Uiso 0.534(13) 1 calc PR B 2 C27 C 0.0439(10) 1.2354(7) 0.8032(5) 0.085(3) Uani 1 1 d . . . H27C H -0.0213 1.2902 0.7578 0.128 Uiso 1 1 calc R B . H27B H 0.0933 1.2947 0.8155 0.128 Uiso 1 1 calc R . . H27A H -0.0203 1.2006 0.8546 0.128 Uiso 1 1 calc R . . C28 C 0.0966(7) 1.0200(6) 0.7628(4) 0.0501(17) Uani 1 1 d . . . H28C H 0.0375 1.0651 0.7140 0.075 Uiso 1 1 calc R B . H28B H 0.0276 0.9925 0.8140 0.075 Uiso 1 1 calc R . . H28A H 0.1799 0.9368 0.7515 0.075 Uiso 1 1 calc R . . B1 B 0.5113(7) 0.6485(6) 0.6723(4) 0.0281(14) Uani 1 1 d . . . H1A H 0.514(6) 0.564(6) 0.643(3) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0353(3) 0.0257(2) 0.0522(3) -0.00264(19) -0.0228(2) -0.01095(18) P1 0.0895(15) 0.0181(7) 0.0756(13) -0.0178(8) -0.0467(12) 0.0047(8) O1 0.049(16) 0.080(18) 0.09(4) -0.05(2) -0.04(2) 0.010(12) O1' 0.07(2) 0.059(7) 0.055(17) -0.009(8) -0.038(16) -0.011(8) N1 0.030(3) 0.024(2) 0.032(3) -0.010(2) 0.005(2) -0.010(2) N2 0.034(3) 0.034(3) 0.060(4) 0.002(2) 0.011(3) -0.011(2) N3 0.022(2) 0.045(3) 0.026(3) -0.002(2) -0.006(2) -0.010(2) N4 0.030(3) 0.036(3) 0.044(3) 0.002(2) -0.018(2) -0.016(2) N5 0.015(2) 0.057(3) 0.023(2) -0.009(2) -0.0004(19) -0.017(2) N6 0.019(2) 0.042(3) 0.027(3) 0.003(2) -0.0048(19) -0.011(2) N7 0.162(8) 0.033(4) 0.236(10) -0.055(5) -0.128(8) 0.007(4) N8 0.023(7) 0.034(6) 0.059(8) -0.034(5) -0.015(6) 0.003(5) N9 0.068(4) 0.027(3) 0.042(3) -0.010(2) -0.010(3) 0.007(2) C1 0.079(6) 0.048(4) 0.113(7) -0.040(4) -0.062(5) 0.001(4) C6 0.057(12) 0.086(14) 0.036(11) -0.009(10) 0.008(9) -0.032(9) C6' 0.062(10) 0.088(12) 0.037(11) 0.005(9) 0.020(8) -0.039(9) C7 0.052(5) 0.044(4) 0.079(6) 0.020(4) 0.036(4) 0.001(4) C8 0.074(5) 0.031(3) 0.047(4) 0.012(3) 0.025(4) 0.009(3) C9 0.047(4) 0.018(3) 0.030(3) -0.008(2) 0.007(3) 0.000(2) C10 0.053(4) 0.041(3) 0.032(3) -0.002(3) -0.010(3) -0.001(3) C11 0.038(4) 0.084(5) 0.046(4) -0.034(4) 0.001(3) 0.001(3) C12 0.021(3) 0.051(4) 0.030(3) -0.003(3) -0.003(3) -0.002(3) C13 0.020(3) 0.062(4) 0.049(4) 0.006(3) -0.007(3) -0.003(3) C14 0.023(3) 0.058(4) 0.062(4) 0.021(3) -0.025(3) -0.019(3) C15 0.047(4) 0.073(5) 0.127(7) 0.019(5) -0.039(5) -0.039(4) C16 0.042(4) 0.152(8) 0.056(5) -0.052(5) -0.018(4) -0.024(5) C17 0.015(3) 0.113(6) 0.026(3) -0.026(4) -0.002(3) -0.015(3) C18 0.020(3) 0.114(6) 0.027(4) 0.003(4) -0.008(3) -0.008(4) C19 0.017(3) 0.070(4) 0.028(3) 0.016(3) 0.001(3) -0.007(3) C20 0.042(4) 0.054(4) 0.059(5) 0.030(4) -0.002(3) 0.001(3) C21 0.166(11) 0.042(5) 0.263(15) -0.040(7) -0.050(10) -0.048(6) C22 0.134(16) 0.058(8) 0.098(14) -0.036(8) -0.008(12) -0.054(9) C22' 0.044(12) 0.048(11) 0.11(2) -0.054(13) 0.017(12) -0.032(8) C24 0.031(8) 0.056(9) 0.027(7) -0.014(6) -0.006(6) -0.002(7) C27 0.104(7) 0.049(4) 0.065(5) -0.023(4) -0.023(5) 0.036(4) C28 0.038(4) 0.051(4) 0.045(4) -0.009(3) 0.006(3) -0.002(3) B1 0.024(3) 0.040(4) 0.026(3) -0.014(3) 0.001(3) -0.014(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 C1 1.813(7) . ? Rh1 N4 2.112(5) . ? Rh1 N6 2.122(4) . ? Rh1 P1 2.252(2) . ? Rh1 B1 3.201(6) . ? Rh1 N2 3.854(5) . ? P1 N8 1.567(9) . ? P1 N7 1.649(7) . ? P1 N9 1.682(6) . ? P1 N8' 1.814(9) . ? O1 C1 1.14(2) . ? O1' C1 1.26(3) . ? N1 C9 1.358(6) . ? N1 N2 1.375(6) . ? N1 B1 1.529(7) . ? N2 C7 1.326(8) . ? N3 C12 1.355(7) . ? N3 N4 1.375(6) . ? N3 B1 1.540(7) . ? N4 C14 1.358(7) . ? N5 C17 1.357(6) . ? N5 N6 1.377(6) . ? N5 B1 1.546(7) . ? N6 C19 1.345(6) . ? N7 C21 1.462(13) . ? N7 C22 1.543(15) . ? N7 C22' 1.653(19) . ? N8 C23 1.453(13) . ? N8 C24 1.467(13) . ? N8' C24' 1.472(12) . ? N8' C23' 1.486(12) . ? N9 C28 1.453(8) . ? N9 C27 1.462(8) . ? C6 C7 1.519(19) . ? C6' C7 1.65(2) . ? C7 C8 1.384(10) . ? C8 C9 1.375(8) . ? C9 C10 1.497(8) . ? C11 C12 1.481(9) . ? C12 C13 1.368(8) . ? C13 C14 1.397(9) . ? C14 C15 1.500(9) . ? C16 C17 1.472(10) . ? C17 C18 1.375(10) . ? C18 C19 1.371(10) . ? C19 C20 1.509(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 N4 90.3(3) . . ? C1 Rh1 N6 172.4(2) . . ? N4 Rh1 N6 83.05(16) . . ? C1 Rh1 P1 85.5(2) . . ? N4 Rh1 P1 175.44(13) . . ? N6 Rh1 P1 101.29(13) . . ? C1 Rh1 B1 120.2(2) . . ? N4 Rh1 B1 51.98(16) . . ? N6 Rh1 B1 52.56(16) . . ? P1 Rh1 B1 131.97(13) . . ? C1 Rh1 N2 112.7(3) . . ? N4 Rh1 N2 88.33(14) . . ? N6 Rh1 N2 63.73(14) . . ? P1 Rh1 N2 94.85(10) . . ? B1 Rh1 N2 39.46(14) . . ? N8 P1 N7 88.8(5) . . ? N8 P1 N9 122.0(5) . . ? N7 P1 N9 99.6(3) . . ? N8 P1 N8' 24.8(4) . . ? N7 P1 N8' 106.0(5) . . ? N9 P1 N8' 100.7(4) . . ? N8 P1 Rh1 107.8(3) . . ? N7 P1 Rh1 118.1(4) . . ? N9 P1 Rh1 117.30(19) . . ? N8' P1 Rh1 112.9(3) . . ? C9 N1 N2 109.8(4) . . ? C9 N1 B1 132.3(4) . . ? N2 N1 B1 115.6(4) . . ? C7 N2 N1 105.9(5) . . ? C7 N2 Rh1 114.6(5) . . ? N1 N2 Rh1 51.3(2) . . ? C12 N3 N4 109.8(4) . . ? C12 N3 B1 130.2(5) . . ? N4 N3 B1 120.0(4) . . ? C14 N4 N3 106.3(5) . . ? C14 N4 Rh1 135.0(4) . . ? N3 N4 Rh1 118.5(3) . . ? C17 N5 N6 109.6(5) . . ? C17 N5 B1 128.6(5) . . ? N6 N5 B1 121.1(4) . . ? C19 N6 N5 106.3(5) . . ? C19 N6 Rh1 136.7(4) . . ? N5 N6 Rh1 117.0(3) . . ? C21 N7 C22 123.0(10) . . ? C21 N7 P1 119.5(6) . . ? C22 N7 P1 110.6(6) . . ? C21 N7 C22' 84.7(12) . . ? C22 N7 C22' 46.9(9) . . ? P1 N7 C22' 118.1(7) . . ? C23 N8 C24 115.4(11) . . ? C23 N8 P1 119.2(8) . . ? C24 N8 P1 114.3(7) . . ? C24' N8' C23' 110.0(9) . . ? C24' N8' P1 120.4(8) . . ? C23' N8' P1 124.2(7) . . ? C28 N9 C27 111.9(6) . . ? C28 N9 P1 116.9(4) . . ? C27 N9 P1 122.5(5) . . ? O1 C1 O1' 35(3) . . ? O1 C1 Rh1 161(6) . . ? O1' C1 Rh1 163(3) . . ? N2 C7 C8 111.2(6) . . ? N2 C7 C6 127.5(10) . . ? C8 C7 C6 117.4(12) . . ? N2 C7 C6' 111.4(10) . . ? C8 C7 C6' 135.5(8) . . ? C6 C7 C6' 35.2(7) . . ? C9 C8 C7 105.6(6) . . ? N1 C9 C8 107.5(5) . . ? N1 C9 C10 124.2(5) . . ? C8 C9 C10 128.3(6) . . ? N3 C12 C13 108.1(6) . . ? N3 C12 C11 123.0(5) . . ? C13 C12 C11 128.9(6) . . ? C12 C13 C14 106.5(5) . . ? N4 C14 C13 109.3(6) . . ? N4 C14 C15 120.7(7) . . ? C13 C14 C15 130.0(6) . . ? N5 C17 C18 107.0(6) . . ? N5 C17 C16 123.4(6) . . ? C18 C17 C16 129.6(6) . . ? C19 C18 C17 107.3(5) . . ? N6 C19 C18 109.8(6) . . ? N6 C19 C20 121.3(6) . . ? C18 C19 C20 128.9(6) . . ? N1 B1 N3 112.2(4) . . ? N1 B1 N5 109.8(4) . . ? N3 B1 N5 108.3(4) . . ? N1 B1 Rh1 75.4(3) . . ? N3 B1 Rh1 69.3(3) . . ? N5 B1 Rh1 68.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 105.0(4) . . . . ? N3 B1 N1 N2 164.9(4) . . . . ? N5 B1 N1 N2 44.4(6) . . . . ? B1 N1 N2 C9 165.1(6) . . . . ? H1A B1 N1 N2 -76(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.038 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.102 data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H43 B N6 O P Rh' _chemical_formula_weight 732.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 10.8099(17) _cell_length_b 12.0504(18) _cell_length_c 13.737(3) _cell_angle_alpha 96.536(12) _cell_angle_beta 93.879(12) _cell_angle_gamma 92.424(12) _cell_volume 1771.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 143 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow-green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.799760 _exptl_absorpt_correction_T_max 0.925177 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15270 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6205 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0331P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6205 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.003 _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 0.243674(17) 0.425143(15) 0.341538(14) 0.01715(7) Uani 1 1 d . . . P1 P 0.26160(6) 0.23925(5) 0.35343(5) 0.01840(14) Uani 1 1 d . . . O1 O 0.51356(17) 0.47607(15) 0.38788(15) 0.0369(5) Uani 1 1 d . . . N1 N 0.19445(18) 0.44194(15) 0.11642(14) 0.0201(4) Uani 1 1 d . . . N2 N 0.15808(19) 0.33493(16) 0.07452(15) 0.0237(5) Uani 1 1 d . . . N3 N 0.14754(18) 0.61112(15) 0.23517(14) 0.0212(5) Uani 1 1 d . . . N4 N 0.22007(17) 0.59289(15) 0.31800(14) 0.0197(4) Uani 1 1 d . . . N5 N 0.00703(18) 0.44013(15) 0.21842(14) 0.0197(4) Uani 1 1 d . . . N6 N 0.05085(18) 0.41306(15) 0.30915(14) 0.0188(4) Uani 1 1 d . . . C1 C 0.4090(2) 0.45235(19) 0.37113(18) 0.0231(6) Uani 1 1 d . . . C6 C 0.3828(3) 0.5774(2) 0.1302(2) 0.0377(7) Uani 1 1 d . . . H28A H 0.3875 0.5947 0.2018 0.056 Uiso 1 1 calc R . . H28B H 0.3377 0.6352 0.0999 0.056 Uiso 1 1 calc R . . H28C H 0.4668 0.5753 0.1077 0.056 Uiso 1 1 calc R . . C7 C 0.3156(2) 0.4657(2) 0.10122(18) 0.0249(6) Uani 1 1 d . . . C8 C 0.3589(2) 0.3717(2) 0.05140(19) 0.0304(6) Uani 1 1 d . . . H25A H 0.4405 0.3619 0.0315 0.036 Uiso 1 1 calc R . . C9 C 0.2585(2) 0.2934(2) 0.03579(18) 0.0265(6) Uani 1 1 d . . . C10 C 0.2521(3) 0.1754(2) -0.0141(2) 0.0381(7) Uani 1 1 d . . . H27A H 0.1683 0.1420 -0.0119 0.057 Uiso 1 1 calc R . . H27B H 0.3121 0.1316 0.0198 0.057 Uiso 1 1 calc R . . H27C H 0.2718 0.1758 -0.0827 0.057 Uiso 1 1 calc R . . C11 C 0.0612(3) 0.7723(2) 0.1558(2) 0.0396(7) Uani 1 1 d . . . H23A H 0.0905 0.7457 0.0916 0.059 Uiso 1 1 calc R . . H23B H 0.0709 0.8540 0.1668 0.059 Uiso 1 1 calc R . . H23C H -0.0265 0.7489 0.1572 0.059 Uiso 1 1 calc R . . C12 C 0.1362(2) 0.72323(19) 0.23511(19) 0.0253(6) Uani 1 1 d . . . C13 C 0.2027(2) 0.7765(2) 0.3172(2) 0.0299(6) Uani 1 1 d . . . H20A H 0.2118 0.8549 0.3361 0.036 Uiso 1 1 calc R . . C14 C 0.2544(2) 0.69290(19) 0.36743(18) 0.0220(5) Uani 1 1 d . . . C15 C 0.3362(2) 0.7047(2) 0.46051(19) 0.0301(6) Uani 1 1 d . . . H22A H 0.3240 0.6382 0.4944 0.045 Uiso 1 1 calc R . . H22B H 0.3151 0.7711 0.5030 0.045 Uiso 1 1 calc R . . H22C H 0.4232 0.7125 0.4452 0.045 Uiso 1 1 calc R . . C16 C -0.1922(2) 0.4356(2) 0.11492(19) 0.0330(7) Uani 1 1 d . . . H32A H -0.1565 0.3940 0.0589 0.049 Uiso 1 1 calc R . . H32B H -0.1907 0.5153 0.1065 0.049 Uiso 1 1 calc R . . H32C H -0.2781 0.4079 0.1186 0.049 Uiso 1 1 calc R . . C17 C -0.1178(2) 0.41960(19) 0.20746(18) 0.0233(6) Uani 1 1 d . . . C18 C -0.1542(2) 0.3815(2) 0.29312(19) 0.0263(6) Uani 1 1 d . . . H30A H -0.2365 0.3611 0.3070 0.032 Uiso 1 1 calc R . . C19 C -0.0474(2) 0.37891(19) 0.35482(18) 0.0210(5) Uani 1 1 d . . . C20 C -0.0332(2) 0.3484(2) 0.45748(18) 0.0293(6) Uani 1 1 d . . . H33A H 0.0552 0.3484 0.4787 0.044 Uiso 1 1 calc R . . H33B H -0.0720 0.2738 0.4594 0.044 Uiso 1 1 calc R . . H33C H -0.0736 0.4030 0.5016 0.044 Uiso 1 1 calc R . . C21 C 0.3716(2) 0.16549(19) 0.27468(18) 0.0225(6) Uani 1 1 d . . . C22 C 0.4892(3) 0.2127(2) 0.2690(3) 0.0630(11) Uani 1 1 d . . . H18A H 0.5120 0.2841 0.3038 0.076 Uiso 1 1 calc R . . C23 C 0.5740(3) 0.1570(3) 0.2131(3) 0.0751(14) Uani 1 1 d . . . H17A H 0.6550 0.1898 0.2106 0.090 Uiso 1 1 calc R . . C24 C 0.5415(3) 0.0533(2) 0.1604(2) 0.0381(7) Uani 1 1 d . . . H16A H 0.5996 0.0168 0.1205 0.046 Uiso 1 1 calc R . . C25 C 0.4261(2) 0.00338(19) 0.16567(17) 0.0228(6) Uani 1 1 d . . . C26 C 0.3424(2) 0.06094(19) 0.22335(18) 0.0222(5) Uani 1 1 d . . . H14A H 0.2623 0.0270 0.2275 0.027 Uiso 1 1 calc R . . C27 C 0.3911(3) -0.1106(2) 0.1120(2) 0.0427(8) Uani 1 1 d . . . H37A H 0.4520 -0.1303 0.0640 0.064 Uiso 1 1 calc R . . H37B H 0.3086 -0.1099 0.0779 0.064 Uiso 1 1 calc R . . H37C H 0.3900 -0.1658 0.1591 0.064 Uiso 1 1 calc R . . C28 C 0.3101(2) 0.20315(19) 0.47573(18) 0.0216(5) Uani 1 1 d . . . C29 C 0.3548(2) 0.0980(2) 0.4905(2) 0.0276(6) Uani 1 1 d . . . H12A H 0.3665 0.0447 0.4358 0.033 Uiso 1 1 calc R . . C30 C 0.3817(2) 0.0725(2) 0.5855(2) 0.0315(6) Uani 1 1 d . . . H11A H 0.4118 0.0015 0.5958 0.038 Uiso 1 1 calc R . . C31 C 0.3648(2) 0.1500(2) 0.6652(2) 0.0310(6) Uani 1 1 d . . . H10A H 0.3840 0.1314 0.7297 0.037 Uiso 1 1 calc R . . C32 C 0.3203(2) 0.2545(2) 0.65325(19) 0.0265(6) Uani 1 1 d . . . C33 C 0.2950(2) 0.28013(19) 0.55707(18) 0.0229(6) Uani 1 1 d . . . H8A H 0.2669 0.3519 0.5472 0.027 Uiso 1 1 calc R . . C34 C 0.2977(3) 0.3377(2) 0.7394(2) 0.0399(7) Uani 1 1 d . . . H36A H 0.3278 0.3095 0.8004 0.060 Uiso 1 1 calc R . . H36B H 0.2085 0.3490 0.7406 0.060 Uiso 1 1 calc R . . H36C H 0.3420 0.4090 0.7335 0.060 Uiso 1 1 calc R . . C35 C 0.1182(2) 0.15319(18) 0.31931(17) 0.0189(5) Uani 1 1 d . . . C36 C 0.0657(2) 0.0802(2) 0.37848(19) 0.0283(6) Uani 1 1 d . . . H6A H 0.1045 0.0724 0.4413 0.034 Uiso 1 1 calc R . . C37 C -0.0435(2) 0.0190(2) 0.3452(2) 0.0346(7) Uani 1 1 d . . . H5A H -0.0791 -0.0311 0.3855 0.042 Uiso 1 1 calc R . . C38 C -0.1012(2) 0.0300(2) 0.2543(2) 0.0299(6) Uani 1 1 d . . . H4B H -0.1764 -0.0119 0.2330 0.036 Uiso 1 1 calc R . . C39 C -0.0502(2) 0.10187(19) 0.19346(18) 0.0238(6) Uani 1 1 d . . . C40 C 0.0588(2) 0.16334(19) 0.22722(18) 0.0212(5) Uani 1 1 d . . . H2A H 0.0939 0.2135 0.1869 0.025 Uiso 1 1 calc R . . C41 C -0.1105(2) 0.1165(2) 0.0934(2) 0.0330(6) Uani 1 1 d . . . H35A H -0.1595 0.0481 0.0669 0.050 Uiso 0.50 1 calc PR . . H35B H -0.0461 0.1314 0.0490 0.050 Uiso 0.50 1 calc PR . . H35C H -0.1650 0.1795 0.0994 0.050 Uiso 0.50 1 calc PR . . H35D H -0.0876 0.1912 0.0766 0.050 Uiso 0.50 1 calc PR . . H35E H -0.2010 0.1080 0.0945 0.050 Uiso 0.50 1 calc PR . . H35F H -0.0821 0.0598 0.0441 0.050 Uiso 0.50 1 calc PR . . B1 B 0.0906(3) 0.5128(2) 0.1605(2) 0.0216(6) Uani 1 1 d . . . H1A H 0.030(2) 0.548(2) 0.102(2) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01763(11) 0.01691(10) 0.01714(11) 0.00284(7) 0.00108(7) 0.00173(7) P1 0.0176(3) 0.0178(3) 0.0201(4) 0.0029(3) 0.0020(3) 0.0013(3) O1 0.0213(11) 0.0334(11) 0.0534(13) -0.0006(9) -0.0054(9) -0.0006(8) N1 0.0251(12) 0.0190(10) 0.0166(11) 0.0038(8) 0.0026(9) 0.0002(9) N2 0.0300(12) 0.0204(11) 0.0211(12) 0.0017(9) 0.0048(9) 0.0021(9) N3 0.0268(12) 0.0180(10) 0.0192(11) 0.0034(8) 0.0016(9) 0.0036(9) N4 0.0205(11) 0.0203(11) 0.0183(11) 0.0023(8) 0.0008(9) 0.0034(9) N5 0.0200(11) 0.0210(11) 0.0178(11) 0.0008(8) 0.0004(9) 0.0044(9) N6 0.0201(11) 0.0196(10) 0.0165(11) 0.0014(8) 0.0000(9) 0.0039(9) C1 0.0267(15) 0.0184(13) 0.0246(15) 0.0046(10) 0.0011(11) 0.0026(11) C6 0.0362(17) 0.0459(18) 0.0298(17) 0.0013(13) 0.0078(13) -0.0107(14) C7 0.0262(14) 0.0322(15) 0.0175(14) 0.0075(11) 0.0049(11) -0.0011(12) C8 0.0258(15) 0.0425(17) 0.0254(15) 0.0078(12) 0.0105(12) 0.0078(13) C9 0.0366(16) 0.0271(14) 0.0180(14) 0.0060(11) 0.0070(12) 0.0097(12) C10 0.053(2) 0.0314(15) 0.0316(17) 0.0028(13) 0.0111(14) 0.0125(14) C11 0.054(2) 0.0281(15) 0.0383(18) 0.0109(13) -0.0057(15) 0.0110(14) C12 0.0318(15) 0.0167(13) 0.0282(15) 0.0037(11) 0.0026(12) 0.0050(11) C13 0.0392(17) 0.0153(13) 0.0350(17) 0.0013(11) 0.0031(13) 0.0024(12) C14 0.0246(14) 0.0201(13) 0.0206(14) -0.0015(10) 0.0036(11) -0.0001(11) C15 0.0290(15) 0.0273(14) 0.0321(16) -0.0028(12) -0.0002(12) -0.0015(12) C16 0.0239(15) 0.0444(17) 0.0291(16) 0.0009(13) -0.0045(12) 0.0035(13) C17 0.0195(14) 0.0228(13) 0.0262(15) -0.0026(11) -0.0009(11) 0.0031(11) C18 0.0153(13) 0.0296(14) 0.0335(16) 0.0000(12) 0.0051(11) 0.0010(11) C19 0.0212(13) 0.0189(12) 0.0233(14) -0.0003(10) 0.0064(11) 0.0036(10) C20 0.0258(15) 0.0361(15) 0.0281(15) 0.0082(12) 0.0082(12) 0.0040(12) C21 0.0211(13) 0.0190(13) 0.0280(15) 0.0026(10) 0.0041(11) 0.0040(10) C22 0.0377(19) 0.0272(16) 0.118(3) -0.0303(18) 0.039(2) -0.0136(14) C23 0.041(2) 0.0355(18) 0.145(4) -0.027(2) 0.053(2) -0.0138(16) C24 0.0342(17) 0.0255(15) 0.057(2) 0.0001(13) 0.0231(14) 0.0063(13) C25 0.0264(14) 0.0238(13) 0.0189(14) 0.0034(10) 0.0012(11) 0.0074(11) C26 0.0190(13) 0.0234(13) 0.0240(14) 0.0045(11) -0.0005(11) -0.0015(11) C27 0.0354(17) 0.0403(17) 0.048(2) -0.0171(14) 0.0062(14) 0.0047(14) C28 0.0162(13) 0.0228(13) 0.0266(15) 0.0069(11) 0.0014(10) 0.0013(10) C29 0.0247(14) 0.0244(14) 0.0342(16) 0.0050(12) 0.0025(12) 0.0032(11) C30 0.0302(16) 0.0294(15) 0.0380(17) 0.0158(13) -0.0002(13) 0.0086(12) C31 0.0273(15) 0.0400(16) 0.0284(16) 0.0162(13) -0.0008(12) 0.0036(13) C32 0.0210(14) 0.0354(15) 0.0237(15) 0.0076(12) -0.0003(11) -0.0014(12) C33 0.0209(13) 0.0207(13) 0.0279(15) 0.0067(11) 0.0006(11) 0.0024(11) C34 0.0497(19) 0.0452(18) 0.0249(16) 0.0040(13) 0.0022(14) 0.0053(15) C35 0.0166(13) 0.0177(12) 0.0225(14) 0.0013(10) 0.0043(10) 0.0020(10) C36 0.0285(15) 0.0337(15) 0.0238(15) 0.0094(12) 0.0022(12) -0.0021(12) C37 0.0328(16) 0.0379(16) 0.0349(17) 0.0163(13) 0.0035(13) -0.0136(13) C38 0.0220(14) 0.0313(15) 0.0349(17) 0.0015(12) 0.0018(12) -0.0098(12) C39 0.0226(14) 0.0232(13) 0.0252(15) -0.0001(11) 0.0029(11) 0.0032(11) C40 0.0230(14) 0.0170(12) 0.0247(14) 0.0048(10) 0.0061(11) 0.0018(10) C41 0.0294(16) 0.0348(15) 0.0330(17) 0.0025(12) -0.0058(12) -0.0037(12) B1 0.0259(16) 0.0217(15) 0.0171(15) 0.0024(12) 0.0003(12) 0.0021(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.813(3) . ? Rh1 N6 2.0972(19) . ? Rh1 N4 2.1064(19) . ? Rh1 P1 2.2799(7) . ? Rh1 B1 3.198(3) . ? Rh1 N2 3.747(2) . ? P1 C28 1.831(2) . ? P1 C35 1.831(2) . ? P1 C21 1.849(2) . ? O1 C1 1.156(3) . ? N1 C7 1.364(3) . ? N1 N2 1.381(3) . ? N1 B1 1.553(3) . ? N2 C9 1.333(3) . ? N3 C12 1.362(3) . ? N3 N4 1.381(3) . ? N3 B1 1.552(3) . ? N4 C14 1.339(3) . ? N5 C17 1.356(3) . ? N5 N6 1.382(3) . ? N5 B1 1.551(3) . ? N6 C19 1.342(3) . ? C6 C7 1.501(4) . ? C7 C8 1.371(3) . ? C8 C9 1.396(4) . ? C9 C10 1.503(3) . ? C11 C12 1.503(3) . ? C12 C13 1.373(4) . ? C13 C14 1.399(3) . ? C14 C15 1.494(3) . ? C16 C17 1.493(3) . ? C17 C18 1.386(3) . ? C18 C19 1.390(3) . ? C19 C20 1.497(3) . ? C21 C22 1.381(4) . ? C21 C26 1.385(3) . ? C22 C23 1.383(4) . ? C23 C24 1.389(4) . ? C24 C25 1.372(4) . ? C25 C26 1.397(3) . ? C25 C27 1.504(3) . ? C28 C33 1.392(3) . ? C28 C29 1.406(3) . ? C29 C30 1.389(4) . ? C30 C31 1.384(4) . ? C31 C32 1.390(3) . ? C32 C33 1.402(3) . ? C32 C34 1.502(4) . ? C35 C36 1.392(3) . ? C35 C40 1.400(3) . ? C36 C37 1.387(4) . ? C37 C38 1.380(4) . ? C38 C39 1.392(4) . ? C39 C40 1.388(3) . ? C39 C41 1.513(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 N6 173.61(9) . . ? C1 Rh1 N4 91.64(9) . . ? N6 Rh1 N4 82.17(7) . . ? C1 Rh1 P1 91.15(7) . . ? N6 Rh1 P1 95.14(5) . . ? N4 Rh1 P1 174.99(6) . . ? C1 Rh1 B1 124.54(9) . . ? N6 Rh1 B1 52.36(7) . . ? N4 Rh1 B1 53.08(7) . . ? P1 Rh1 B1 121.98(5) . . ? C1 Rh1 N2 113.88(8) . . ? N6 Rh1 N2 67.90(6) . . ? N4 Rh1 N2 89.91(6) . . ? P1 Rh1 N2 85.16(4) . . ? B1 Rh1 N2 41.05(6) . . ? C28 P1 C35 103.56(11) . . ? C28 P1 C21 102.74(11) . . ? C35 P1 C21 101.43(11) . . ? C28 P1 Rh1 115.73(8) . . ? C35 P1 Rh1 114.49(7) . . ? C21 P1 Rh1 116.88(8) . . ? C7 N1 N2 110.34(18) . . ? C7 N1 B1 133.4(2) . . ? N2 N1 B1 115.95(19) . . ? C9 N2 N1 105.5(2) . . ? C9 N2 Rh1 107.27(15) . . ? N1 N2 Rh1 53.67(10) . . ? C12 N3 N4 108.76(19) . . ? C12 N3 B1 129.6(2) . . ? N4 N3 B1 121.67(18) . . ? C14 N4 N3 107.57(18) . . ? C14 N4 Rh1 135.49(16) . . ? N3 N4 Rh1 116.85(14) . . ? C17 N5 N6 109.05(19) . . ? C17 N5 B1 129.1(2) . . ? N6 N5 B1 119.60(19) . . ? C19 N6 N5 107.51(19) . . ? C19 N6 Rh1 135.18(16) . . ? N5 N6 Rh1 117.23(14) . . ? O1 C1 Rh1 175.7(2) . . ? N1 C7 C8 107.1(2) . . ? N1 C7 C6 124.6(2) . . ? C8 C7 C6 128.2(2) . . ? C7 C8 C9 106.1(2) . . ? N2 C9 C8 110.9(2) . . ? N2 C9 C10 119.5(2) . . ? C8 C9 C10 129.6(2) . . ? N3 C12 C13 108.0(2) . . ? N3 C12 C11 122.7(2) . . ? C13 C12 C11 129.3(2) . . ? C12 C13 C14 106.7(2) . . ? N4 C14 C13 109.0(2) . . ? N4 C14 C15 122.0(2) . . ? C13 C14 C15 128.9(2) . . ? N5 C17 C18 107.5(2) . . ? N5 C17 C16 122.1(2) . . ? C18 C17 C16 130.4(2) . . ? C17 C18 C19 106.8(2) . . ? N6 C19 C18 109.1(2) . . ? N6 C19 C20 121.4(2) . . ? C18 C19 C20 129.5(2) . . ? C22 C21 C26 117.8(2) . . ? C22 C21 P1 119.85(19) . . ? C26 C21 P1 122.26(19) . . ? C21 C22 C23 120.6(3) . . ? C22 C23 C24 120.4(3) . . ? C25 C24 C23 120.4(2) . . ? C24 C25 C26 118.1(2) . . ? C24 C25 C27 121.0(2) . . ? C26 C25 C27 120.9(2) . . ? C21 C26 C25 122.6(2) . . ? C33 C28 C29 119.1(2) . . ? C33 C28 P1 118.64(17) . . ? C29 C28 P1 122.18(19) . . ? C30 C29 C28 119.6(2) . . ? C31 C30 C29 120.3(2) . . ? C30 C31 C32 121.6(2) . . ? C31 C32 C33 117.7(2) . . ? C31 C32 C34 121.9(2) . . ? C33 C32 C34 120.3(2) . . ? C28 C33 C32 121.7(2) . . ? C36 C35 C40 118.9(2) . . ? C36 C35 P1 124.50(19) . . ? C40 C35 P1 116.56(17) . . ? C37 C36 C35 119.6(2) . . ? C38 C37 C36 120.8(2) . . ? C37 C38 C39 120.7(2) . . ? C40 C39 C38 118.3(2) . . ? C40 C39 C41 119.3(2) . . ? C38 C39 C41 122.4(2) . . ? C39 C40 C35 121.6(2) . . ? N5 B1 N3 106.53(19) . . ? N5 B1 N1 109.90(19) . . ? N3 B1 N1 110.6(2) . . ? N5 B1 Rh1 68.27(12) . . ? N3 B1 Rh1 68.36(12) . . ? N1 B1 Rh1 73.50(12) . . ? 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 Rh1 B1 N1 N2 101.66(16) . . . . ? N3 B1 N1 N2 160.18(18) . . . . ? N5 B1 N1 N2 42.8(3) . . . . ? B1 N1 N2 C9 175.6(2) . . . . ? H1A B1 N1 N2 -78.4(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.319 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.059 data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H37 B N6 O4 P Rh' _chemical_formula_weight 738.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 10.4975(17) _cell_length_b 12.1867(17) _cell_length_c 13.7717(15) _cell_angle_alpha 87.865(8) _cell_angle_beta 87.751(9) _cell_angle_gamma 78.014(12) _cell_volume 1721.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 126 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.922509 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17504 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7766 _reflns_number_gt 6293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0333P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7766 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.225 _refine_ls_shift/su_mean 0.007 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 0.293989(16) 0.304157(14) 0.166978(11) 0.02321(5) Uani 1 1 d . . . B1 B 0.2532(2) 0.0457(2) 0.15160(17) 0.0263(5) Uani 1 1 d . . . H1 H 0.2269(18) -0.0323(16) 0.1376(13) 0.017(5) Uiso 1 1 d . . . N2 N 0.43069(17) 0.10343(14) 0.24402(12) 0.0274(4) Uani 1 1 d . . . N1 N 0.35486(16) 0.02645(14) 0.23151(11) 0.0244(4) Uani 1 1 d . . . N3 N 0.30783(16) 0.09224(14) 0.05587(11) 0.0242(4) Uani 1 1 d . . . N4 N 0.32451(16) 0.20101(14) 0.04508(11) 0.0240(4) Uani 1 1 d . . . N5 N 0.12629(16) 0.13013(14) 0.18231(11) 0.0241(4) Uani 1 1 d . . . N6 N 0.11991(16) 0.24510(14) 0.17938(11) 0.0243(4) Uani 1 1 d . . . P1 P 0.25548(5) 0.41014(4) 0.29321(4) 0.02228(12) Uani 1 1 d . . . O1 O 0.53989(18) 0.38627(17) 0.13503(13) 0.0556(5) Uani 1 1 d . . . O2 O 0.37079(13) 0.38418(12) 0.36868(9) 0.0258(3) Uani 1 1 d . . . O3 O 0.24047(14) 0.54421(12) 0.28142(10) 0.0283(3) Uani 1 1 d . . . O4 O 0.12772(13) 0.40953(12) 0.36227(10) 0.0268(3) Uani 1 1 d . . . C1 C 0.3568(2) 0.41908(19) 0.46604(14) 0.0270(5) Uani 1 1 d . . . C2 C 0.3648(3) 0.3362(2) 0.53745(16) 0.0431(6) Uani 1 1 d . . . H2A H 0.3734 0.2600 0.5207 0.052 Uiso 1 1 calc R . . C3 C 0.3603(3) 0.3651(3) 0.63426(18) 0.0557(8) Uani 1 1 d . . . H3A H 0.3670 0.3084 0.6841 0.067 Uiso 1 1 calc R . . C4 C 0.3462(2) 0.4757(3) 0.65811(18) 0.0489(7) Uani 1 1 d . . . H4A H 0.3417 0.4956 0.7244 0.059 Uiso 1 1 calc R . . C5 C 0.3385(2) 0.5577(2) 0.58553(18) 0.0444(6) Uani 1 1 d . . . H5A H 0.3292 0.6339 0.6022 0.053 Uiso 1 1 calc R . . C6 C 0.3442(2) 0.5298(2) 0.48771(16) 0.0331(5) Uani 1 1 d . . . H6A H 0.3396 0.5860 0.4376 0.040 Uiso 1 1 calc R . . C7 C 0.1625(2) 0.60802(17) 0.21037(15) 0.0297(5) Uani 1 1 d . . . C8 C 0.2170(3) 0.6239(2) 0.11956(16) 0.0389(6) Uani 1 1 d . . . H8A H 0.3058 0.5918 0.1046 0.047 Uiso 1 1 calc R . . C9 C 0.1388(4) 0.6881(2) 0.05040(19) 0.0574(8) Uani 1 1 d . . . H9A H 0.1745 0.6993 -0.0128 0.069 Uiso 1 1 calc R . . C10 C 0.0120(4) 0.7352(2) 0.0716(2) 0.0643(10) Uani 1 1 d . . . H10A H -0.0405 0.7779 0.0233 0.077 Uiso 1 1 calc R . . C11 C -0.0402(3) 0.7206(2) 0.1636(3) 0.0584(8) Uani 1 1 d . . . H11A H -0.1284 0.7544 0.1786 0.070 Uiso 1 1 calc R . . C12 C 0.0355(2) 0.65680(19) 0.23443(19) 0.0407(6) Uani 1 1 d . . . H12A H 0.0003 0.6472 0.2980 0.049 Uiso 1 1 calc R . . C13 C 0.0973(2) 0.31577(18) 0.41232(14) 0.0262(5) Uani 1 1 d . . . C14 C 0.1730(2) 0.20891(19) 0.40758(15) 0.0310(5) Uani 1 1 d . . . H14A H 0.2502 0.1945 0.3677 0.037 Uiso 1 1 calc R . . C15 C 0.1345(2) 0.1234(2) 0.46185(17) 0.0398(6) Uani 1 1 d . . . H15A H 0.1860 0.0496 0.4593 0.048 Uiso 1 1 calc R . . C16 C 0.0220(3) 0.1436(2) 0.52006(18) 0.0488(7) Uani 1 1 d . . . H16A H -0.0037 0.0842 0.5572 0.059 Uiso 1 1 calc R . . C17 C -0.0524(3) 0.2509(2) 0.52348(19) 0.0510(7) Uani 1 1 d . . . H17A H -0.1298 0.2652 0.5632 0.061 Uiso 1 1 calc R . . C18 C -0.0156(2) 0.3383(2) 0.46965(17) 0.0375(6) Uani 1 1 d . . . H18A H -0.0670 0.4122 0.4721 0.045 Uiso 1 1 calc R . . C19 C 0.5057(2) 0.06558(18) 0.31929(14) 0.0286(5) Uani 1 1 d . . . C20 C 0.4787(2) -0.0361(2) 0.35514(16) 0.0360(5) Uani 1 1 d . . . H20A H 0.5182 -0.0805 0.4083 0.043 Uiso 1 1 calc R . . C21 C 0.3836(2) -0.05921(19) 0.29821(16) 0.0325(5) Uani 1 1 d . . . C22 C 0.6025(2) 0.1291(2) 0.35192(18) 0.0419(6) Uani 1 1 d . . . H22A H 0.5973 0.1978 0.3116 0.063 Uiso 0.50 1 calc PR . . H22B H 0.6903 0.0825 0.3455 0.063 Uiso 0.50 1 calc PR . . H22C H 0.5833 0.1488 0.4201 0.063 Uiso 0.50 1 calc PR . . H22D H 0.6500 0.0883 0.4065 0.063 Uiso 0.50 1 calc PR . . H22E H 0.5570 0.2036 0.3726 0.063 Uiso 0.50 1 calc PR . . H22F H 0.6640 0.1373 0.2981 0.063 Uiso 0.50 1 calc PR . . C23 C 0.3178(3) -0.1573(2) 0.3032(2) 0.0553(8) Uani 1 1 d . . . H23A H 0.2249 -0.1314 0.3194 0.083 Uiso 1 1 calc R . . H23B H 0.3576 -0.2115 0.3533 0.083 Uiso 1 1 calc R . . H23C H 0.3279 -0.1933 0.2401 0.083 Uiso 1 1 calc R . . C24 C 0.3623(2) 0.21658(19) -0.04758(14) 0.0278(5) Uani 1 1 d . . . C25 C 0.3711(2) 0.11699(19) -0.09692(14) 0.0297(5) Uani 1 1 d . . . H25A H 0.3966 0.1045 -0.1632 0.036 Uiso 1 1 calc R . . C26 C 0.33563(19) 0.04045(18) -0.03036(14) 0.0262(5) Uani 1 1 d . . . C27 C 0.3867(3) 0.3267(2) -0.08479(16) 0.0445(6) Uani 1 1 d . . . H27A H 0.3273 0.3873 -0.0511 0.067 Uiso 1 1 calc R . . H27B H 0.3718 0.3345 -0.1547 0.067 Uiso 1 1 calc R . . H27C H 0.4770 0.3310 -0.0731 0.067 Uiso 1 1 calc R . . C28 C 0.3282(2) -0.07913(19) -0.04394(16) 0.0357(5) Uani 1 1 d . . . H28A H 0.2997 -0.1112 0.0174 0.054 Uiso 0.50 1 calc PR . . H28B H 0.4144 -0.1219 -0.0639 0.054 Uiso 0.50 1 calc PR . . H28C H 0.2658 -0.0827 -0.0942 0.054 Uiso 0.50 1 calc PR . . H28D H 0.3535 -0.0993 -0.1112 0.054 Uiso 0.50 1 calc PR . . H28E H 0.2388 -0.0887 -0.0299 0.054 Uiso 0.50 1 calc PR . . H28F H 0.3874 -0.1278 0.0004 0.054 Uiso 0.50 1 calc PR . . C29 C 0.0042(2) 0.11115(19) 0.19605(15) 0.0286(5) Uani 1 1 d . . . C34 C 0.4442(2) 0.35625(19) 0.14699(15) 0.0317(5) Uani 1 1 d . . . C30 C -0.0808(2) 0.21310(19) 0.20138(15) 0.0315(5) Uani 1 1 d . . . H30A H -0.1726 0.2253 0.2113 0.038 Uiso 1 1 calc R . . C31 C -0.0064(2) 0.29489(18) 0.18943(14) 0.0268(5) Uani 1 1 d . . . C32 C -0.0253(2) -0.0038(2) 0.2005(2) 0.0446(6) Uani 1 1 d . . . H32A H 0.0286 -0.0502 0.2493 0.067 Uiso 1 1 calc R . . H32B H -0.0061 -0.0377 0.1368 0.067 Uiso 1 1 calc R . . H32C H -0.1176 0.0013 0.2183 0.067 Uiso 1 1 calc R . . C33 C -0.0517(2) 0.41916(19) 0.18112(17) 0.0364(5) Uani 1 1 d . . . H33A H 0.0170 0.4524 0.1492 0.055 Uiso 1 1 calc R . . H33B H -0.0715 0.4495 0.2462 0.055 Uiso 1 1 calc R . . H33C H -0.1302 0.4372 0.1426 0.055 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 0.02622(9) 0.02370(9) 0.02044(8) -0.00396(6) 0.00283(6) -0.00689(6) B1 0.0291(13) 0.0238(12) 0.0256(12) -0.0032(10) 0.0034(10) -0.0051(10) N2 0.0318(10) 0.0233(9) 0.0259(9) -0.0016(7) 0.0008(7) -0.0031(8) N1 0.0280(9) 0.0207(9) 0.0231(8) 0.0005(7) 0.0040(7) -0.0029(7) N3 0.0290(9) 0.0228(9) 0.0201(8) -0.0041(7) 0.0017(7) -0.0037(7) N4 0.0276(9) 0.0238(9) 0.0207(8) -0.0013(7) 0.0023(7) -0.0058(7) N5 0.0260(9) 0.0226(9) 0.0240(9) -0.0014(7) 0.0010(7) -0.0058(7) N6 0.0281(9) 0.0215(9) 0.0236(8) -0.0036(7) 0.0018(7) -0.0056(7) P1 0.0252(3) 0.0209(3) 0.0203(3) -0.0013(2) -0.0003(2) -0.0035(2) O1 0.0456(11) 0.0724(14) 0.0577(12) -0.0173(10) 0.0142(9) -0.0330(10) O2 0.0268(8) 0.0283(8) 0.0207(7) -0.0044(6) -0.0006(6) -0.0012(6) O3 0.0385(9) 0.0219(8) 0.0252(7) 0.0004(6) -0.0079(6) -0.0068(7) O4 0.0264(8) 0.0251(8) 0.0271(7) -0.0023(6) 0.0037(6) -0.0018(6) C1 0.0233(11) 0.0360(12) 0.0215(10) -0.0049(9) -0.0014(8) -0.0047(9) C2 0.0578(17) 0.0442(15) 0.0286(12) 0.0005(11) -0.0087(11) -0.0128(13) C3 0.072(2) 0.074(2) 0.0255(13) 0.0081(13) -0.0073(12) -0.0270(17) C4 0.0417(15) 0.080(2) 0.0264(12) -0.0134(14) 0.0002(11) -0.0139(14) C5 0.0332(13) 0.0519(17) 0.0480(15) -0.0251(13) -0.0020(11) -0.0044(12) C6 0.0280(12) 0.0365(13) 0.0342(12) -0.0077(10) -0.0024(9) -0.0035(10) C7 0.0414(13) 0.0177(10) 0.0311(11) 0.0001(9) -0.0106(10) -0.0072(9) C8 0.0561(16) 0.0312(13) 0.0318(12) 0.0025(10) -0.0066(11) -0.0138(12) C9 0.105(3) 0.0340(15) 0.0364(14) 0.0076(12) -0.0213(15) -0.0195(17) C10 0.102(3) 0.0256(14) 0.066(2) 0.0063(14) -0.0504(19) -0.0083(16) C11 0.0526(18) 0.0293(14) 0.092(2) -0.0067(15) -0.0303(17) 0.0007(13) C12 0.0428(15) 0.0266(12) 0.0515(15) -0.0052(11) -0.0067(11) -0.0026(11) C13 0.0279(11) 0.0307(12) 0.0211(10) -0.0022(9) 0.0008(8) -0.0088(9) C14 0.0331(12) 0.0327(12) 0.0260(11) -0.0042(9) 0.0068(9) -0.0048(10) C15 0.0511(16) 0.0300(13) 0.0371(13) -0.0031(10) 0.0093(11) -0.0069(11) C16 0.0633(18) 0.0414(15) 0.0446(15) -0.0005(12) 0.0193(13) -0.0214(14) C17 0.0484(16) 0.0500(17) 0.0543(16) -0.0076(13) 0.0281(13) -0.0140(13) C18 0.0330(13) 0.0365(13) 0.0419(13) -0.0077(11) 0.0127(10) -0.0064(11) C19 0.0282(11) 0.0305(12) 0.0238(10) -0.0013(9) 0.0025(9) 0.0013(9) C20 0.0341(13) 0.0401(14) 0.0295(12) 0.0115(10) -0.0011(10) 0.0002(11) C21 0.0331(12) 0.0291(12) 0.0317(12) 0.0065(10) 0.0071(9) -0.0007(10) C22 0.0395(14) 0.0455(15) 0.0398(13) -0.0038(12) -0.0058(11) -0.0052(12) C23 0.0545(18) 0.0435(16) 0.0684(19) 0.0282(14) -0.0056(14) -0.0154(14) C24 0.0269(11) 0.0339(12) 0.0212(10) 0.0007(9) 0.0005(8) -0.0035(9) C25 0.0286(12) 0.0397(13) 0.0179(10) -0.0056(9) 0.0022(8) -0.0005(10) C26 0.0223(10) 0.0306(12) 0.0237(10) -0.0073(9) -0.0026(8) 0.0006(9) C27 0.0618(18) 0.0460(16) 0.0273(12) 0.0015(11) 0.0076(11) -0.0169(13) C28 0.0385(13) 0.0333(13) 0.0335(12) -0.0106(10) -0.0001(10) -0.0019(11) C29 0.0286(12) 0.0322(12) 0.0264(11) 0.0027(9) -0.0010(9) -0.0101(10) C34 0.0402(14) 0.0296(12) 0.0259(11) -0.0055(9) 0.0057(9) -0.0088(10) C30 0.0234(11) 0.0379(13) 0.0329(12) -0.0023(10) 0.0013(9) -0.0060(10) C31 0.0254(11) 0.0302(12) 0.0238(10) -0.0044(9) -0.0011(8) -0.0032(9) C32 0.0363(14) 0.0355(14) 0.0640(17) 0.0084(13) -0.0010(12) -0.0139(11) C33 0.0310(13) 0.0300(12) 0.0461(14) -0.0066(11) -0.0044(10) 0.0002(10) _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 C34 1.826(2) . ? Rh1 N6 2.0974(17) . ? Rh1 N4 2.1092(16) . ? Rh1 P1 2.1792(6) . ? Rh1 N2 2.7635(18) . ? Rh1 B1 3.281(3) . ? B1 N1 1.541(3) . ? B1 N3 1.552(3) . ? B1 N5 1.559(3) . ? N2 C19 1.336(3) . ? N2 N1 1.370(2) . ? N1 C21 1.358(3) . ? N3 C26 1.359(2) . ? N3 N4 1.375(2) . ? N4 C24 1.340(2) . ? N5 C29 1.354(3) . ? N5 N6 1.388(2) . ? N6 C31 1.343(3) . ? P1 O2 1.6002(15) . ? P1 O3 1.6113(15) . ? P1 O4 1.6146(14) . ? O1 C34 1.143(3) . ? O2 C1 1.415(2) . ? O3 C7 1.405(2) . ? O4 C13 1.400(2) . ? C1 C6 1.371(3) . ? C1 C2 1.375(3) . ? C2 C3 1.388(3) . ? C3 C4 1.376(4) . ? C4 C5 1.379(4) . ? C5 C6 1.398(3) . ? C7 C12 1.375(3) . ? C7 C8 1.379(3) . ? C8 C9 1.390(4) . ? C9 C10 1.361(4) . ? C10 C11 1.380(4) . ? C11 C12 1.391(4) . ? C13 C14 1.380(3) . ? C13 C18 1.382(3) . ? C14 C15 1.378(3) . ? C15 C16 1.385(3) . ? C16 C17 1.378(4) . ? C17 C18 1.386(3) . ? C19 C20 1.396(3) . ? C19 C22 1.491(3) . ? C20 C21 1.373(3) . ? C21 C23 1.498(3) . ? C24 C25 1.397(3) . ? C24 C27 1.487(3) . ? C25 C26 1.380(3) . ? C26 C28 1.494(3) . ? C29 C30 1.373(3) . ? C29 C32 1.494(3) . ? C30 C31 1.390(3) . ? C31 C33 1.492(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 Rh1 N6 175.99(8) . . ? C34 Rh1 N4 94.98(8) . . ? N6 Rh1 N4 81.93(6) . . ? C34 Rh1 P1 86.92(7) . . ? N6 Rh1 P1 96.15(5) . . ? N4 Rh1 P1 178.03(5) . . ? C34 Rh1 N2 91.07(8) . . ? N6 Rh1 N2 90.76(6) . . ? N4 Rh1 N2 77.73(6) . . ? P1 Rh1 N2 102.77(4) . . ? C34 Rh1 B1 127.97(8) . . ? N6 Rh1 B1 51.64(6) . . ? N4 Rh1 B1 51.46(6) . . ? P1 Rh1 B1 127.51(4) . . ? N2 Rh1 B1 48.49(6) . . ? N1 B1 N3 111.30(18) . . ? N1 B1 N5 112.15(16) . . ? N3 B1 N5 107.70(17) . . ? N1 B1 Rh1 81.08(12) . . ? N3 B1 Rh1 66.73(11) . . ? N5 B1 Rh1 66.57(11) . . ? C19 N2 N1 106.53(17) . . ? C19 N2 Rh1 139.30(14) . . ? N1 N2 Rh1 105.79(11) . . ? C21 N1 N2 110.09(17) . . ? C21 N1 B1 129.53(19) . . ? N2 N1 B1 120.37(16) . . ? C26 N3 N4 109.28(16) . . ? C26 N3 B1 128.00(18) . . ? N4 N3 B1 122.50(15) . . ? C24 N4 N3 107.42(16) . . ? C24 N4 Rh1 133.51(15) . . ? N3 N4 Rh1 119.04(11) . . ? C29 N5 N6 108.75(16) . . ? C29 N5 B1 128.41(18) . . ? N6 N5 B1 121.60(16) . . ? C31 N6 N5 107.07(16) . . ? C31 N6 Rh1 134.08(14) . . ? N5 N6 Rh1 118.79(12) . . ? O2 P1 O3 99.02(8) . . ? O2 P1 O4 102.68(7) . . ? O3 P1 O4 97.72(8) . . ? O2 P1 Rh1 112.88(5) . . ? O3 P1 Rh1 120.88(6) . . ? O4 P1 Rh1 120.12(6) . . ? C1 O2 P1 123.70(12) . . ? C7 O3 P1 122.08(12) . . ? C13 O4 P1 125.83(13) . . ? C6 C1 C2 121.8(2) . . ? C6 C1 O2 121.2(2) . . ? C2 C1 O2 116.86(19) . . ? C1 C2 C3 119.3(2) . . ? C4 C3 C2 120.1(3) . . ? C3 C4 C5 119.8(2) . . ? C4 C5 C6 120.7(2) . . ? C1 C6 C5 118.2(2) . . ? C12 C7 C8 121.8(2) . . ? C12 C7 O3 119.2(2) . . ? C8 C7 O3 119.0(2) . . ? C7 C8 C9 118.3(3) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 120.4(3) . . ? C7 C12 C11 118.5(3) . . ? C14 C13 C18 121.5(2) . . ? C14 C13 O4 123.94(18) . . ? C18 C13 O4 114.55(19) . . ? C15 C14 C13 118.7(2) . . ? C14 C15 C16 121.0(2) . . ? C17 C16 C15 119.3(2) . . ? C16 C17 C18 120.8(2) . . ? C13 C18 C17 118.7(2) . . ? N2 C19 C20 109.8(2) . . ? N2 C19 C22 120.6(2) . . ? C20 C19 C22 129.5(2) . . ? C21 C20 C19 106.3(2) . . ? N1 C21 C20 107.2(2) . . ? N1 C21 C23 123.1(2) . . ? C20 C21 C23 129.7(2) . . ? N4 C24 C25 109.18(19) . . ? N4 C24 C27 121.55(19) . . ? C25 C24 C27 129.27(19) . . ? C26 C25 C24 106.45(18) . . ? N3 C26 C25 107.67(19) . . ? N3 C26 C28 123.19(19) . . ? C25 C26 C28 129.14(19) . . ? N5 C29 C30 108.17(19) . . ? N5 C29 C32 123.1(2) . . ? C30 C29 C32 128.7(2) . . ? O1 C34 Rh1 178.3(2) . . ? C29 C30 C31 106.75(19) . . ? N6 C31 C30 109.24(19) . . ? N6 C31 C33 122.11(19) . . ? C30 C31 C33 128.5(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 Rh1 B1 N1 N2 -19.05(15) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.369 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.060 data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H52 B N6 P2 Rh' _chemical_formula_weight 960.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 11.4436(11) _cell_length_b 18.7695(18) _cell_length_c 23.137(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.323(8) _cell_angle_gamma 90.00 _cell_volume 4968.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 352 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.450 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.870920 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31048 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11340 _reflns_number_gt 9052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0451P)^2^+0.3115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11340 _refine_ls_number_parameters 609 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.816980(13) 0.805373(9) 0.792781(7) 0.01868(5) Uani 1 1 d . . . P1 P 0.95794(5) 0.83087(3) 0.85939(2) 0.02112(12) Uani 1 1 d . . . P2 P 0.68365(5) 0.88235(3) 0.82769(2) 0.02146(12) Uani 1 1 d . . . N2 N 0.88521(16) 0.92309(10) 0.66978(8) 0.0273(4) Uani 1 1 d . . . N1 N 0.95331(15) 0.86283(10) 0.66810(8) 0.0240(4) Uani 1 1 d . . . N3 N 0.76065(15) 0.79360(9) 0.66692(7) 0.0217(4) Uani 1 1 d . . . N4 N 0.71097(15) 0.77830(10) 0.71916(8) 0.0219(4) Uani 1 1 d . . . N5 N 0.94437(14) 0.72914(10) 0.69779(8) 0.0228(4) Uani 1 1 d . . . N6 N 0.91419(15) 0.72490(10) 0.75491(8) 0.0221(4) Uani 1 1 d . . . B1 B 0.8954(2) 0.78941(14) 0.65810(11) 0.0232(5) Uani 1 1 d . . . H1A H 0.910(2) 0.7739(15) 0.6132(12) 0.050 Uiso 1 1 d . . . C1 C 1.08138(18) 0.76774(13) 0.86152(10) 0.0264(5) Uani 1 1 d . . . C2 C 1.1143(2) 0.72734(14) 0.90912(11) 0.0368(6) Uani 1 1 d . . . H2 H 1.0737 0.7328 0.9442 0.044 Uiso 1 1 calc R . . C3 C 1.2063(3) 0.67872(17) 0.90646(15) 0.0538(8) Uani 1 1 d . . . H3 H 1.2285 0.6516 0.9396 0.065 Uiso 1 1 calc R . . C4 C 1.2642(3) 0.67042(19) 0.85584(16) 0.0610(10) Uani 1 1 d . . . H4 H 1.3255 0.6365 0.8536 0.073 Uiso 1 1 calc R . . C5 C 1.2343(2) 0.71097(17) 0.80822(14) 0.0509(8) Uani 1 1 d . . . H5 H 1.2756 0.7053 0.7734 0.061 Uiso 1 1 calc R . . C6 C 1.14421(19) 0.75996(15) 0.81090(11) 0.0358(6) Uani 1 1 d . . . H6 H 1.1250 0.7885 0.7781 0.043 Uiso 1 1 calc R . . C7 C 0.92054(18) 0.83436(13) 0.93621(9) 0.0250(5) Uani 1 1 d . . . C8 C 0.9570(2) 0.88742(14) 0.97452(10) 0.0314(5) Uani 1 1 d . . . H8 H 1.0062 0.9246 0.9615 0.038 Uiso 1 1 calc R . . C9 C 0.9221(2) 0.88676(15) 1.03182(11) 0.0375(6) Uani 1 1 d . . . H9 H 0.9472 0.9235 1.0575 0.045 Uiso 1 1 calc R . . C10 C 0.8518(2) 0.83334(17) 1.05126(11) 0.0436(7) Uani 1 1 d . . . H10 H 0.8279 0.8331 1.0903 0.052 Uiso 1 1 calc R . . C11 C 0.8160(3) 0.78015(17) 1.01420(12) 0.0483(7) Uani 1 1 d . . . H11 H 0.7681 0.7427 1.0278 0.058 Uiso 1 1 calc R . . C12 C 0.8494(2) 0.78089(15) 0.95692(11) 0.0371(6) Uani 1 1 d . . . H12 H 0.8230 0.7442 0.9315 0.044 Uiso 1 1 calc R . . C13 C 1.04400(18) 0.91243(12) 0.84867(9) 0.0249(5) Uani 1 1 d . . . C14 C 1.1505(2) 0.92308(13) 0.87893(11) 0.0317(5) Uani 1 1 d . . . H14 H 1.1777 0.8883 0.9059 0.038 Uiso 1 1 calc R . . C15 C 1.2160(2) 0.98383(14) 0.86983(11) 0.0357(6) Uani 1 1 d . . . H15 H 1.2874 0.9908 0.8909 0.043 Uiso 1 1 calc R . . C16 C 1.1782(2) 1.03425(14) 0.83031(12) 0.0374(6) Uani 1 1 d . . . H16 H 1.2233 1.0760 0.8241 0.045 Uiso 1 1 calc R . . C17 C 1.0746(2) 1.02387(14) 0.79981(11) 0.0376(6) Uani 1 1 d . . . H17 H 1.0485 1.0586 0.7726 0.045 Uiso 1 1 calc R . . C18 C 1.0079(2) 0.96272(13) 0.80860(10) 0.0296(5) Uani 1 1 d . . . H18 H 0.9374 0.9557 0.7869 0.035 Uiso 1 1 calc R . . C19 C 0.9580(2) 0.97776(13) 0.66385(10) 0.0301(5) Uani 1 1 d . . . C20 C 1.0727(2) 0.95386(13) 0.65810(11) 0.0328(5) Uani 1 1 d . . . H20 H 1.1407 0.9822 0.6537 0.039 Uiso 1 1 calc R . . C21 C 1.06660(19) 0.88080(13) 0.66013(10) 0.0280(5) Uani 1 1 d . . . C22 C 0.9109(2) 1.05272(14) 0.66456(13) 0.0436(7) Uani 1 1 d . . . H22A H 0.8261 1.0514 0.6693 0.065 Uiso 0.50 1 calc PR . . H22B H 0.9287 1.0764 0.6281 0.065 Uiso 0.50 1 calc PR . . H22C H 0.9474 1.0791 0.6968 0.065 Uiso 0.50 1 calc PR . . H22D H 0.9753 1.0865 0.6601 0.065 Uiso 0.50 1 calc PR . . H22E H 0.8728 1.0615 0.7014 0.065 Uiso 0.50 1 calc PR . . H22F H 0.8540 1.0589 0.6326 0.065 Uiso 0.50 1 calc PR . . C23 C 1.1607(2) 0.82653(14) 0.65090(13) 0.0381(6) Uani 1 1 d . . . H23A H 1.1596 0.7912 0.6821 0.057 Uiso 1 1 calc R . . H23B H 1.2370 0.8502 0.6509 0.057 Uiso 1 1 calc R . . H23C H 1.1469 0.8027 0.6137 0.057 Uiso 1 1 calc R . . C24 C 0.59887(18) 0.76263(12) 0.70767(10) 0.0272(5) Uani 1 1 d . . . C25 C 0.57426(19) 0.77005(13) 0.64904(10) 0.0303(5) Uani 1 1 d . . . H25 H 0.5009 0.7629 0.6298 0.036 Uiso 1 1 calc R . . C26 C 0.6773(2) 0.78986(12) 0.62435(10) 0.0274(5) Uani 1 1 d . . . C27 C 0.5189(2) 0.73610(15) 0.75326(12) 0.0404(6) Uani 1 1 d . . . H27A H 0.5653 0.7142 0.7847 0.061 Uiso 1 1 calc R . . H27B H 0.4653 0.7006 0.7364 0.061 Uiso 1 1 calc R . . H27C H 0.4739 0.7761 0.7685 0.061 Uiso 1 1 calc R . . C28 C 0.7009(2) 0.80703(15) 0.56312(11) 0.0393(6) Uani 1 1 d . . . H28A H 0.7543 0.8477 0.5615 0.059 Uiso 1 1 calc R . . H28B H 0.6273 0.8190 0.5429 0.059 Uiso 1 1 calc R . . H28C H 0.7365 0.7657 0.5446 0.059 Uiso 1 1 calc R . . C29 C 0.99102(18) 0.66556(13) 0.68178(10) 0.0270(5) Uani 1 1 d . . . C30 C 0.99181(19) 0.62085(12) 0.72861(10) 0.0288(5) Uani 1 1 d . . . H30 H 1.0211 0.5735 0.7304 0.035 Uiso 1 1 calc R . . C31 C 0.94052(18) 0.65929(12) 0.77337(10) 0.0253(5) Uani 1 1 d . . . C33 C 0.9103(2) 0.63408(13) 0.83195(11) 0.0349(6) Uani 1 1 d . . . H33A H 0.8718 0.6725 0.8529 0.052 Uiso 1 1 calc R . . H33B H 0.9818 0.6199 0.8531 0.052 Uiso 1 1 calc R . . H33C H 0.8575 0.5931 0.8286 0.052 Uiso 1 1 calc R . . C35 C 0.72610(18) 0.96927(12) 0.85921(10) 0.0259(5) Uani 1 1 d . . . C36 C 0.7484(2) 0.97611(14) 0.91835(11) 0.0329(5) Uani 1 1 d . . . H36 H 0.7385 0.9363 0.9431 0.039 Uiso 1 1 calc R . . C37 C 0.7853(2) 1.04111(15) 0.94142(12) 0.0413(7) Uani 1 1 d . . . H37 H 0.8007 1.0453 0.9818 0.050 Uiso 1 1 calc R . . C38 C 0.7996(2) 1.09928(15) 0.90605(13) 0.0450(7) Uani 1 1 d . . . H38 H 0.8248 1.1435 0.9220 0.054 Uiso 1 1 calc R . . C39 C 0.7772(2) 1.09337(14) 0.84745(13) 0.0397(6) Uani 1 1 d . . . H39 H 0.7869 1.1335 0.8231 0.048 Uiso 1 1 calc R . . C40 C 0.74054(19) 1.02868(13) 0.82399(11) 0.0326(5) Uani 1 1 d . . . H41 H 0.7252 1.0250 0.7836 0.039 Uiso 1 1 calc R . . C41 C 0.59268(19) 0.84559(14) 0.88498(10) 0.0304(5) Uani 1 1 d . . . C42 C 0.5196(2) 0.88753(18) 0.91835(11) 0.0434(7) Uani 1 1 d . . . H42 H 0.5156 0.9375 0.9121 0.052 Uiso 1 1 calc R . . C43 C 0.4523(3) 0.8560(3) 0.96099(13) 0.0662(11) Uani 1 1 d . . . H43 H 0.4030 0.8845 0.9840 0.079 Uiso 1 1 calc R . . C44 C 0.4577(3) 0.7831(3) 0.96966(14) 0.0768(13) Uani 1 1 d . . . H44 H 0.4120 0.7617 0.9987 0.092 Uiso 1 1 calc R . . C45 C 0.5279(3) 0.7418(2) 0.93688(14) 0.0685(11) Uani 1 1 d . . . H45 H 0.5303 0.6918 0.9429 0.082 Uiso 1 1 calc R . . C46 C 0.5961(2) 0.77243(17) 0.89469(12) 0.0442(7) Uani 1 1 d . . . H46 H 0.6456 0.7432 0.8723 0.053 Uiso 1 1 calc R . . C47 C 0.57490(18) 0.91133(12) 0.77244(9) 0.0227(4) Uani 1 1 d . . . C48 C 0.61661(19) 0.93036(12) 0.71834(10) 0.0246(5) Uani 1 1 d . . . H48 H 0.6981 0.9285 0.7115 0.030 Uiso 1 1 calc R . . C49 C 0.5397(2) 0.95197(12) 0.67465(10) 0.0293(5) Uani 1 1 d . . . H49 H 0.5686 0.9648 0.6379 0.035 Uiso 1 1 calc R . . C50 C 0.4201(2) 0.95498(13) 0.68427(11) 0.0330(5) Uani 1 1 d . . . H50 H 0.3677 0.9702 0.6543 0.040 Uiso 1 1 calc R . . C51 C 0.37807(19) 0.93582(14) 0.73736(11) 0.0329(6) Uani 1 1 d . . . H51 H 0.2964 0.9372 0.7438 0.040 Uiso 1 1 calc R . . C52 C 0.45434(18) 0.91451(13) 0.78135(10) 0.0280(5) Uani 1 1 d . . . H52 H 0.4246 0.9019 0.8180 0.034 Uiso 1 1 calc R . . C74 C 1.0269(2) 0.64810(14) 0.62164(11) 0.0387(6) Uani 1 1 d . . . H74A H 1.0823 0.6841 0.6084 0.058 Uiso 1 1 calc R . . H74B H 0.9578 0.6477 0.5958 0.058 Uiso 1 1 calc R . . H74C H 1.0641 0.6011 0.6213 0.058 Uiso 1 1 calc R . . C100 C 0.981(3) 1.0395(9) 0.5000(5) 0.205(13) Uani 0.50 1 d P . . C101 C 0.881(2) 1.0161(14) 0.4997(5) 0.22(2) Uani 0.50 1 d P . . C102 C 0.769(2) 1.0755(8) 0.4996(5) 0.178(10) Uani 0.50 1 d P . . C103 C 0.708(3) 1.0205(8) 0.4996(5) 0.219(12) Uani 0.50 1 d P . . C104 C 0.6016(13) 1.0761(6) 0.4993(6) 0.117(4) Uani 0.50 1 d P . . C105 C 0.5000 1.0000 0.5000 0.360(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01700(8) 0.02179(9) 0.01724(9) -0.00156(6) 0.00008(6) -0.00074(6) P1 0.0189(3) 0.0261(3) 0.0183(3) -0.0018(2) -0.0006(2) -0.0002(2) P2 0.0176(3) 0.0269(3) 0.0198(3) -0.0021(2) 0.0009(2) -0.0003(2) N2 0.0238(9) 0.0272(11) 0.0310(11) 0.0026(8) 0.0027(8) 0.0028(8) N1 0.0201(9) 0.0285(11) 0.0236(10) 0.0016(8) 0.0024(7) 0.0008(8) N3 0.0216(9) 0.0256(10) 0.0176(9) -0.0019(7) -0.0010(7) -0.0008(7) N4 0.0189(8) 0.0245(10) 0.0223(9) -0.0041(7) 0.0001(7) -0.0023(7) N5 0.0195(9) 0.0265(10) 0.0225(9) -0.0038(7) 0.0012(7) 0.0011(7) N6 0.0205(9) 0.0234(10) 0.0224(9) -0.0021(7) -0.0013(7) 0.0000(7) B1 0.0206(12) 0.0299(15) 0.0191(12) -0.0017(10) 0.0017(9) 0.0005(10) C1 0.0208(11) 0.0316(13) 0.0265(12) -0.0067(9) -0.0037(9) 0.0005(9) C2 0.0356(14) 0.0411(15) 0.0336(14) -0.0040(11) -0.0047(11) 0.0118(12) C3 0.0479(17) 0.054(2) 0.058(2) -0.0070(15) -0.0172(15) 0.0231(14) C4 0.0344(16) 0.070(2) 0.078(2) -0.0297(19) -0.0134(15) 0.0251(15) C5 0.0224(13) 0.077(2) 0.0532(19) -0.0300(16) 0.0042(12) 0.0023(13) C6 0.0221(11) 0.0522(17) 0.0332(14) -0.0107(11) 0.0019(10) -0.0034(11) C7 0.0212(11) 0.0331(13) 0.0205(11) -0.0017(9) -0.0018(8) 0.0051(9) C8 0.0282(12) 0.0405(15) 0.0252(12) -0.0067(10) -0.0020(9) 0.0037(10) C9 0.0332(13) 0.0538(17) 0.0253(13) -0.0120(11) -0.0020(10) 0.0067(12) C10 0.0428(15) 0.068(2) 0.0203(13) -0.0031(12) 0.0040(11) 0.0093(14) C11 0.0542(18) 0.0588(19) 0.0325(15) 0.0028(13) 0.0123(13) -0.0098(15) C12 0.0414(14) 0.0434(15) 0.0266(13) -0.0030(11) 0.0057(11) -0.0052(12) C13 0.0222(10) 0.0286(12) 0.0239(11) -0.0046(9) 0.0018(8) -0.0019(9) C14 0.0265(12) 0.0360(14) 0.0323(13) -0.0044(10) -0.0030(10) -0.0027(10) C15 0.0249(12) 0.0407(15) 0.0414(15) -0.0124(12) 0.0003(10) -0.0067(11) C16 0.0376(14) 0.0308(14) 0.0441(16) -0.0083(11) 0.0112(11) -0.0095(11) C17 0.0423(14) 0.0318(14) 0.0388(15) 0.0026(11) 0.0042(11) -0.0012(11) C18 0.0261(12) 0.0326(14) 0.0299(13) -0.0009(10) 0.0000(9) -0.0013(10) C19 0.0290(12) 0.0293(13) 0.0320(13) 0.0044(10) 0.0029(10) -0.0021(10) C20 0.0245(12) 0.0360(14) 0.0381(14) 0.0024(11) 0.0054(10) -0.0068(10) C21 0.0212(11) 0.0343(14) 0.0285(12) -0.0017(10) 0.0035(9) -0.0008(9) C22 0.0379(15) 0.0324(15) 0.0607(19) 0.0077(13) 0.0028(13) -0.0007(12) C23 0.0225(12) 0.0391(15) 0.0531(17) -0.0041(12) 0.0099(11) -0.0009(10) C24 0.0212(11) 0.0268(13) 0.0335(13) -0.0082(10) 0.0011(9) -0.0039(9) C25 0.0221(11) 0.0341(14) 0.0342(13) -0.0088(10) -0.0086(9) -0.0010(10) C26 0.0294(12) 0.0275(13) 0.0249(12) -0.0054(9) -0.0065(9) 0.0023(9) C27 0.0303(13) 0.0476(17) 0.0438(16) -0.0112(12) 0.0096(11) -0.0157(12) C28 0.0406(14) 0.0523(17) 0.0248(13) 0.0020(11) -0.0074(10) 0.0052(12) C29 0.0201(10) 0.0285(12) 0.0322(13) -0.0084(10) -0.0015(9) 0.0017(9) C30 0.0264(11) 0.0237(12) 0.0361(13) -0.0052(10) -0.0037(10) 0.0032(9) C31 0.0223(11) 0.0249(12) 0.0285(12) -0.0019(9) -0.0050(9) -0.0013(9) C33 0.0425(14) 0.0266(13) 0.0354(14) 0.0026(10) -0.0018(11) -0.0014(11) C35 0.0183(10) 0.0284(12) 0.0308(12) -0.0070(9) -0.0025(9) 0.0058(9) C36 0.0287(12) 0.0347(14) 0.0349(14) -0.0066(11) -0.0069(10) 0.0089(10) C37 0.0423(15) 0.0407(16) 0.0400(15) -0.0174(12) -0.0146(12) 0.0087(12) C38 0.0394(15) 0.0313(15) 0.064(2) -0.0168(13) -0.0164(13) 0.0067(12) C39 0.0351(14) 0.0262(14) 0.0572(18) -0.0012(12) -0.0106(12) 0.0003(11) C40 0.0269(12) 0.0319(14) 0.0386(14) -0.0042(11) -0.0044(10) 0.0013(10) C41 0.0204(11) 0.0503(16) 0.0206(11) -0.0007(10) 0.0015(8) -0.0050(10) C42 0.0251(12) 0.078(2) 0.0269(14) -0.0055(13) 0.0025(10) 0.0037(13) C43 0.0310(15) 0.138(4) 0.0299(16) -0.0110(19) 0.0102(12) -0.0087(19) C44 0.057(2) 0.139(4) 0.0349(18) 0.013(2) 0.0107(15) -0.047(2) C45 0.074(2) 0.086(3) 0.0454(19) 0.0155(18) 0.0063(17) -0.044(2) C46 0.0438(15) 0.0563(19) 0.0325(15) 0.0066(13) 0.0013(12) -0.0178(14) C47 0.0215(10) 0.0224(11) 0.0240(11) -0.0044(9) -0.0014(8) 0.0014(9) C48 0.0219(11) 0.0246(12) 0.0275(12) -0.0044(9) 0.0005(9) 0.0007(9) C49 0.0341(12) 0.0267(13) 0.0270(12) -0.0025(9) -0.0007(10) -0.0005(10) C50 0.0304(12) 0.0340(14) 0.0339(14) -0.0030(10) -0.0114(10) 0.0046(10) C51 0.0183(11) 0.0419(15) 0.0384(14) -0.0082(11) -0.0030(9) 0.0020(10) C52 0.0215(11) 0.0356(14) 0.0269(12) -0.0050(10) -0.0002(9) 0.0009(9) C74 0.0399(14) 0.0391(15) 0.0372(15) -0.0117(11) 0.0045(11) 0.0087(12) C100 0.41(3) 0.141(12) 0.060(7) -0.050(8) -0.073(13) 0.173(18) C101 0.34(4) 0.28(4) 0.022(5) 0.005(9) -0.014(10) -0.19(4) C102 0.36(3) 0.098(10) 0.079(8) 0.038(7) -0.049(12) -0.088(14) C103 0.50(4) 0.091(11) 0.064(8) -0.011(7) -0.012(14) -0.022(18) C104 0.149(11) 0.081(8) 0.124(10) -0.011(7) 0.022(8) 0.001(8) C105 0.55(4) 0.45(3) 0.073(8) 0.020(13) -0.052(15) 0.29(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 N6 2.0813(18) . ? Rh1 N4 2.1298(17) . ? Rh1 P1 2.2564(6) . ? Rh1 P2 2.2638(6) . ? Rh1 B1 3.276(3) . ? Rh1 N2 3.7003(19) . ? P1 C7 1.839(2) . ? P1 C13 1.840(2) . ? P1 C1 1.844(2) . ? P2 C41 1.839(2) . ? P2 C47 1.845(2) . ? P2 C35 1.847(2) . ? N2 C19 1.331(3) . ? N2 N1 1.375(3) . ? N1 C21 1.356(3) . ? N1 B1 1.544(3) . ? N3 C26 1.357(3) . ? N3 N4 1.378(2) . ? N3 B1 1.562(3) . ? N4 C24 1.337(3) . ? N5 C29 1.362(3) . ? N5 N6 1.376(2) . ? N5 B1 1.554(3) . ? N6 C31 1.336(3) . ? C1 C2 1.382(3) . ? C1 C6 1.396(3) . ? C2 C3 1.395(4) . ? C3 C4 1.368(5) . ? C4 C5 1.376(5) . ? C5 C6 1.384(4) . ? C7 C12 1.385(3) . ? C7 C8 1.391(3) . ? C8 C9 1.393(3) . ? C9 C10 1.368(4) . ? C10 C11 1.372(4) . ? C11 C12 1.388(3) . ? C13 C18 1.380(3) . ? C13 C14 1.405(3) . ? C14 C15 1.384(3) . ? C15 C16 1.379(4) . ? C16 C17 1.379(4) . ? C17 C18 1.396(3) . ? C19 C20 1.397(3) . ? C19 C22 1.507(3) . ? C20 C21 1.374(3) . ? C21 C23 1.501(3) . ? C24 C25 1.386(3) . ? C24 C27 1.497(3) . ? C25 C26 1.373(3) . ? C26 C28 1.484(3) . ? C29 C30 1.370(3) . ? C29 C74 1.496(3) . ? C30 C31 1.402(3) . ? C31 C33 1.484(3) . ? C35 C36 1.392(3) . ? C35 C40 1.393(3) . ? C36 C37 1.393(4) . ? C37 C38 1.376(4) . ? C38 C39 1.378(4) . ? C39 C40 1.391(3) . ? C41 C46 1.392(4) . ? C41 C42 1.395(3) . ? C42 C43 1.397(4) . ? C43 C44 1.384(6) . ? C44 C45 1.360(6) . ? C45 C46 1.388(4) . ? C47 C48 1.396(3) . ? C47 C52 1.401(3) . ? C48 C49 1.386(3) . ? C49 C50 1.392(3) . ? C50 C51 1.378(3) . ? C51 C52 1.384(3) . ? C100 C101 1.23(4) . ? C100 C100 1.55(2) 3_776 ? C101 C102 1.70(3) . ? C101 C103 1.98(4) . ? C102 C103 1.25(2) . ? C102 C104 1.92(3) . ? C103 C104 1.60(3) . ? C104 C105 1.842(13) . ? 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 N6 Rh1 N4 77.89(7) . . ? N6 Rh1 P1 93.49(5) . . ? N4 Rh1 P1 169.07(5) . . ? N6 Rh1 P2 169.93(5) . . ? N4 Rh1 P2 93.52(5) . . ? P1 Rh1 P2 95.63(2) . . ? N6 Rh1 B1 51.13(7) . . ? N4 Rh1 B1 51.74(6) . . ? P1 Rh1 B1 117.51(5) . . ? P2 Rh1 B1 126.82(5) . . ? N6 Rh1 N2 89.15(6) . . ? N4 Rh1 N2 69.74(6) . . ? P1 Rh1 N2 103.79(4) . . ? P2 Rh1 N2 92.82(3) . . ? B1 Rh1 N2 41.91(5) . . ? C7 P1 C13 103.76(10) . . ? C7 P1 C1 101.09(10) . . ? C13 P1 C1 97.25(10) . . ? C7 P1 Rh1 119.28(7) . . ? C13 P1 Rh1 117.44(7) . . ? C1 P1 Rh1 114.66(7) . . ? C41 P2 C47 103.06(10) . . ? C41 P2 C35 101.23(11) . . ? C47 P2 C35 100.38(10) . . ? C41 P2 Rh1 114.53(9) . . ? C47 P2 Rh1 112.97(7) . . ? C35 P2 Rh1 122.09(7) . . ? C19 N2 N1 105.96(18) . . ? C19 N2 Rh1 133.12(15) . . ? N1 N2 Rh1 70.15(10) . . ? C21 N1 N2 110.09(18) . . ? C21 N1 B1 127.60(19) . . ? N2 N1 B1 119.78(17) . . ? C26 N3 N4 109.18(17) . . ? C26 N3 B1 125.59(18) . . ? N4 N3 B1 122.19(17) . . ? C24 N4 N3 106.56(17) . . ? C24 N4 Rh1 137.54(15) . . ? N3 N4 Rh1 114.39(12) . . ? C29 N5 N6 108.62(18) . . ? C29 N5 B1 127.99(19) . . ? N6 N5 B1 120.97(17) . . ? C31 N6 N5 107.50(17) . . ? C31 N6 Rh1 130.79(15) . . ? N5 N6 Rh1 120.72(13) . . ? N1 B1 N5 114.41(18) . . ? N1 B1 N3 110.93(18) . . ? N5 B1 N3 107.67(17) . . ? N1 B1 Rh1 84.38(12) . . ? N5 B1 Rh1 66.89(11) . . ? N3 B1 Rh1 65.06(10) . . ? C2 C1 C6 118.4(2) . . ? C2 C1 P1 124.65(18) . . ? C6 C1 P1 116.99(18) . . ? C1 C2 C3 121.0(3) . . ? C4 C3 C2 119.6(3) . . ? C3 C4 C5 120.4(3) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C1 120.4(3) . . ? C12 C7 C8 117.9(2) . . ? C12 C7 P1 117.42(18) . . ? C8 C7 P1 124.64(19) . . ? C7 C8 C9 120.8(2) . . ? C10 C9 C8 120.2(2) . . ? C9 C10 C11 119.8(2) . . ? C10 C11 C12 120.3(3) . . ? C7 C12 C11 121.0(2) . . ? C18 C13 C14 118.7(2) . . ? C18 C13 P1 120.46(17) . . ? C14 C13 P1 120.77(18) . . ? C15 C14 C13 120.5(2) . . ? C16 C15 C14 120.2(2) . . ? C15 C16 C17 119.7(2) . . ? C16 C17 C18 120.5(2) . . ? C13 C18 C17 120.3(2) . . ? N2 C19 C20 110.7(2) . . ? N2 C19 C22 119.6(2) . . ? C20 C19 C22 129.7(2) . . ? C21 C20 C19 105.6(2) . . ? N1 C21 C20 107.6(2) . . ? N1 C21 C23 122.8(2) . . ? C20 C21 C23 129.4(2) . . ? N4 C24 C25 110.2(2) . . ? N4 C24 C27 122.2(2) . . ? C25 C24 C27 127.5(2) . . ? C26 C25 C24 106.10(19) . . ? N3 C26 C25 107.9(2) . . ? N3 C26 C28 122.8(2) . . ? C25 C26 C28 129.3(2) . . ? N5 C29 C30 108.5(2) . . ? N5 C29 C74 124.2(2) . . ? C30 C29 C74 127.2(2) . . ? C29 C30 C31 105.9(2) . . ? N6 C31 C30 109.5(2) . . ? N6 C31 C33 122.0(2) . . ? C30 C31 C33 128.4(2) . . ? C36 C35 C40 118.7(2) . . ? C36 C35 P2 120.67(19) . . ? C40 C35 P2 120.63(18) . . ? C35 C36 C37 120.3(3) . . ? C38 C37 C36 120.4(3) . . ? C37 C38 C39 119.9(2) . . ? C38 C39 C40 120.1(3) . . ? C39 C40 C35 120.6(2) . . ? C46 C41 C42 118.9(2) . . ? C46 C41 P2 118.17(18) . . ? C42 C41 P2 123.0(2) . . ? C41 C42 C43 119.9(3) . . ? C44 C43 C42 119.9(3) . . ? C45 C44 C43 120.5(3) . . ? C44 C45 C46 120.4(4) . . ? C45 C46 C41 120.5(3) . . ? C48 C47 C52 118.6(2) . . ? C48 C47 P2 117.22(15) . . ? C52 C47 P2 124.15(17) . . ? C49 C48 C47 120.3(2) . . ? C48 C49 C50 120.4(2) . . ? C51 C50 C49 119.8(2) . . ? C50 C51 C52 120.2(2) . . ? C51 C52 C47 120.7(2) . . ? C101 C100 C100 85(3) . 3_776 ? C100 C101 C102 118(2) . . ? C100 C101 C103 157(3) . . ? C102 C101 C103 38.7(8) . . ? C103 C102 C101 83.1(18) . . ? C103 C102 C104 56.2(18) . . ? C101 C102 C104 139.2(13) . . ? C102 C103 C104 83.5(17) . . ? C102 C103 C101 58.2(18) . . ? C104 C103 C101 141.7(16) . . ? C103 C104 C105 88.5(11) . . ? C103 C104 C102 40.4(9) . . ? C105 C104 C102 128.9(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 -75.15(17) . . . . ? N3 B1 N1 N2 -14.6(3) . . . . ? N5 B1 N1 N2 -136.60(19) . . . . ? B1 N1 N2 C19 -164.4(2) . . . . ? H1A B1 N1 N2 103.3(15) . . . . ? Rh1 B1 N2 N1 100.52(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.618 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.083 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H37 B N6 O P Rh' _chemical_formula_weight 690.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 9.428(3) _cell_length_b 16.510(4) _cell_length_c 20.735(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.73(3) _cell_angle_gamma 90.00 _cell_volume 3198.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 174 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14466 _diffrn_reflns_av_R_equivalents 0.1000 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.19 _reflns_number_total 5582 _reflns_number_gt 4668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material '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^)+(0.0558P)^2^+21.7512P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5582 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.73585(5) 0.08675(3) 0.75243(2) 0.02270(17) Uani 1 1 d . . . N1 N 1.0679(5) -0.0006(3) 0.8162(2) 0.0289(11) Uani 1 1 d . . . N2 N 0.9571(5) -0.0023(3) 0.8542(2) 0.0242(11) Uani 1 1 d . . . N3 N 0.7647(5) 0.0810(3) 0.8988(2) 0.0206(10) Uani 1 1 d . . . N4 N 0.6635(5) 0.0882(3) 0.84433(19) 0.0194(10) Uani 1 1 d . . . N5 N 0.9679(5) 0.1493(3) 0.8554(2) 0.0243(11) Uani 1 1 d . . . N6 N 0.8899(5) 0.1705(3) 0.7964(2) 0.0231(10) Uani 1 1 d . . . O1 O 0.4964(5) -0.0184(3) 0.6964(2) 0.0402(12) Uani 1 1 d . . . B1 B 0.9264(7) 0.0742(4) 0.8922(3) 0.0236(14) Uani 1 1 d . . . H1 H 0.9836 0.0727 0.9365 0.036(19) Uiso 1 1 calc R . . P1 P 0.81902(16) 0.07416(9) 0.65503(7) 0.0222(3) Uani 1 1 d . . . C1 C 0.9649(6) 0.1404(4) 0.6385(3) 0.0233(12) Uani 1 1 d . . . C2 C 1.0931(6) 0.1393(4) 0.6820(3) 0.0283(13) Uani 1 1 d . . . H2A H 1.1051 0.1027 0.7176 0.034 Uiso 1 1 calc R . . C3 C 1.2010(7) 0.1923(4) 0.6718(3) 0.0366(15) Uani 1 1 d . . . H3A H 1.2880 0.1917 0.7008 0.044 Uiso 1 1 calc R . . C4 C 1.1852(8) 0.2463(5) 0.6202(3) 0.0417(17) Uani 1 1 d . . . H4A H 1.2600 0.2831 0.6145 0.050 Uiso 1 1 calc R . . C5 C 1.0595(7) 0.2463(4) 0.5768(3) 0.0347(15) Uani 1 1 d . . . H5A H 1.0484 0.2825 0.5409 0.042 Uiso 1 1 calc R . . C6 C 0.9502(7) 0.1933(4) 0.5862(3) 0.0293(13) Uani 1 1 d . . . H6A H 0.8643 0.1932 0.5565 0.035 Uiso 1 1 calc R . . C7 C 0.6840(6) 0.0906(4) 0.5846(3) 0.0259(13) Uani 1 1 d . . . C8 C 0.5671(8) 0.1413(4) 0.5904(3) 0.0371(16) Uani 1 1 d . . . H8A H 0.5560 0.1638 0.6316 0.044 Uiso 1 1 calc R . . C9 C 0.4676(8) 0.1591(5) 0.5367(4) 0.049(2) Uani 1 1 d . . . H9A H 0.3896 0.1941 0.5414 0.059 Uiso 1 1 calc R . . C10 C 0.4807(8) 0.1269(5) 0.4774(4) 0.047(2) Uani 1 1 d . . . H10A H 0.4123 0.1396 0.4409 0.057 Uiso 1 1 calc R . . C11 C 0.5928(8) 0.0758(5) 0.4703(3) 0.0429(19) Uani 1 1 d . . . H11A H 0.6014 0.0533 0.4288 0.052 Uiso 1 1 calc R . . C12 C 0.6936(7) 0.0568(4) 0.5235(3) 0.0334(15) Uani 1 1 d . . . H12A H 0.7695 0.0206 0.5182 0.040 Uiso 1 1 calc R . . C13 C 0.8871(7) -0.0272(4) 0.6387(3) 0.0276(13) Uani 1 1 d . . . C14 C 0.8298(7) -0.0951(4) 0.6637(3) 0.0352(15) Uani 1 1 d . . . H14A H 0.7625 -0.0890 0.6936 0.042 Uiso 1 1 calc R . . C15 C 0.8684(7) -0.1729(4) 0.6460(4) 0.0372(16) Uani 1 1 d . . . H15A H 0.8272 -0.2193 0.6633 0.045 Uiso 1 1 calc R . . C16 C 0.9669(8) -0.1814(4) 0.6033(3) 0.0407(17) Uani 1 1 d . . . H16A H 0.9931 -0.2339 0.5904 0.049 Uiso 1 1 calc R . . C17 C 1.0267(9) -0.1151(5) 0.5794(4) 0.049(2) Uani 1 1 d . . . H17A H 1.0957 -0.1219 0.5505 0.059 Uiso 1 1 calc R . . C18 C 0.9893(8) -0.0370(4) 0.5965(4) 0.0402(17) Uani 1 1 d . . . H18A H 1.0327 0.0088 0.5796 0.048 Uiso 1 1 calc R . . C19 C 1.0865(6) -0.0770(4) 0.7995(3) 0.0277(13) Uani 1 1 d . . . C20 C 0.9934(7) -0.1280(4) 0.8261(3) 0.0288(14) Uani 1 1 d . . . H20A H 0.9865 -0.1851 0.8211 0.035 Uiso 1 1 calc R . . C21 C 0.9140(6) -0.0805(4) 0.8605(3) 0.0250(13) Uani 1 1 d . . . C22 C 1.1995(7) -0.0974(5) 0.7569(4) 0.0393(16) Uani 1 1 d . . . H22A H 1.2478 -0.0476 0.7461 0.059 Uiso 1 1 calc R . . H22B H 1.1544 -0.1233 0.7168 0.059 Uiso 1 1 calc R . . H22C H 1.2697 -0.1345 0.7802 0.059 Uiso 1 1 calc R . . C23 C 0.7998(7) -0.1026(4) 0.9008(3) 0.0344(15) Uani 1 1 d . . . H23A H 0.7634 -0.0534 0.9193 0.052 Uiso 1 1 calc R . . H23B H 0.8397 -0.1389 0.9361 0.052 Uiso 1 1 calc R . . H23C H 0.7214 -0.1301 0.8735 0.052 Uiso 1 1 calc R . . C24 C 0.5357(6) 0.0930(4) 0.8651(3) 0.0236(12) Uani 1 1 d . . . C25 C 0.5538(7) 0.0869(4) 0.9329(3) 0.0283(13) Uani 1 1 d . . . H25A H 0.4806 0.0876 0.9602 0.034 Uiso 1 1 calc R . . C26 C 0.6988(7) 0.0798(4) 0.9524(3) 0.0250(12) Uani 1 1 d . . . C27 C 0.4012(7) 0.1071(5) 0.8201(3) 0.0382(17) Uani 1 1 d . . . H27A H 0.4224 0.1084 0.7751 0.057 Uiso 1 1 calc R . . H27B H 0.3592 0.1589 0.8306 0.057 Uiso 1 1 calc R . . H27C H 0.3333 0.0632 0.8249 0.057 Uiso 1 1 calc R . . C28 C 0.7780(7) 0.0723(5) 1.0205(3) 0.0347(15) Uani 1 1 d . . . H28A H 0.8810 0.0682 1.0184 0.052 Uiso 1 1 calc R . . H28B H 0.7454 0.0237 1.0413 0.052 Uiso 1 1 calc R . . H28C H 0.7590 0.1202 1.0459 0.052 Uiso 1 1 calc R . . C29 C 1.0636(6) 0.2083(4) 0.8738(3) 0.0251(13) Uani 1 1 d . . . C30 C 1.0454(7) 0.2689(4) 0.8278(3) 0.0293(13) Uani 1 1 d . . . H30A H 1.0971 0.3183 0.8283 0.035 Uiso 1 1 calc R . . C31 C 0.9355(6) 0.2430(4) 0.7803(3) 0.0247(12) Uani 1 1 d . . . C32 C 1.1681(7) 0.2034(4) 0.9352(3) 0.0360(16) Uani 1 1 d . . . H32A H 1.1543 0.1523 0.9576 0.054 Uiso 1 1 calc R . . H32B H 1.1521 0.2489 0.9637 0.054 Uiso 1 1 calc R . . H32C H 1.2660 0.2058 0.9243 0.054 Uiso 1 1 calc R . . C33 C 0.8695(7) 0.2877(4) 0.7218(3) 0.0302(14) Uani 1 1 d . . . H33A H 0.7947 0.2542 0.6975 0.045 Uiso 1 1 calc R . . H33B H 0.9429 0.3002 0.6940 0.045 Uiso 1 1 calc R . . H33C H 0.8271 0.3381 0.7352 0.045 Uiso 1 1 calc R . . C34 C 0.5892(6) 0.0212(4) 0.7178(3) 0.0274(13) 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 Rh1 0.0251(3) 0.0217(3) 0.0187(2) -0.00071(17) -0.00634(17) -0.00096(19) N1 0.027(3) 0.025(3) 0.033(3) 0.001(2) 0.000(2) 0.005(2) N2 0.021(2) 0.022(3) 0.027(3) 0.004(2) -0.0049(19) -0.002(2) N3 0.019(2) 0.019(2) 0.022(2) 0.0026(19) -0.0037(18) 0.0043(19) N4 0.030(3) 0.018(2) 0.0068(19) -0.0005(17) -0.0113(17) -0.002(2) N5 0.022(2) 0.026(3) 0.022(2) 0.001(2) -0.0044(19) 0.002(2) N6 0.022(2) 0.019(3) 0.025(2) 0.0001(19) -0.0091(19) -0.001(2) O1 0.030(2) 0.045(3) 0.045(3) -0.010(2) 0.002(2) -0.015(2) B1 0.021(3) 0.028(4) 0.019(3) 0.003(3) -0.007(2) -0.003(3) P1 0.0226(7) 0.0215(8) 0.0205(7) -0.0005(6) -0.0039(6) 0.0004(6) C1 0.023(3) 0.023(3) 0.024(3) -0.005(2) 0.002(2) -0.003(2) C2 0.024(3) 0.033(4) 0.026(3) 0.001(3) -0.005(2) 0.000(3) C3 0.030(3) 0.037(4) 0.039(4) 0.004(3) -0.007(3) -0.005(3) C4 0.042(4) 0.044(4) 0.038(4) -0.002(3) 0.003(3) -0.013(3) C5 0.042(4) 0.035(4) 0.024(3) 0.004(3) -0.005(3) -0.011(3) C6 0.034(3) 0.026(3) 0.026(3) -0.004(3) -0.002(3) -0.004(3) C7 0.029(3) 0.020(3) 0.027(3) 0.002(2) 0.000(2) -0.009(3) C8 0.041(4) 0.041(4) 0.027(3) 0.003(3) -0.004(3) 0.006(3) C9 0.039(4) 0.060(5) 0.044(4) 0.017(4) -0.010(3) 0.010(4) C10 0.044(4) 0.056(5) 0.035(4) 0.017(4) -0.018(3) -0.014(4) C11 0.051(4) 0.053(5) 0.021(3) 0.001(3) -0.007(3) -0.022(4) C12 0.039(4) 0.036(4) 0.023(3) 0.000(3) -0.003(3) -0.013(3) C13 0.030(3) 0.028(3) 0.021(3) -0.003(2) -0.007(2) 0.000(3) C14 0.038(4) 0.031(4) 0.037(4) 0.004(3) 0.006(3) 0.002(3) C15 0.038(4) 0.021(3) 0.051(4) 0.000(3) 0.000(3) -0.002(3) C16 0.054(4) 0.026(4) 0.042(4) -0.001(3) 0.006(3) 0.004(3) C17 0.068(5) 0.036(4) 0.049(4) -0.006(3) 0.029(4) 0.001(4) C18 0.054(4) 0.024(3) 0.046(4) 0.000(3) 0.019(3) -0.003(3) C19 0.026(3) 0.025(3) 0.030(3) -0.001(2) -0.005(2) 0.002(3) C20 0.030(3) 0.023(3) 0.029(3) 0.002(3) -0.010(2) 0.004(3) C21 0.024(3) 0.025(3) 0.023(3) 0.002(2) -0.008(2) -0.005(2) C22 0.033(3) 0.037(4) 0.048(4) -0.002(3) 0.006(3) 0.006(3) C23 0.042(4) 0.035(4) 0.027(3) -0.006(3) 0.004(3) -0.008(3) C24 0.014(3) 0.028(3) 0.027(3) -0.003(2) -0.001(2) 0.000(2) C25 0.027(3) 0.031(3) 0.026(3) -0.001(3) 0.003(2) 0.004(3) C26 0.032(3) 0.022(3) 0.020(3) -0.002(2) -0.001(2) -0.004(3) C27 0.020(3) 0.062(5) 0.030(3) -0.007(3) -0.006(2) 0.003(3) C28 0.035(3) 0.046(4) 0.020(3) 0.004(3) -0.005(3) 0.005(3) C29 0.023(3) 0.025(3) 0.024(3) -0.003(2) -0.008(2) 0.003(2) C30 0.030(3) 0.024(3) 0.031(3) -0.005(3) -0.005(2) -0.006(3) C31 0.024(3) 0.022(3) 0.027(3) 0.000(2) 0.000(2) 0.001(2) C32 0.035(4) 0.035(4) 0.033(3) 0.001(3) -0.014(3) -0.003(3) C33 0.040(4) 0.021(3) 0.027(3) 0.000(2) -0.002(3) 0.004(3) C34 0.020(3) 0.032(3) 0.028(3) -0.001(3) -0.001(2) 0.000(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 C34 1.825(6) . ? Rh1 N4 2.108(4) . ? Rh1 N6 2.120(5) . ? Rh1 P1 2.2721(16) . ? Rh1 N2 3.128(5) . ? Rh1 B1 3.205(6) . ? N1 C19 1.326(8) . ? N1 N2 1.391(7) . ? N2 C21 1.366(8) . ? N2 B1 1.536(8) . ? N3 C26 1.344(8) . ? N3 N4 1.383(6) . ? N3 B1 1.553(8) . ? N4 C24 1.335(7) . ? N5 C29 1.347(8) . ? N5 N6 1.383(6) . ? N5 B1 1.535(8) . ? N6 C31 1.331(8) . ? O1 C34 1.134(7) . ? B1 H1 1.0000 . ? P1 C1 1.825(6) . ? P1 C7 1.824(6) . ? P1 C13 1.841(7) . ? C1 C6 1.384(9) . ? C1 C2 1.408(8) . ? C2 C3 1.379(9) . ? C2 H2A 0.9500 . ? C3 C4 1.386(10) . ? C3 H3A 0.9500 . ? C4 C5 1.388(9) . ? C4 H4A 0.9500 . ? C5 C6 1.386(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.398(9) . ? C7 C8 1.402(9) . ? C8 C9 1.388(9) . ? C8 H8A 0.9500 . ? C9 C10 1.359(12) . ? C9 H9A 0.9500 . ? C10 C11 1.376(12) . ? C10 H10A 0.9500 . ? C11 C12 1.391(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.377(9) . ? C13 C18 1.395(9) . ? C14 C15 1.397(9) . ? C14 H14A 0.9500 . ? C15 C16 1.374(10) . ? C15 H15A 0.9500 . ? C16 C17 1.356(10) . ? C16 H16A 0.9500 . ? C17 C18 1.394(10) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.383(9) . ? C19 C22 1.510(9) . ? C20 C21 1.351(9) . ? C20 H20A 0.9500 . ? C21 C23 1.496(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.397(8) . ? C24 C27 1.487(8) . ? C25 C26 1.377(9) . ? C25 H25A 0.9500 . ? C26 C28 1.510(8) . ? 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 C30 1.378(9) . ? C29 C32 1.502(8) . ? C30 C31 1.397(8) . ? C30 H30A 0.9500 . ? C31 C33 1.483(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 C34 Rh1 N4 92.4(2) . . ? C34 Rh1 N6 174.0(2) . . ? N4 Rh1 N6 83.65(18) . . ? C34 Rh1 P1 85.99(19) . . ? N4 Rh1 P1 175.21(13) . . ? N6 Rh1 P1 98.28(14) . . ? C34 Rh1 N2 112.8(2) . . ? N4 Rh1 N2 70.30(16) . . ? N6 Rh1 N2 70.11(16) . . ? P1 Rh1 N2 106.16(10) . . ? C34 Rh1 B1 128.3(2) . . ? N4 Rh1 B1 52.66(17) . . ? N6 Rh1 B1 52.02(18) . . ? P1 Rh1 B1 125.41(13) . . ? N2 Rh1 B1 28.04(15) . . ? C19 N1 N2 105.4(5) . . ? C21 N2 N1 109.1(5) . . ? C21 N2 B1 130.6(5) . . ? N1 N2 B1 118.8(5) . . ? C21 N2 Rh1 109.2(3) . . ? N1 N2 Rh1 95.2(3) . . ? B1 N2 Rh1 78.8(3) . . ? C26 N3 N4 109.4(5) . . ? C26 N3 B1 129.8(5) . . ? N4 N3 B1 120.8(4) . . ? C24 N4 N3 107.2(4) . . ? C24 N4 Rh1 135.0(4) . . ? N3 N4 Rh1 117.8(4) . . ? C29 N5 N6 109.0(5) . . ? C29 N5 B1 130.4(5) . . ? N6 N5 B1 120.2(5) . . ? C31 N6 N5 107.3(5) . . ? C31 N6 Rh1 134.8(4) . . ? N5 N6 Rh1 117.9(4) . . ? N5 B1 N2 109.3(5) . . ? N5 B1 N3 107.7(5) . . ? N2 B1 N3 111.1(5) . . ? N5 B1 Rh1 69.3(3) . . ? N2 B1 Rh1 73.2(3) . . ? N3 B1 Rh1 68.7(3) . . ? N5 B1 H1 109.6 . . ? N2 B1 H1 109.6 . . ? N3 B1 H1 109.6 . . ? Rh1 B1 H1 177.2 . . ? C1 P1 C7 102.9(3) . . ? C1 P1 C13 102.7(3) . . ? C7 P1 C13 102.2(3) . . ? C1 P1 Rh1 118.13(19) . . ? C7 P1 Rh1 114.3(2) . . ? C13 P1 Rh1 114.7(2) . . ? C6 C1 C2 119.8(6) . . ? C6 C1 P1 121.8(5) . . ? C2 C1 P1 118.4(5) . . ? C3 C2 C1 118.8(6) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 121.4(6) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 119.7(6) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C1 C6 C5 120.7(6) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C12 C7 C8 117.6(6) . . ? C12 C7 P1 122.9(5) . . ? C8 C7 P1 119.5(5) . . ? C9 C8 C7 120.8(7) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C10 C9 C8 120.5(8) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 120.1(6) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 120.4(7) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.5(7) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? C14 C13 C18 118.8(6) . . ? C14 C13 P1 120.5(5) . . ? C18 C13 P1 120.6(5) . . ? C13 C14 C15 121.4(6) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 119.0(6) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C15 120.2(7) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 121.5(7) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C13 C18 C17 119.1(6) . . ? C13 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? N1 C19 C20 111.2(6) . . ? N1 C19 C22 119.5(6) . . ? C20 C19 C22 129.3(6) . . ? C21 C20 C19 106.5(6) . . ? C21 C20 H20A 126.7 . . ? C19 C20 H20A 126.7 . . ? C20 C21 N2 107.8(5) . . ? C20 C21 C23 130.2(6) . . ? N2 C21 C23 122.0(6) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C25 109.0(5) . . ? N4 C24 C27 122.5(5) . . ? C25 C24 C27 128.4(5) . . ? C26 C25 C24 106.5(5) . . ? C26 C25 H25A 126.7 . . ? C24 C25 H25A 126.7 . . ? N3 C26 C25 107.8(5) . . ? N3 C26 C28 123.2(5) . . ? C25 C26 C28 128.9(6) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 108.1(5) . . ? N5 C29 C32 122.7(6) . . ? C30 C29 C32 129.2(6) . . ? C29 C30 C31 106.2(5) . . ? C29 C30 H30A 126.9 . . ? C31 C30 H30A 126.9 . . ? N6 C31 C30 109.4(5) . . ? N6 C31 C33 122.6(5) . . ? C30 C31 C33 128.0(6) . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O1 C34 Rh1 178.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 B1 N1 N2 -81.9(5) . . . . ? N3 B1 N1 N2 -43.2(6) . . . . ? N5 B1 N1 N2 -152.1(6) . . . . ? B1 N1 N2 C19 -168.8(5) . . . . ? H1 B1 N1 N2 99.3 . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.211 _refine_diff_density_min -1.881 _refine_diff_density_rms 0.138