Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Clarke, Matthew L.' 'Slawin, A.' 'Woollins, Derek' _publ_contact_author_name 'Prof Derek Woollins' _publ_contact_author_address ; Chemistry U of St Andrews Dept of Chemistry University of St Andrews St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email 'JDW3@ST-AND.AC.UK' _publ_section_title ; Highly electron rich alkyl- and dialkyl- N-pyrrolidinyl phosphines: An evaluation of their electronic and structural properties ; data_13 _database_code_CSD 171245 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H52 Cl N2 O P2 Rh' _chemical_formula_sum 'C25 H52 Cl N2 O P2 Rh' _chemical_formula_weight 596.99 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' '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.7010(8) _cell_length_b 15.1617(5) _cell_length_c 24.5230(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.033(2) _cell_angle_gamma 90.00 _cell_volume 8920.5(4) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 108 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .18 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.767656 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22067 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6403 _reflns_number_gt 4491 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.7903P] 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 0.00000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6403 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.732 _refine_ls_shift/su_mean 0.005 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 -0.160820(14) 0.03573(2) 0.501938(14) 0.03747(12) Uani 1 1 d . . . Cl1 Cl -0.08446(6) 0.12227(11) 0.50743(7) 0.0816(5) Uani 1 1 d . . . P1 P -0.17568(5) -0.02638(8) 0.40734(5) 0.0377(3) Uani 1 1 d . . . N1 N -0.21091(15) -0.1220(2) 0.39453(16) 0.0475(10) Uani 1 1 d . . . C2 C -0.1939(2) -0.1922(3) 0.4402(2) 0.0741(16) Uani 1 1 d . . . H2A H -0.1574 -0.2145 0.4477 0.089 Uiso 1 1 calc R . . H2B H -0.1922 -0.1699 0.4781 0.089 Uiso 1 1 calc R . . C3 C -0.2343(3) -0.2600(5) 0.4169(3) 0.137(3) Uani 1 1 d . . . H3A H -0.2629 -0.2523 0.4308 0.165 Uiso 1 1 calc R . . H3B H -0.2171 -0.3173 0.4301 0.165 Uiso 1 1 calc R . . C4 C -0.2587(4) -0.2527(5) 0.3500(3) 0.133(3) Uani 1 1 d . . . H4A H -0.2418 -0.2955 0.3338 0.159 Uiso 1 1 calc R . . H4B H -0.2985 -0.2637 0.3323 0.159 Uiso 1 1 calc R . . C5 C -0.2478(2) -0.1630(3) 0.3358(2) 0.0694(16) Uani 1 1 d . . . H5A H -0.2823 -0.1301 0.3161 0.083 Uiso 1 1 calc R . . H5B H -0.2297 -0.1644 0.3091 0.083 Uiso 1 1 calc R . . C6 C -0.2235(2) 0.0509(3) 0.34623(19) 0.0495(12) Uani 1 1 d . . . C7 C -0.2003(2) 0.1440(3) 0.3621(2) 0.0723(16) Uani 1 1 d . . . H7A H -0.1939 0.1577 0.4029 0.108 Uiso 1 1 calc R . . H7B H -0.2267 0.1851 0.3346 0.108 Uiso 1 1 calc R . . H7C H -0.1659 0.1480 0.3588 0.108 Uiso 1 1 calc R . . C8 C -0.2799(2) 0.0499(4) 0.3485(2) 0.0696(16) Uani 1 1 d . . . H8A H -0.2960 -0.0079 0.3382 0.104 Uiso 1 1 calc R . . H8B H -0.3044 0.0921 0.3201 0.104 Uiso 1 1 calc R . . H8C H -0.2747 0.0649 0.3887 0.104 Uiso 1 1 calc R . . C9 C -0.2328(2) 0.0305(4) 0.2809(2) 0.0768(17) Uani 1 1 d . . . H9A H -0.2478 -0.0279 0.2699 0.115 Uiso 1 1 calc R . . H9B H -0.1979 0.0343 0.2785 0.115 Uiso 1 1 calc R . . H9C H -0.2585 0.0725 0.2535 0.115 Uiso 1 1 calc R . . C10 C -0.1105(2) -0.0544(3) 0.3971(2) 0.0538(13) Uani 1 1 d . . . C11 C -0.0846(2) 0.0260(4) 0.3814(3) 0.0792(18) Uani 1 1 d . . . H11A H -0.0765 0.0704 0.4120 0.119 Uiso 1 1 calc R . . H11B H -0.1102 0.0492 0.3428 0.119 Uiso 1 1 calc R . . H11C H -0.0507 0.0088 0.3797 0.119 Uiso 1 1 calc R . . C12 C -0.0688(2) -0.0919(4) 0.4582(2) 0.0763(17) Uani 1 1 d . . . H12A H -0.0608 -0.0483 0.4893 0.115 Uiso 1 1 calc R . . H12B H -0.0350 -0.1079 0.4559 0.115 Uiso 1 1 calc R . . H12C H -0.0845 -0.1432 0.4678 0.115 Uiso 1 1 calc R . . C13 C -0.1219(2) -0.1244(3) 0.3483(2) 0.0741(17) Uani 1 1 d . . . H13A H -0.1381 -0.1755 0.3575 0.111 Uiso 1 1 calc R . . H13B H -0.0876 -0.1406 0.3473 0.111 Uiso 1 1 calc R . . H13C H -0.1473 -0.1013 0.3095 0.111 Uiso 1 1 calc R . . P2 P -0.14812(4) 0.08163(7) 0.59976(5) 0.0362(3) Uani 1 1 d . . . N21 N -0.20982(14) 0.0862(3) 0.60292(14) 0.0471(10) Uani 1 1 d . . . C22 C -0.2232(2) 0.0689(4) 0.6539(2) 0.0707(17) Uani 1 1 d . . . H22A H -0.2078 0.1145 0.6846 0.085 Uiso 1 1 calc R . . H22B H -0.2086 0.0122 0.6723 0.085 Uiso 1 1 calc R . . C23 C -0.2847(2) 0.0695(6) 0.6269(3) 0.114(3) Uani 1 1 d . . . H23A H -0.2983 0.0103 0.6272 0.137 Uiso 1 1 calc R . . H23B H -0.2971 0.1074 0.6503 0.137 Uiso 1 1 calc R . . C24 C -0.3064(2) 0.1015(4) 0.5648(2) 0.0800(18) Uani 1 1 d . . . H24A H -0.3330 0.1487 0.5580 0.096 Uiso 1 1 calc R . . H24B H -0.3247 0.0543 0.5362 0.096 Uiso 1 1 calc R . . C25 C -0.25720(19) 0.1344(4) 0.5574(2) 0.0660(15) Uani 1 1 d . . . H25A H -0.2612 0.1222 0.5169 0.079 Uiso 1 1 calc R . . H25B H -0.2526 0.1975 0.5646 0.079 Uiso 1 1 calc R . . C26 C -0.10688(17) -0.0092(3) 0.65329(19) 0.0427(11) Uani 1 1 d . . . C27 C -0.1428(2) -0.0932(3) 0.6362(2) 0.0676(15) Uani 1 1 d . . . H27A H -0.1561 -0.1046 0.5936 0.101 Uiso 1 1 calc R . . H27B H -0.1740 -0.0852 0.6453 0.101 Uiso 1 1 calc R . . H27C H -0.1208 -0.1422 0.6590 0.101 Uiso 1 1 calc R . . C28 C -0.05642(19) -0.0277(4) 0.6407(2) 0.0647(14) Uani 1 1 d . . . H28A H -0.0689 -0.0395 0.5983 0.097 Uiso 1 1 calc R . . H28B H -0.0365 -0.0780 0.6639 0.097 Uiso 1 1 calc R . . H28C H -0.0322 0.0227 0.6521 0.097 Uiso 1 1 calc R . . C29 C -0.0859(2) 0.0086(4) 0.7208(2) 0.0635(14) Uani 1 1 d . . . H29A H -0.1170 0.0202 0.7296 0.095 Uiso 1 1 calc R . . H29B H -0.0615 0.0589 0.7321 0.095 Uiso 1 1 calc R . . H29C H -0.0659 -0.0420 0.7435 0.095 Uiso 1 1 calc R . . C30 C -0.1147(2) 0.1922(3) 0.6299(2) 0.0547(13) Uani 1 1 d . . . C31 C -0.0510(2) 0.1945(4) 0.6523(2) 0.0759(17) Uani 1 1 d . . . H31A H -0.0338 0.1535 0.6851 0.114 Uiso 1 1 calc R . . H31B H -0.0375 0.2529 0.6660 0.114 Uiso 1 1 calc R . . H31C H -0.0422 0.1785 0.6196 0.114 Uiso 1 1 calc R . . C32 C -0.1273(3) 0.2243(4) 0.6823(2) 0.0858(19) Uani 1 1 d . . . H32A H -0.1105 0.1848 0.7161 0.129 Uiso 1 1 calc R . . H32B H -0.1668 0.2256 0.6690 0.129 Uiso 1 1 calc R . . H32C H -0.1123 0.2825 0.6944 0.129 Uiso 1 1 calc R . . C33 C -0.1417(2) 0.2587(3) 0.5774(3) 0.0793(17) Uani 1 1 d . . . H33A H -0.1814 0.2581 0.5632 0.119 Uiso 1 1 calc R . . H33B H -0.1329 0.2426 0.5448 0.119 Uiso 1 1 calc R . . H33C H -0.1277 0.3168 0.5915 0.119 Uiso 1 1 calc R . . C34 C -0.2214(2) -0.0228(3) 0.49581(19) 0.0489(12) Uani 1 1 d . . . O34 O -0.25931(14) -0.0577(2) 0.49222(14) 0.0667(10) Uani 1 1 d . . . Rh2 Rh 0.0000 0.59711(3) 0.7500 0.03621(15) Uani 1 2 d S . . Cl2 Cl 0.0000 0.75380(11) 0.7500 0.0703(6) Uani 1 2 d S . . P3 P 0.00212(5) 0.58996(7) 0.65424(5) 0.0368(3) Uani 1 1 d . . . N41 N 0.03054(15) 0.4938(2) 0.64667(15) 0.0472(10) Uani 1 1 d . . . C42 C 0.0847(2) 0.4644(4) 0.6927(2) 0.0677(15) Uani 1 1 d . . . H42A H 0.0870 0.4704 0.7331 0.081 Uiso 1 1 calc R . . H42B H 0.1146 0.4982 0.6905 0.081 Uiso 1 1 calc R . . C43 C 0.0879(3) 0.3702(4) 0.6777(2) 0.095(2) Uani 1 1 d . . . H43A H 0.1263 0.3514 0.6922 0.114 Uiso 1 1 calc R . . H43B H 0.0696 0.3328 0.6956 0.114 Uiso 1 1 calc R . . C44 C 0.0588(3) 0.3665(4) 0.6110(3) 0.109(3) Uani 1 1 d . . . H44A H 0.0393 0.3108 0.5978 0.131 Uiso 1 1 calc R . . H44B H 0.0852 0.3723 0.5939 0.131 Uiso 1 1 calc R . . C45 C 0.0180(2) 0.4418(3) 0.5909(2) 0.0681(16) Uani 1 1 d . . . H45A H 0.0230 0.4775 0.5608 0.082 Uiso 1 1 calc R . . H45B H -0.0200 0.4201 0.5735 0.082 Uiso 1 1 calc R . . C46 C -0.07291(18) 0.5857(3) 0.59570(19) 0.0461(12) Uani 1 1 d . . . C47 C -0.0976(2) 0.4996(3) 0.6063(2) 0.0648(15) Uani 1 1 d . . . H47A H -0.0907 0.4960 0.6481 0.097 Uiso 1 1 calc R . . H47B H -0.0805 0.4503 0.5965 0.097 Uiso 1 1 calc R . . H47C H -0.1371 0.4986 0.5809 0.097 Uiso 1 1 calc R . . C48 C -0.0835(2) 0.5917(4) 0.52923(19) 0.0669(15) Uani 1 1 d . . . H48A H -0.0641 0.5448 0.5203 0.100 Uiso 1 1 calc R . . H48B H -0.0703 0.6475 0.5222 0.100 Uiso 1 1 calc R . . H48C H -0.1228 0.5867 0.5035 0.100 Uiso 1 1 calc R . . C49 C -0.1041(2) 0.6616(4) 0.6090(2) 0.0684(15) Uani 1 1 d . . . H49A H -0.0977 0.6588 0.6506 0.103 Uiso 1 1 calc R . . H49B H -0.1433 0.6565 0.5831 0.103 Uiso 1 1 calc R . . H49C H -0.0907 0.7170 0.6016 0.103 Uiso 1 1 calc R . . C50 C 0.0416(2) 0.6786(3) 0.6341(2) 0.0594(14) Uani 1 1 d . . . C51 C 0.0579(2) 0.6478(4) 0.5843(3) 0.0841(18) Uani 1 1 d . . . H51A H 0.0248 0.6379 0.5473 0.126 Uiso 1 1 calc R . . H51B H 0.0788 0.5940 0.5968 0.126 Uiso 1 1 calc R . . H51C H 0.0802 0.6923 0.5777 0.126 Uiso 1 1 calc R . . C52 C 0.0950(2) 0.6965(4) 0.6925(3) 0.091(2) Uani 1 1 d . . . H52A H 0.0853 0.7168 0.7237 0.136 Uiso 1 1 calc R . . H52B H 0.1168 0.7407 0.6848 0.136 Uiso 1 1 calc R . . H52C H 0.1163 0.6431 0.7056 0.136 Uiso 1 1 calc R . . C53 C 0.0091(2) 0.7657(3) 0.6137(3) 0.0790(17) Uani 1 1 d . . . H53A H -0.0010 0.7861 0.6446 0.119 Uiso 1 1 calc R . . H53B H -0.0240 0.7562 0.5767 0.119 Uiso 1 1 calc R . . H53C H 0.0320 0.8092 0.6070 0.119 Uiso 1 1 calc R . . C54 C 0.0000 0.4791(5) 0.7500 0.0483(17) Uani 1 2 d S . . O54 O 0.0000 0.4030(3) 0.7500 0.0739(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 0.0346(2) 0.0485(2) 0.03156(19) -0.00463(17) 0.01662(15) -0.00601(17) Cl1 0.0760(10) 0.1085(12) 0.0780(9) -0.0356(9) 0.0501(8) -0.0463(9) P1 0.0424(7) 0.0418(7) 0.0328(6) -0.0014(5) 0.0201(5) -0.0027(6) N1 0.056(2) 0.044(2) 0.039(2) -0.0022(19) 0.0184(19) -0.0090(19) C2 0.099(5) 0.051(3) 0.071(4) 0.008(3) 0.036(3) -0.005(3) C3 0.161(8) 0.083(5) 0.119(7) 0.024(5) 0.016(6) -0.059(5) C4 0.182(8) 0.092(5) 0.087(5) -0.009(4) 0.025(5) -0.075(5) C5 0.083(4) 0.063(4) 0.050(3) -0.014(3) 0.018(3) -0.024(3) C6 0.059(3) 0.052(3) 0.035(3) 0.000(2) 0.020(2) 0.006(2) C7 0.102(4) 0.049(3) 0.070(4) 0.006(3) 0.041(3) 0.006(3) C8 0.065(4) 0.079(4) 0.053(3) 0.010(3) 0.015(3) 0.019(3) C9 0.110(5) 0.079(4) 0.038(3) 0.005(3) 0.028(3) 0.013(4) C10 0.059(3) 0.058(3) 0.058(3) -0.009(3) 0.038(3) -0.002(3) C11 0.080(4) 0.093(5) 0.098(4) -0.017(4) 0.070(4) -0.024(3) C12 0.050(3) 0.106(5) 0.074(4) 0.005(4) 0.028(3) 0.016(3) C13 0.094(4) 0.071(4) 0.088(4) -0.010(3) 0.067(4) 0.005(3) P2 0.0348(6) 0.0425(7) 0.0292(6) -0.0007(5) 0.0122(5) 0.0016(5) N21 0.036(2) 0.074(3) 0.031(2) 0.0039(19) 0.0146(17) 0.009(2) C22 0.062(4) 0.120(5) 0.039(3) 0.004(3) 0.031(3) 0.012(3) C23 0.050(4) 0.216(9) 0.084(5) 0.053(5) 0.035(3) 0.014(4) C24 0.043(3) 0.124(5) 0.071(4) 0.011(4) 0.024(3) 0.015(3) C25 0.052(3) 0.100(4) 0.044(3) 0.017(3) 0.020(3) 0.028(3) C26 0.035(3) 0.050(3) 0.038(3) 0.006(2) 0.011(2) 0.003(2) C27 0.069(4) 0.050(3) 0.066(3) 0.013(3) 0.013(3) 0.001(3) C28 0.052(3) 0.075(4) 0.062(3) 0.003(3) 0.020(3) 0.018(3) C29 0.053(3) 0.088(4) 0.038(3) 0.007(3) 0.011(2) 0.011(3) C30 0.062(3) 0.049(3) 0.048(3) -0.013(2) 0.019(3) -0.008(3) C31 0.082(4) 0.066(4) 0.066(4) -0.016(3) 0.021(3) -0.035(3) C32 0.118(5) 0.070(4) 0.069(4) -0.029(3) 0.041(4) 0.000(4) C33 0.104(5) 0.042(3) 0.085(4) 0.001(3) 0.036(4) -0.001(3) C34 0.056(3) 0.063(3) 0.029(2) -0.005(2) 0.020(2) 0.000(3) O34 0.050(2) 0.099(3) 0.053(2) -0.0084(19) 0.0242(18) -0.028(2) Rh2 0.0441(3) 0.0331(3) 0.0326(3) 0.000 0.0178(2) 0.000 Cl2 0.1133(17) 0.0375(10) 0.0608(11) 0.000 0.0387(12) 0.000 P3 0.0374(6) 0.0398(7) 0.0351(6) 0.0042(5) 0.0176(5) 0.0014(6) N41 0.055(3) 0.050(2) 0.037(2) 0.0028(18) 0.021(2) 0.0144(19) C42 0.066(4) 0.080(4) 0.054(3) 0.011(3) 0.024(3) 0.026(3) C43 0.117(5) 0.097(5) 0.065(4) 0.010(4) 0.034(4) 0.058(4) C44 0.172(7) 0.090(5) 0.062(4) 0.011(4) 0.047(4) 0.075(5) C45 0.096(4) 0.070(4) 0.043(3) -0.001(3) 0.035(3) 0.026(3) C46 0.042(3) 0.052(3) 0.040(3) -0.002(2) 0.014(2) 0.002(2) C47 0.047(3) 0.077(4) 0.062(3) -0.003(3) 0.016(3) -0.015(3) C48 0.074(4) 0.080(4) 0.033(3) 0.005(3) 0.011(3) 0.010(3) C49 0.046(3) 0.085(4) 0.062(3) -0.004(3) 0.014(3) 0.014(3) C50 0.063(3) 0.060(3) 0.062(3) 0.006(3) 0.034(3) -0.008(3) C51 0.090(4) 0.100(5) 0.091(4) 0.013(4) 0.066(4) -0.011(4) C52 0.066(4) 0.098(5) 0.105(5) 0.004(4) 0.036(4) -0.036(4) C53 0.104(5) 0.056(4) 0.085(4) 0.021(3) 0.049(4) -0.010(3) C54 0.071(5) 0.042(5) 0.036(4) 0.000 0.027(3) 0.000 O54 0.128(5) 0.037(3) 0.070(3) 0.000 0.056(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C34 1.793(5) . ? Rh1 P1 2.3702(11) . ? Rh1 P2 2.3749(11) . ? Rh1 Cl1 2.3782(13) . ? P1 N1 1.681(4) . ? P1 C6 1.889(5) . ? P1 C10 1.912(5) . ? N1 C2 1.465(6) . ? N1 C5 1.479(5) . ? C2 C3 1.417(7) . ? C3 C4 1.480(9) . ? C4 C5 1.464(8) . ? C6 C7 1.522(6) . ? C6 C8 1.533(6) . ? C6 C9 1.541(6) . ? C10 C12 1.532(7) . ? C10 C13 1.527(6) . ? C10 C11 1.531(7) . ? P2 N21 1.684(3) . ? P2 C26 1.887(4) . ? P2 C30 1.891(5) . ? N21 C25 1.463(5) . ? N21 C22 1.468(5) . ? C22 C23 1.475(7) . ? C23 C24 1.455(7) . ? C24 C25 1.488(7) . ? C26 C29 1.522(6) . ? C26 C27 1.538(6) . ? C26 C28 1.534(6) . ? C30 C33 1.542(7) . ? C30 C31 1.540(7) . ? C30 C32 1.543(6) . ? C34 O34 1.111(5) . ? Rh2 C54 1.789(7) . ? Rh2 P3 2.3761(10) 2_556 ? Rh2 P3 2.3762(10) . ? Rh2 Cl2 2.3757(18) . ? P3 N41 1.691(4) . ? P3 C46 1.885(4) . ? P3 C50 1.903(5) . ? N41 C42 1.460(6) . ? N41 C45 1.485(5) . ? C42 C43 1.487(7) . ? C43 C44 1.471(7) . ? C44 C45 1.502(7) . ? C46 C48 1.530(6) . ? C46 C47 1.536(6) . ? C46 C49 1.537(6) . ? C50 C53 1.538(7) . ? C50 C51 1.538(7) . ? C50 C52 1.539(7) . ? C54 O54 1.154(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 P1 87.94(14) . . ? C34 Rh1 P2 87.32(13) . . ? P1 Rh1 P2 173.43(4) . . ? C34 Rh1 Cl1 175.98(16) . . ? P1 Rh1 Cl1 92.62(4) . . ? P2 Rh1 Cl1 92.43(4) . . ? N1 P1 C6 105.0(2) . . ? N1 P1 C10 104.5(2) . . ? C6 P1 C10 111.7(2) . . ? N1 P1 Rh1 111.41(13) . . ? C6 P1 Rh1 107.14(14) . . ? C10 P1 Rh1 116.48(15) . . ? C2 N1 C5 106.8(4) . . ? C2 N1 P1 121.6(3) . . ? C5 N1 P1 128.6(3) . . ? C3 C2 N1 107.0(5) . . ? C2 C3 C4 106.2(6) . . ? C5 C4 C3 107.2(5) . . ? C4 C5 N1 106.0(4) . . ? C7 C6 C8 107.2(4) . . ? C7 C6 C9 108.3(4) . . ? C8 C6 C9 108.9(4) . . ? C7 C6 P1 108.4(3) . . ? C8 C6 P1 107.3(3) . . ? C9 C6 P1 116.4(3) . . ? C12 C10 C13 108.5(4) . . ? C12 C10 C11 109.1(4) . . ? C13 C10 C11 108.3(4) . . ? C12 C10 P1 105.4(3) . . ? C13 C10 P1 112.2(3) . . ? C11 C10 P1 113.2(3) . . ? N21 P2 C26 106.38(19) . . ? N21 P2 C30 104.4(2) . . ? C26 P2 C30 110.1(2) . . ? N21 P2 Rh1 110.46(12) . . ? C26 P2 Rh1 105.65(14) . . ? C30 P2 Rh1 119.21(15) . . ? C25 N21 C22 106.7(3) . . ? C25 N21 P2 121.4(3) . . ? C22 N21 P2 129.9(3) . . ? N21 C22 C23 104.8(4) . . ? C24 C23 C22 109.1(4) . . ? C23 C24 C25 105.7(4) . . ? N21 C25 C24 104.7(4) . . ? C29 C26 C27 109.4(4) . . ? C29 C26 C28 108.3(4) . . ? C27 C26 C28 106.9(4) . . ? C29 C26 P2 116.8(3) . . ? C27 C26 P2 108.1(3) . . ? C28 C26 P2 106.8(3) . . ? C33 C30 C31 108.8(4) . . ? C33 C30 C32 107.3(4) . . ? C31 C30 C32 107.8(4) . . ? C33 C30 P2 106.6(3) . . ? C31 C30 P2 114.6(3) . . ? C32 C30 P2 111.5(4) . . ? O34 C34 Rh1 178.8(5) . . ? C54 Rh2 P3 87.39(3) . 2_556 ? C54 Rh2 P3 87.39(3) . . ? P3 Rh2 P3 174.77(6) 2_556 . ? C54 Rh2 Cl2 180.000(1) . . ? P3 Rh2 Cl2 92.61(3) 2_556 . ? P3 Rh2 Cl2 92.61(3) . . ? N41 P3 C46 105.4(2) . . ? N41 P3 C50 104.7(2) . . ? C46 P3 C50 110.6(2) . . ? N41 P3 Rh2 110.75(13) . . ? C46 P3 Rh2 106.01(14) . . ? C50 P3 Rh2 118.71(16) . . ? C42 N41 C45 107.2(4) . . ? C42 N41 P3 121.2(3) . . ? C45 N41 P3 129.0(3) . . ? N41 C42 C43 104.3(4) . . ? C44 C43 C42 104.6(5) . . ? C43 C44 C45 106.8(5) . . ? N41 C45 C44 105.3(4) . . ? C48 C46 C47 109.8(4) . . ? C48 C46 C49 108.5(4) . . ? C47 C46 C49 106.8(4) . . ? C48 C46 P3 116.6(3) . . ? C47 C46 P3 107.0(3) . . ? C49 C46 P3 107.9(3) . . ? C53 C50 C51 108.6(4) . . ? C53 C50 C52 108.2(5) . . ? C51 C50 C52 108.9(4) . . ? C53 C50 P3 113.1(4) . . ? C51 C50 P3 111.9(4) . . ? C52 C50 P3 106.0(3) . . ? O54 C54 Rh2 180.000(1) . . ? 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 C34 Rh1 P1 N1 -25.5(2) . . . . ? P2 Rh1 P1 N1 18.4(4) . . . . ? Cl1 Rh1 P1 N1 158.50(15) . . . . ? C34 Rh1 P1 C6 88.8(2) . . . . ? P2 Rh1 P1 C6 132.7(4) . . . . ? Cl1 Rh1 P1 C6 -87.18(17) . . . . ? C34 Rh1 P1 C10 -145.2(2) . . . . ? P2 Rh1 P1 C10 -101.4(4) . . . . ? Cl1 Rh1 P1 C10 38.73(18) . . . . ? C6 P1 N1 C2 -165.3(4) . . . . ? C10 P1 N1 C2 76.9(4) . . . . ? Rh1 P1 N1 C2 -49.7(4) . . . . ? C6 P1 N1 C5 37.0(5) . . . . ? C10 P1 N1 C5 -80.7(5) . . . . ? Rh1 P1 N1 C5 152.7(4) . . . . ? C5 N1 C2 C3 -22.3(7) . . . . ? P1 N1 C2 C3 175.8(5) . . . . ? N1 C2 C3 C4 26.5(9) . . . . ? C2 C3 C4 C5 -20.9(10) . . . . ? C3 C4 C5 N1 7.0(9) . . . . ? C2 N1 C5 C4 8.9(7) . . . . ? P1 N1 C5 C4 169.1(5) . . . . ? N1 P1 C6 C7 168.2(3) . . . . ? C10 P1 C6 C7 -79.0(4) . . . . ? Rh1 P1 C6 C7 49.7(3) . . . . ? N1 P1 C6 C8 52.8(4) . . . . ? C10 P1 C6 C8 165.6(3) . . . . ? Rh1 P1 C6 C8 -65.7(3) . . . . ? N1 P1 C6 C9 -69.4(4) . . . . ? C10 P1 C6 C9 43.3(4) . . . . ? Rh1 P1 C6 C9 172.0(3) . . . . ? N1 P1 C10 C12 -84.0(4) . . . . ? C6 P1 C10 C12 163.0(3) . . . . ? Rh1 P1 C10 C12 39.4(4) . . . . ? N1 P1 C10 C13 33.9(4) . . . . ? C6 P1 C10 C13 -79.1(4) . . . . ? Rh1 P1 C10 C13 157.3(3) . . . . ? N1 P1 C10 C11 156.9(3) . . . . ? C6 P1 C10 C11 43.8(4) . . . . ? Rh1 P1 C10 C11 -79.7(4) . . . . ? C34 Rh1 P2 N21 -28.3(2) . . . . ? P1 Rh1 P2 N21 -72.2(4) . . . . ? Cl1 Rh1 P2 N21 147.71(16) . . . . ? C34 Rh1 P2 C26 86.4(2) . . . . ? P1 Rh1 P2 C26 42.5(4) . . . . ? Cl1 Rh1 P2 C26 -97.63(15) . . . . ? C34 Rh1 P2 C30 -149.1(2) . . . . ? P1 Rh1 P2 C30 167.0(4) . . . . ? Cl1 Rh1 P2 C30 26.85(19) . . . . ? C26 P2 N21 C25 -165.6(4) . . . . ? C30 P2 N21 C25 77.9(4) . . . . ? Rh1 P2 N21 C25 -51.4(4) . . . . ? C26 P2 N21 C22 33.0(5) . . . . ? C30 P2 N21 C22 -83.5(5) . . . . ? Rh1 P2 N21 C22 147.2(4) . . . . ? C25 N21 C22 C23 25.3(6) . . . . ? P2 N21 C22 C23 -171.2(5) . . . . ? N21 C22 C23 C24 -9.9(8) . . . . ? C22 C23 C24 C25 -8.9(8) . . . . ? C22 N21 C25 C24 -31.0(6) . . . . ? P2 N21 C25 C24 163.8(4) . . . . ? C23 C24 C25 N21 24.3(7) . . . . ? N21 P2 C26 C29 -70.6(4) . . . . ? C30 P2 C26 C29 42.0(4) . . . . ? Rh1 P2 C26 C29 171.9(3) . . . . ? N21 P2 C26 C27 53.2(4) . . . . ? C30 P2 C26 C27 165.7(3) . . . . ? Rh1 P2 C26 C27 -64.3(3) . . . . ? N21 P2 C26 C28 167.9(3) . . . . ? C30 P2 C26 C28 -79.5(3) . . . . ? Rh1 P2 C26 C28 50.5(3) . . . . ? N21 P2 C30 C33 -79.5(4) . . . . ? C26 P2 C30 C33 166.6(3) . . . . ? Rh1 P2 C30 C33 44.3(4) . . . . ? N21 P2 C30 C31 160.1(3) . . . . ? C26 P2 C30 C31 46.2(4) . . . . ? Rh1 P2 C30 C31 -76.1(4) . . . . ? N21 P2 C30 C32 37.2(4) . . . . ? C26 P2 C30 C32 -76.6(4) . . . . ? Rh1 P2 C30 C32 161.1(3) . . . . ? P1 Rh1 C34 O34 -129(21) . . . . ? P2 Rh1 C34 O34 55(21) . . . . ? Cl1 Rh1 C34 O34 -31(23) . . . . ? C54 Rh2 P3 N41 -25.09(15) . . . . ? P3 Rh2 P3 N41 -25.10(15) 2_556 . . . ? Cl2 Rh2 P3 N41 154.91(15) . . . . ? C54 Rh2 P3 C46 88.72(15) . . . . ? P3 Rh2 P3 C46 88.72(16) 2_556 . . . ? Cl2 Rh2 P3 C46 -91.28(15) . . . . ? C54 Rh2 P3 C50 -146.27(19) . . . . ? P3 Rh2 P3 C50 -146.28(19) 2_556 . . . ? Cl2 Rh2 P3 C50 33.73(19) . . . . ? C46 P3 N41 C42 -166.6(4) . . . . ? C50 P3 N41 C42 76.7(4) . . . . ? Rh2 P3 N41 C42 -52.4(4) . . . . ? C46 P3 N41 C45 34.1(5) . . . . ? C50 P3 N41 C45 -82.6(4) . . . . ? Rh2 P3 N41 C45 148.3(4) . . . . ? C45 N41 C42 C43 -30.6(5) . . . . ? P3 N41 C42 C43 166.1(4) . . . . ? N41 C42 C43 C44 34.8(6) . . . . ? C42 C43 C44 C45 -26.0(8) . . . . ? C42 N41 C45 C44 14.5(6) . . . . ? P3 N41 C45 C44 176.0(4) . . . . ? C43 C44 C45 N41 7.4(7) . . . . ? N41 P3 C46 C48 -69.5(4) . . . . ? C50 P3 C46 C48 43.2(4) . . . . ? Rh2 P3 C46 C48 173.1(3) . . . . ? N41 P3 C46 C47 53.7(3) . . . . ? C50 P3 C46 C47 166.4(3) . . . . ? Rh2 P3 C46 C47 -63.7(3) . . . . ? N41 P3 C46 C49 168.3(3) . . . . ? C50 P3 C46 C49 -79.1(4) . . . . ? Rh2 P3 C46 C49 50.8(3) . . . . ? N41 P3 C50 C53 157.3(4) . . . . ? C46 P3 C50 C53 44.3(4) . . . . ? Rh2 P3 C50 C53 -78.5(4) . . . . ? N41 P3 C50 C51 34.3(4) . . . . ? C46 P3 C50 C51 -78.7(4) . . . . ? Rh2 P3 C50 C51 158.5(3) . . . . ? N41 P3 C50 C52 -84.2(4) . . . . ? C46 P3 C50 C52 162.7(4) . . . . ? Rh2 P3 C50 C52 39.9(4) . . . . ? P3 Rh2 C54 O54 -117(100) 2_556 . . . ? P3 Rh2 C54 O54 63(100) . . . . ? Cl2 Rh2 C54 O54 0(100) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.340 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.073 data_mcdw16 _database_code_CSD 171246 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H66 Cl O P2 Rh' _chemical_formula_sum 'C37 H66 Cl O P2 Rh' _chemical_formula_weight 727.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.95740(10) _cell_length_b 10.25750(10) _cell_length_c 10.81250(10) _cell_angle_alpha 113.7820(10) _cell_angle_beta 109.1770(10) _cell_angle_gamma 90.8190(10) _cell_volume 940.650(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.780727 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5876 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 23.24 _reflns_number_total 4978 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4978 _refine_ls_number_parameters 379 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.038 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 0.64446(14) 0.67290(16) 0.62144(15) 0.03146(8) Uani 1 1 d . . . Cl1 Cl 0.7960(4) 0.7506(5) 0.5202(4) 0.0747(10) Uani 1 1 d . . . P1 P 0.8467(2) 0.7031(2) 0.8255(2) 0.0309(6) Uani 1 1 d . . . C1 C 0.8969(10) 0.5291(10) 0.8170(9) 0.043(3) Uani 1 1 d . . . H1A H 0.9878 0.5529 0.8994 0.052 Uiso 1 1 calc R . . C2 C 0.9312(11) 0.4472(12) 0.6834(13) 0.041(3) Uani 1 1 d . . . H2A H 0.8455 0.4268 0.5985 0.049 Uiso 1 1 calc R . . H2B H 1.0051 0.5084 0.6817 0.049 Uiso 1 1 calc R . . C3 C 0.9816(13) 0.3093(13) 0.6733(14) 0.052(3) Uani 1 1 d . . . H3A H 1.0731 0.3293 0.7521 0.062 Uiso 1 1 calc R . . H3B H 0.9970 0.2610 0.5825 0.062 Uiso 1 1 calc R . . C4 C 0.8717(11) 0.2093(11) 0.6810(13) 0.056(3) Uani 1 1 d . . . H4A H 0.7814 0.1841 0.5995 0.067 Uiso 1 1 calc R . . H4B H 0.9079 0.1210 0.6772 0.067 Uiso 1 1 calc R . . C5 C 0.8475(14) 0.2893(12) 0.8240(14) 0.064(4) Uani 1 1 d . . . H5A H 0.9363 0.3075 0.9053 0.077 Uiso 1 1 calc R . . H5B H 0.7744 0.2302 0.8291 0.077 Uiso 1 1 calc R . . C6 C 0.7982(11) 0.4353(11) 0.8331(12) 0.051(3) Uani 1 1 d . . . H6A H 0.7041 0.4149 0.7579 0.061 Uiso 1 1 calc R . . H6B H 0.7879 0.4869 0.9260 0.061 Uiso 1 1 calc R . . C7 C 0.8112(10) 0.7852(10) 0.9996(8) 0.032(2) Uani 1 1 d . . . H7A H 0.7350 0.7152 0.9884 0.038 Uiso 1 1 calc R . . C8 C 0.9357(11) 0.8056(14) 1.1379(12) 0.044(3) Uani 1 1 d . . . H8A H 0.9780 0.7184 1.1209 0.053 Uiso 1 1 calc R . . H8B H 1.0098 0.8844 1.1636 0.053 Uiso 1 1 calc R . . C9 C 0.8843(10) 0.8376(13) 1.2568(12) 0.053(3) Uani 1 1 d . . . H9A H 0.9643 0.8508 1.3439 0.064 Uiso 1 1 calc R . . H9B H 0.8136 0.7567 1.2329 0.064 Uiso 1 1 calc R . . C10 C 0.8166(12) 0.9733(14) 1.2851(11) 0.058(3) Uani 1 1 d . . . H10A H 0.8895 1.0557 1.3173 0.070 Uiso 1 1 calc R . . H10B H 0.7793 0.9904 1.3617 0.070 Uiso 1 1 calc R . . C11 C 0.6922(13) 0.9580(15) 1.1456(12) 0.059(4) Uani 1 1 d . . . H11A H 0.6562 1.0485 1.1624 0.071 Uiso 1 1 calc R . . H11B H 0.6135 0.8837 1.1199 0.071 Uiso 1 1 calc R . . C12 C 0.7508(12) 0.9164(13) 1.0191(12) 0.055(3) Uani 1 1 d . . . H12A H 0.6729 0.9019 0.9301 0.066 Uiso 1 1 calc R . . H12B H 0.8243 0.9942 1.0418 0.066 Uiso 1 1 calc R . . C13 C 1.0188(10) 0.8024(10) 0.8481(11) 0.039(3) Uani 1 1 d . . . H13A H 1.0225 0.7643 0.7505 0.046 Uiso 1 1 calc R . . C14 C 1.1613(9) 0.7849(12) 0.9430(13) 0.045(3) Uani 1 1 d . . . H14A H 1.1717 0.8339 1.0442 0.055 Uiso 1 1 calc R . . H14B H 1.1634 0.6832 0.9185 0.055 Uiso 1 1 calc R . . C15 C 1.2811(12) 0.8466(15) 0.9206(15) 0.063(3) Uani 1 1 d . . . H15A H 1.2721 0.7949 0.8201 0.076 Uiso 1 1 calc R . . H15B H 1.3720 0.8346 0.9810 0.076 Uiso 1 1 calc R . . C16 C 1.2812(11) 1.0061(16) 0.9581(18) 0.073(4) Uani 1 1 d . . . H16A H 1.3030 1.0587 1.0616 0.088 Uiso 1 1 calc R . . H16B H 1.3575 1.0413 0.9363 0.088 Uiso 1 1 calc R . . C17 C 1.1399(13) 1.0386(14) 0.8776(15) 0.080(4) Uani 1 1 d . . . H17A H 1.1415 1.1422 0.9170 0.095 Uiso 1 1 calc R . . H17B H 1.1260 1.0032 0.7757 0.095 Uiso 1 1 calc R . . C18 C 1.0180(11) 0.9657(12) 0.8936(14) 0.046(3) Uani 1 1 d . . . H18A H 0.9269 0.9788 0.8346 0.055 Uiso 1 1 calc R . . H18B H 1.0254 1.0119 0.9941 0.055 Uiso 1 1 calc R . . P2 P 0.44253(18) 0.6437(2) 0.4166(2) 0.0304(7) Uani 1 1 d . . . C19 C 0.3877(9) 0.8207(9) 0.4264(10) 0.031(2) Uani 1 1 d . . . H19A H 0.2966 0.8010 0.3454 0.037 Uiso 1 1 calc R . . C20 C 0.3630(13) 0.9061(13) 0.5714(12) 0.053(3) Uani 1 1 d . . . H20A H 0.4517 0.9258 0.6532 0.064 Uiso 1 1 calc R . . H20B H 0.2898 0.8486 0.5782 0.064 Uiso 1 1 calc R . . C21 C 0.3135(13) 1.0519(13) 0.5764(15) 0.058(3) Uani 1 1 d . . . H21A H 0.2198 1.0318 0.5006 0.069 Uiso 1 1 calc R . . H21B H 0.3045 1.1079 0.6692 0.069 Uiso 1 1 calc R . . C22 C 0.4207(12) 1.1372(11) 0.5554(13) 0.060(3) Uani 1 1 d . . . H22A H 0.5102 1.1681 0.6387 0.071 Uiso 1 1 calc R . . H22B H 0.3843 1.2233 0.5516 0.071 Uiso 1 1 calc R . . C23 C 0.4515(12) 1.0551(12) 0.4208(11) 0.049(3) Uani 1 1 d . . . H23A H 0.5235 1.1158 0.4161 0.058 Uiso 1 1 calc R . . H23B H 0.3641 1.0328 0.3368 0.058 Uiso 1 1 calc R . . C24 C 0.5048(11) 0.9167(12) 0.4142(12) 0.048(3) Uani 1 1 d . . . H24A H 0.5961 0.9377 0.4934 0.057 Uiso 1 1 calc R . . H24B H 0.5192 0.8651 0.3234 0.057 Uiso 1 1 calc R . . C25 C 0.4759(10) 0.5649(10) 0.2485(10) 0.043(3) Uani 1 1 d . . . H25A H 0.5498 0.6379 0.2604 0.051 Uiso 1 1 calc R . . C26 C 0.5494(11) 0.4230(11) 0.2212(12) 0.044(3) Uani 1 1 d . . . H26A H 0.6340 0.4411 0.3064 0.053 Uiso 1 1 calc R . . H26B H 0.4821 0.3441 0.2065 0.053 Uiso 1 1 calc R . . C27 C 0.5924(13) 0.3802(14) 0.0923(14) 0.060(4) Uani 1 1 d . . . H27A H 0.6718 0.4522 0.1148 0.072 Uiso 1 1 calc R . . H27B H 0.6273 0.2890 0.0744 0.072 Uiso 1 1 calc R . . C28 C 0.4770(13) 0.3650(13) -0.0402(12) 0.064(4) Uani 1 1 d . . . H28A H 0.4044 0.2827 -0.0718 0.077 Uiso 1 1 calc R . . H28B H 0.5163 0.3452 -0.1159 0.077 Uiso 1 1 calc R . . C29 C 0.4072(12) 0.4946(14) -0.0227(10) 0.061(3) Uani 1 1 d . . . H29A H 0.3257 0.4737 -0.1113 0.073 Uiso 1 1 calc R . . H29B H 0.4754 0.5734 -0.0071 0.073 Uiso 1 1 calc R . . C30 C 0.3533(13) 0.5434(15) 0.1086(12) 0.050(3) Uani 1 1 d . . . H30A H 0.3163 0.6331 0.1218 0.060 Uiso 1 1 calc R . . H30B H 0.2752 0.4706 0.0872 0.060 Uiso 1 1 calc R . . C31 C 0.2766(9) 0.5398(11) 0.3960(11) 0.035(2) Uani 1 1 d . . . H31A H 0.2766 0.5782 0.4949 0.042 Uiso 1 1 calc R . . C32 C 0.1310(11) 0.5650(13) 0.3083(14) 0.055(3) Uani 1 1 d . . . H32A H 0.1208 0.5288 0.2072 0.067 Uiso 1 1 calc R . . H32B H 0.1283 0.6679 0.3449 0.067 Uiso 1 1 calc R . . C33 C 0.0015(11) 0.4851(14) 0.3204(16) 0.065(4) Uani 1 1 d . . . H33A H 0.0044 0.5316 0.4194 0.078 Uiso 1 1 calc R . . H33B H -0.0890 0.4953 0.2577 0.078 Uiso 1 1 calc R . . C34 C 0.0060(13) 0.3280(15) 0.2794(17) 0.074(4) Uani 1 1 d . . . H34A H -0.0102 0.2777 0.1769 0.088 Uiso 1 1 calc R . . H34B H -0.0695 0.2862 0.2975 0.088 Uiso 1 1 calc R . . C35 C 0.1505(11) 0.3116(12) 0.3676(15) 0.063(4) Uani 1 1 d . . . H35A H 0.1535 0.2092 0.3377 0.076 Uiso 1 1 calc R . . H35B H 0.1599 0.3534 0.4687 0.076 Uiso 1 1 calc R . . C36 C 0.2817(11) 0.3815(13) 0.3564(14) 0.048(3) Uani 1 1 d . . . H36A H 0.3703 0.3710 0.4215 0.058 Uiso 1 1 calc R . . H36B H 0.2805 0.3332 0.2581 0.058 Uiso 1 1 calc R . . C37 C 0.5236(11) 0.6097(11) 0.7010(11) 0.072(4) Uani 1 1 d . . . O37 O 0.4707(11) 0.5870(13) 0.7303(11) 0.092(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02910(14) 0.03900(15) 0.02667(13) 0.01648(10) 0.00782(9) 0.00405(10) Cl1 0.0561(15) 0.100(2) 0.0588(18) 0.0383(16) 0.0055(12) 0.0044(13) P1 0.0370(14) 0.0315(16) 0.0225(16) 0.0120(13) 0.0085(12) 0.0043(12) C1 0.052(6) 0.044(6) 0.018(4) 0.006(4) 0.005(4) -0.002(4) C2 0.039(5) 0.035(6) 0.054(6) 0.022(5) 0.020(4) 0.007(4) C3 0.068(7) 0.042(5) 0.054(6) 0.015(5) 0.040(5) 0.014(4) C4 0.051(6) 0.042(7) 0.059(7) 0.010(6) 0.015(6) 0.018(5) C5 0.074(7) 0.037(7) 0.090(9) 0.043(7) 0.021(6) 0.008(5) C6 0.053(5) 0.045(6) 0.070(7) 0.027(5) 0.039(5) 0.024(4) C7 0.043(5) 0.038(6) 0.012(4) 0.003(4) 0.018(4) 0.004(4) C8 0.038(5) 0.061(8) 0.034(6) 0.023(6) 0.010(5) 0.012(5) C9 0.043(5) 0.059(6) 0.046(6) 0.019(4) 0.008(4) 0.007(4) C10 0.062(7) 0.070(8) 0.039(6) 0.024(6) 0.013(5) -0.006(6) C11 0.066(8) 0.069(8) 0.039(6) 0.011(5) 0.030(6) 0.019(6) C12 0.054(5) 0.065(7) 0.038(6) 0.014(5) 0.018(4) 0.004(5) C13 0.039(5) 0.029(5) 0.042(6) 0.011(4) 0.014(5) -0.008(4) C14 0.023(4) 0.054(7) 0.067(7) 0.039(6) 0.008(4) 0.018(4) C15 0.041(5) 0.062(7) 0.085(8) 0.042(6) 0.007(5) 0.003(4) C16 0.031(6) 0.078(9) 0.122(12) 0.057(8) 0.023(7) -0.002(6) C17 0.059(8) 0.069(8) 0.099(10) 0.033(7) 0.019(7) -0.006(6) C18 0.037(5) 0.042(6) 0.064(7) 0.032(6) 0.012(4) 0.015(4) P2 0.0227(13) 0.0360(17) 0.0322(17) 0.0183(15) 0.0053(12) 0.0035(12) C19 0.024(4) 0.027(5) 0.053(6) 0.029(4) 0.013(4) 0.009(3) C20 0.077(7) 0.045(6) 0.035(5) 0.012(4) 0.026(5) 0.010(5) C21 0.061(6) 0.034(5) 0.061(6) 0.012(4) 0.012(5) 0.012(4) C22 0.080(8) 0.032(6) 0.063(8) 0.028(6) 0.014(6) -0.005(5) C23 0.052(5) 0.053(7) 0.046(6) 0.025(6) 0.020(5) 0.006(5) C24 0.055(5) 0.039(6) 0.053(6) 0.029(5) 0.013(4) -0.009(4) C25 0.034(5) 0.035(6) 0.054(6) 0.028(5) 0.000(4) 0.005(4) C26 0.051(5) 0.038(5) 0.048(6) 0.022(5) 0.019(4) 0.032(4) C27 0.057(7) 0.045(6) 0.069(9) 0.015(6) 0.025(7) 0.010(5) C28 0.070(8) 0.058(7) 0.045(7) -0.008(5) 0.039(7) -0.003(6) C29 0.081(7) 0.081(8) 0.016(4) 0.019(4) 0.014(5) -0.002(6) C30 0.061(7) 0.055(8) 0.031(6) 0.020(6) 0.012(6) 0.014(6) C31 0.023(4) 0.054(6) 0.037(6) 0.032(5) 0.006(4) 0.022(4) C32 0.042(6) 0.055(7) 0.055(6) 0.023(6) 0.001(5) -0.012(5) C33 0.023(4) 0.069(7) 0.111(10) 0.049(7) 0.022(5) 0.011(4) C34 0.056(7) 0.056(7) 0.103(10) 0.038(7) 0.019(7) -0.008(6) C35 0.050(6) 0.053(7) 0.129(10) 0.071(7) 0.041(7) 0.018(5) C36 0.038(5) 0.047(7) 0.061(7) 0.027(6) 0.015(4) -0.005(4) C37 0.044(5) 0.049(4) 0.051(5) -0.003(4) -0.040(4) 0.014(3) O37 0.088(6) 0.139(7) 0.048(4) 0.047(4) 0.013(4) 0.048(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C37 1.928(12) . ? Rh1 P1 2.352(3) . ? Rh1 P2 2.358(3) . ? Rh1 Cl1 2.422(4) . ? P1 C1 1.835(11) . ? P1 C13 1.872(9) . ? P1 C7 1.883(7) . ? C1 C6 1.464(13) . ? C1 C2 1.504(14) . ? C2 C3 1.482(17) . ? C3 C4 1.534(14) . ? C4 C5 1.532(15) . ? C5 C6 1.558(15) . ? C7 C12 1.448(14) . ? C7 C8 1.530(15) . ? C8 C9 1.456(14) . ? C9 C10 1.519(18) . ? C10 C11 1.552(16) . ? C11 C12 1.566(14) . ? C13 C14 1.516(14) . ? C13 C18 1.545(14) . ? C14 C15 1.474(14) . ? C15 C16 1.519(19) . ? C16 C17 1.513(17) . ? C17 C18 1.510(15) . ? P2 C25 1.813(10) . ? P2 C31 1.852(9) . ? P2 C19 1.876(9) . ? C19 C20 1.561(14) . ? C19 C24 1.587(12) . ? C20 C21 1.567(18) . ? C21 C22 1.500(15) . ? C22 C23 1.494(15) . ? C23 C24 1.506(16) . ? C25 C30 1.529(16) . ? C25 C26 1.603(13) . ? C26 C27 1.491(15) . ? C27 C28 1.460(18) . ? C28 C29 1.482(18) . ? C29 C30 1.578(14) . ? C31 C36 1.509(15) . ? C31 C32 1.541(14) . ? C32 C33 1.587(14) . ? C33 C34 1.494(19) . ? C34 C35 1.498(17) . ? C35 C36 1.545(13) . ? C37 O37 0.773(18) . ? 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 C37 Rh1 P1 89.1(3) . . ? C37 Rh1 P2 91.2(3) . . ? P1 Rh1 P2 179.62(12) . . ? C37 Rh1 Cl1 179.6(4) . . ? P1 Rh1 Cl1 91.00(11) . . ? P2 Rh1 Cl1 88.65(11) . . ? C1 P1 C13 102.1(4) . . ? C1 P1 C7 103.4(4) . . ? C13 P1 C7 109.7(5) . . ? C1 P1 Rh1 111.8(3) . . ? C13 P1 Rh1 116.0(3) . . ? C7 P1 Rh1 112.6(3) . . ? C6 C1 C2 110.6(8) . . ? C6 C1 P1 117.1(7) . . ? C2 C1 P1 111.1(7) . . ? C3 C2 C1 114.4(9) . . ? C2 C3 C4 111.3(8) . . ? C5 C4 C3 108.2(9) . . ? C4 C5 C6 109.6(9) . . ? C1 C6 C5 114.2(9) . . ? C12 C7 C8 110.9(9) . . ? C12 C7 P1 112.9(7) . . ? C8 C7 P1 116.4(6) . . ? C9 C8 C7 110.3(8) . . ? C8 C9 C10 110.7(9) . . ? C9 C10 C11 110.7(9) . . ? C10 C11 C12 108.9(9) . . ? C7 C12 C11 109.6(9) . . ? C14 C13 C18 108.0(9) . . ? C14 C13 P1 119.3(6) . . ? C18 C13 P1 113.0(7) . . ? C15 C14 C13 109.7(9) . . ? C14 C15 C16 111.2(10) . . ? C17 C16 C15 113.9(11) . . ? C18 C17 C16 109.1(9) . . ? C17 C18 C13 112.7(9) . . ? C25 P2 C31 109.4(5) . . ? C25 P2 C19 104.1(4) . . ? C31 P2 C19 103.2(4) . . ? C25 P2 Rh1 113.1(3) . . ? C31 P2 Rh1 113.9(3) . . ? C19 P2 Rh1 112.3(3) . . ? C20 C19 C24 109.6(8) . . ? C20 C19 P2 110.2(6) . . ? C24 C19 P2 111.8(6) . . ? C19 C20 C21 109.6(9) . . ? C22 C21 C20 110.4(9) . . ? C21 C22 C23 113.6(9) . . ? C22 C23 C24 113.0(9) . . ? C23 C24 C19 108.3(9) . . ? C30 C25 C26 109.5(9) . . ? C30 C25 P2 117.7(7) . . ? C26 C25 P2 116.0(6) . . ? C27 C26 C25 111.7(8) . . ? C28 C27 C26 114.5(10) . . ? C27 C28 C29 113.6(9) . . ? C28 C29 C30 112.1(9) . . ? C25 C30 C29 110.9(9) . . ? C36 C31 C32 112.4(9) . . ? C36 C31 P2 114.2(6) . . ? C32 C31 P2 117.3(6) . . ? C31 C32 C33 110.4(9) . . ? C34 C33 C32 113.0(9) . . ? C33 C34 C35 109.1(11) . . ? C34 C35 C36 115.5(9) . . ? C31 C36 C35 109.7(9) . . ? O37 C37 Rh1 175.8(17) . . ? 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 C37 Rh1 P1 C1 75.0(5) . . . . ? P2 Rh1 P1 C1 -126(24) . . . . ? Cl1 Rh1 P1 C1 -104.6(4) . . . . ? C37 Rh1 P1 C13 -168.5(5) . . . . ? P2 Rh1 P1 C13 -9(24) . . . . ? Cl1 Rh1 P1 C13 11.9(4) . . . . ? C37 Rh1 P1 C7 -40.9(4) . . . . ? P2 Rh1 P1 C7 118(24) . . . . ? Cl1 Rh1 P1 C7 139.5(3) . . . . ? C13 P1 C1 C6 166.2(8) . . . . ? C7 P1 C1 C6 52.2(8) . . . . ? Rh1 P1 C1 C6 -69.2(8) . . . . ? C13 P1 C1 C2 -65.5(8) . . . . ? C7 P1 C1 C2 -179.4(7) . . . . ? Rh1 P1 C1 C2 59.1(7) . . . . ? C6 C1 C2 C3 -51.8(12) . . . . ? P1 C1 C2 C3 176.4(8) . . . . ? C1 C2 C3 C4 56.3(13) . . . . ? C2 C3 C4 C5 -58.0(13) . . . . ? C3 C4 C5 C6 56.4(12) . . . . ? C2 C1 C6 C5 51.1(13) . . . . ? P1 C1 C6 C5 179.7(8) . . . . ? C4 C5 C6 C1 -55.7(13) . . . . ? C1 P1 C7 C12 -172.3(7) . . . . ? C13 P1 C7 C12 79.4(8) . . . . ? Rh1 P1 C7 C12 -51.5(8) . . . . ? C1 P1 C7 C8 57.8(8) . . . . ? C13 P1 C7 C8 -50.6(9) . . . . ? Rh1 P1 C7 C8 178.6(7) . . . . ? C12 C7 C8 C9 62.3(12) . . . . ? P1 C7 C8 C9 -166.8(8) . . . . ? C7 C8 C9 C10 -58.8(13) . . . . ? C8 C9 C10 C11 56.7(12) . . . . ? C9 C10 C11 C12 -54.1(12) . . . . ? C8 C7 C12 C11 -60.1(11) . . . . ? P1 C7 C12 C11 167.2(8) . . . . ? C10 C11 C12 C7 56.6(13) . . . . ? C1 P1 C13 C14 -38.1(10) . . . . ? C7 P1 C13 C14 71.1(9) . . . . ? Rh1 P1 C13 C14 -159.9(8) . . . . ? C1 P1 C13 C18 -166.7(8) . . . . ? C7 P1 C13 C18 -57.5(9) . . . . ? Rh1 P1 C13 C18 71.6(8) . . . . ? C18 C13 C14 C15 -61.1(12) . . . . ? P1 C13 C14 C15 168.1(8) . . . . ? C13 C14 C15 C16 59.5(14) . . . . ? C14 C15 C16 C17 -54.9(16) . . . . ? C15 C16 C17 C18 50.5(16) . . . . ? C16 C17 C18 C13 -53.4(14) . . . . ? C14 C13 C18 C17 59.4(12) . . . . ? P1 C13 C18 C17 -166.4(8) . . . . ? C37 Rh1 P2 C25 -139.1(5) . . . . ? P1 Rh1 P2 C25 62(24) . . . . ? Cl1 Rh1 P2 C25 40.5(3) . . . . ? C37 Rh1 P2 C31 -13.4(5) . . . . ? P1 Rh1 P2 C31 -172(100) . . . . ? Cl1 Rh1 P2 C31 166.2(4) . . . . ? C37 Rh1 P2 C19 103.5(4) . . . . ? P1 Rh1 P2 C19 -56(24) . . . . ? Cl1 Rh1 P2 C19 -76.9(3) . . . . ? C25 P2 C19 C20 -176.9(7) . . . . ? C31 P2 C19 C20 68.9(7) . . . . ? Rh1 P2 C19 C20 -54.2(7) . . . . ? C25 P2 C19 C24 -54.9(7) . . . . ? C31 P2 C19 C24 -169.1(7) . . . . ? Rh1 P2 C19 C24 67.8(7) . . . . ? C24 C19 C20 C21 58.1(11) . . . . ? P2 C19 C20 C21 -178.6(7) . . . . ? C19 C20 C21 C22 -55.4(13) . . . . ? C20 C21 C22 C23 54.4(14) . . . . ? C21 C22 C23 C24 -56.9(13) . . . . ? C22 C23 C24 C19 57.2(12) . . . . ? C20 C19 C24 C23 -58.5(11) . . . . ? P2 C19 C24 C23 179.2(7) . . . . ? C31 P2 C25 C30 53.0(9) . . . . ? C19 P2 C25 C30 -56.8(9) . . . . ? Rh1 P2 C25 C30 -178.9(7) . . . . ? C31 P2 C25 C26 -79.6(8) . . . . ? C19 P2 C25 C26 170.6(7) . . . . ? Rh1 P2 C25 C26 48.5(8) . . . . ? C30 C25 C26 C27 52.4(12) . . . . ? P2 C25 C26 C27 -171.3(8) . . . . ? C25 C26 C27 C28 -52.7(14) . . . . ? C26 C27 C28 C29 53.8(14) . . . . ? C27 C28 C29 C30 -53.1(13) . . . . ? C26 C25 C30 C29 -52.4(12) . . . . ? P2 C25 C30 C29 172.1(8) . . . . ? C28 C29 C30 C25 54.0(13) . . . . ? C25 P2 C31 C36 58.4(9) . . . . ? C19 P2 C31 C36 168.8(8) . . . . ? Rh1 P2 C31 C36 -69.2(9) . . . . ? C25 P2 C31 C32 -76.2(9) . . . . ? C19 P2 C31 C32 34.1(10) . . . . ? Rh1 P2 C31 C32 156.1(8) . . . . ? C36 C31 C32 C33 52.6(13) . . . . ? P2 C31 C32 C33 -172.0(8) . . . . ? C31 C32 C33 C34 -53.7(15) . . . . ? C32 C33 C34 C35 54.0(16) . . . . ? C33 C34 C35 C36 -56.1(16) . . . . ? C32 C31 C36 C35 -52.8(12) . . . . ? P2 C31 C36 C35 170.4(8) . . . . ? C34 C35 C36 C31 55.7(15) . . . . ? P1 Rh1 C37 O37 147(21) . . . . ? P2 Rh1 C37 O37 -33(21) . . . . ? Cl1 Rh1 C37 O37 -106(50) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.316 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.044 data_16 _database_code_CSD 171247 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C28 H42 Cl2 N4 P2 Pt' _chemical_formula_sum 'C28 H42 Cl2 N4 P2 Pt' _chemical_formula_weight 762.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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 9.80770(10) _cell_length_b 10.4935(3) _cell_length_c 16.7513(5) _cell_angle_alpha 94.161(2) _cell_angle_beta 101.821(2) _cell_angle_gamma 116.6040(10) _cell_volume 1481.95(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 5.048 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.45862 _exptl_absorpt_correction_T_max 0.693217 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6486 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4186 _reflns_number_gt 3384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^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 4186 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 Pt1 Pt 0.98147(4) 0.41667(3) 0.72031(2) 0.03421(13) Uani 1 1 d . . . Cl1 Cl 0.7927(3) 0.4302(3) 0.61427(15) 0.0571(6) Uani 1 1 d . . . Cl2 Cl 0.9524(3) 0.5900(3) 0.80640(15) 0.0569(6) Uani 1 1 d . . . P1 P 0.9882(2) 0.2460(2) 0.63396(13) 0.0317(5) Uani 1 1 d . . . N1 N 1.1723(7) 0.3009(7) 0.6264(4) 0.0392(17) Uani 1 1 d . . . C2 C 1.2253(10) 0.2128(10) 0.5825(6) 0.053(2) Uani 1 1 d . . . H2A H 1.1386 0.1411 0.5374 0.063 Uiso 1 1 calc R . . H2B H 1.2632 0.1628 0.6202 0.063 Uiso 1 1 calc R . . C3 C 1.3552(13) 0.3138(12) 0.5494(9) 0.110(6) Uani 1 1 d . . . H3A H 1.4394 0.2875 0.5562 0.132 Uiso 1 1 calc R . . H3B H 1.3160 0.3111 0.4909 0.132 Uiso 1 1 calc R . . C4 C 1.4127(13) 0.4582(12) 0.5977(8) 0.082(4) Uani 1 1 d . . . H4A H 1.4447 0.5307 0.5630 0.098 Uiso 1 1 calc R . . H4B H 1.5032 0.4811 0.6436 0.098 Uiso 1 1 calc R . . C5 C 1.2777(9) 0.4567(9) 0.6300(6) 0.047(2) Uani 1 1 d . . . H5A H 1.3166 0.5105 0.6865 0.056 Uiso 1 1 calc R . . H5B H 1.2229 0.4985 0.5952 0.056 Uiso 1 1 calc R . . N6 N 0.8787(7) 0.1904(7) 0.5349(4) 0.0358(16) Uani 1 1 d . . . C7 C 0.9240(10) 0.2823(9) 0.4721(5) 0.046(2) Uani 1 1 d . . . H7A H 1.0233 0.2947 0.4629 0.055 Uiso 1 1 calc R . . H7B H 0.9333 0.3770 0.4888 0.055 Uiso 1 1 calc R . . C8 C 0.7888(12) 0.1974(11) 0.3956(6) 0.061(3) Uani 1 1 d . . . H8A H 0.7778 0.2608 0.3584 0.074 Uiso 1 1 calc R . . H8B H 0.8043 0.1240 0.3661 0.074 Uiso 1 1 calc R . . C9 C 0.6481(11) 0.1297(13) 0.4288(6) 0.079(4) Uani 1 1 d . . . H9A H 0.5672 0.0406 0.3916 0.095 Uiso 1 1 calc R . . H9B H 0.6042 0.1952 0.4346 0.095 Uiso 1 1 calc R . . C10 C 0.7032(9) 0.0985(9) 0.5122(5) 0.046(2) Uani 1 1 d . . . H10A H 0.6581 0.1253 0.5527 0.055 Uiso 1 1 calc R . . H10B H 0.6742 -0.0035 0.5085 0.055 Uiso 1 1 calc R . . C11 C 0.9093(8) 0.0772(8) 0.6703(5) 0.0311(18) Uani 1 1 d . . . C12 C 0.8035(10) 0.0529(10) 0.7188(6) 0.052(2) Uani 1 1 d . . . H12A H 0.7779 0.1254 0.7325 0.062 Uiso 1 1 calc R . . C13 C 0.7373(14) -0.0727(13) 0.7464(8) 0.083(4) Uani 1 1 d . . . H13A H 0.6646 -0.0869 0.7773 0.100 Uiso 1 1 calc R . . C14 C 0.7763(13) -0.1787(12) 0.7293(8) 0.074(3) Uani 1 1 d . . . H14A H 0.7372 -0.2616 0.7524 0.089 Uiso 1 1 calc R . . C15 C 0.8701(14) -0.1645(11) 0.6796(7) 0.076(3) Uani 1 1 d . . . H15A H 0.8905 -0.2404 0.6655 0.091 Uiso 1 1 calc R . . C16 C 0.9375(11) -0.0385(9) 0.6488(5) 0.050(2) Uani 1 1 d . . . H16A H 1.0019 -0.0305 0.6136 0.060 Uiso 1 1 calc R . . P2 P 1.1609(2) 0.4233(2) 0.83239(13) 0.0335(5) Uani 1 1 d . . . N16 N 1.0749(8) 0.3512(7) 0.9046(4) 0.0410(17) Uani 1 1 d . . . C17 C 0.9171(10) 0.3229(10) 0.9105(6) 0.050(2) Uani 1 1 d . . . H17A H 0.8411 0.2819 0.8564 0.060 Uiso 1 1 calc R . . H17B H 0.9184 0.4114 0.9330 0.060 Uiso 1 1 calc R . . C18 C 0.8771(13) 0.2157(13) 0.9683(7) 0.086(4) Uani 1 1 d . . . H18A H 0.8527 0.2531 1.0150 0.103 Uiso 1 1 calc R . . H18B H 0.7857 0.1245 0.9394 0.103 Uiso 1 1 calc R . . C19 C 1.0161(15) 0.1933(11) 0.9977(7) 0.078(4) Uani 1 1 d . . . H19A H 1.0011 0.1037 0.9673 0.093 Uiso 1 1 calc R . . H19B H 1.0349 0.1899 1.0564 0.093 Uiso 1 1 calc R . . C20 C 1.1502(11) 0.3211(10) 0.9815(5) 0.052(2) Uani 1 1 d . . . H20A H 1.1954 0.4032 1.0269 0.063 Uiso 1 1 calc R . . H20B H 1.2324 0.2982 0.9734 0.063 Uiso 1 1 calc R . . N21 N 1.3003(8) 0.5953(7) 0.8704(4) 0.0426(18) Uani 1 1 d . . . C22 C 1.4043(11) 0.6439(9) 0.9550(6) 0.053(2) Uani 1 1 d . . . H22A H 1.4573 0.5856 0.9660 0.064 Uiso 1 1 calc R . . H22B H 1.3451 0.6384 0.9956 0.064 Uiso 1 1 calc R . . C23 C 1.5230(14) 0.8010(10) 0.9568(7) 0.079(4) Uani 1 1 d . . . H23A H 1.5541 0.8601 1.0112 0.095 Uiso 1 1 calc R . . H23B H 1.6168 0.8068 0.9432 0.095 Uiso 1 1 calc R . . C24 C 1.4370(12) 0.8487(10) 0.8933(6) 0.060(3) Uani 1 1 d . . . H24A H 1.5102 0.9286 0.8727 0.073 Uiso 1 1 calc R . . H24B H 1.3702 0.8789 0.9157 0.073 Uiso 1 1 calc R . . C25 C 1.3384(11) 0.7156(9) 0.8250(6) 0.051(2) Uani 1 1 d . . . H25A H 1.2431 0.7159 0.7945 0.061 Uiso 1 1 calc R . . H25B H 1.3982 0.7102 0.7866 0.061 Uiso 1 1 calc R . . C26 C 1.2780(10) 0.3301(9) 0.8229(5) 0.040(2) Uani 1 1 d . . . C27 C 1.2158(11) 0.1826(10) 0.8214(5) 0.048(2) Uani 1 1 d . . . H27A H 1.1149 0.1310 0.8285 0.057 Uiso 1 1 calc R . . C28 C 1.3006(12) 0.1101(11) 0.8095(6) 0.062(3) Uani 1 1 d . . . H28A H 1.2552 0.0102 0.8065 0.074 Uiso 1 1 calc R . . C30 C 1.4541(13) 0.1879(13) 0.8020(6) 0.069(3) Uani 1 1 d . . . H30A H 1.5122 0.1405 0.7940 0.082 Uiso 1 1 calc R . . C31 C 1.5185(11) 0.3347(13) 0.8065(6) 0.061(3) Uani 1 1 d . . . H31A H 1.6218 0.3868 0.8027 0.073 Uiso 1 1 calc R . . C32 C 1.4332(10) 0.4087(11) 0.8167(5) 0.052(2) Uani 1 1 d . . . H32B H 1.4787 0.5085 0.8193 0.063 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 Pt1 0.03221(18) 0.03264(19) 0.0341(2) 0.00363(13) 0.00535(13) 0.01410(14) Cl1 0.0560(14) 0.0655(16) 0.0500(15) 0.0044(12) -0.0047(12) 0.0378(12) Cl2 0.0676(15) 0.0530(14) 0.0566(15) -0.0012(12) 0.0105(13) 0.0383(12) P1 0.0292(11) 0.0313(11) 0.0302(12) 0.0051(9) 0.0055(9) 0.0118(9) N1 0.033(4) 0.032(4) 0.046(4) 0.005(3) 0.013(3) 0.009(3) C2 0.045(5) 0.057(6) 0.066(7) 0.013(5) 0.022(5) 0.029(5) C3 0.074(8) 0.082(9) 0.154(13) -0.030(9) 0.074(9) 0.010(7) C4 0.073(8) 0.079(8) 0.091(9) 0.032(7) 0.052(7) 0.020(6) C5 0.038(5) 0.043(5) 0.047(6) 0.005(4) 0.011(4) 0.009(4) N6 0.032(4) 0.030(4) 0.033(4) 0.007(3) 0.005(3) 0.005(3) C7 0.049(5) 0.043(5) 0.040(5) 0.013(4) 0.013(4) 0.017(4) C8 0.079(7) 0.069(7) 0.040(6) 0.019(5) 0.003(5) 0.042(6) C9 0.047(6) 0.111(9) 0.043(6) 0.018(6) 0.002(5) 0.010(6) C10 0.035(5) 0.039(5) 0.038(5) 0.001(4) -0.002(4) 0.001(4) C11 0.027(4) 0.034(4) 0.027(4) 0.009(4) 0.006(3) 0.010(3) C12 0.051(6) 0.043(5) 0.066(7) 0.017(5) 0.029(5) 0.020(5) C13 0.084(8) 0.069(8) 0.100(10) 0.041(7) 0.049(8) 0.026(7) C14 0.070(7) 0.057(7) 0.091(9) 0.037(7) 0.029(7) 0.019(6) C15 0.104(9) 0.040(6) 0.088(9) 0.016(6) 0.041(8) 0.031(6) C16 0.072(6) 0.044(5) 0.042(6) 0.017(4) 0.027(5) 0.029(5) P2 0.0316(11) 0.0325(12) 0.0299(12) 0.0043(10) 0.0041(10) 0.0116(9) N16 0.037(4) 0.041(4) 0.046(4) 0.015(4) 0.012(3) 0.018(3) C17 0.051(5) 0.053(6) 0.050(6) 0.012(5) 0.029(5) 0.021(5) C18 0.066(8) 0.095(9) 0.069(8) 0.032(7) 0.022(6) 0.010(7) C19 0.128(11) 0.049(6) 0.071(8) 0.030(6) 0.044(8) 0.044(7) C20 0.074(7) 0.064(6) 0.042(6) 0.029(5) 0.026(5) 0.045(5) N21 0.042(4) 0.037(4) 0.034(4) 0.005(3) 0.002(3) 0.009(3) C22 0.054(6) 0.049(6) 0.044(6) 0.004(5) -0.004(5) 0.021(5) C23 0.088(8) 0.041(6) 0.062(7) -0.002(5) -0.012(6) 0.005(6) C24 0.072(7) 0.043(6) 0.048(6) 0.002(5) 0.006(5) 0.017(5) C25 0.049(5) 0.039(5) 0.050(6) 0.021(5) 0.016(5) 0.006(4) C26 0.051(5) 0.042(5) 0.026(5) 0.007(4) 0.013(4) 0.019(4) C27 0.045(5) 0.064(7) 0.036(5) 0.007(5) 0.002(4) 0.033(5) C28 0.068(7) 0.062(6) 0.057(7) 0.005(5) -0.005(5) 0.042(6) C30 0.076(8) 0.094(9) 0.051(7) -0.004(6) 0.005(6) 0.059(7) C31 0.041(5) 0.093(9) 0.061(7) 0.019(6) 0.017(5) 0.040(6) C32 0.040(5) 0.071(7) 0.045(6) 0.016(5) 0.012(5) 0.024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.252(2) . ? Pt1 P2 2.268(2) . ? Pt1 Cl1 2.351(2) . ? Pt1 Cl2 2.393(2) . ? P1 N1 1.667(6) . ? P1 N6 1.678(7) . ? P1 C11 1.797(8) . ? N1 C2 1.468(10) . ? N1 C5 1.481(10) . ? C2 C3 1.489(14) . ? C3 C4 1.461(14) . ? C4 C5 1.525(12) . ? N6 C7 1.479(10) . ? N6 C10 1.494(10) . ? C7 C8 1.508(12) . ? C8 C9 1.487(13) . ? C9 C10 1.505(13) . ? C11 C12 1.392(11) . ? C11 C16 1.399(11) . ? C12 C13 1.349(13) . ? C13 C14 1.358(15) . ? C14 C15 1.330(14) . ? C15 C16 1.382(13) . ? P2 N16 1.652(7) . ? P2 N21 1.673(7) . ? P2 C26 1.833(9) . ? N16 C17 1.466(10) . ? N16 C20 1.477(11) . ? C17 C18 1.509(14) . ? C18 C19 1.478(15) . ? C19 C20 1.490(13) . ? N21 C25 1.465(10) . ? N21 C22 1.464(10) . ? C22 C23 1.528(13) . ? C23 C24 1.477(14) . ? C24 C25 1.516(12) . ? C26 C27 1.382(12) . ? C26 C32 1.400(11) . ? C27 C28 1.388(12) . ? C28 C30 1.393(14) . ? C30 C31 1.368(14) . ? C31 C32 1.397(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 P1 Pt1 P2 96.39(7) . . ? P1 Pt1 Cl1 90.40(8) . . ? P2 Pt1 Cl1 173.21(8) . . ? P1 Pt1 Cl2 175.41(8) . . ? P2 Pt1 Cl2 87.44(8) . . ? Cl1 Pt1 Cl2 85.77(8) . . ? N1 P1 N6 103.8(3) . . ? N1 P1 C11 112.6(3) . . ? N6 P1 C11 99.8(3) . . ? N1 P1 Pt1 110.0(2) . . ? N6 P1 Pt1 121.2(2) . . ? C11 P1 Pt1 109.2(3) . . ? C2 N1 C5 109.6(6) . . ? C2 N1 P1 125.5(5) . . ? C5 N1 P1 119.9(5) . . ? N1 C2 C3 107.1(8) . . ? C4 C3 C2 105.9(8) . . ? C3 C4 C5 107.4(8) . . ? N1 C5 C4 104.0(7) . . ? C7 N6 C10 109.6(6) . . ? C7 N6 P1 120.9(5) . . ? C10 N6 P1 122.0(5) . . ? N6 C7 C8 103.0(7) . . ? C9 C8 C7 103.9(7) . . ? C8 C9 C10 106.9(8) . . ? N6 C10 C9 103.9(7) . . ? C12 C11 C16 116.2(8) . . ? C12 C11 P1 118.9(6) . . ? C16 C11 P1 124.7(6) . . ? C13 C12 C11 121.9(9) . . ? C14 C13 C12 120.2(11) . . ? C15 C14 C13 120.3(11) . . ? C14 C15 C16 120.8(10) . . ? C15 C16 C11 120.2(9) . . ? N16 P2 N21 110.2(3) . . ? N16 P2 C26 102.2(4) . . ? N21 P2 C26 102.5(4) . . ? N16 P2 Pt1 111.0(3) . . ? N21 P2 Pt1 109.4(3) . . ? C26 P2 Pt1 120.9(3) . . ? C17 N16 C20 106.6(7) . . ? C17 N16 P2 126.7(6) . . ? C20 N16 P2 126.3(6) . . ? N16 C17 C18 104.4(8) . . ? C19 C18 C17 107.7(9) . . ? C18 C19 C20 104.6(9) . . ? N16 C20 C19 103.0(8) . . ? C25 N21 C22 110.9(6) . . ? C25 N21 P2 125.9(6) . . ? C22 N21 P2 123.2(6) . . ? N21 C22 C23 103.9(7) . . ? C24 C23 C22 104.3(9) . . ? C23 C24 C25 104.2(8) . . ? N21 C25 C24 103.3(7) . . ? C27 C26 C32 119.0(8) . . ? C27 C26 P2 121.1(6) . . ? C32 C26 P2 119.8(7) . . ? C26 C27 C28 121.4(9) . . ? C30 C28 C27 119.5(10) . . ? C31 C30 C28 119.3(9) . . ? C30 C31 C32 121.8(9) . . ? C31 C32 C26 118.9(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 P2 Pt1 P1 N1 -57.7(3) . . . . ? Cl1 Pt1 P1 N1 122.5(3) . . . . ? Cl2 Pt1 P1 N1 155.8(11) . . . . ? P2 Pt1 P1 N6 -178.8(3) . . . . ? Cl1 Pt1 P1 N6 1.4(3) . . . . ? Cl2 Pt1 P1 N6 34.7(12) . . . . ? P2 Pt1 P1 C11 66.2(3) . . . . ? Cl1 Pt1 P1 C11 -113.6(3) . . . . ? Cl2 Pt1 P1 C11 -80.2(11) . . . . ? N6 P1 N1 C2 -55.4(8) . . . . ? C11 P1 N1 C2 51.6(8) . . . . ? Pt1 P1 N1 C2 173.6(6) . . . . ? N6 P1 N1 C5 96.9(6) . . . . ? C11 P1 N1 C5 -156.1(6) . . . . ? Pt1 P1 N1 C5 -34.2(7) . . . . ? C5 N1 C2 C3 -6.4(11) . . . . ? P1 N1 C2 C3 148.2(8) . . . . ? N1 C2 C3 C4 19.5(14) . . . . ? C2 C3 C4 C5 -25.1(15) . . . . ? C2 N1 C5 C4 -8.6(10) . . . . ? P1 N1 C5 C4 -164.9(7) . . . . ? C3 C4 C5 N1 20.9(13) . . . . ? N1 P1 N6 C7 -48.9(7) . . . . ? C11 P1 N6 C7 -165.2(6) . . . . ? Pt1 P1 N6 C7 75.1(6) . . . . ? N1 P1 N6 C10 164.4(6) . . . . ? C11 P1 N6 C10 48.0(7) . . . . ? Pt1 P1 N6 C10 -71.6(7) . . . . ? C10 N6 C7 C8 -25.2(9) . . . . ? P1 N6 C7 C8 -175.6(6) . . . . ? N6 C7 C8 C9 35.0(10) . . . . ? C7 C8 C9 C10 -32.9(12) . . . . ? C7 N6 C10 C9 5.3(10) . . . . ? P1 N6 C10 C9 155.4(7) . . . . ? C8 C9 C10 N6 17.2(11) . . . . ? N1 P1 C11 C12 147.4(6) . . . . ? N6 P1 C11 C12 -103.1(7) . . . . ? Pt1 P1 C11 C12 25.0(7) . . . . ? N1 P1 C11 C16 -37.2(8) . . . . ? N6 P1 C11 C16 72.3(7) . . . . ? Pt1 P1 C11 C16 -159.6(6) . . . . ? C16 C11 C12 C13 2.7(13) . . . . ? P1 C11 C12 C13 178.5(8) . . . . ? C11 C12 C13 C14 1.9(17) . . . . ? C12 C13 C14 C15 -5.5(19) . . . . ? C13 C14 C15 C16 4.1(19) . . . . ? C14 C15 C16 C11 0.7(16) . . . . ? C12 C11 C16 C15 -4.0(13) . . . . ? P1 C11 C16 C15 -179.5(8) . . . . ? P1 Pt1 P2 N16 -109.4(3) . . . . ? Cl1 Pt1 P2 N16 68.8(8) . . . . ? Cl2 Pt1 P2 N16 68.1(3) . . . . ? P1 Pt1 P2 N21 128.8(3) . . . . ? Cl1 Pt1 P2 N21 -53.1(8) . . . . ? Cl2 Pt1 P2 N21 -53.8(3) . . . . ? P1 Pt1 P2 C26 10.2(3) . . . . ? Cl1 Pt1 P2 C26 -171.7(7) . . . . ? Cl2 Pt1 P2 C26 -172.4(3) . . . . ? N21 P2 N16 C17 105.0(7) . . . . ? C26 P2 N16 C17 -146.6(7) . . . . ? Pt1 P2 N16 C17 -16.4(7) . . . . ? N21 P2 N16 C20 -66.3(8) . . . . ? C26 P2 N16 C20 42.1(8) . . . . ? Pt1 P2 N16 C20 172.3(6) . . . . ? C20 N16 C17 C18 -25.2(10) . . . . ? P2 N16 C17 C18 162.2(7) . . . . ? N16 C17 C18 C19 3.5(12) . . . . ? C17 C18 C19 C20 19.0(12) . . . . ? C17 N16 C20 C19 37.1(9) . . . . ? P2 N16 C20 C19 -150.2(7) . . . . ? C18 C19 C20 N16 -33.9(10) . . . . ? N16 P2 N21 C25 -143.3(7) . . . . ? C26 P2 N21 C25 108.6(7) . . . . ? Pt1 P2 N21 C25 -21.0(8) . . . . ? N16 P2 N21 C22 38.4(8) . . . . ? C26 P2 N21 C22 -69.8(7) . . . . ? Pt1 P2 N21 C22 160.7(6) . . . . ? C25 N21 C22 C23 -5.7(10) . . . . ? P2 N21 C22 C23 172.8(7) . . . . ? N21 C22 C23 C24 26.4(11) . . . . ? C22 C23 C24 C25 -36.7(11) . . . . ? C22 N21 C25 C24 -16.4(10) . . . . ? P2 N21 C25 C24 165.0(7) . . . . ? C23 C24 C25 N21 32.8(10) . . . . ? N16 P2 C26 C27 43.1(8) . . . . ? N21 P2 C26 C27 157.3(7) . . . . ? Pt1 P2 C26 C27 -80.8(7) . . . . ? N16 P2 C26 C32 -137.1(7) . . . . ? N21 P2 C26 C32 -22.9(8) . . . . ? Pt1 P2 C26 C32 99.1(7) . . . . ? C32 C26 C27 C28 -3.5(13) . . . . ? P2 C26 C27 C28 176.3(7) . . . . ? C26 C27 C28 C30 2.5(14) . . . . ? C27 C28 C30 C31 0.0(15) . . . . ? C28 C30 C31 C32 -1.4(16) . . . . ? C30 C31 C32 C26 0.4(15) . . . . ? C27 C26 C32 C31 2.1(13) . . . . ? P2 C26 C32 C31 -177.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.983 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.132 data_24 _database_code_CSD 171248 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 B F4 Fe N2 O2 P' _chemical_formula_sum 'C21 H26 B F4 Fe N2 O2 P' _chemical_formula_weight 512.07 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' 'Fe' 'Fe' 0.3463 0.8444 '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 11.6620(2) _cell_length_b 14.63060(10) _cell_length_c 13.7467(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.2380(10) _cell_angle_gamma 90.00 _cell_volume 2326.80(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.875832 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9918 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3326 _reflns_number_gt 2466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+1.4694P] 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 0.0022(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3326 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 Fe1 Fe 0.03840(4) 0.56687(3) 0.76595(3) 0.0448(2) Uani 1 1 d . . . P1 P -0.11552(8) 0.65762(6) 0.75939(6) 0.0432(3) Uani 1 1 d . . . N1 N -0.2257(2) 0.6236(2) 0.6805(2) 0.0547(8) Uani 1 1 d . . . C2 C -0.2274(4) 0.5539(4) 0.6038(4) 0.0979(17) Uani 1 1 d . . . H2A H -0.1805 0.5730 0.5540 0.117 Uiso 1 1 calc R . . H2B H -0.1974 0.4964 0.6315 0.117 Uiso 1 1 calc R . . C3 C -0.3471(5) 0.5439(5) 0.5621(5) 0.115(2) Uani 1 1 d . . . H3A H -0.3807 0.4903 0.5888 0.138 Uiso 1 1 calc R . . H3B H -0.3526 0.5372 0.4914 0.138 Uiso 1 1 calc R . . C4 C -0.4080(5) 0.6266(4) 0.5873(5) 0.121(2) Uani 1 1 d . . . H4A H -0.4867 0.6120 0.5976 0.145 Uiso 1 1 calc R . . H4B H -0.4102 0.6713 0.5350 0.145 Uiso 1 1 calc R . . C5 C -0.3425(4) 0.6633(3) 0.6792(4) 0.0820(14) Uani 1 1 d . . . H5A H -0.3396 0.7295 0.6778 0.098 Uiso 1 1 calc R . . H5B H -0.3775 0.6441 0.7363 0.098 Uiso 1 1 calc R . . N6 N -0.1610(3) 0.6739(2) 0.8673(2) 0.0558(8) Uani 1 1 d . . . C7 C -0.1906(4) 0.5955(3) 0.9273(3) 0.0814(14) Uani 1 1 d . . . H7A H -0.2392 0.5522 0.8876 0.098 Uiso 1 1 calc R . . H7B H -0.1212 0.5644 0.9564 0.098 Uiso 1 1 calc R . . C8 C -0.2530(7) 0.6356(6) 1.0035(5) 0.147(3) Uani 1 1 d . . . H8A H -0.3334 0.6169 0.9935 0.176 Uiso 1 1 calc R . . H8B H -0.2192 0.6147 1.0677 0.176 Uiso 1 1 calc R . . C9 C -0.2452(6) 0.7318(6) 0.9981(4) 0.127(2) Uani 1 1 d . . . H9A H -0.1863 0.7541 1.0487 0.152 Uiso 1 1 calc R . . H9B H -0.3185 0.7593 1.0083 0.152 Uiso 1 1 calc R . . C10 C -0.2152(5) 0.7572(4) 0.9002(4) 0.0953(16) Uani 1 1 d . . . H10A H -0.2838 0.7732 0.8560 0.114 Uiso 1 1 calc R . . H10B H -0.1617 0.8083 0.9046 0.114 Uiso 1 1 calc R . . C11 C -0.0794(3) 0.7734(2) 0.7250(3) 0.0470(9) Uani 1 1 d . . . C12 C -0.1208(4) 0.8084(3) 0.6344(3) 0.0615(10) Uani 1 1 d . . . H12A H -0.1722 0.7744 0.5916 0.074 Uiso 1 1 calc R . . C13 C -0.0862(4) 0.8942(3) 0.6068(3) 0.0741(13) Uani 1 1 d . . . H13A H -0.1143 0.9171 0.5454 0.089 Uiso 1 1 calc R . . C14 C -0.0116(4) 0.9451(3) 0.6689(4) 0.0793(14) Uani 1 1 d . . . H14A H 0.0099 1.0032 0.6505 0.095 Uiso 1 1 calc R . . C15 C 0.0315(4) 0.9103(3) 0.7585(4) 0.0764(13) Uani 1 1 d . . . H15A H 0.0829 0.9448 0.8009 0.092 Uiso 1 1 calc R . . C16 C -0.0005(4) 0.8247(3) 0.7863(3) 0.0653(11) Uani 1 1 d . . . H16A H 0.0310 0.8010 0.8465 0.078 Uiso 1 1 calc R . . C17 C 0.0639(4) 0.6082(3) 0.6251(3) 0.0636(11) Uani 1 1 d . . . H17A H 0.0110 0.6415 0.5830 0.076 Uiso 1 1 calc R . . C18 C 0.1510(4) 0.6450(3) 0.6935(3) 0.0632(11) Uani 1 1 d . . . H18A H 0.1655 0.7068 0.7052 0.076 Uiso 1 1 calc R . . C19 C 0.2125(4) 0.5717(3) 0.7412(3) 0.0692(12) Uani 1 1 d . . . H19A H 0.2754 0.5768 0.7896 0.083 Uiso 1 1 calc R . . C20 C 0.1627(4) 0.4893(3) 0.7034(3) 0.0679(12) Uani 1 1 d . . . H20A H 0.1864 0.4306 0.7226 0.082 Uiso 1 1 calc R . . C21 C 0.0702(4) 0.5122(3) 0.6310(3) 0.0630(11) Uani 1 1 d . . . H21A H 0.0219 0.4712 0.5938 0.076 Uiso 1 1 calc R . . C30 C -0.0403(4) 0.4693(3) 0.7955(3) 0.0608(10) Uani 1 1 d . . . O30 O -0.0892(4) 0.4058(2) 0.8125(3) 0.1026(12) Uani 1 1 d . . . C40 C 0.0823(3) 0.6027(3) 0.8882(3) 0.0607(10) Uani 1 1 d . . . O40 O 0.1144(3) 0.6250(3) 0.9659(2) 0.0913(10) Uani 1 1 d . . . B1 B 0.0974(5) 0.2517(4) 0.6435(4) 0.0726(15) Uani 1 1 d . . . F1 F 0.0682(3) 0.16301(19) 0.6292(3) 0.1236(12) Uani 1 1 d . . . F2 F 0.0200(3) 0.3070(2) 0.5923(3) 0.1402(15) Uani 1 1 d . . . F3 F 0.2017(3) 0.2664(3) 0.6135(3) 0.1558(15) Uani 1 1 d . . . F4 F 0.1115(4) 0.2729(2) 0.7387(2) 0.1380(14) 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 Fe1 0.0516(3) 0.0405(3) 0.0430(3) 0.0011(2) 0.0085(2) 0.0008(2) P1 0.0474(5) 0.0392(5) 0.0430(5) -0.0024(4) 0.0060(4) -0.0022(4) N1 0.0485(18) 0.054(2) 0.0601(19) -0.0060(16) 0.0004(14) -0.0029(15) C2 0.091(4) 0.090(4) 0.103(4) -0.043(3) -0.025(3) -0.007(3) C3 0.091(4) 0.122(5) 0.121(5) -0.038(4) -0.031(3) -0.014(4) C4 0.088(4) 0.113(5) 0.146(5) 0.001(4) -0.052(4) 0.001(4) C5 0.056(3) 0.077(3) 0.108(4) -0.006(3) -0.008(3) 0.002(2) N6 0.065(2) 0.0520(19) 0.0548(19) -0.0081(15) 0.0233(15) 0.0018(16) C7 0.101(4) 0.081(3) 0.070(3) 0.005(2) 0.042(3) -0.012(3) C8 0.198(8) 0.147(7) 0.118(5) 0.000(5) 0.107(5) 0.015(6) C9 0.138(5) 0.168(7) 0.083(4) -0.028(4) 0.045(4) 0.037(5) C10 0.112(4) 0.087(4) 0.093(4) -0.021(3) 0.037(3) 0.019(3) C11 0.050(2) 0.037(2) 0.054(2) -0.0027(17) 0.0065(17) 0.0005(16) C12 0.068(3) 0.051(2) 0.065(3) 0.001(2) 0.003(2) -0.001(2) C13 0.091(3) 0.051(3) 0.080(3) 0.023(2) 0.010(3) 0.005(2) C14 0.083(3) 0.046(3) 0.113(4) 0.010(3) 0.028(3) -0.006(2) C15 0.069(3) 0.054(3) 0.105(4) -0.014(3) 0.006(3) -0.018(2) C16 0.068(3) 0.053(3) 0.072(3) -0.006(2) -0.003(2) -0.004(2) C17 0.076(3) 0.069(3) 0.051(2) 0.009(2) 0.031(2) 0.006(2) C18 0.067(3) 0.058(3) 0.071(3) -0.003(2) 0.032(2) -0.011(2) C19 0.053(2) 0.072(3) 0.084(3) -0.014(3) 0.016(2) 0.003(2) C20 0.063(3) 0.064(3) 0.081(3) -0.010(2) 0.023(2) 0.011(2) C21 0.077(3) 0.061(3) 0.055(2) -0.016(2) 0.021(2) 0.003(2) C30 0.081(3) 0.047(2) 0.059(2) 0.000(2) 0.027(2) 0.000(2) O30 0.151(3) 0.053(2) 0.115(3) 0.0014(18) 0.063(2) -0.025(2) C40 0.067(3) 0.064(3) 0.051(3) 0.009(2) 0.003(2) 0.007(2) O40 0.103(2) 0.119(3) 0.0460(18) -0.0029(18) -0.0115(16) 0.003(2) B1 0.082(4) 0.060(4) 0.072(4) -0.002(3) -0.003(3) 0.000(3) F1 0.157(3) 0.0543(18) 0.146(3) 0.0080(17) -0.033(2) -0.0088(18) F2 0.162(3) 0.071(2) 0.164(3) 0.021(2) -0.073(3) 0.013(2) F3 0.125(3) 0.167(4) 0.184(4) -0.011(3) 0.054(3) -0.024(3) F4 0.219(4) 0.115(3) 0.077(2) -0.0055(19) 0.006(2) 0.034(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 Fe1 C40 1.773(4) . ? Fe1 C30 1.772(4) . ? Fe1 C17 2.085(4) . ? Fe1 C18 2.086(4) . ? Fe1 C21 2.095(4) . ? Fe1 C19 2.101(4) . ? Fe1 C20 2.108(4) . ? Fe1 P1 2.2254(10) . ? P1 N1 1.650(3) . ? P1 N6 1.655(3) . ? P1 C11 1.823(4) . ? N1 C2 1.465(5) . ? N1 C5 1.479(5) . ? C2 C3 1.448(7) . ? C3 C4 1.467(8) . ? C4 C5 1.491(7) . ? N6 C10 1.470(5) . ? N6 C7 1.478(5) . ? C7 C8 1.472(7) . ? C8 C9 1.413(9) . ? C9 C10 1.480(7) . ? C11 C12 1.376(5) . ? C11 C16 1.386(5) . ? C12 C13 1.385(6) . ? C13 C14 1.362(6) . ? C14 C15 1.369(6) . ? C15 C16 1.375(6) . ? C17 C21 1.407(6) . ? C17 C18 1.402(6) . ? C18 C19 1.404(6) . ? C19 C20 1.409(6) . ? C20 C21 1.414(6) . ? C30 O30 1.130(5) . ? C40 O40 1.135(4) . ? B1 F4 1.335(6) . ? B1 F2 1.344(6) . ? B1 F3 1.350(6) . ? B1 F1 1.350(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Fe1 C30 96.71(19) . . ? C40 Fe1 C17 137.41(19) . . ? C30 Fe1 C17 125.83(18) . . ? C40 Fe1 C18 99.57(18) . . ? C30 Fe1 C18 157.87(17) . . ? C17 Fe1 C18 39.27(16) . . ? C40 Fe1 C21 152.82(18) . . ? C30 Fe1 C21 92.88(17) . . ? C17 Fe1 C21 39.35(16) . . ? C18 Fe1 C21 66.06(17) . . ? C40 Fe1 C19 88.49(18) . . ? C30 Fe1 C19 127.12(19) . . ? C17 Fe1 C19 65.54(18) . . ? C18 Fe1 C19 39.19(16) . . ? C21 Fe1 C19 65.64(17) . . ? C40 Fe1 C20 114.46(18) . . ? C30 Fe1 C20 93.58(18) . . ? C17 Fe1 C20 65.89(17) . . ? C18 Fe1 C20 66.03(17) . . ? C21 Fe1 C20 39.31(16) . . ? C19 Fe1 C20 39.12(16) . . ? C40 Fe1 P1 89.85(13) . . ? C30 Fe1 P1 92.95(13) . . ? C17 Fe1 P1 89.90(12) . . ? C18 Fe1 P1 101.94(13) . . ? C21 Fe1 P1 115.05(13) . . ? C19 Fe1 P1 139.81(14) . . ? C20 Fe1 P1 153.84(13) . . ? N1 P1 N6 108.75(16) . . ? N1 P1 C11 107.23(16) . . ? N6 P1 C11 102.08(16) . . ? N1 P1 Fe1 113.83(12) . . ? N6 P1 Fe1 113.45(12) . . ? C11 P1 Fe1 110.70(12) . . ? C2 N1 C5 109.6(3) . . ? C2 N1 P1 128.4(3) . . ? C5 N1 P1 122.0(3) . . ? C3 C2 N1 106.3(4) . . ? C2 C3 C4 107.1(4) . . ? C3 C4 C5 106.6(4) . . ? N1 C5 C4 104.0(4) . . ? C10 N6 C7 109.4(3) . . ? C10 N6 P1 126.4(3) . . ? C7 N6 P1 120.8(3) . . ? C8 C7 N6 105.0(5) . . ? C9 C8 C7 108.6(5) . . ? C8 C9 C10 108.8(5) . . ? N6 C10 C9 103.4(5) . . ? C12 C11 C16 118.6(4) . . ? C12 C11 P1 120.9(3) . . ? C16 C11 P1 120.2(3) . . ? C11 C12 C13 120.2(4) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 119.6(4) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C11 120.5(4) . . ? C21 C17 C18 108.5(4) . . ? C21 C17 Fe1 70.7(2) . . ? C18 C17 Fe1 70.4(2) . . ? C19 C18 C17 107.7(4) . . ? C19 C18 Fe1 71.0(2) . . ? C17 C18 Fe1 70.3(2) . . ? C18 C19 C20 108.6(4) . . ? C18 C19 Fe1 69.8(2) . . ? C20 C19 Fe1 70.7(2) . . ? C19 C20 C21 107.4(4) . . ? C19 C20 Fe1 70.2(2) . . ? C21 C20 Fe1 69.9(2) . . ? C17 C21 C20 107.9(4) . . ? C17 C21 Fe1 69.9(2) . . ? C20 C21 Fe1 70.8(2) . . ? O30 C30 Fe1 178.2(4) . . ? O40 C40 Fe1 177.6(4) . . ? F4 B1 F2 111.4(5) . . ? F4 B1 F3 105.0(5) . . ? F2 B1 F3 108.4(5) . . ? F4 B1 F1 111.4(5) . . ? F2 B1 F1 111.2(4) . . ? F3 B1 F1 109.2(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 C40 Fe1 P1 N1 -153.85(18) . . . . ? C30 Fe1 P1 N1 -57.13(18) . . . . ? C17 Fe1 P1 N1 68.74(18) . . . . ? C18 Fe1 P1 N1 106.40(18) . . . . ? C21 Fe1 P1 N1 37.43(18) . . . . ? C19 Fe1 P1 N1 118.7(2) . . . . ? C20 Fe1 P1 N1 47.2(3) . . . . ? C40 Fe1 P1 N6 -28.78(19) . . . . ? C30 Fe1 P1 N6 67.94(18) . . . . ? C17 Fe1 P1 N6 -166.19(18) . . . . ? C18 Fe1 P1 N6 -128.53(18) . . . . ? C21 Fe1 P1 N6 162.51(18) . . . . ? C19 Fe1 P1 N6 -116.3(2) . . . . ? C20 Fe1 P1 N6 172.2(3) . . . . ? C40 Fe1 P1 C11 85.29(18) . . . . ? C30 Fe1 P1 C11 -178.00(18) . . . . ? C17 Fe1 P1 C11 -52.12(18) . . . . ? C18 Fe1 P1 C11 -14.47(18) . . . . ? C21 Fe1 P1 C11 -83.43(18) . . . . ? C19 Fe1 P1 C11 -2.2(2) . . . . ? C20 Fe1 P1 C11 -73.7(3) . . . . ? N6 P1 N1 C2 -140.0(4) . . . . ? C11 P1 N1 C2 110.3(4) . . . . ? Fe1 P1 N1 C2 -12.5(4) . . . . ? N6 P1 N1 C5 40.0(4) . . . . ? C11 P1 N1 C5 -69.7(4) . . . . ? Fe1 P1 N1 C5 167.5(3) . . . . ? C5 N1 C2 C3 -5.7(6) . . . . ? P1 N1 C2 C3 174.4(4) . . . . ? N1 C2 C3 C4 19.6(7) . . . . ? C2 C3 C4 C5 -26.2(8) . . . . ? C2 N1 C5 C4 -10.1(5) . . . . ? P1 N1 C5 C4 169.9(4) . . . . ? C3 C4 C5 N1 21.9(6) . . . . ? N1 P1 N6 C10 -84.9(4) . . . . ? C11 P1 N6 C10 28.2(4) . . . . ? Fe1 P1 N6 C10 147.4(4) . . . . ? N1 P1 N6 C7 72.2(4) . . . . ? C11 P1 N6 C7 -174.7(3) . . . . ? Fe1 P1 N6 C7 -55.6(4) . . . . ? C10 N6 C7 C8 -6.0(6) . . . . ? P1 N6 C7 C8 -166.6(4) . . . . ? N6 C7 C8 C9 -8.3(8) . . . . ? C7 C8 C9 C10 19.6(9) . . . . ? C7 N6 C10 C9 17.1(6) . . . . ? P1 N6 C10 C9 176.3(4) . . . . ? C8 C9 C10 N6 -22.4(7) . . . . ? N1 P1 C11 C12 -15.3(4) . . . . ? N6 P1 C11 C12 -129.6(3) . . . . ? Fe1 P1 C11 C12 109.4(3) . . . . ? N1 P1 C11 C16 170.9(3) . . . . ? N6 P1 C11 C16 56.7(3) . . . . ? Fe1 P1 C11 C16 -64.4(3) . . . . ? C16 C11 C12 C13 -1.7(6) . . . . ? P1 C11 C12 C13 -175.6(3) . . . . ? C11 C12 C13 C14 -0.4(7) . . . . ? C12 C13 C14 C15 1.4(7) . . . . ? C13 C14 C15 C16 -0.4(7) . . . . ? C14 C15 C16 C11 -1.8(7) . . . . ? C12 C11 C16 C15 2.8(6) . . . . ? P1 C11 C16 C15 176.7(3) . . . . ? C40 Fe1 C17 C21 138.3(3) . . . . ? C30 Fe1 C17 C21 -38.5(3) . . . . ? C18 Fe1 C17 C21 118.7(4) . . . . ? C19 Fe1 C17 C21 80.8(3) . . . . ? C20 Fe1 C17 C21 37.7(3) . . . . ? P1 Fe1 C17 C21 -132.1(2) . . . . ? C40 Fe1 C17 C18 19.5(4) . . . . ? C30 Fe1 C17 C18 -157.2(3) . . . . ? C21 Fe1 C17 C18 -118.7(4) . . . . ? C19 Fe1 C17 C18 -37.9(2) . . . . ? C20 Fe1 C17 C18 -81.0(3) . . . . ? P1 Fe1 C17 C18 109.2(2) . . . . ? C21 C17 C18 C19 0.7(4) . . . . ? Fe1 C17 C18 C19 61.5(3) . . . . ? C21 C17 C18 Fe1 -60.8(3) . . . . ? C40 Fe1 C18 C19 75.6(3) . . . . ? C30 Fe1 C18 C19 -61.3(6) . . . . ? C17 Fe1 C18 C19 -117.7(4) . . . . ? C21 Fe1 C18 C19 -80.2(3) . . . . ? C20 Fe1 C18 C19 -37.0(2) . . . . ? P1 Fe1 C18 C19 167.5(2) . . . . ? C40 Fe1 C18 C17 -166.7(3) . . . . ? C30 Fe1 C18 C17 56.4(6) . . . . ? C21 Fe1 C18 C17 37.5(3) . . . . ? C19 Fe1 C18 C17 117.7(4) . . . . ? C20 Fe1 C18 C17 80.7(3) . . . . ? P1 Fe1 C18 C17 -74.8(3) . . . . ? C17 C18 C19 C20 -0.8(5) . . . . ? Fe1 C18 C19 C20 60.3(3) . . . . ? C17 C18 C19 Fe1 -61.1(3) . . . . ? C40 Fe1 C19 C18 -107.2(3) . . . . ? C30 Fe1 C19 C18 155.5(3) . . . . ? C17 Fe1 C19 C18 38.0(2) . . . . ? C21 Fe1 C19 C18 81.4(3) . . . . ? C20 Fe1 C19 C18 119.3(4) . . . . ? P1 Fe1 C19 C18 -19.2(3) . . . . ? C40 Fe1 C19 C20 133.5(3) . . . . ? C30 Fe1 C19 C20 36.3(4) . . . . ? C17 Fe1 C19 C20 -81.3(3) . . . . ? C18 Fe1 C19 C20 -119.3(4) . . . . ? C21 Fe1 C19 C20 -37.9(3) . . . . ? P1 Fe1 C19 C20 -138.5(2) . . . . ? C18 C19 C20 C21 0.5(5) . . . . ? Fe1 C19 C20 C21 60.3(3) . . . . ? C18 C19 C20 Fe1 -59.8(3) . . . . ? C40 Fe1 C20 C19 -52.8(3) . . . . ? C30 Fe1 C20 C19 -151.8(3) . . . . ? C17 Fe1 C20 C19 80.3(3) . . . . ? C18 Fe1 C20 C19 37.1(3) . . . . ? C21 Fe1 C20 C19 118.0(4) . . . . ? P1 Fe1 C20 C19 104.1(4) . . . . ? C40 Fe1 C20 C21 -170.8(3) . . . . ? C30 Fe1 C20 C21 90.2(3) . . . . ? C17 Fe1 C20 C21 -37.7(3) . . . . ? C18 Fe1 C20 C21 -80.9(3) . . . . ? C19 Fe1 C20 C21 -118.0(4) . . . . ? P1 Fe1 C20 C21 -14.0(5) . . . . ? C18 C17 C21 C20 -0.4(4) . . . . ? Fe1 C17 C21 C20 -61.0(3) . . . . ? C18 C17 C21 Fe1 60.6(3) . . . . ? C19 C20 C21 C17 -0.1(4) . . . . ? Fe1 C20 C21 C17 60.4(3) . . . . ? C19 C20 C21 Fe1 -60.5(3) . . . . ? C40 Fe1 C21 C17 -99.6(4) . . . . ? C30 Fe1 C21 C17 149.7(3) . . . . ? C18 Fe1 C21 C17 -37.4(3) . . . . ? C19 Fe1 C21 C17 -80.5(3) . . . . ? C20 Fe1 C21 C17 -118.2(4) . . . . ? P1 Fe1 C21 C17 55.0(3) . . . . ? C40 Fe1 C21 C20 18.6(5) . . . . ? C30 Fe1 C21 C20 -92.1(3) . . . . ? C17 Fe1 C21 C20 118.2(4) . . . . ? C18 Fe1 C21 C20 80.8(3) . . . . ? C19 Fe1 C21 C20 37.7(3) . . . . ? P1 Fe1 C21 C20 173.3(2) . . . . ? C40 Fe1 C30 O30 -136(14) . . . . ? C17 Fe1 C30 O30 41(14) . . . . ? C18 Fe1 C30 O30 1(15) . . . . ? C21 Fe1 C30 O30 18(14) . . . . ? C19 Fe1 C30 O30 -43(14) . . . . ? C20 Fe1 C30 O30 -21(14) . . . . ? P1 Fe1 C30 O30 133(14) . . . . ? C30 Fe1 C40 O40 116(9) . . . . ? C17 Fe1 C40 O40 -62(9) . . . . ? C18 Fe1 C40 O40 -49(9) . . . . ? C21 Fe1 C40 O40 6(10) . . . . ? C19 Fe1 C40 O40 -11(9) . . . . ? C20 Fe1 C40 O40 19(9) . . . . ? P1 Fe1 C40 O40 -151(9) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.391 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.047