# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 data_Gandelman-158 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Gandelman-58 (Yuri)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H40 Cl4 F6 N3 O6 P2 Pt S2' _chemical_formula_weight 1223.69 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' S S 0.1246 0.1234 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 20.729(1) _cell_length_b 16.7382(8) _cell_length_c 13.9693(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.679(2) _cell_angle_gamma 90.00 _cell_volume 4836.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2420 _exptl_absorpt_coefficient_mu 3.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Bruker APEX2 DUO' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 22824 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4574 _reflns_number_gt 3762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2010.7.0.0' _computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 3.0' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+5.9027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4574 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.257 _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 Pt1 Pt 0.0000 0.253251(12) 0.7500 0.02672(8) Uani 1 2 d S . . P1 P 0.05241(5) 0.25992(6) 0.61113(7) 0.0289(2) Uani 1 1 d . . . S1 S 0.35691(5) 0.45286(7) 0.07199(8) 0.0380(3) Uani 1 1 d . . . Cl1 Cl 0.22343(8) 0.35766(9) 0.30253(11) 0.0681(4) Uani 1 1 d . . . Cl2 Cl 0.15103(7) 0.49714(10) 0.35720(13) 0.0773(4) Uani 1 1 d . . . N1 N 0.0000 0.1266(3) 0.7500 0.0255(9) Uani 1 2 d S . . N2 N 0.03999(14) 0.07660(18) 0.7063(2) 0.0250(7) Uani 1 1 d . . . O1 O 0.34091(15) 0.4718(2) 0.1682(2) 0.0502(8) Uani 1 1 d . . . O2 O 0.42059(15) 0.4201(2) 0.0639(2) 0.0595(10) Uani 1 1 d . . . O3 O 0.33782(17) 0.5120(2) 0.0015(3) 0.0642(10) Uani 1 1 d . . . F1 F 0.3150(2) 0.3081(2) 0.0963(3) 0.1041(13) Uani 1 1 d . . . F2 F 0.3145(2) 0.3455(3) -0.0503(3) 0.1023(13) Uani 1 1 d . . . F3 F 0.24311(16) 0.3895(3) 0.0422(3) 0.1085(14) Uani 1 1 d . . . C1 C 0.09233(17) 0.1076(2) 0.6506(3) 0.0288(8) Uani 1 1 d . . . H1A H 0.1169 0.0622 0.6257 0.035 Uiso 1 1 calc R . . H1B H 0.1224 0.1395 0.6932 0.035 Uiso 1 1 calc R . . C2 C 0.06691(19) 0.1594(2) 0.5670(3) 0.0307(9) Uani 1 1 d . . . H2A H 0.0262 0.1365 0.5378 0.037 Uiso 1 1 calc R . . H2B H 0.0989 0.1612 0.5173 0.037 Uiso 1 1 calc R . . C3 C 0.02583(17) -0.0001(2) 0.7218(3) 0.0256(8) Uani 1 1 d . . . C4 C 0.0589(2) -0.0725(2) 0.6871(3) 0.0363(9) Uani 1 1 d . . . H4A H 0.1064 -0.0665 0.6971 0.044 Uiso 1 1 calc R . . H4B H 0.0479 -0.0806 0.6178 0.044 Uiso 1 1 calc R . . C5 C 0.0361(3) -0.1435(3) 0.7442(5) 0.0664(16) Uani 1 1 d . . . H5A H 0.0478 -0.1934 0.7116 0.080 Uiso 1 1 calc R . . H5B H 0.0591 -0.1432 0.8085 0.080 Uiso 1 1 calc R . . C6 C 0.0000 0.3767(4) 0.7500 0.0558(19) Uani 1 2 d S . . C7 C 0.13311(19) 0.3018(2) 0.6275(3) 0.0352(9) Uani 1 1 d . . . C8 C 0.1705(2) 0.3144(4) 0.5512(4) 0.0638(16) Uani 1 1 d . . . H8 H 0.1530 0.3043 0.4879 0.077 Uiso 1 1 calc R . . C9 C 0.2334(3) 0.3417(4) 0.5654(4) 0.0749(18) Uani 1 1 d . . . H9 H 0.2583 0.3516 0.5120 0.090 Uiso 1 1 calc R . . C10 C 0.2597(2) 0.3544(3) 0.6573(4) 0.0589(14) Uani 1 1 d . . . H10 H 0.3025 0.3743 0.6677 0.071 Uiso 1 1 calc R . . C11 C 0.2241(2) 0.3384(3) 0.7318(4) 0.0552(13) Uani 1 1 d . . . H11 H 0.2429 0.3446 0.7952 0.066 Uiso 1 1 calc R . . C12 C 0.16080(10) 0.31293(14) 0.71843(16) 0.0459(11) Uani 1 1 d . . . H12 H 0.1363 0.3031 0.7724 0.055 Uiso 1 1 calc R . . C13 C 0.00783(10) 0.31246(14) 0.51575(16) 0.0404(10) Uani 1 1 d R . . C14 C 0.02928(10) 0.38333(14) 0.47679(16) 0.0987(11) Uani 1 1 d R . . H14 H 0.0705 0.4042 0.4972 0.118 Uiso 1 1 calc R . . C15 C -0.00962(10) 0.42371(14) 0.40795(16) 0.0987(11) Uani 1 1 d R . . H15 H 0.0050 0.4722 0.3813 0.118 Uiso 1 1 calc R . . C16 C -0.06995(10) 0.39322(14) 0.37807(16) 0.0987(11) Uani 1 1 d R . . H16 H -0.0965 0.4208 0.3310 0.118 Uiso 1 1 calc R . . C17 C -0.09140(10) 0.32235(14) 0.41702(16) 0.0987(11) Uani 1 1 d R . . H17 H -0.1326 0.3015 0.3966 0.118 Uiso 1 1 calc R . . C18 C -0.05251(10) 0.28197(14) 0.48586(16) 0.0987(11) Uani 1 1 d R . . H18 H -0.0672 0.2335 0.5125 0.118 Uiso 1 1 calc R . . C19 C 0.3038(3) 0.3701(4) 0.0388(4) 0.0618(14) Uani 1 1 d . . . C20 C 0.2237(2) 0.4615(3) 0.3170(4) 0.0638(15) Uani 1 1 d . . . H20A H 0.2595 0.4767 0.3636 0.077 Uiso 1 1 calc R . . H20B H 0.2315 0.4871 0.2549 0.077 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 0.03130(12) 0.02252(12) 0.02645(12) 0.000 0.00279(8) 0.000 P1 0.0296(5) 0.0307(6) 0.0260(5) 0.0062(4) 0.0002(4) -0.0059(4) S1 0.0287(5) 0.0470(6) 0.0384(6) 0.0077(5) 0.0032(4) 0.0047(5) Cl1 0.0809(10) 0.0571(8) 0.0668(9) 0.0029(7) 0.0082(7) -0.0013(7) Cl2 0.0621(9) 0.0780(10) 0.0935(12) 0.0077(9) 0.0196(8) 0.0070(8) N1 0.024(2) 0.027(2) 0.026(2) 0.000 0.0041(18) 0.000 N2 0.0269(16) 0.0268(17) 0.0219(15) -0.0006(13) 0.0050(12) 0.0029(13) O1 0.0472(18) 0.064(2) 0.0398(18) -0.0004(16) 0.0041(14) 0.0137(16) O2 0.0343(17) 0.088(3) 0.056(2) -0.0192(19) -0.0049(15) 0.0168(17) O3 0.066(2) 0.068(2) 0.060(2) 0.0363(19) 0.0264(18) 0.0191(19) F1 0.157(4) 0.059(2) 0.097(3) 0.020(2) 0.013(3) -0.026(2) F2 0.120(3) 0.123(3) 0.061(2) -0.022(2) -0.018(2) -0.032(3) F3 0.045(2) 0.152(4) 0.127(3) 0.018(3) -0.006(2) -0.029(2) C1 0.0268(19) 0.031(2) 0.030(2) 0.0023(17) 0.0093(16) -0.0017(16) C2 0.031(2) 0.037(2) 0.024(2) 0.0019(17) 0.0051(16) -0.0038(17) C3 0.0297(19) 0.0241(19) 0.0231(19) 0.0002(15) 0.0022(15) 0.0011(15) C4 0.045(2) 0.026(2) 0.038(2) -0.0036(18) 0.0079(19) 0.0058(18) C5 0.089(4) 0.031(2) 0.083(4) 0.003(3) 0.034(3) 0.012(3) C6 0.064(5) 0.028(3) 0.078(5) 0.000 0.017(4) 0.000 C7 0.035(2) 0.031(2) 0.039(2) 0.0092(18) -0.0021(18) -0.0075(17) C8 0.048(3) 0.097(4) 0.046(3) 0.027(3) -0.003(2) -0.029(3) C9 0.050(3) 0.106(5) 0.069(4) 0.030(3) 0.002(3) -0.031(3) C10 0.041(3) 0.049(3) 0.085(4) 0.008(3) -0.005(3) -0.016(2) C11 0.051(3) 0.055(3) 0.057(3) -0.010(3) -0.017(3) -0.004(2) C12 0.043(3) 0.050(3) 0.044(3) 0.000(2) -0.005(2) -0.003(2) C13 0.036(2) 0.046(3) 0.039(2) 0.016(2) -0.0023(19) -0.0041(19) C14 0.0681(19) 0.110(2) 0.113(3) 0.058(2) -0.0314(17) -0.0063(17) C15 0.0681(19) 0.110(2) 0.113(3) 0.058(2) -0.0314(17) -0.0063(17) C16 0.0681(19) 0.110(2) 0.113(3) 0.058(2) -0.0314(17) -0.0063(17) C17 0.0681(19) 0.110(2) 0.113(3) 0.058(2) -0.0314(17) -0.0063(17) C18 0.0681(19) 0.110(2) 0.113(3) 0.058(2) -0.0314(17) -0.0063(17) C19 0.064(4) 0.074(4) 0.045(3) 0.008(3) -0.009(3) -0.009(3) C20 0.051(3) 0.056(3) 0.085(4) 0.005(3) 0.014(3) -0.002(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 Pt1 C6 2.066(6) . ? Pt1 N1 2.121(4) . ? Pt1 P1 2.2861(10) . ? Pt1 P1 2.2861(10) 2_556 ? P1 C13 1.801(2) . ? P1 C7 1.815(4) . ? P1 C2 1.824(4) . ? S1 O3 1.433(3) . ? S1 O1 1.440(3) . ? S1 O2 1.440(3) . ? S1 C19 1.810(6) . ? Cl1 C20 1.750(5) . ? Cl2 C20 1.745(5) . ? N1 N2 1.350(4) . ? N1 N2 1.350(4) 2_556 ? N2 C3 1.338(5) . ? N2 C1 1.470(4) . ? F1 C19 1.324(6) . ? F2 C19 1.344(6) . ? F3 C19 1.304(7) . ? C1 C2 1.521(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C3 1.370(7) 2_556 ? C3 C4 1.490(5) . ? C4 C5 1.523(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C5 1.515(11) 2_556 ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C12 1.373(5) . ? C7 C8 1.374(6) . ? C8 C9 1.382(7) . ? C8 H8 0.9500 . ? C9 C10 1.379(8) . ? C9 H9 0.9500 . ? C10 C11 1.341(8) . ? C10 H10 0.9500 . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pt1 N1 180.000(1) . . ? C6 Pt1 P1 87.20(3) . . ? N1 Pt1 P1 92.80(3) . . ? C6 Pt1 P1 87.20(3) . 2_556 ? N1 Pt1 P1 92.80(3) . 2_556 ? P1 Pt1 P1 174.40(5) . 2_556 ? C13 P1 C7 109.24(15) . . ? C13 P1 C2 106.75(15) . . ? C7 P1 C2 103.19(19) . . ? C13 P1 Pt1 113.73(9) . . ? C7 P1 Pt1 113.37(14) . . ? C2 P1 Pt1 109.84(13) . . ? O3 S1 O1 114.8(2) . . ? O3 S1 O2 115.0(2) . . ? O1 S1 O2 115.10(19) . . ? O3 S1 C19 102.5(2) . . ? O1 S1 C19 103.5(2) . . ? O2 S1 C19 103.5(3) . . ? N2 N1 N2 103.5(4) . 2_556 ? N2 N1 Pt1 128.27(19) . . ? N2 N1 Pt1 128.26(19) 2_556 . ? C3 N2 N1 112.0(3) . . ? C3 N2 C1 127.0(3) . . ? N1 N2 C1 121.1(3) . . ? N2 C1 C2 112.1(3) . . ? N2 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N2 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 P1 108.8(3) . . ? C1 C2 H2A 109.9 . . ? P1 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? P1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C3 C3 106.3(2) . 2_556 ? N2 C3 C4 128.2(3) . . ? C3 C3 C4 125.5(2) 2_556 . ? C3 C4 C5 107.4(3) . . ? C3 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? C3 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C5 C5 C4 113.5(4) 2_556 . ? C5 C5 H5A 108.9 2_556 . ? C4 C5 H5A 108.9 . . ? C5 C5 H5B 108.9 2_556 . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C12 C7 C8 118.3(4) . . ? C12 C7 P1 119.7(3) . . ? C8 C7 P1 121.6(3) . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.1(5) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 121.5(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C7 C12 C11 120.3(3) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 122.99(17) . . ? C18 C13 P1 116.87(17) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? F3 C19 F1 107.8(5) . . ? F3 C19 F2 109.1(5) . . ? F1 C19 F2 106.8(5) . . ? F3 C19 S1 111.9(4) . . ? F1 C19 S1 111.4(4) . . ? F2 C19 S1 109.8(4) . . ? Cl2 C20 Cl1 112.4(3) . . ? Cl2 C20 H20A 109.1 . . ? Cl1 C20 H20A 109.1 . . ? Cl2 C20 H20B 109.1 . . ? Cl1 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.422 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 961443' data_Gandelman-157 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Gandelman-157 (Yuri)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H61 F12 K N3 O13 P3 Pt S4' _chemical_formula_weight 1715.46 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' 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' S S 0.1246 0.1234 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _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 13.7780(3) _cell_length_b 14.7720(3) _cell_length_c 17.4760(4) _cell_angle_alpha 84.622(1) _cell_angle_beta 82.600(1) _cell_angle_gamma 83.819(1) _cell_volume 3495.21(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23777 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 26.1 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.255 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.155 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _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 'Bruker APEX2 DUO' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 23777 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12873 _reflns_number_gt 11211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2010.7.0.0' _computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 3.0' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12873 _refine_ls_number_parameters 854 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.029 _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 Pt1 Pt 0.798184(15) 0.256634(15) 0.227707(12) 0.02910(12) Uani 1 1 d . . . P1 P 0.88091(13) 0.19541(13) 0.11611(10) 0.0360(4) Uani 1 1 d . . . P3 P 0.64478(12) 0.23204(12) 0.20486(10) 0.0340(4) Uani 1 1 d . . . P2 P 0.74842(12) 0.33459(12) 0.34099(9) 0.0333(4) Uani 1 1 d . . . S1 S 0.7924(2) 0.6310(2) 0.03672(15) 0.0758(8) Uani 1 1 d . . . S2 S 0.13050(18) 0.73141(17) 0.37453(12) 0.0588(5) Uani 1 1 d . . . S3 S 0.2126(2) 1.1044(2) 0.25256(17) 0.0708(7) Uani 1 1 d . . . S4 S -0.11660(15) 0.95615(14) 0.44608(12) 0.0503(5) Uani 1 1 d . . . N1 N 0.9395(4) 0.2675(4) 0.2603(3) 0.0282(11) Uani 1 1 d . . . N2 N 1.0090(4) 0.3136(4) 0.2192(3) 0.0348(12) Uani 1 1 d . . . N3 N 0.9605(4) 0.2617(4) 0.3342(3) 0.0347(12) Uani 1 1 d . . . F1 F 0.7068(15) 0.7891(8) -0.0003(10) 0.236(8) Uani 1 1 d . . . F2 F 0.6794(13) 0.7510(10) 0.1156(8) 0.215(7) Uani 1 1 d . . . F3 F 0.6079(9) 0.6899(8) 0.0411(7) 0.157(4) Uani 1 1 d . . . F4 F 0.2999(8) 0.6536(9) 0.3985(6) 0.171(5) Uani 1 1 d . . . F5 F 0.2413(11) 0.5987(7) 0.3095(6) 0.169(5) Uani 1 1 d . . . F6 F 0.2945(7) 0.7227(9) 0.2829(6) 0.147(4) Uani 1 1 d . . . F7 F 0.3416(8) 1.0170(10) 0.1592(7) 0.184(6) Uani 1 1 d . . . F8 F 0.2203(12) 0.9450(7) 0.2070(8) 0.183(6) Uani 1 1 d . . . F9 F 0.2057(9) 1.0496(9) 0.1158(5) 0.158(5) Uani 1 1 d . . . F10 F -0.2380(7) 0.9088(6) 0.3609(5) 0.113(3) Uani 1 1 d . . . F11 F -0.1336(6) 0.7993(5) 0.3961(6) 0.108(3) Uani 1 1 d . . . F12 F -0.2547(6) 0.8478(7) 0.4742(5) 0.123(3) Uani 1 1 d . . . O1 O 0.7893(6) 0.6098(6) -0.0404(4) 0.079(2) Uani 1 1 d . . . O2 O 0.7656(7) 0.5593(7) 0.0927(5) 0.105(3) Uani 1 1 d . . . O3 O 0.8772(9) 0.6750(9) 0.0476(6) 0.142(5) Uani 1 1 d . . . O4 O 0.0818(7) 0.7479(7) 0.3071(5) 0.093(2) Uani 1 1 d . . . O5 O 0.1560(7) 0.8113(5) 0.4051(5) 0.089(2) Uani 1 1 d . . . O6 O 0.0933(8) 0.6649(8) 0.4320(5) 0.111(3) Uani 1 1 d . . . O7 O 0.1088(6) 1.1130(7) 0.2624(5) 0.100(3) Uani 1 1 d . . . O8 O 0.2493(9) 1.0589(11) 0.3182(6) 0.139(5) Uani 1 1 d . . . O9 O 0.2544(11) 1.1823(8) 0.2205(10) 0.175(6) Uani 1 1 d . . . O10 O -0.0677(6) 0.9080(5) 0.5081(4) 0.076(2) Uani 1 1 d . . . O11 O -0.1863(5) 1.0290(5) 0.4699(4) 0.0737(18) Uani 1 1 d . . . O12 O -0.0521(5) 0.9794(5) 0.3772(4) 0.0698(18) Uani 1 1 d . . . C1 C 1.0723(5) 0.3369(5) 0.2643(4) 0.0396(15) Uani 1 1 d . . . C2 C 1.0405(5) 0.3042(5) 0.3389(4) 0.0387(14) Uani 1 1 d . . . C3 C 1.0177(6) 0.3181(6) 0.1345(4) 0.0464(18) Uani 1 1 d . . . H3A H 1.0813 0.3375 0.1129 0.056 Uiso 1 1 calc R . . H3B H 0.9672 0.3626 0.1160 0.056 Uiso 1 1 calc R . . C4 C 1.0068(6) 0.2258(6) 0.1085(4) 0.0498(19) Uani 1 1 d . . . H4A H 1.0443 0.1798 0.1390 0.060 Uiso 1 1 calc R . . H4B H 1.0355 0.2239 0.0549 0.060 Uiso 1 1 calc R . . C5 C 0.8989(5) 0.2104(5) 0.3940(4) 0.0400(15) Uani 1 1 d . . . H5A H 0.9340 0.1952 0.4389 0.048 Uiso 1 1 calc R . . H5B H 0.8873 0.1536 0.3746 0.048 Uiso 1 1 calc R . . C6 C 0.7990(5) 0.2639(6) 0.4190(4) 0.0436(17) Uani 1 1 d . . . H6A H 0.8071 0.3023 0.4594 0.052 Uiso 1 1 calc R . . H6B H 0.7524 0.2208 0.4408 0.052 Uiso 1 1 calc R . . C7 C 1.0893(6) 0.3113(6) 0.4085(5) 0.0540(19) Uani 1 1 d . . . H7A H 1.1247 0.2533 0.4232 0.065 Uiso 1 1 calc R . . H7B H 1.0409 0.3281 0.4515 0.065 Uiso 1 1 calc R . . C8 C 1.1608(9) 0.3851(9) 0.3879(6) 0.077(3) Uani 1 1 d . . . H8A H 1.1237 0.4447 0.3895 0.092 Uiso 1 1 calc R . . H8B H 1.2058 0.3801 0.4268 0.092 Uiso 1 1 calc R . . C9 C 1.2193(8) 0.3790(9) 0.3098(7) 0.077(3) Uani 1 1 d . . . H9A H 1.2590 0.3206 0.3095 0.093 Uiso 1 1 calc R . . H9B H 1.2641 0.4263 0.3023 0.093 Uiso 1 1 calc R . . C10 C 1.1610(6) 0.3883(6) 0.2423(5) 0.053(2) Uani 1 1 d . . . H10A H 1.1410 0.4522 0.2290 0.064 Uiso 1 1 calc R . . H10B H 1.2008 0.3636 0.1977 0.064 Uiso 1 1 calc R . . C11 C 0.8891(5) 0.0727(5) 0.1199(4) 0.0425(16) Uani 1 1 d . . . C12 C 0.8563(6) 0.0244(7) 0.0659(5) 0.057(2) Uani 1 1 d . . . H12 H 0.8299 0.0546 0.0231 0.069 Uiso 1 1 calc R . . C13 C 0.8636(8) -0.0715(7) 0.0772(8) 0.077(3) Uani 1 1 d . . . H13 H 0.8409 -0.1038 0.0410 0.093 Uiso 1 1 calc R . . C14 C 0.9005(9) -0.1174(7) 0.1361(7) 0.074(3) Uani 1 1 d . . . H14 H 0.9024 -0.1808 0.1420 0.088 Uiso 1 1 calc R . . C15 C 0.9374(9) -0.0697(6) 0.1902(6) 0.072(3) Uani 1 1 d . . . H15 H 0.9670 -0.1009 0.2313 0.087 Uiso 1 1 calc R . . C16 C 0.9286(8) 0.0251(6) 0.1809(6) 0.063(2) Uani 1 1 d . . . H16 H 0.9504 0.0572 0.2176 0.076 Uiso 1 1 calc R . . C17 C 0.8455(6) 0.2505(5) 0.0262(4) 0.0451(17) Uani 1 1 d . . . C18 C 0.7935(6) 0.3377(6) 0.0259(5) 0.0514(18) Uani 1 1 d . . . H18 H 0.7723 0.3629 0.0728 0.062 Uiso 1 1 calc R . . C19 C 0.7735(9) 0.3860(8) -0.0411(6) 0.075(3) Uani 1 1 d . . . H19 H 0.7421 0.4449 -0.0405 0.090 Uiso 1 1 calc R . . C20 C 0.8010(11) 0.3458(9) -0.1113(7) 0.087(4) Uani 1 1 d . . . H20 H 0.7843 0.3765 -0.1574 0.105 Uiso 1 1 calc R . . C21 C 0.8525(11) 0.2610(9) -0.1117(6) 0.090(4) Uani 1 1 d . . . H21 H 0.8725 0.2352 -0.1585 0.108 Uiso 1 1 calc R . . C22 C 0.8744(8) 0.2145(8) -0.0448(5) 0.067(2) Uani 1 1 d . . . H22 H 0.9097 0.1572 -0.0462 0.080 Uiso 1 1 calc R . . C23 C 0.8157(5) 0.4348(5) 0.3292(4) 0.0405(15) Uani 1 1 d . . . C24 C 0.8415(6) 0.4785(5) 0.2561(5) 0.0479(17) Uani 1 1 d . . . H24 H 0.8249 0.4540 0.2130 0.057 Uiso 1 1 calc R . . C25 C 0.8902(7) 0.5561(7) 0.2448(6) 0.067(2) Uani 1 1 d . . . H25 H 0.9003 0.5880 0.1964 0.080 Uiso 1 1 calc R . . C26 C 0.9247(9) 0.5855(7) 0.3123(8) 0.080(3) Uani 1 1 d . . . H26 H 0.9672 0.6311 0.3066 0.096 Uiso 1 1 calc R . . C27 C 0.8959(9) 0.5477(7) 0.3822(7) 0.079(3) Uani 1 1 d . . . H27 H 0.9093 0.5747 0.4252 0.095 Uiso 1 1 calc R . . C28 C 0.8467(8) 0.4694(7) 0.3938(5) 0.062(2) Uani 1 1 d . . . H28 H 0.8343 0.4403 0.4431 0.074 Uiso 1 1 calc R . . C29 C 0.6237(6) 0.3753(6) 0.3811(5) 0.054(2) Uani 1 1 d . . . C30 C 0.5702(7) 0.3268(7) 0.4395(6) 0.066(2) Uani 1 1 d . . . H30 H 0.5960 0.2696 0.4588 0.079 Uiso 1 1 calc R . . C31 C 0.4786(8) 0.3626(11) 0.4696(8) 0.095(4) Uani 1 1 d . . . H31 H 0.4457 0.3333 0.5132 0.114 Uiso 1 1 calc R . . C32 C 0.4342(8) 0.4437(12) 0.4343(10) 0.106(5) Uani 1 1 d . . . H32 H 0.3691 0.4646 0.4493 0.127 Uiso 1 1 calc R . . C33 C 0.4886(10) 0.4886(10) 0.3794(8) 0.102(5) Uani 1 1 d . . . H33 H 0.4621 0.5447 0.3588 0.123 Uiso 1 1 calc R . . C34 C 0.5833(8) 0.4570(10) 0.3505(7) 0.088(4) Uani 1 1 d . . . H34 H 0.6187 0.4909 0.3110 0.106 Uiso 1 1 calc R . . C35 C 0.5685(5) 0.3325(5) 0.1705(4) 0.0431(16) Uani 1 1 d . . . C36 C 0.4794(6) 0.3236(7) 0.1491(5) 0.060(2) Uani 1 1 d . . . H36 H 0.4566 0.2663 0.1511 0.072 Uiso 1 1 calc R . . C37 C 0.4213(7) 0.4031(8) 0.1236(6) 0.075(3) Uani 1 1 d . . . H37 H 0.3600 0.3980 0.1086 0.090 Uiso 1 1 calc R . . C38 C 0.4557(9) 0.4897(9) 0.1208(10) 0.102(5) Uani 1 1 d . . . H38 H 0.4181 0.5415 0.1027 0.122 Uiso 1 1 calc R . . C39 C 0.5427(9) 0.4970(8) 0.1443(8) 0.083(3) Uani 1 1 d . . . H39 H 0.5642 0.5546 0.1440 0.099 Uiso 1 1 calc R . . C40 C 0.6028(6) 0.4194(6) 0.1698(6) 0.057(2) Uani 1 1 d . . . H40 H 0.6635 0.4253 0.1857 0.069 Uiso 1 1 calc R . . C41 C 0.6340(6) 0.1471(6) 0.1370(5) 0.0501(19) Uani 1 1 d . . . C42 C 0.6258(6) 0.1759(8) 0.0600(5) 0.064(3) Uani 1 1 d . . . H42 H 0.6296 0.2369 0.0423 0.077 Uiso 1 1 calc R . . C43 C 0.6112(8) 0.1091(12) 0.0074(8) 0.104(5) Uani 1 1 d . . . H43 H 0.6036 0.1254 -0.0443 0.125 Uiso 1 1 calc R . . C44 C 0.6094(9) 0.0156(12) 0.0408(11) 0.119(7) Uani 1 1 d . . . H44 H 0.6028 -0.0300 0.0091 0.143 Uiso 1 1 calc R . . C45 C 0.6169(9) -0.0064(9) 0.1146(9) 0.084(3) Uani 1 1 d . . . H45 H 0.6137 -0.0670 0.1338 0.100 Uiso 1 1 calc R . . C46 C 0.6293(8) 0.0562(7) 0.1635(7) 0.079(3) Uani 1 1 d . . . H46 H 0.6346 0.0380 0.2153 0.095 Uiso 1 1 calc R . . C47 C 0.5821(5) 0.1834(5) 0.2963(4) 0.0401(15) Uani 1 1 d . . . C48 C 0.4797(6) 0.2020(7) 0.3143(6) 0.060(2) Uani 1 1 d . . . H48 H 0.4426 0.2413 0.2821 0.072 Uiso 1 1 calc R . . C49 C 0.4371(7) 0.1594(8) 0.3815(6) 0.071(3) Uani 1 1 d . . . H49 H 0.3691 0.1668 0.3932 0.085 Uiso 1 1 calc R . . C50 C 0.4922(7) 0.1059(9) 0.4320(7) 0.082(4) Uani 1 1 d . . . H50 H 0.4618 0.0824 0.4792 0.099 Uiso 1 1 calc R . . C51 C 0.5899(7) 0.0872(7) 0.4137(6) 0.070(3) Uani 1 1 d . . . H51 H 0.6267 0.0480 0.4462 0.084 Uiso 1 1 calc R . . C52 C 0.6350(5) 0.1285(5) 0.3442(5) 0.0484(18) Uani 1 1 d . . . H52 H 0.7026 0.1174 0.3313 0.058 Uiso 1 1 calc R . . C53 C 0.6930(16) 0.7203(11) 0.0492(12) 0.125(7) Uani 1 1 d . . . C54 C 0.2442(13) 0.6781(12) 0.3413(9) 0.115(6) Uani 1 1 d . . . C55 C 0.2472(11) 1.0283(12) 0.1741(9) 0.105(5) Uani 1 1 d . . . C56 C -0.1910(7) 0.8730(7) 0.4170(6) 0.060(2) Uani 1 1 d . . . K5 K 0.1238(3) 0.9673(2) 0.38897(19) 0.1019(9) Uani 1 1 d . . . O13 O 0.531(2) 0.7974(18) 0.348(2) 0.36(2) Uani 1 1 d D . . C58 C 0.549(4) 0.738(4) 0.288(3) 0.36(3) Uiso 1 1 d D . . H58A H 0.5461 0.7684 0.2363 0.437 Uiso 1 1 calc R . . H58B H 0.5102 0.6859 0.2959 0.437 Uiso 1 1 calc R . . C59 C 0.654(4) 0.718(4) 0.312(3) 0.41(3) Uiso 1 1 d D . . H59A H 0.6938 0.6787 0.2764 0.617 Uiso 1 1 calc R . . H59B H 0.6511 0.6878 0.3632 0.617 Uiso 1 1 calc R . . H59C H 0.6837 0.7740 0.3108 0.617 Uiso 1 1 calc R . . C60 C 0.474(2) 0.8751(18) 0.3183(19) 0.221(13) Uiso 1 1 d D . . H60A H 0.4486 0.8654 0.2709 0.266 Uiso 1 1 calc R . . H60B H 0.5083 0.9301 0.3116 0.266 Uiso 1 1 calc R . . C61 C 0.398(3) 0.873(3) 0.389(2) 0.274(18) Uiso 1 1 d D . . H61A H 0.3627 0.9323 0.3928 0.411 Uiso 1 1 calc R . . H61B H 0.4293 0.8551 0.4342 0.411 Uiso 1 1 calc R . . H61C H 0.3523 0.8294 0.3833 0.411 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 0.02697(16) 0.03490(17) 0.02566(17) -0.00231(10) -0.00190(10) -0.00567(10) P1 0.0359(9) 0.0455(9) 0.0262(8) -0.0088(7) 0.0014(7) -0.0030(7) P3 0.0274(8) 0.0406(9) 0.0355(9) -0.0067(7) -0.0034(7) -0.0069(7) P2 0.0337(8) 0.0403(9) 0.0255(8) -0.0036(6) -0.0035(6) -0.0007(7) S1 0.0879(18) 0.0980(19) 0.0470(13) 0.0039(12) -0.0002(12) -0.0526(16) S2 0.0663(13) 0.0717(13) 0.0410(11) -0.0060(9) -0.0094(9) -0.0142(11) S3 0.0654(15) 0.0775(16) 0.0716(16) -0.0196(13) -0.0126(12) 0.0008(12) S4 0.0511(11) 0.0492(10) 0.0478(11) 0.0040(8) -0.0055(9) 0.0010(8) N1 0.023(2) 0.037(3) 0.024(3) 0.000(2) -0.009(2) -0.001(2) N2 0.033(3) 0.041(3) 0.029(3) 0.001(2) 0.001(2) -0.010(2) N3 0.034(3) 0.038(3) 0.031(3) -0.003(2) -0.001(2) -0.007(2) F1 0.35(2) 0.088(7) 0.248(16) 0.028(9) 0.049(15) -0.058(10) F2 0.295(19) 0.182(12) 0.162(11) -0.098(10) 0.035(11) -0.008(12) F3 0.144(9) 0.140(9) 0.165(10) -0.009(7) 0.044(8) 0.005(7) F4 0.162(9) 0.204(11) 0.126(7) -0.022(7) -0.053(7) 0.124(9) F5 0.268(15) 0.100(7) 0.133(8) -0.053(6) -0.026(9) 0.048(8) F6 0.096(6) 0.234(13) 0.103(7) -0.031(7) 0.039(5) -0.021(7) F7 0.109(8) 0.271(16) 0.159(10) -0.085(10) 0.014(7) 0.064(9) F8 0.264(16) 0.086(6) 0.205(13) -0.052(7) -0.032(11) 0.001(8) F9 0.173(10) 0.223(12) 0.073(5) -0.040(6) -0.035(6) 0.057(9) F10 0.127(6) 0.117(6) 0.110(6) -0.004(5) -0.057(5) -0.027(5) F11 0.091(5) 0.071(4) 0.165(8) -0.045(5) -0.002(5) -0.006(4) F12 0.108(6) 0.143(7) 0.122(7) -0.021(5) 0.028(5) -0.076(6) O1 0.080(5) 0.110(6) 0.053(4) -0.008(4) -0.005(3) -0.038(4) O2 0.114(7) 0.133(8) 0.073(5) 0.038(5) -0.017(5) -0.068(6) O3 0.162(10) 0.209(12) 0.076(6) 0.003(7) -0.005(6) -0.135(10) O4 0.093(6) 0.129(7) 0.061(4) 0.008(4) -0.029(4) -0.019(5) O5 0.108(6) 0.078(5) 0.088(5) -0.038(4) -0.028(5) 0.008(4) O6 0.137(8) 0.142(8) 0.058(5) 0.023(5) -0.004(5) -0.058(7) O7 0.073(5) 0.124(7) 0.098(6) -0.035(5) -0.003(4) 0.023(5) O8 0.121(8) 0.215(13) 0.085(7) -0.019(7) -0.051(6) 0.022(8) O9 0.185(13) 0.100(8) 0.235(16) -0.042(9) 0.055(12) -0.058(9) O10 0.087(5) 0.066(4) 0.077(5) 0.013(3) -0.042(4) 0.010(4) O11 0.073(4) 0.063(4) 0.081(5) -0.013(3) -0.003(4) 0.009(3) O12 0.077(4) 0.078(4) 0.054(4) -0.002(3) 0.004(3) -0.021(4) C1 0.035(3) 0.042(4) 0.043(4) -0.001(3) -0.007(3) -0.008(3) C2 0.034(3) 0.048(4) 0.036(4) -0.007(3) -0.006(3) -0.008(3) C3 0.042(4) 0.060(5) 0.038(4) 0.004(3) 0.001(3) -0.026(4) C4 0.043(4) 0.073(5) 0.032(4) -0.014(3) 0.015(3) -0.014(4) C5 0.048(4) 0.034(3) 0.035(4) 0.011(3) -0.003(3) -0.008(3) C6 0.032(3) 0.070(5) 0.029(3) 0.005(3) -0.007(3) -0.012(3) C7 0.050(4) 0.072(5) 0.045(4) -0.006(4) -0.020(4) -0.011(4) C8 0.086(7) 0.097(8) 0.059(6) -0.006(5) -0.025(5) -0.044(6) C9 0.064(6) 0.101(8) 0.075(7) -0.012(6) -0.008(5) -0.043(6) C10 0.048(4) 0.061(5) 0.054(5) 0.003(4) -0.003(4) -0.028(4) C11 0.038(4) 0.044(4) 0.043(4) -0.010(3) 0.006(3) 0.000(3) C12 0.052(5) 0.073(6) 0.052(5) -0.023(4) -0.011(4) -0.008(4) C13 0.068(6) 0.068(6) 0.103(9) -0.048(6) -0.004(6) -0.012(5) C14 0.091(7) 0.045(5) 0.076(7) -0.007(5) 0.011(6) 0.009(5) C15 0.097(8) 0.047(5) 0.068(6) 0.000(4) -0.006(5) 0.008(5) C16 0.083(7) 0.055(5) 0.053(5) -0.011(4) -0.002(5) -0.007(4) C17 0.043(4) 0.056(4) 0.036(4) -0.009(3) 0.000(3) -0.005(3) C18 0.052(4) 0.052(4) 0.051(5) 0.002(3) -0.019(4) -0.001(3) C19 0.090(7) 0.075(6) 0.055(6) 0.004(5) -0.018(5) 0.015(5) C20 0.122(10) 0.087(8) 0.054(6) 0.013(5) -0.034(6) -0.001(7) C21 0.126(10) 0.106(9) 0.036(5) -0.005(5) -0.010(6) -0.001(8) C22 0.077(6) 0.085(7) 0.033(4) -0.011(4) 0.002(4) 0.004(5) C23 0.041(4) 0.046(4) 0.036(4) -0.005(3) -0.009(3) -0.004(3) C24 0.050(4) 0.043(4) 0.052(4) 0.001(3) -0.013(3) -0.006(3) C25 0.063(6) 0.064(5) 0.076(6) 0.004(5) -0.013(5) -0.022(4) C26 0.081(7) 0.062(6) 0.109(9) -0.012(6) -0.034(6) -0.028(5) C27 0.104(8) 0.058(5) 0.089(8) -0.025(5) -0.041(7) -0.018(5) C28 0.078(6) 0.066(5) 0.047(5) -0.020(4) -0.010(4) -0.014(5) C29 0.041(4) 0.075(5) 0.042(4) -0.030(4) 0.014(3) 0.006(4) C30 0.058(5) 0.056(5) 0.079(7) -0.008(5) 0.009(5) 0.004(4) C31 0.054(6) 0.127(11) 0.107(9) -0.050(9) 0.027(6) -0.028(7) C32 0.040(5) 0.147(13) 0.132(12) -0.062(11) 0.004(7) 0.015(7) C33 0.082(8) 0.111(10) 0.091(9) 0.008(7) -0.003(7) 0.066(8) C34 0.052(6) 0.136(11) 0.074(7) -0.036(7) 0.011(5) 0.009(6) C35 0.041(4) 0.049(4) 0.037(4) 0.002(3) -0.001(3) -0.003(3) C36 0.043(4) 0.078(6) 0.055(5) 0.005(4) -0.009(4) 0.001(4) C37 0.041(5) 0.106(8) 0.071(6) 0.017(6) -0.015(4) 0.009(5) C38 0.066(7) 0.084(8) 0.141(13) 0.025(8) 0.003(8) 0.013(6) C39 0.071(7) 0.060(6) 0.106(9) 0.025(6) -0.009(6) 0.013(5) C40 0.041(4) 0.051(4) 0.079(6) 0.020(4) -0.021(4) -0.001(3) C41 0.037(4) 0.066(5) 0.050(5) -0.025(4) 0.003(3) -0.009(3) C42 0.045(4) 0.100(7) 0.055(5) -0.037(5) -0.012(4) -0.011(4) C43 0.054(6) 0.173(15) 0.099(9) -0.084(10) -0.019(6) -0.001(7) C44 0.072(8) 0.141(14) 0.161(16) -0.104(13) 0.020(9) -0.047(8) C45 0.073(7) 0.081(7) 0.104(10) -0.043(7) -0.002(6) -0.018(6) C46 0.080(7) 0.062(6) 0.094(8) -0.043(5) 0.038(6) -0.030(5) C47 0.033(3) 0.041(4) 0.046(4) -0.008(3) 0.003(3) -0.009(3) C48 0.034(4) 0.075(6) 0.066(6) 0.011(4) -0.006(4) -0.003(4) C49 0.038(4) 0.103(8) 0.063(6) 0.029(5) 0.007(4) -0.008(5) C50 0.045(5) 0.110(8) 0.084(7) 0.050(6) -0.009(5) -0.021(5) C51 0.064(6) 0.071(6) 0.068(6) 0.025(5) 0.004(5) -0.016(5) C52 0.031(3) 0.052(4) 0.059(5) 0.006(3) 0.004(3) -0.006(3) C53 0.153(17) 0.083(10) 0.130(14) -0.028(9) 0.051(12) -0.030(10) C54 0.131(13) 0.130(12) 0.083(9) -0.041(9) -0.034(9) 0.048(10) C55 0.094(10) 0.119(12) 0.106(11) -0.043(9) -0.036(8) 0.029(8) C56 0.061(5) 0.067(6) 0.052(5) -0.007(4) 0.000(4) -0.010(4) K5 0.109(2) 0.098(2) 0.096(2) -0.0080(16) -0.0107(17) -0.0018(17) O13 0.32(3) 0.27(3) 0.54(5) -0.11(3) -0.32(4) 0.15(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 Pt1 N1 2.124(5) . ? Pt1 P3 2.2734(17) . ? Pt1 P1 2.3359(16) . ? Pt1 P2 2.3713(16) . ? P1 C17 1.800(8) . ? P1 C11 1.799(7) . ? P1 C4 1.823(8) . ? P3 C35 1.824(8) . ? P3 C41 1.835(8) . ? P3 C47 1.838(8) . ? P2 C6 1.804(7) . ? P2 C23 1.812(7) . ? P2 C29 1.831(7) . ? S1 O2 1.419(8) . ? S1 O1 1.420(7) . ? S1 O3 1.438(9) . ? S1 C53 1.80(2) . ? S2 O6 1.423(8) . ? S2 O4 1.418(8) . ? S2 O5 1.435(8) . ? S2 C54 1.731(16) . ? S2 K5 3.507(4) . ? S3 O9 1.381(12) . ? S3 O8 1.399(11) . ? S3 O7 1.411(9) . ? S3 C55 1.838(14) . ? S3 K5 3.188(5) . ? S4 O11 1.419(7) . ? S4 O10 1.441(6) . ? S4 O12 1.438(7) . ? S4 C56 1.828(10) . ? S4 K5 3.180(4) 2_576 ? S4 K5 3.351(4) . ? N1 N2 1.330(7) . ? N1 N3 1.351(7) . ? N2 C1 1.338(9) . ? N2 C3 1.466(9) . ? N3 C2 1.341(9) . ? N3 C5 1.466(8) . ? F1 C53 1.29(2) . ? F2 C53 1.27(2) . ? F3 C53 1.33(2) . ? F4 C54 1.336(16) . ? F5 C54 1.352(18) . ? F6 C54 1.32(2) . ? F7 C55 1.289(18) . ? F8 C55 1.38(2) . ? F8 K5 3.318(15) . ? F9 C55 1.231(16) . ? F10 C56 1.286(12) . ? F11 C56 1.325(12) . ? F12 C56 1.298(12) . ? O5 K5 2.296(9) . ? O7 K5 2.949(11) . ? O8 K5 2.447(15) . ? O10 K5 2.680(8) 2_576 ? O10 K5 3.288(9) . ? O11 K5 2.723(8) 2_576 ? O12 K5 2.445(8) . ? C1 C2 1.380(10) . ? C1 C10 1.497(10) . ? C2 C7 1.481(10) . ? C3 C4 1.506(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.545(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.534(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.498(16) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.498(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.362(13) . ? C11 C12 1.382(11) . ? C12 C13 1.405(14) . ? C12 H12 0.9300 . ? C13 C14 1.306(16) . ? C13 H13 0.9300 . ? C14 C15 1.407(16) . ? C14 H14 0.9300 . ? C15 C16 1.389(13) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.389(11) . ? C17 C18 1.405(11) . ? C18 C19 1.357(12) . ? C18 H18 0.9300 . ? C19 C20 1.404(17) . ? C19 H19 0.9300 . ? C20 C21 1.372(18) . ? C20 H20 0.9300 . ? C21 C22 1.352(15) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.397(11) . ? C23 C28 1.413(11) . ? C24 C25 1.375(12) . ? C24 H24 0.9300 . ? C25 C26 1.445(15) . ? C25 H25 0.9300 . ? C26 C27 1.325(17) . ? C26 H26 0.9300 . ? C27 C28 1.390(14) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.372(13) . ? C29 C34 1.366(16) . ? C30 C31 1.374(14) . ? C30 H30 0.9300 . ? C31 C32 1.41(2) . ? C31 H31 0.9300 . ? C32 C33 1.31(2) . ? C32 H32 0.9300 . ? C33 C34 1.385(15) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.352(12) . ? C35 C40 1.413(11) . ? C36 C37 1.418(13) . ? C36 H36 0.9300 . ? C37 C38 1.405(18) . ? C37 H37 0.9300 . ? C38 C39 1.334(19) . ? C38 H38 0.9300 . ? C39 C40 1.411(12) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C46 1.384(14) . ? C41 C42 1.388(13) . ? C42 C43 1.454(14) . ? C42 H42 0.9300 . ? C43 C44 1.45(2) . ? C43 H43 0.9300 . ? C44 C45 1.31(2) . ? C44 H44 0.9300 . ? C45 C46 1.355(14) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.339(11) . ? C47 C48 1.408(11) . ? C48 C49 1.372(12) . ? C48 H48 0.9300 . ? C49 C50 1.376(13) . ? C49 H49 0.9300 . ? C50 C51 1.348(14) . ? C50 H50 0.9300 . ? C51 C52 1.407(12) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? K5 O10 2.680(8) 2_576 ? K5 O11 2.723(8) 2_576 ? K5 S4 3.180(4) 2_576 ? O13 C60 1.418(10) . ? O13 C58 1.419(10) . ? C58 C59 1.56(4) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.51(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 P3 173.15(14) . . ? N1 Pt1 P1 86.44(15) . . ? P3 Pt1 P1 96.14(6) . . ? N1 Pt1 P2 81.48(15) . . ? P3 Pt1 P2 96.49(6) . . ? P1 Pt1 P2 166.73(6) . . ? C17 P1 C11 113.3(4) . . ? C17 P1 C4 99.9(4) . . ? C11 P1 C4 106.3(4) . . ? C17 P1 Pt1 115.3(3) . . ? C11 P1 Pt1 114.0(2) . . ? C4 P1 Pt1 106.2(2) . . ? C35 P3 C41 103.8(4) . . ? C35 P3 C47 108.4(3) . . ? C41 P3 C47 102.8(4) . . ? C35 P3 Pt1 115.9(2) . . ? C41 P3 Pt1 117.9(3) . . ? C47 P3 Pt1 107.1(2) . . ? C6 P2 C23 104.5(3) . . ? C6 P2 C29 105.1(4) . . ? C23 P2 C29 104.8(4) . . ? C6 P2 Pt1 106.2(3) . . ? C23 P2 Pt1 105.8(2) . . ? C29 P2 Pt1 128.3(3) . . ? O2 S1 O1 113.2(5) . . ? O2 S1 O3 116.6(6) . . ? O1 S1 O3 114.4(5) . . ? O2 S1 C53 104.9(7) . . ? O1 S1 C53 102.3(8) . . ? O3 S1 C53 103.3(9) . . ? O6 S2 O4 116.4(6) . . ? O6 S2 O5 114.1(6) . . ? O4 S2 O5 115.4(6) . . ? O6 S2 C54 102.0(8) . . ? O4 S2 C54 103.5(6) . . ? O5 S2 C54 102.6(7) . . ? O6 S2 K5 127.3(5) . . ? O4 S2 K5 90.3(4) . . ? O5 S2 K5 25.5(4) . . ? C54 S2 K5 115.2(7) . . ? O9 S3 O8 117.7(10) . . ? O9 S3 O7 114.7(8) . . ? O8 S3 O7 110.7(7) . . ? O9 S3 C55 101.0(9) . . ? O8 S3 C55 106.4(8) . . ? O7 S3 C55 104.6(6) . . ? O9 S3 K5 155.9(7) . . ? O8 S3 K5 46.6(6) . . ? O7 S3 K5 67.4(4) . . ? C55 S3 K5 101.4(6) . . ? O11 S4 O10 113.8(5) . . ? O11 S4 O12 113.9(5) . . ? O10 S4 O12 114.5(5) . . ? O11 S4 C56 104.1(5) . . ? O10 S4 C56 104.4(5) . . ? O12 S4 C56 104.4(4) . . ? O11 S4 K5 58.5(3) . 2_576 ? O10 S4 K5 56.9(3) . 2_576 ? O12 S4 K5 127.0(3) . 2_576 ? C56 S4 K5 128.6(3) . 2_576 ? O11 S4 K5 126.8(3) . . ? O10 S4 K5 75.0(3) . . ? O12 S4 K5 40.6(3) . . ? C56 S4 K5 125.1(3) . . ? K5 S4 K5 97.75(10) 2_576 . ? N2 N1 N3 105.3(5) . . ? N2 N1 Pt1 125.5(4) . . ? N3 N1 Pt1 124.6(4) . . ? C1 N2 N1 111.3(5) . . ? C1 N2 C3 128.6(6) . . ? N1 N2 C3 119.1(5) . . ? C2 N3 N1 110.7(5) . . ? C2 N3 C5 130.5(6) . . ? N1 N3 C5 118.7(5) . . ? C55 F8 K5 108.9(8) . . ? S2 O5 K5 139.0(5) . . ? S3 O7 K5 86.4(5) . . ? S3 O8 K5 108.9(7) . . ? S4 O10 K5 96.4(4) . 2_576 ? S4 O10 K5 79.9(3) . . ? K5 O10 K5 110.7(3) 2_576 . ? S4 O11 K5 95.1(4) . 2_576 ? S4 O12 K5 116.9(4) . . ? N2 C1 C2 106.5(6) . . ? N2 C1 C10 129.2(7) . . ? C2 C1 C10 124.3(7) . . ? N3 C2 C1 106.1(6) . . ? N3 C2 C7 127.8(7) . . ? C1 C2 C7 126.0(7) . . ? N2 C3 C4 110.0(6) . . ? N2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 P1 115.4(6) . . ? C3 C4 H4A 108.4 . . ? P1 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? P1 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C6 112.8(5) . . ? N3 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N3 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 P2 113.7(5) . . ? C5 C6 H6A 108.8 . . ? P2 C6 H6A 108.8 . . ? C5 C6 H6B 108.8 . . ? P2 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C2 C7 C8 107.2(7) . . ? C2 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? C2 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C9 C8 C7 113.8(8) . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 115.9(9) . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C1 C10 C9 108.4(7) . . ? C1 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? C1 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 118.3(8) . . ? C16 C11 P1 117.4(6) . . ? C12 C11 P1 124.3(7) . . ? C11 C12 C13 118.6(9) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C14 C13 C12 123.3(9) . . ? C14 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C13 C14 C15 119.0(9) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 118.3(10) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C11 C16 C15 122.4(9) . . ? C11 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C22 C17 C18 117.6(8) . . ? C22 C17 P1 123.1(7) . . ? C18 C17 P1 119.1(6) . . ? C19 C18 C17 121.5(9) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.1(10) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.8(9) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.5(10) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C17 121.5(10) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? C24 C23 C28 117.9(7) . . ? C24 C23 P2 121.4(5) . . ? C28 C23 P2 120.7(6) . . ? C25 C24 C23 123.2(8) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 116.4(10) . . ? C24 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? C27 C26 C25 120.2(9) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 122.6(9) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 118.7(9) . . ? C27 C28 H28 120.7 . . ? C23 C28 H28 120.7 . . ? C30 C29 C34 119.6(8) . . ? C30 C29 P2 122.6(7) . . ? C34 C29 P2 117.8(7) . . ? C29 C30 C31 120.0(10) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 120.0(12) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 117.4(10) . . ? C33 C32 H32 121.3 . . ? C31 C32 H32 121.3 . . ? C32 C33 C34 123.8(12) . . ? C32 C33 H33 118.1 . . ? C34 C33 H33 118.1 . . ? C33 C34 C29 118.7(12) . . ? C33 C34 H34 120.7 . . ? C29 C34 H34 120.6 . . ? C36 C35 C40 121.1(8) . . ? C36 C35 P3 120.2(7) . . ? C40 C35 P3 118.7(6) . . ? C35 C36 C37 118.8(9) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 120.6(10) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.4(11) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 121.6(11) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C39 C40 C35 118.4(8) . . ? C39 C40 H40 120.8 . . ? C35 C40 H40 120.8 . . ? C46 C41 C42 120.7(8) . . ? C46 C41 P3 120.0(7) . . ? C42 C41 P3 119.2(7) . . ? C41 C42 C43 119.0(12) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C44 C43 C42 115.8(13) . . ? C44 C43 H43 122.1 . . ? C42 C43 H43 122.1 . . ? C45 C44 C43 121.7(11) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C44 C45 C46 122.3(14) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C45 C46 C41 120.5(12) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.7 . . ? C52 C47 C48 120.9(7) . . ? C52 C47 P3 118.9(5) . . ? C48 C47 P3 120.2(6) . . ? C49 C48 C47 117.0(8) . . ? C49 C48 H48 121.5 . . ? C47 C48 H48 121.5 . . ? C50 C49 C48 121.8(8) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C51 C50 C49 120.6(9) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 118.5(9) . . ? C50 C51 H51 120.8 . . ? C52 C51 H51 120.8 . . ? C47 C52 C51 121.0(7) . . ? C47 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? F2 C53 F1 106.5(15) . . ? F2 C53 F3 104.6(16) . . ? F1 C53 F3 109(2) . . ? F2 C53 S1 114.7(19) . . ? F1 C53 S1 111.3(14) . . ? F3 C53 S1 110.8(11) . . ? F6 C54 F4 110.4(17) . . ? F6 C54 F5 99.3(12) . . ? F4 C54 F5 103.0(13) . . ? F6 C54 S2 115.7(12) . . ? F4 C54 S2 112.1(10) . . ? F5 C54 S2 114.9(14) . . ? F9 C55 F7 113.0(16) . . ? F9 C55 F8 109.1(16) . . ? F7 C55 F8 105.1(14) . . ? F9 C55 S3 115.1(11) . . ? F7 C55 S3 109.9(11) . . ? F8 C55 S3 103.7(11) . . ? F10 C56 F12 108.2(10) . . ? F10 C56 F11 110.6(9) . . ? F12 C56 F11 107.9(10) . . ? F10 C56 S4 109.8(7) . . ? F12 C56 S4 110.5(7) . . ? F11 C56 S4 109.7(7) . . ? O5 K5 O12 100.1(3) . . ? O5 K5 O8 119.5(4) . . ? O12 K5 O8 128.5(3) . . ? O5 K5 O10 131.4(3) . 2_576 ? O12 K5 O10 83.1(2) . 2_576 ? O8 K5 O10 92.6(4) . 2_576 ? O5 K5 O11 86.5(3) . 2_576 ? O12 K5 O11 120.1(2) . 2_576 ? O8 K5 O11 95.5(3) . 2_576 ? O10 K5 O11 52.66(19) 2_576 2_576 ? O5 K5 O7 139.1(3) . . ? O12 K5 O7 78.9(2) . . ? O8 K5 O7 49.7(3) . . ? O10 K5 O7 89.4(2) 2_576 . ? O11 K5 O7 129.8(3) 2_576 . ? O5 K5 S4 107.5(2) . 2_576 ? O12 K5 S4 99.7(2) . 2_576 ? O8 K5 S4 98.2(3) . 2_576 ? O10 K5 S4 26.76(13) 2_576 2_576 ? O11 K5 S4 26.39(14) 2_576 2_576 ? O7 K5 S4 113.0(2) . 2_576 ? O5 K5 S3 128.2(3) . . ? O12 K5 S3 104.8(2) . . ? O8 K5 S3 24.5(2) . . ? O10 K5 S3 96.5(2) 2_576 . ? O11 K5 S3 117.0(2) 2_576 . ? O7 K5 S3 26.22(18) . . ? S4 K5 S3 111.98(12) 2_576 . ? O5 K5 O10 77.8(3) . . ? O12 K5 O10 47.2(2) . . ? O8 K5 O10 161.3(4) . . ? O10 K5 O10 69.3(3) 2_576 . ? O11 K5 O10 77.6(2) 2_576 . ? O7 K5 O10 122.7(2) . . ? S4 K5 O10 67.85(15) 2_576 . ? S3 K5 O10 148.43(16) . . ? O5 K5 F8 85.1(3) . . ? O12 K5 F8 101.4(3) . . ? O8 K5 F8 55.2(4) . . ? O10 K5 F8 142.4(3) 2_576 . ? O11 K5 F8 138.5(3) 2_576 . ? O7 K5 F8 55.8(3) . . ? S4 K5 F8 153.0(3) 2_576 . ? S3 K5 F8 46.0(2) . . ? O10 K5 F8 139.1(3) . . ? O5 K5 S4 92.1(3) . . ? O12 K5 S4 22.50(16) . . ? O8 K5 S4 146.0(3) . . ? O10 K5 S4 72.59(19) 2_576 . ? O11 K5 S4 98.88(19) 2_576 . ? O7 K5 S4 98.66(19) . . ? S4 K5 S4 82.25(10) 2_576 . ? S3 K5 S4 124.88(12) . . ? O10 K5 S4 25.05(11) . . ? F8 K5 S4 122.0(3) . . ? O5 K5 S2 15.6(2) . . ? O12 K5 S2 88.3(2) . . ? O8 K5 S2 122.2(3) . . ? O10 K5 S2 140.2(2) 2_576 . ? O11 K5 S2 101.24(18) 2_576 . ? O7 K5 S2 126.9(2) . . ? S4 K5 S2 119.90(11) 2_576 . ? S3 K5 S2 123.19(11) . . ? O10 K5 S2 76.39(15) . . ? F8 K5 S2 77.4(2) . . ? S4 K5 S2 84.86(10) . . ? C60 O13 C58 105(3) . . ? O13 C58 C59 86(3) . . ? O13 C58 H58A 114.4 . . ? C59 C58 H58A 114.4 . . ? O13 C58 H58B 114.4 . . ? C59 C58 H58B 114.4 . . ? H58A C58 H58B 111.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O13 C60 C61 93(2) . . ? O13 C60 H60A 113.1 . . ? C61 C60 H60A 113.2 . . ? O13 C60 H60B 113.2 . . ? C61 C60 H60B 113.2 . . ? H60A C60 H60B 110.5 . . ? C60 C61 H61A 109.4 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? loop_ # start Validation Reply Form _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for O8 RESPONSE: Slightly disordered CF3-SO3 group ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.623 _refine_diff_density_min -2.992 _refine_diff_density_rms 0.291 _database_code_depnum_ccdc_archive 'CCDC 961444' data_Gandelman-155 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Gandelman-155 (Saha)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 F12 N3 O3.50 P4 Rh' _chemical_formula_weight 1193.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.854(2) _cell_length_b 22.376(3) _cell_length_c 19.553(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.609(4) _cell_angle_gamma 90.00 _cell_volume 5709.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(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 'Bruker APEX2 DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 19090 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.25 _reflns_number_total 10067 _reflns_number_gt 7559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v2010.7.0.0' _computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1817P)^2^+3.2076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10067 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.2551 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.012 _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 0.25328(3) 0.107160(17) -0.07037(2) 0.03474(19) Uani 1 1 d . . . P1 P 0.39273(10) 0.13522(6) 0.02791(7) 0.0335(3) Uani 1 1 d . . . P2 P 0.11777(10) 0.08139(6) -0.17296(7) 0.0376(3) Uani 1 1 d . . . P3 P 0.40557(17) 0.13922(9) -0.32078(11) 0.0668(5) Uani 1 1 d . . . P4 P 0.00899(17) 0.28662(13) -0.42761(12) 0.0849(7) Uani 1 1 d . . . C35 C 0.2471(6) 0.0189(3) -0.0291(4) 0.0592(17) Uani 1 1 d . . . H35A H 0.2584 0.0213 0.0220 0.071 Uiso 1 1 d R . . H35B H 0.1808 0.0019 -0.0535 0.071 Uiso 1 1 d R . . N1 N 0.2228(3) 0.24050(19) -0.0470(2) 0.0385(10) Uani 1 1 d . . . N2 N 0.2198(3) 0.1965(2) -0.0942(2) 0.0385(10) Uani 1 1 d . . . N3 N 0.1855(3) 0.2235(2) -0.1594(2) 0.0402(10) Uani 1 1 d . . . F3 F 0.3957(4) 0.1262(2) -0.2431(2) 0.0832(13) Uani 1 1 d . . . C32 C 0.2019(6) -0.0835(4) -0.2822(4) 0.076(2) Uani 1 1 d . . . H32 H 0.2219 -0.1169 -0.3024 0.091 Uiso 1 1 d R . . F1 F 0.4106(5) 0.1520(2) -0.4003(3) 0.0949(16) Uani 1 1 d . . . F2 F 0.2898(5) 0.1556(4) -0.3488(3) 0.137(3) Uani 1 1 d . . . C4 C 0.1521(9) 0.3888(3) -0.1762(5) 0.091(3) Uani 1 1 d . . . H4A H 0.2249 0.3972 -0.1619 0.109 Uiso 1 1 d R . . H4B H 0.1161 0.4189 -0.2111 0.109 Uiso 1 1 d R . . C5 C 0.1185(9) 0.3922(4) -0.1102(5) 0.092(3) Uani 1 1 d . . . H5A H 0.0473 0.3802 -0.1239 0.110 Uiso 1 1 d R . . H5B H 0.1235 0.4333 -0.0935 0.110 Uiso 1 1 d R . . C11 C 0.4161(4) 0.0944(2) 0.1131(3) 0.0425(12) Uani 1 1 d . . . F5 F 0.3812(5) 0.0714(2) -0.3406(3) 0.1103(19) Uani 1 1 d . . . C1 C 0.1910(4) 0.2934(2) -0.0810(3) 0.0456(13) Uani 1 1 d . . . C2 C 0.1673(4) 0.2818(2) -0.1541(3) 0.0434(12) Uani 1 1 d . . . C17 C 0.5139(4) 0.1346(3) 0.0107(3) 0.0418(12) Uani 1 1 d . . . C16 C 0.3624(6) 0.1081(3) 0.1584(4) 0.066(2) Uani 1 1 d . . . H16 H 0.3161 0.1396 0.1463 0.079 Uiso 1 1 d R . . C7 C 0.2655(4) 0.2298(3) 0.0317(3) 0.0439(12) Uani 1 1 d . . . H7A H 0.2282 0.1977 0.0450 0.053 Uiso 1 1 d R . . H7B H 0.2584 0.2655 0.0578 0.053 Uiso 1 1 d R . . C18 C 0.5148(5) 0.1239(3) -0.0577(3) 0.0498(14) Uani 1 1 d . . . H18 H 0.4538 0.1140 -0.0940 0.060 Uiso 1 1 d R . . C9 C 0.1747(5) 0.1887(3) -0.2252(3) 0.0451(13) Uani 1 1 d . . . H9A H 0.2387 0.1683 -0.2197 0.054 Uiso 1 1 d R . . H9B H 0.1602 0.2155 -0.2664 0.054 Uiso 1 1 d R . . C12 C 0.4813(5) 0.0471(3) 0.1310(4) 0.0604(17) Uani 1 1 d . . . H12 H 0.5182 0.0368 0.1008 0.072 Uiso 1 1 d R . . C8 C 0.3782(4) 0.2131(2) 0.0526(3) 0.0412(12) Uani 1 1 d . . . H8A H 0.4112 0.2182 0.1045 0.049 Uiso 1 1 d R . . H8B H 0.4116 0.2394 0.0281 0.049 Uiso 1 1 d R . . C29 C 0.1429(4) 0.0165(3) -0.2205(3) 0.0459(13) Uani 1 1 d . . . F4 F 0.5209(5) 0.1212(4) -0.2921(4) 0.153(3) Uani 1 1 d . . . F6 F 0.4291(9) 0.2050(3) -0.3007(4) 0.171(4) Uani 1 1 d . . . C30 C 0.1129(5) -0.0406(3) -0.2069(4) 0.0569(16) Uani 1 1 d . . . H30 H 0.0733 -0.0454 -0.1772 0.068 Uiso 1 1 d R . . C24 C -0.0141(5) 0.0683(3) -0.0943(4) 0.0586(16) Uani 1 1 d . . . H24 H 0.0427 0.0784 -0.0545 0.070 Uiso 1 1 d R . . C23 C -0.0044(4) 0.0653(3) -0.1618(3) 0.0469(13) Uani 1 1 d . . . C22 C 0.6061(5) 0.1495(3) 0.0653(4) 0.0581(16) Uani 1 1 d . . . H22 H 0.6074 0.1569 0.1124 0.070 Uiso 1 1 d R . . C10 C 0.0884(5) 0.1425(3) -0.2397(3) 0.0478(13) Uani 1 1 d . . . H10A H 0.0750 0.1257 -0.2878 0.057 Uiso 1 1 d R . . H10B H 0.0266 0.1625 -0.2393 0.057 Uiso 1 1 d R . . C34 C 0.2017(5) 0.0235(3) -0.2667(4) 0.0583(16) Uani 1 1 d . . . H34 H 0.2206 0.0613 -0.2774 0.070 Uiso 1 1 d R . . C6 C 0.1834(6) 0.3524(3) -0.0477(4) 0.0584(16) Uani 1 1 d . . . H6A H 0.2510 0.3695 -0.0251 0.070 Uiso 1 1 d R . . H6B H 0.1507 0.3481 -0.0112 0.070 Uiso 1 1 d R . . C36 C 0.3221(5) 0.0193(3) -0.0574(4) 0.0584(17) Uani 1 1 d . . . H36A H 0.3158 0.0031 -0.1041 0.070 Uiso 1 1 d R . . H36B H 0.3933 0.0225 -0.0286 0.070 Uiso 1 1 d R . . F7 F 0.1221(4) 0.2991(4) -0.3752(3) 0.120(2) Uani 1 1 d . . . C13 C 0.4939(5) 0.0140(3) 0.1931(4) 0.0611(17) Uani 1 1 d . . . H13 H 0.5380 -0.0187 0.2038 0.073 Uiso 1 1 d R . . C31 C 0.1419(6) -0.0899(3) -0.2375(5) 0.070(2) Uani 1 1 d . . . H31 H 0.1217 -0.1279 -0.2283 0.084 Uiso 1 1 d R . . F8 F -0.1028(5) 0.2690(5) -0.4759(4) 0.167(4) Uani 1 1 d . . . C3 C 0.1310(6) 0.3274(3) -0.2119(4) 0.0654(18) Uani 1 1 d . . . H3A H 0.0582 0.3226 -0.2374 0.079 Uiso 1 1 d R . . H3B H 0.1667 0.3231 -0.2466 0.079 Uiso 1 1 d R . . C14 C 0.4428(6) 0.0287(3) 0.2382(4) 0.0690(19) Uani 1 1 d . . . H14 H 0.4529 0.0070 0.2806 0.083 Uiso 1 1 d R . . C28 C -0.0889(5) 0.0512(3) -0.2222(4) 0.0637(17) Uani 1 1 d . . . H28 H -0.0837 0.0497 -0.2684 0.076 Uiso 1 1 d R . . C25 C -0.1067(7) 0.0566(4) -0.0842(5) 0.083(2) Uani 1 1 d . . . H25 H -0.1122 0.0568 -0.0381 0.100 Uiso 1 1 d R . . F9 F 0.0511(5) 0.2342(4) -0.4632(5) 0.170(4) Uani 1 1 d . . . C19 C 0.6044(6) 0.1270(4) -0.0746(4) 0.0660(18) Uani 1 1 d . . . H19 H 0.6035 0.1189 -0.1215 0.079 Uiso 1 1 d R . . C27 C -0.1815(6) 0.0394(4) -0.2113(5) 0.081(2) Uani 1 1 d . . . H27 H -0.2377 0.0276 -0.2507 0.097 Uiso 1 1 d R . . C20 C 0.6943(5) 0.1424(3) -0.0214(5) 0.0655(19) Uani 1 1 d . . . H20 H 0.7543 0.1458 -0.0325 0.079 Uiso 1 1 d R . . C33 C 0.2307(7) -0.0273(4) -0.2959(4) 0.078(2) Uani 1 1 d . . . H33 H 0.2708 -0.0231 -0.3254 0.094 Uiso 1 1 d R . . C21 C 0.6959(5) 0.1531(4) 0.0482(5) 0.075(2) Uani 1 1 d . . . H21 H 0.7575 0.1627 0.0842 0.090 Uiso 1 1 d R . . C26 C -0.1923(6) 0.0444(4) -0.1464(6) 0.089(3) Uani 1 1 d . . . H26 H -0.2567 0.0400 -0.1420 0.107 Uiso 1 1 d R . . C15 C 0.3745(7) 0.0768(4) 0.2210(4) 0.081(2) Uani 1 1 d . . . H15 H 0.3380 0.0873 0.2513 0.097 Uiso 1 1 d R . . F10 F 0.0345(9) 0.3253(6) -0.4845(5) 0.225(5) Uani 1 1 d . . . F11 F -0.0302(8) 0.3366(5) -0.3908(7) 0.224(6) Uani 1 1 d . . . F12 F -0.0067(7) 0.2486(6) -0.3682(4) 0.207(6) Uani 1 1 d . . . O1 O 0.0836(5) 0.7484(3) 0.7206(4) 0.101(2) Uani 1 1 d . . . C37 C 0.1710(8) 0.7293(5) 0.7771(7) 0.104(3) Uani 1 1 d . . . H37A H 0.1617 0.6890 0.7922 0.125 Uiso 1 1 d R . . H37B H 0.1859 0.7558 0.8186 0.125 Uiso 1 1 d R . . C40 C 0.1018(9) 0.7412(6) 0.6565(6) 0.113(4) Uani 1 1 d . . . H40A H 0.0846 0.7777 0.6283 0.135 Uiso 1 1 d R . . H40B H 0.0589 0.7093 0.6286 0.135 Uiso 1 1 d R . . C41 C 0.4236(9) 0.2709(6) 0.8404(8) 0.117(4) Uani 1 1 d . . . H41A H 0.3726 0.2874 0.7976 0.140 Uiso 1 1 d R . . H41B H 0.4167 0.2277 0.8389 0.140 Uiso 1 1 d R . . C38 C 0.2533(11) 0.7314(9) 0.7464(12) 0.174(7) Uani 1 1 d . . . H38A H 0.2912 0.7686 0.7592 0.209 Uiso 1 1 d R . . H38B H 0.3003 0.6984 0.7646 0.209 Uiso 1 1 d R . . C42 C 0.5297(10) 0.2887(7) 0.8425(10) 0.145(5) Uani 1 1 d . . . H42A H 0.5709 0.2538 0.8416 0.174 Uiso 1 1 d R . . H42B H 0.5271 0.3146 0.8022 0.174 Uiso 1 1 d R . . C47 C 0.173(3) 0.5964(17) 1.0136(11) 0.34(2) Uani 1 1 d . . . H47A H 0.2201 0.5648 1.0374 0.404 Uiso 1 1 d R . . H47B H 0.1969 0.6341 1.0379 0.404 Uiso 1 1 d R . . C39 C 0.2080(14) 0.7266(9) 0.6706(11) 0.171(7) Uani 1 1 d . . . H39A H 0.2150 0.6865 0.6541 0.205 Uiso 1 1 d R . . H39B H 0.2389 0.7546 0.6462 0.205 Uiso 1 1 d R . . C44 C 0.492(2) 0.3207(11) 0.9444(11) 0.249(14) Uani 1 1 d . . . H44A H 0.5167 0.3015 0.9915 0.299 Uiso 1 1 d R . . H44B H 0.4746 0.3618 0.9512 0.299 Uiso 1 1 d R . . C48 C 0.160(2) 0.6007(16) 0.9336(14) 0.299(19) Uani 1 1 d . . . H48A H 0.1506 0.6420 0.9176 0.359 Uiso 1 1 d R . . H48B H 0.2193 0.5849 0.9244 0.359 Uiso 1 1 d R . . C43 C 0.5702(14) 0.3196(11) 0.9113(14) 0.229(12) Uani 1 1 d . . . H43A H 0.6306 0.2992 0.9429 0.275 Uiso 1 1 d R . . H43B H 0.5893 0.3600 0.9034 0.275 Uiso 1 1 d R . . O2 O 0.4096(7) 0.2926(4) 0.9011(6) 0.129(3) Uani 1 1 d . . . O3 O 0.0735(14) 0.5663(8) 0.8954(6) 0.209(6) Uani 1 1 d . . . C45 C 0.008(2) 0.5735(17) 0.9373(10) 0.292(16) Uani 1 1 d . . . H45A H -0.0300 0.5370 0.9365 0.350 Uiso 1 1 d R . . H45B H -0.0393 0.6064 0.9201 0.350 Uiso 1 1 d R . . C46 C 0.079(2) 0.5835(17) 1.0099(14) 0.294(18) Uani 1 1 d . . . H46A H 0.0540 0.6170 1.0303 0.353 Uiso 1 1 d R . . H46B H 0.0810 0.5490 1.0402 0.353 Uiso 1 1 d R . . O49 O 0.512(4) 0.5111(10) 0.9666(15) 0.32(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0356(3) 0.0297(3) 0.0399(3) -0.00176(15) 0.01391(19) -0.00086(15) P1 0.0326(7) 0.0319(7) 0.0375(7) -0.0020(5) 0.0138(5) 0.0012(5) P2 0.0355(7) 0.0347(7) 0.0421(7) -0.0034(6) 0.0125(6) -0.0043(5) P3 0.0903(14) 0.0539(10) 0.0611(11) 0.0195(8) 0.0320(10) 0.0125(9) P4 0.0665(13) 0.127(2) 0.0668(12) 0.0230(13) 0.0295(10) 0.0212(13) C35 0.069(4) 0.035(3) 0.062(4) 0.000(3) 0.008(3) -0.003(3) N1 0.042(2) 0.033(2) 0.042(2) 0.0012(18) 0.0172(19) 0.0054(19) N2 0.040(2) 0.037(2) 0.036(2) -0.0029(18) 0.0104(19) 0.0013(19) N3 0.041(2) 0.038(2) 0.041(2) 0.0023(19) 0.0125(19) -0.0050(19) F3 0.109(4) 0.083(3) 0.065(3) 0.026(2) 0.038(3) 0.013(3) C32 0.083(5) 0.068(5) 0.072(5) -0.032(4) 0.020(4) 0.001(4) F1 0.142(5) 0.080(3) 0.084(3) 0.026(3) 0.066(3) 0.019(3) F2 0.117(5) 0.205(7) 0.104(4) 0.069(5) 0.057(4) 0.088(5) C4 0.135(9) 0.045(4) 0.079(6) 0.022(4) 0.019(5) 0.020(4) C5 0.126(8) 0.056(5) 0.084(6) 0.002(4) 0.022(6) 0.033(5) C11 0.039(3) 0.037(3) 0.048(3) -0.001(2) 0.010(2) 0.002(2) F5 0.182(6) 0.069(3) 0.089(4) 0.004(3) 0.058(4) -0.024(3) C1 0.045(3) 0.038(3) 0.054(3) 0.003(2) 0.017(3) 0.005(2) C2 0.041(3) 0.037(3) 0.052(3) 0.003(2) 0.015(2) 0.001(2) C17 0.037(3) 0.044(3) 0.046(3) 0.002(2) 0.016(2) 0.000(2) C16 0.085(5) 0.061(4) 0.063(4) 0.019(3) 0.040(4) 0.032(4) C7 0.052(3) 0.039(3) 0.043(3) -0.006(2) 0.018(2) 0.007(2) C18 0.046(3) 0.057(3) 0.052(3) 0.001(3) 0.023(3) 0.004(3) C9 0.054(3) 0.044(3) 0.041(3) 0.000(2) 0.021(3) 0.003(3) C12 0.049(3) 0.069(4) 0.065(4) 0.015(3) 0.022(3) 0.022(3) C8 0.045(3) 0.032(3) 0.042(3) -0.008(2) 0.008(2) -0.001(2) C29 0.045(3) 0.045(3) 0.048(3) -0.013(3) 0.016(2) -0.006(2) F4 0.084(4) 0.232(9) 0.143(6) 0.080(6) 0.038(4) 0.013(5) F6 0.360(13) 0.067(3) 0.094(4) 0.004(3) 0.087(6) -0.031(5) C30 0.069(4) 0.043(3) 0.059(4) -0.007(3) 0.021(3) -0.015(3) C24 0.055(4) 0.066(4) 0.062(4) -0.011(3) 0.029(3) -0.005(3) C23 0.041(3) 0.041(3) 0.061(3) -0.009(3) 0.020(3) -0.010(2) C22 0.039(3) 0.079(5) 0.055(4) -0.011(3) 0.013(3) -0.009(3) C10 0.050(3) 0.044(3) 0.041(3) 0.005(2) 0.004(2) 0.001(3) C34 0.064(4) 0.062(4) 0.054(4) -0.011(3) 0.027(3) -0.008(3) C6 0.074(4) 0.034(3) 0.073(4) -0.001(3) 0.032(4) 0.011(3) C36 0.058(4) 0.040(3) 0.062(4) -0.009(3) 0.000(3) 0.007(3) F7 0.084(4) 0.202(7) 0.084(4) -0.017(4) 0.043(3) -0.012(4) C13 0.062(4) 0.053(4) 0.064(4) 0.015(3) 0.015(3) 0.008(3) C31 0.078(5) 0.045(4) 0.085(5) -0.009(4) 0.024(4) -0.007(3) F8 0.073(4) 0.278(11) 0.129(5) -0.021(6) 0.007(4) 0.038(5) C3 0.075(5) 0.052(4) 0.064(4) 0.019(3) 0.016(3) 0.006(3) C14 0.079(5) 0.071(5) 0.056(4) 0.021(3) 0.022(4) 0.006(4) C28 0.042(3) 0.078(5) 0.066(4) -0.007(4) 0.012(3) -0.007(3) C25 0.089(6) 0.092(6) 0.091(6) -0.012(5) 0.058(5) -0.017(5) F9 0.096(5) 0.205(8) 0.215(9) -0.090(7) 0.061(5) 0.003(5) C19 0.066(5) 0.074(5) 0.073(5) 0.003(4) 0.043(4) 0.004(4) C27 0.051(4) 0.107(6) 0.086(6) -0.008(5) 0.023(4) -0.029(4) C20 0.047(4) 0.071(5) 0.090(5) 0.000(4) 0.039(4) -0.005(3) C33 0.092(6) 0.084(6) 0.063(4) -0.022(4) 0.033(4) 0.009(4) C21 0.038(4) 0.095(6) 0.084(5) 0.007(4) 0.013(3) -0.011(4) C26 0.057(5) 0.105(7) 0.115(7) -0.003(6) 0.040(5) -0.017(4) C15 0.123(7) 0.070(5) 0.071(5) 0.018(4) 0.063(5) 0.017(5) F10 0.280(13) 0.265(13) 0.115(6) 0.097(8) 0.046(7) -0.019(10) F11 0.163(8) 0.231(11) 0.235(11) -0.091(9) 0.011(7) 0.099(8) F12 0.143(7) 0.363(16) 0.120(6) 0.081(8) 0.051(5) -0.066(8) O1 0.083(4) 0.128(6) 0.102(5) -0.012(4) 0.042(4) 0.003(4) C37 0.094(7) 0.098(7) 0.126(9) -0.021(7) 0.045(7) -0.006(6) C40 0.116(9) 0.147(10) 0.096(7) -0.031(7) 0.063(7) -0.027(7) C41 0.103(8) 0.119(9) 0.141(10) 0.002(8) 0.058(8) -0.016(7) C38 0.096(10) 0.181(16) 0.25(2) -0.005(16) 0.058(13) 0.006(9) C42 0.112(10) 0.133(11) 0.220(17) -0.016(11) 0.095(11) -0.019(8) C47 0.31(4) 0.58(6) 0.096(14) -0.01(2) 0.035(18) -0.21(4) C39 0.158(15) 0.212(18) 0.182(16) -0.077(15) 0.110(13) -0.012(13) C44 0.32(3) 0.30(3) 0.190(19) -0.130(18) 0.18(2) -0.21(2) C48 0.23(3) 0.50(5) 0.15(2) 0.05(2) 0.036(18) -0.15(3) C43 0.125(13) 0.26(3) 0.29(3) -0.14(2) 0.060(16) -0.080(15) O2 0.110(6) 0.152(7) 0.152(7) -0.020(6) 0.077(6) -0.023(5) O3 0.238(15) 0.269(17) 0.087(7) -0.019(9) 0.012(8) 0.006(12) C45 0.28(3) 0.51(5) 0.068(9) 0.033(19) 0.038(14) -0.05(3) C46 0.26(3) 0.49(5) 0.18(3) -0.10(3) 0.14(2) -0.16(3) O49 0.76(8) 0.115(16) 0.18(2) 0.015(16) 0.27(4) -0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 2.070(4) . ? Rh1 C35 2.146(6) . ? Rh1 C36 2.163(6) . ? Rh1 P1 2.3081(13) . ? Rh1 P2 2.3137(14) . ? P1 C17 1.820(5) . ? P1 C11 1.830(6) . ? P1 C8 1.837(5) . ? P2 C23 1.813(6) . ? P2 C29 1.820(6) . ? P2 C10 1.839(6) . ? P3 F6 1.531(6) . ? P3 F2 1.555(6) . ? P3 F4 1.558(7) . ? P3 F5 1.574(6) . ? P3 F3 1.598(4) . ? P3 F1 1.606(5) . ? P4 F12 1.513(7) . ? P4 F11 1.525(8) . ? P4 F10 1.541(8) . ? P4 F9 1.572(8) . ? P4 F8 1.569(8) . ? P4 F7 1.583(6) . ? C35 C36 1.331(10) . ? C35 H35A 0.9599 . ? C35 H35B 0.9601 . ? N1 N2 1.341(6) . ? N1 C1 1.356(7) . ? N1 C7 1.471(7) . ? N2 N3 1.344(6) . ? N3 C2 1.340(7) . ? N3 C9 1.468(7) . ? C32 C33 1.372(12) . ? C32 C31 1.402(11) . ? C32 H32 0.9303 . ? C4 C5 1.514(14) . ? C4 C3 1.523(11) . ? C4 H4A 0.9701 . ? C4 H4B 0.9700 . ? C5 C6 1.535(11) . ? C5 H5A 0.9701 . ? C5 H5B 0.9699 . ? C11 C12 1.360(8) . ? C11 C16 1.369(9) . ? C1 C2 1.379(8) . ? C1 C6 1.491(8) . ? C2 C3 1.480(8) . ? C17 C18 1.364(8) . ? C17 C22 1.402(8) . ? C16 C15 1.370(10) . ? C16 H16 0.9301 . ? C7 C8 1.522(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9702 . ? C18 C19 1.389(9) . ? C18 H18 0.9300 . ? C9 C10 1.533(8) . ? C9 H9A 0.9702 . ? C9 H9B 0.9699 . ? C12 C13 1.382(9) . ? C12 H12 0.9302 . ? C8 H8A 0.9700 . ? C8 H8B 0.9699 . ? C29 C30 1.397(8) . ? C29 C34 1.414(9) . ? C30 C31 1.377(10) . ? C30 H30 0.9298 . ? C24 C23 1.373(9) . ? C24 C25 1.386(10) . ? C24 H24 0.9300 . ? C23 C28 1.392(9) . ? C22 C21 1.395(9) . ? C22 H22 0.9299 . ? C10 H10A 0.9699 . ? C10 H10B 0.9700 . ? C34 C33 1.390(10) . ? C34 H34 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C36 H36A 0.9602 . ? C36 H36B 0.9601 . ? C13 C14 1.344(10) . ? C13 H13 0.9300 . ? C31 H31 0.9300 . ? C3 H3A 0.9700 . ? C3 H3B 0.9701 . ? C14 C15 1.398(11) . ? C14 H14 0.9299 . ? C28 C27 1.394(10) . ? C28 H28 0.9300 . ? C25 C26 1.412(13) . ? C25 H25 0.9300 . ? C19 C20 1.372(11) . ? C19 H19 0.9300 . ? C27 C26 1.332(12) . ? C27 H27 0.9300 . ? C20 C21 1.375(11) . ? C20 H20 0.9300 . ? C33 H33 0.9302 . ? C21 H21 0.9300 . ? C26 H26 0.9300 . ? C15 H15 0.9298 . ? O1 C40 1.370(11) . ? O1 C37 1.404(13) . ? C37 C38 1.455(18) . ? C37 H37A 0.9701 . ? C37 H37B 0.9700 . ? C40 C39 1.440(19) . ? C40 H40A 0.9701 . ? C40 H40B 0.9700 . ? C41 O2 1.354(13) . ? C41 C42 1.511(15) . ? C41 H41A 0.9700 . ? C41 H41B 0.9701 . ? C38 C39 1.41(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9701 . ? C42 C43 1.45(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9701 . ? C47 C46 1.31(3) . ? C47 C48 1.51(3) . ? C47 H47A 0.9699 . ? C47 H47B 0.9701 . ? C39 H39A 0.9698 . ? C39 H39B 0.9700 . ? C44 O2 1.33(2) . ? C44 C43 1.44(2) . ? C44 H44A 0.9699 . ? C44 H44B 0.9701 . ? C48 O3 1.41(3) . ? C48 H48A 0.9699 . ? C48 H48B 0.9700 . ? C43 H43A 0.9699 . ? C43 H43B 0.9701 . ? O3 C45 1.42(2) . ? C45 C46 1.45(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9701 . ? C46 H46A 0.9698 . ? C46 H46B 0.9701 . ? O49 O49 1.53(4) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 C35 159.9(2) . . ? N2 Rh1 C36 164.0(2) . . ? C35 Rh1 C36 36.0(3) . . ? N2 Rh1 P1 89.24(12) . . ? C35 Rh1 P1 93.74(18) . . ? C36 Rh1 P1 86.36(17) . . ? N2 Rh1 P2 89.42(12) . . ? C35 Rh1 P2 88.48(19) . . ? C36 Rh1 P2 94.18(17) . . ? P1 Rh1 P2 176.89(5) . . ? C17 P1 C11 105.8(3) . . ? C17 P1 C8 104.2(3) . . ? C11 P1 C8 103.6(3) . . ? C17 P1 Rh1 114.24(19) . . ? C11 P1 Rh1 117.70(18) . . ? C8 P1 Rh1 110.01(18) . . ? C23 P2 C29 104.4(3) . . ? C23 P2 C10 103.9(3) . . ? C29 P2 C10 105.4(3) . . ? C23 P2 Rh1 117.6(2) . . ? C29 P2 Rh1 113.78(19) . . ? C10 P2 Rh1 110.61(19) . . ? F6 P3 F2 88.2(5) . . ? F6 P3 F4 93.0(6) . . ? F2 P3 F4 178.5(4) . . ? F6 P3 F5 179.3(3) . . ? F2 P3 F5 91.7(4) . . ? F4 P3 F5 87.0(5) . . ? F6 P3 F3 90.6(3) . . ? F2 P3 F3 88.3(3) . . ? F4 P3 F3 90.9(3) . . ? F5 P3 F3 88.8(3) . . ? F6 P3 F1 90.2(3) . . ? F2 P3 F1 89.5(3) . . ? F4 P3 F1 91.3(4) . . ? F5 P3 F1 90.5(3) . . ? F3 P3 F1 177.7(3) . . ? F12 P4 F11 83.5(7) . . ? F12 P4 F10 175.3(6) . . ? F11 P4 F10 97.6(8) . . ? F12 P4 F9 95.1(7) . . ? F11 P4 F9 178.3(6) . . ? F10 P4 F9 83.7(6) . . ? F12 P4 F8 87.3(5) . . ? F11 P4 F8 91.9(5) . . ? F10 P4 F8 97.2(6) . . ? F9 P4 F8 89.1(4) . . ? F12 P4 F7 88.1(4) . . ? F11 P4 F7 89.8(5) . . ? F10 P4 F7 87.3(5) . . ? F9 P4 F7 89.1(4) . . ? F8 P4 F7 175.0(5) . . ? C36 C35 Rh1 72.7(4) . . ? C36 C35 H35A 123.7 . . ? Rh1 C35 H35A 109.2 . . ? C36 C35 H35B 123.1 . . ? Rh1 C35 H35B 109.3 . . ? H35A C35 H35B 109.5 . . ? N2 N1 C1 111.9(4) . . ? N2 N1 C7 120.6(4) . . ? C1 N1 C7 127.3(5) . . ? N1 N2 N3 104.1(4) . . ? N1 N2 Rh1 126.9(3) . . ? N3 N2 Rh1 128.9(3) . . ? C2 N3 N2 112.3(4) . . ? C2 N3 C9 128.2(5) . . ? N2 N3 C9 119.5(4) . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.5 . . ? C5 C4 C3 111.7(7) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.5(7) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C12 C11 C16 117.7(6) . . ? C12 C11 P1 121.5(5) . . ? C16 C11 P1 120.7(4) . . ? N1 C1 C2 105.7(5) . . ? N1 C1 C6 128.1(6) . . ? C2 C1 C6 126.2(5) . . ? N3 C2 C1 106.1(5) . . ? N3 C2 C3 129.6(6) . . ? C1 C2 C3 124.4(5) . . ? C18 C17 C22 118.9(5) . . ? C18 C17 P1 119.7(4) . . ? C22 C17 P1 121.2(4) . . ? C15 C16 C11 122.3(6) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.8 . . ? N1 C7 C8 109.7(4) . . ? N1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N1 C7 H7B 109.8 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C17 C18 C19 121.8(6) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? N3 C9 C10 111.3(5) . . ? N3 C9 H9A 109.4 . . ? C10 C9 H9A 109.3 . . ? N3 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C12 C13 121.4(6) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C7 C8 P1 110.8(4) . . ? C7 C8 H8A 109.4 . . ? P1 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C30 C29 C34 119.6(6) . . ? C30 C29 P2 120.9(5) . . ? C34 C29 P2 119.2(5) . . ? C31 C30 C29 120.1(7) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 119.9 . . ? C23 C24 C25 121.5(7) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.3 . . ? C24 C23 C28 120.0(6) . . ? C24 C23 P2 120.2(5) . . ? C28 C23 P2 119.8(5) . . ? C21 C22 C17 119.3(6) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.4 . . ? C9 C10 P2 113.4(4) . . ? C9 C10 H10A 108.9 . . ? P2 C10 H10A 108.9 . . ? C9 C10 H10B 108.8 . . ? P2 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C33 C34 C29 118.7(7) . . ? C33 C34 H34 120.6 . . ? C29 C34 H34 120.7 . . ? C1 C6 C5 106.0(6) . . ? C1 C6 H6A 110.4 . . ? C5 C6 H6A 110.6 . . ? C1 C6 H6B 110.7 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.7 . . ? C35 C36 Rh1 71.3(4) . . ? C35 C36 H36A 124.0 . . ? Rh1 C36 H36A 109.6 . . ? C35 C36 H36B 123.3 . . ? Rh1 C36 H36B 109.1 . . ? H36A C36 H36B 109.5 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.9 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.6 . . ? C2 C3 C4 107.9(6) . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3A 110.0 . . ? C2 C3 H3B 110.1 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.4 . . ? C13 C14 C15 119.6(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.3 . . ? C23 C28 C27 118.0(7) . . ? C23 C28 H28 121.0 . . ? C27 C28 H28 121.1 . . ? C24 C25 C26 117.6(8) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C20 C19 C18 119.2(7) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C26 C27 C28 122.2(8) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 119.0 . . ? C19 C20 C21 120.3(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.8 . . ? C32 C33 C34 121.7(7) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.1 . . ? C20 C21 C22 120.4(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.8 . . ? C27 C26 C25 120.5(7) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.7 . . ? C16 C15 C14 118.6(7) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.6 . . ? C40 O1 C37 108.0(8) . . ? O1 C37 C38 104.8(12) . . ? O1 C37 H37A 110.8 . . ? C38 C37 H37A 111.0 . . ? O1 C37 H37B 110.9 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.9 . . ? O1 C40 C39 109.9(12) . . ? O1 C40 H40A 109.6 . . ? C39 C40 H40A 109.9 . . ? O1 C40 H40B 109.6 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? O2 C41 C42 107.8(12) . . ? O2 C41 H41A 110.0 . . ? C42 C41 H41A 110.1 . . ? O2 C41 H41B 110.1 . . ? C42 C41 H41B 110.3 . . ? H41A C41 H41B 108.5 . . ? C39 C38 C37 107.3(13) . . ? C39 C38 H38A 110.4 . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38B 109.6 . . ? C37 C38 H38B 110.3 . . ? H38A C38 H38B 108.5 . . ? C43 C42 C41 102.8(13) . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42A 111.1 . . ? C43 C42 H42B 111.5 . . ? C41 C42 H42B 111.4 . . ? H42A C42 H42B 109.1 . . ? C46 C47 C48 100(2) . . ? C46 C47 H47A 111.1 . . ? C48 C47 H47A 111.8 . . ? C46 C47 H47B 112.9 . . ? C48 C47 H47B 110.7 . . ? H47A C47 H47B 109.6 . . ? C38 C39 C40 104.5(11) . . ? C38 C39 H39A 111.3 . . ? C40 C39 H39A 110.8 . . ? C38 C39 H39B 110.8 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.8 . . ? O2 C44 C43 108.7(14) . . ? O2 C44 H44A 110.4 . . ? C43 C44 H44A 110.0 . . ? O2 C44 H44B 109.6 . . ? C43 C44 H44B 109.8 . . ? H44A C44 H44B 108.3 . . ? O3 C48 C47 107.6(19) . . ? O3 C48 H48A 110.7 . . ? C47 C48 H48A 110.7 . . ? O3 C48 H48B 108.9 . . ? C47 C48 H48B 110.7 . . ? H48A C48 H48B 108.3 . . ? C42 C43 C44 108.2(14) . . ? C42 C43 H43A 110.5 . . ? C44 C43 H43A 110.0 . . ? C42 C43 H43B 109.8 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C44 O2 C41 112.5(11) . . ? C45 O3 C48 102.8(19) . . ? O3 C45 C46 103(2) . . ? O3 C45 H45A 110.1 . . ? C46 C45 H45A 109.6 . . ? O3 C45 H45B 112.0 . . ? C46 C45 H45B 112.5 . . ? H45A C45 H45B 109.2 . . ? C47 C46 C45 115(2) . . ? C47 C46 H46A 107.3 . . ? C45 C46 H46A 107.5 . . ? C47 C46 H46B 109.0 . . ? C45 C46 H46B 110.1 . . ? H46A C46 H46B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.969 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.154 _database_code_depnum_ccdc_archive 'CCDC 961445' data_mg13 # struture Linda JW Shimon, WIS # Mark Gandelman, Technion _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Cl N3 P2 Pt, 2(C F3 O3 S), 2(C H2 Cl2)' _chemical_formula_sum 'C38 H40 Cl5 F6 N3 O6 P2 Pt S2' _chemical_formula_weight 1247.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 26.8737(3) _cell_length_b 12.5922(2) _cell_length_c 16.04680(10) _cell_angle_alpha 90.00 _cell_angle_beta 120.7260(10) _cell_angle_gamma 90.00 _cell_volume 4667.93(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 44905 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 3.522 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3720 _exptl_absorpt_correction_T_max 0.7659 _exptl_absorpt_process_details 'Numabs, Hitashi 1999' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44905 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5338 _reflns_number_gt 4985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+7.8971P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5338 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Pt1 Pt 0.0000 0.272494(11) 0.2500 0.01216(7) Uani 1 2 d S . . Cl1 Cl 0.0000 0.45393(8) 0.2500 0.0173(2) Uani 1 2 d S . . P1 P 0.08919(3) 0.28065(6) 0.39287(6) 0.01304(16) Uani 1 1 d . . . N1 N 0.02669(10) 0.04529(19) 0.32632(17) 0.0135(5) Uani 1 1 d . . . N2 N 0.0000 0.1086(3) 0.2500 0.0126(7) Uani 1 2 d S . . C1 C 0.14735(12) 0.3470(3) 0.3876(2) 0.0170(6) Uani 1 1 d . . . C2 C 0.15798(14) 0.4546(3) 0.4116(2) 0.0229(7) Uani 1 1 d . . . H2 H 0.1342 0.4930 0.4290 0.028 Uiso 1 1 calc R . . C3 C 0.20331(14) 0.5055(3) 0.4099(3) 0.0273(7) Uani 1 1 d . . . H3 H 0.2103 0.5788 0.4257 0.033 Uiso 1 1 calc R . . C4 C 0.23844(14) 0.4497(3) 0.3854(2) 0.0266(7) Uani 1 1 d . . . H4 H 0.2700 0.4843 0.3858 0.032 Uiso 1 1 calc R . . C5 C 0.22759(14) 0.3438(3) 0.3604(3) 0.0273(7) Uani 1 1 d . . . H5 H 0.2514 0.3061 0.3427 0.033 Uiso 1 1 calc R . . C6 C 0.18200(15) 0.2916(3) 0.3608(3) 0.0243(7) Uani 1 1 d . . . H6 H 0.1746 0.2189 0.3430 0.029 Uiso 1 1 calc R . . C7 C 0.08836(13) 0.3400(2) 0.4952(2) 0.0172(6) Uani 1 1 d . . . C8 C 0.03748(15) 0.3612(3) 0.4939(2) 0.0247(7) Uani 1 1 d . . . H8 H 0.0013 0.3512 0.4359 0.030 Uiso 1 1 calc R . . C9 C 0.03919(16) 0.3970(3) 0.5772(3) 0.0301(8) Uani 1 1 d . . . H9 H 0.0041 0.4118 0.5758 0.036 Uiso 1 1 calc R . . C10 C 0.09173(18) 0.4111(3) 0.6621(3) 0.0304(8) Uani 1 1 d . . . H10 H 0.0927 0.4351 0.7191 0.036 Uiso 1 1 calc R . . C11 C 0.14237(17) 0.3905(3) 0.6641(3) 0.0319(8) Uani 1 1 d . . . H11 H 0.1784 0.4003 0.7225 0.038 Uiso 1 1 calc R . . C12 C 0.14129(15) 0.3554(3) 0.5812(2) 0.0249(7) Uani 1 1 d . . . H12 H 0.1765 0.3418 0.5828 0.030 Uiso 1 1 calc R . . C13 C 0.11345(13) 0.1466(2) 0.4378(2) 0.0183(6) Uani 1 1 d . . . H13A H 0.1292 0.1122 0.4007 0.022 Uiso 1 1 calc R . . H13B H 0.1443 0.1487 0.5070 0.022 Uiso 1 1 calc R . . C14 C 0.06131(13) 0.0842(3) 0.4257(2) 0.0181(6) Uani 1 1 d . . . H14A H 0.0748 0.0235 0.4713 0.022 Uiso 1 1 calc R . . H14B H 0.0373 0.1306 0.4410 0.022 Uiso 1 1 calc R . . C15 C 0.01764(12) -0.0577(2) 0.3000(2) 0.0156(6) Uani 1 1 d . . . C16 C 0.04013(14) -0.1539(2) 0.3614(2) 0.0195(6) Uani 1 1 d . . . H16A H 0.0194 -0.1656 0.3968 0.023 Uiso 1 1 calc R . . H16B H 0.0819 -0.1455 0.4094 0.023 Uiso 1 1 calc R . . C17 C 0.03053(17) -0.2486(3) 0.2942(3) 0.0259(8) Uani 1 1 d . . . H17A H 0.0590 -0.2453 0.2726 0.031 Uiso 1 1 calc R . . H17B H 0.0370 -0.3156 0.3306 0.031 Uiso 1 1 calc R . . S1 S 0.38641(3) 0.50717(7) 0.32245(6) 0.02190(17) Uani 1 1 d . . . F1 F 0.31097(12) 0.3530(2) 0.2510(2) 0.0576(7) Uani 1 1 d . . . F2 F 0.34402(12) 0.4020(3) 0.15983(19) 0.0605(8) Uani 1 1 d . . . F3 F 0.28213(10) 0.4983(2) 0.17070(18) 0.0526(7) Uani 1 1 d . . . O1 O 0.43062(11) 0.4278(2) 0.37046(19) 0.0372(7) Uani 1 1 d . . . O2 O 0.35988(11) 0.5415(2) 0.37594(18) 0.0308(6) Uani 1 1 d . . . O3 O 0.40005(11) 0.5901(2) 0.27563(19) 0.0352(6) Uani 1 1 d . . . C18 C 0.32780(17) 0.4367(3) 0.2208(3) 0.0341(8) Uani 1 1 d . . . Cl3 Cl 0.10749(5) 0.34507(11) 0.05662(10) 0.0577(3) Uani 1 1 d . . . Cl2 Cl 0.19678(5) 0.24107(9) 0.03500(9) 0.0400(2) Uani 1 1 d . . . C19 C 0.17452(19) 0.2802(3) 0.1171(3) 0.0335(9) Uani 1 1 d . . . H19A H 0.1716 0.2168 0.1508 0.040 Uiso 1 1 calc R . . H19B H 0.2039 0.3283 0.1666 0.040 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 0.01292(9) 0.01393(10) 0.01051(10) 0.000 0.00661(7) 0.000 Cl1 0.0196(5) 0.0133(4) 0.0178(5) 0.000 0.0088(4) 0.000 P1 0.0125(4) 0.0165(4) 0.0099(4) -0.0022(3) 0.0056(3) -0.0005(3) N1 0.0163(11) 0.0154(11) 0.0081(11) 0.0024(10) 0.0056(9) 0.0023(10) N2 0.0154(16) 0.0197(17) 0.0032(15) 0.000 0.0052(13) 0.000 C1 0.0137(13) 0.0253(15) 0.0093(14) -0.0002(12) 0.0040(11) -0.0009(12) C2 0.0219(15) 0.0273(16) 0.0221(17) -0.0016(14) 0.0130(13) -0.0010(13) C3 0.0260(17) 0.0267(17) 0.0261(18) -0.0008(15) 0.0112(14) -0.0080(14) C4 0.0158(14) 0.042(2) 0.0183(16) 0.0075(15) 0.0064(13) -0.0039(14) C5 0.0211(16) 0.041(2) 0.0244(18) 0.0031(16) 0.0150(14) 0.0045(15) C6 0.0248(17) 0.0292(16) 0.0239(18) -0.0040(14) 0.0159(15) -0.0007(14) C7 0.0231(15) 0.0169(13) 0.0131(14) 0.0005(12) 0.0102(12) 0.0023(12) C8 0.0256(16) 0.0310(17) 0.0216(17) -0.0021(14) 0.0151(14) -0.0019(14) C9 0.0366(19) 0.0324(18) 0.034(2) -0.0028(16) 0.0270(17) 0.0014(16) C10 0.053(2) 0.0259(17) 0.0208(18) -0.0011(15) 0.0249(17) 0.0036(17) C11 0.038(2) 0.0356(19) 0.0165(17) -0.0055(16) 0.0101(15) 0.0020(17) C12 0.0238(16) 0.0307(18) 0.0176(16) -0.0026(14) 0.0085(14) 0.0035(14) C13 0.0185(15) 0.0204(15) 0.0136(15) -0.0020(12) 0.0064(12) 0.0011(12) C14 0.0242(15) 0.0196(14) 0.0088(13) 0.0006(12) 0.0072(12) -0.0003(12) C15 0.0171(14) 0.0138(13) 0.0170(15) 0.0003(12) 0.0095(12) 0.0007(11) C16 0.0232(15) 0.0153(14) 0.0192(16) 0.0033(13) 0.0102(13) 0.0035(12) C17 0.036(2) 0.0182(14) 0.025(2) 0.0034(15) 0.0160(17) 0.0039(15) S1 0.0199(4) 0.0328(4) 0.0165(4) 0.0059(3) 0.0118(3) 0.0030(3) F1 0.0592(17) 0.0500(16) 0.0654(19) -0.0037(14) 0.0331(15) -0.0231(14) F2 0.0596(16) 0.087(2) 0.0415(15) -0.0280(16) 0.0308(13) -0.0107(16) F3 0.0287(12) 0.0750(19) 0.0354(14) 0.0040(14) 0.0028(10) 0.0052(12) O1 0.0319(13) 0.0552(18) 0.0299(14) 0.0148(13) 0.0196(12) 0.0187(13) O2 0.0319(13) 0.0421(15) 0.0260(13) 0.0028(12) 0.0204(11) 0.0083(12) O3 0.0356(14) 0.0446(16) 0.0301(14) 0.0087(13) 0.0202(12) -0.0088(12) C18 0.0336(19) 0.045(2) 0.0274(19) -0.0037(17) 0.0181(16) -0.0050(17) Cl3 0.0485(6) 0.0625(7) 0.0642(8) -0.0078(6) 0.0303(6) 0.0189(6) Cl2 0.0376(6) 0.0454(5) 0.0469(7) -0.0059(5) 0.0289(5) 0.0009(4) C19 0.031(2) 0.043(2) 0.029(2) -0.0024(16) 0.0168(18) -0.0010(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.064(4) . ? Pt1 Cl1 2.2847(10) . ? Pt1 P1 2.3230(8) . ? Pt1 P1 2.3230(8) 2 ? P1 C1 1.812(3) . ? P1 C7 1.815(3) . ? P1 C13 1.821(3) . ? N1 N2 1.323(3) . ? N1 C15 1.347(4) . ? N1 C14 1.460(4) . ? N2 N1 1.323(3) 2 ? C1 C6 1.395(4) . ? C1 C2 1.398(5) . ? C2 C3 1.388(5) . ? C2 H2 0.9500 . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.382(5) . ? C7 C12 1.400(4) . ? C8 C9 1.389(5) . ? C8 H8 0.9500 . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.370(5) . ? C10 H10 0.9500 . ? C11 C12 1.388(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.529(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C15 1.386(6) 2 ? C15 C16 1.482(4) . ? C16 C17 1.539(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C17 1.525(8) 2 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? S1 O2 1.434(2) . ? S1 O1 1.438(3) . ? S1 O3 1.439(3) . ? S1 C18 1.817(4) . ? F1 C18 1.332(5) . ? F2 C18 1.332(4) . ? F3 C18 1.322(5) . ? Cl3 C19 1.751(4) . ? Cl2 C19 1.772(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 Cl1 180.0 . . ? N2 Pt1 P1 92.535(18) . . ? Cl1 Pt1 P1 87.465(18) . . ? N2 Pt1 P1 92.535(18) . 2 ? Cl1 Pt1 P1 87.465(18) . 2 ? P1 Pt1 P1 174.93(4) . 2 ? C1 P1 C7 105.21(14) . . ? C1 P1 C13 107.64(14) . . ? C7 P1 C13 100.98(14) . . ? C1 P1 Pt1 117.00(10) . . ? C7 P1 Pt1 115.33(10) . . ? C13 P1 Pt1 109.28(10) . . ? N2 N1 C15 111.3(2) . . ? N2 N1 C14 123.4(2) . . ? C15 N1 C14 125.3(2) . . ? N1 N2 N1 106.0(3) . 2 ? N1 N2 Pt1 127.01(17) . . ? N1 N2 Pt1 127.01(17) 2 . ? C6 C1 C2 119.6(3) . . ? C6 C1 P1 120.8(3) . . ? C2 C1 P1 119.6(2) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.5(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C8 C7 C12 119.2(3) . . ? C8 C7 P1 122.3(2) . . ? C12 C7 P1 118.2(2) . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 P1 107.8(2) . . ? C14 C13 H13A 110.1 . . ? P1 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? P1 C13 H13B 110.1 . . ? H13A C13 H13B 108.5 . . ? N1 C14 C13 110.1(2) . . ? N1 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? N1 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? N1 C15 C15 105.67(16) . 2 ? N1 C15 C16 129.2(3) . . ? C15 C15 C16 125.14(17) 2 . ? C15 C16 C17 107.6(3) . . ? C15 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? C15 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C17 C17 C16 111.6(3) 2 . ? C17 C17 H17A 109.3 2 . ? C16 C17 H17A 109.3 . . ? C17 C17 H17B 109.3 2 . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? O2 S1 O1 114.59(15) . . ? O2 S1 O3 115.51(17) . . ? O1 S1 O3 115.00(16) . . ? O2 S1 C18 102.50(16) . . ? O1 S1 C18 103.98(19) . . ? O3 S1 C18 102.76(17) . . ? F3 C18 F2 107.2(3) . . ? F3 C18 F1 107.7(3) . . ? F2 C18 F1 107.9(4) . . ? F3 C18 S1 111.6(3) . . ? F2 C18 S1 111.1(3) . . ? F1 C18 S1 111.1(3) . . ? Cl3 C19 Cl2 111.1(2) . . ? Cl3 C19 H19A 109.4 . . ? Cl2 C19 H19A 109.4 . . ? Cl3 C19 H19B 109.4 . . ? Cl2 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pt1 P1 C1 119.68(12) . . . . ? Cl1 Pt1 P1 C1 -60.32(12) . . . . ? N2 Pt1 P1 C7 -115.78(11) . . . . ? Cl1 Pt1 P1 C7 64.22(11) . . . . ? N2 Pt1 P1 C13 -2.89(11) . . . . ? Cl1 Pt1 P1 C13 177.11(11) . . . . ? C15 N1 N2 N1 0.18(15) . . . 2 ? C14 N1 N2 N1 -179.8(3) . . . 2 ? C15 N1 N2 Pt1 -179.82(15) . . . . ? C14 N1 N2 Pt1 0.2(3) . . . . ? P1 Pt1 N2 N1 26.89(13) . . . . ? P1 Pt1 N2 N1 -153.11(13) 2 . . . ? P1 Pt1 N2 N1 -153.11(13) . . . 2 ? P1 Pt1 N2 N1 26.89(13) 2 . . 2 ? C7 P1 C1 C6 143.8(3) . . . . ? C13 P1 C1 C6 36.7(3) . . . . ? Pt1 P1 C1 C6 -86.7(3) . . . . ? C7 P1 C1 C2 -35.6(3) . . . . ? C13 P1 C1 C2 -142.7(3) . . . . ? Pt1 P1 C1 C2 93.9(3) . . . . ? C6 C1 C2 C3 -0.9(5) . . . . ? P1 C1 C2 C3 178.5(3) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? C4 C5 C6 C1 -0.5(5) . . . . ? C2 C1 C6 C5 1.4(5) . . . . ? P1 C1 C6 C5 -178.0(3) . . . . ? C1 P1 C7 C8 141.7(3) . . . . ? C13 P1 C7 C8 -106.4(3) . . . . ? Pt1 P1 C7 C8 11.2(3) . . . . ? C1 P1 C7 C12 -44.3(3) . . . . ? C13 P1 C7 C12 67.6(3) . . . . ? Pt1 P1 C7 C12 -174.8(2) . . . . ? C12 C7 C8 C9 -0.2(5) . . . . ? P1 C7 C8 C9 173.7(3) . . . . ? C7 C8 C9 C10 -0.4(5) . . . . ? C8 C9 C10 C11 0.5(6) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C10 C11 C12 C7 -0.5(6) . . . . ? C8 C7 C12 C11 0.6(5) . . . . ? P1 C7 C12 C11 -173.5(3) . . . . ? C1 P1 C13 C14 -170.2(2) . . . . ? C7 P1 C13 C14 79.8(2) . . . . ? Pt1 P1 C13 C14 -42.2(2) . . . . ? N2 N1 C14 C13 -63.4(3) . . . . ? C15 N1 C14 C13 116.6(3) . . . . ? P1 C13 C14 N1 81.9(3) . . . . ? N2 N1 C15 C15 -0.4(4) . . . 2 ? C14 N1 C15 C15 179.6(3) . . . 2 ? N2 N1 C15 C16 178.7(3) . . . . ? C14 N1 C15 C16 -1.3(5) . . . . ? N1 C15 C16 C17 -165.0(3) . . . . ? C15 C15 C16 C17 14.0(5) 2 . . . ? C15 C16 C17 C17 -46.6(4) . . . 2 ? O2 S1 C18 F3 57.8(3) . . . . ? O1 S1 C18 F3 177.4(3) . . . . ? O3 S1 C18 F3 -62.4(3) . . . . ? O2 S1 C18 F2 177.5(3) . . . . ? O1 S1 C18 F2 -62.9(3) . . . . ? O3 S1 C18 F2 57.3(3) . . . . ? O2 S1 C18 F1 -62.4(3) . . . . ? O1 S1 C18 F1 57.2(3) . . . . ? O3 S1 C18 F1 177.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.063 _refine_diff_density_min -1.784 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 961446' data_mg11 # structure by Linda JW Shimon WIS # Mark Gandelman Technion _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H47 N3 P3 Rh, 2(P F6), 2(C4 H6 O)' _chemical_formula_sum 'C120 H126 F24 N6 O4 P10 Rh2' _chemical_formula_weight 2687.79 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7239(7) _cell_length_b 17.5295(8) _cell_length_c 23.5911(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.188(2) _cell_angle_gamma 90.00 _cell_volume 6244.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 66241 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9535 _exptl_absorpt_correction_T_max 0.9535 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KappaApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66241 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11400 _reflns_number_gt 8216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+26.5890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11400 _refine_ls_number_parameters 787 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.005 _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 0.25424(3) 0.73574(3) 0.101473(18) 0.02300(15) Uani 1 1 d . . . P3 P 0.36891(10) 0.64765(8) 0.11178(6) 0.0245(3) Uani 1 1 d . . . P2 P 0.16617(10) 0.84192(9) 0.08901(7) 0.0295(4) Uani 1 1 d . . . P1 P 0.14665(10) 0.65040(8) 0.06268(6) 0.0232(3) Uani 1 1 d . . . N3 N 0.4261(3) 0.7847(3) 0.1891(2) 0.0265(11) Uani 1 1 d . . . N1 N 0.3601(3) 0.8060(3) 0.1431(2) 0.0270(11) Uani 1 1 d . . . N2 N 0.3843(3) 0.8706(3) 0.1231(2) 0.0297(11) Uani 1 1 d . . . C1 C 0.4510(4) 0.6914(3) 0.0801(2) 0.0269(13) Uani 1 1 d . . . C2 C 0.4212(5) 0.7343(4) 0.0291(3) 0.0401(16) Uani 1 1 d . . . H2 H 0.3594 0.7407 0.0119 0.048 Uiso 1 1 calc R . . C3 C 0.4814(5) 0.7683(4) 0.0027(3) 0.0479(18) Uani 1 1 d . . . H3 H 0.4608 0.7985 -0.0319 0.058 Uiso 1 1 calc R . . C4 C 0.5710(5) 0.7573(4) 0.0275(3) 0.0453(17) Uani 1 1 d . . . H4 H 0.6120 0.7792 0.0093 0.054 Uiso 1 1 calc R . . C5 C 0.6014(5) 0.7154(4) 0.0778(3) 0.0460(18) Uani 1 1 d . . . H5 H 0.6633 0.7095 0.0951 0.055 Uiso 1 1 calc R . . C6 C 0.5414(4) 0.6810(4) 0.1038(3) 0.0398(16) Uani 1 1 d . . . H6 H 0.5627 0.6503 0.1381 0.048 Uiso 1 1 calc R . . C7 C 0.3673(4) 0.5487(3) 0.0879(2) 0.0262(13) Uani 1 1 d . . . C8 C 0.3904(4) 0.5302(4) 0.0375(3) 0.0336(14) Uani 1 1 d . . . H8 H 0.4056 0.5697 0.0146 0.040 Uiso 1 1 calc R . . C9 C 0.3919(4) 0.4549(4) 0.0194(3) 0.0421(17) Uani 1 1 d . . . H9 H 0.4089 0.4428 -0.0152 0.051 Uiso 1 1 calc R . . C10 C 0.3684(4) 0.3977(4) 0.0525(3) 0.0391(16) Uani 1 1 d . . . H10 H 0.3702 0.3459 0.0409 0.047 Uiso 1 1 calc R . . C11 C 0.3424(4) 0.4148(4) 0.1019(3) 0.0367(15) Uani 1 1 d . . . H11 H 0.3251 0.3753 0.1240 0.044 Uiso 1 1 calc R . . C12 C 0.3417(4) 0.4908(3) 0.1196(3) 0.0305(13) Uani 1 1 d . . . H12 H 0.3234 0.5030 0.1537 0.037 Uiso 1 1 calc R . . C13 C 0.1182(4) 0.8645(4) 0.1488(3) 0.0377(15) Uani 1 1 d . . . C14 C 0.1294(4) 0.8130(4) 0.1944(3) 0.0437(17) Uani 1 1 d . . . H14 H 0.1567 0.7651 0.1925 0.052 Uiso 1 1 calc R . . C15 C 0.1001(5) 0.8316(6) 0.2439(3) 0.060(2) Uani 1 1 d . . . H15 H 0.1070 0.7967 0.2756 0.072 Uiso 1 1 calc R . . C16 C 0.0607(5) 0.9027(6) 0.2450(4) 0.068(3) Uani 1 1 d . . . H16 H 0.0417 0.9166 0.2785 0.082 Uiso 1 1 calc R . . C17 C 0.0490(6) 0.9518(6) 0.1998(4) 0.070(3) Uani 1 1 d . . . H17 H 0.0207 0.9993 0.2012 0.084 Uiso 1 1 calc R . . C18 C 0.0776(5) 0.9340(4) 0.1513(4) 0.052(2) Uani 1 1 d . . . H18 H 0.0695 0.9692 0.1197 0.062 Uiso 1 1 calc R . . C19 C 0.0798(4) 0.8552(3) 0.0196(3) 0.0345(15) Uani 1 1 d . . . C20 C 0.1050(5) 0.8506(4) -0.0319(3) 0.0409(16) Uani 1 1 d . . . H20 H 0.1651 0.8409 -0.0303 0.049 Uiso 1 1 calc R . . C21 C 0.0420(5) 0.8602(5) -0.0862(3) 0.056(2) Uani 1 1 d . . . H21 H 0.0589 0.8573 -0.1218 0.068 Uiso 1 1 calc R . . C22 C -0.0453(6) 0.8740(5) -0.0879(4) 0.059(2) Uani 1 1 d . . . H22 H -0.0883 0.8799 -0.1249 0.071 Uiso 1 1 calc R . . C23 C -0.0707(5) 0.8792(4) -0.0373(3) 0.0497(19) Uani 1 1 d . . . H23 H -0.1308 0.8894 -0.0392 0.060 Uiso 1 1 calc R . . C24 C -0.0083(4) 0.8695(4) 0.0175(3) 0.0398(16) Uani 1 1 d . . . H24 H -0.0257 0.8726 0.0529 0.048 Uiso 1 1 calc R . . C25 C 0.0297(4) 0.6775(3) 0.0379(2) 0.0273(13) Uani 1 1 d . . . C26 C -0.0184(4) 0.6780(3) -0.0214(3) 0.0350(15) Uani 1 1 d . . . H26 H 0.0101 0.6669 -0.0510 0.042 Uiso 1 1 calc R . . C27 C -0.1088(5) 0.6949(4) -0.0369(3) 0.0459(18) Uani 1 1 d . . . H27 H -0.1417 0.6960 -0.0773 0.055 Uiso 1 1 calc R . . C28 C -0.1498(5) 0.7097(4) 0.0055(4) 0.0462(18) Uani 1 1 d . . . H28 H -0.2117 0.7197 -0.0057 0.055 Uiso 1 1 calc R . . C29 C -0.1034(4) 0.7103(4) 0.0642(3) 0.0419(16) Uani 1 1 d . . . H29 H -0.1325 0.7217 0.0935 0.050 Uiso 1 1 calc R . . C30 C -0.0140(4) 0.6943(3) 0.0799(3) 0.0329(14) Uani 1 1 d . . . H30 H 0.0183 0.6947 0.1205 0.039 Uiso 1 1 calc R . . C31 C 0.1370(4) 0.5771(3) 0.1159(2) 0.0270(13) Uani 1 1 d . . . C32 C 0.0743(4) 0.5188(4) 0.0997(3) 0.0355(15) Uani 1 1 d . . . H32 H 0.0374 0.5157 0.0603 0.043 Uiso 1 1 calc R . . C33 C 0.0660(5) 0.4655(4) 0.1414(3) 0.0406(16) Uani 1 1 d . . . H33 H 0.0245 0.4251 0.1300 0.049 Uiso 1 1 calc R . . C34 C 0.1175(5) 0.4705(4) 0.1992(3) 0.0383(16) Uani 1 1 d . . . H34 H 0.1124 0.4333 0.2274 0.046 Uiso 1 1 calc R . . C35 C 0.1768(4) 0.5308(3) 0.2157(2) 0.0299(13) Uani 1 1 d . . . H35 H 0.2110 0.5360 0.2556 0.036 Uiso 1 1 calc R . . C36 C 0.1860(4) 0.5829(3) 0.1740(2) 0.0275(13) Uani 1 1 d . . . H36 H 0.2269 0.6237 0.1857 0.033 Uiso 1 1 calc R . . C37 C 0.1655(4) 0.6014(3) -0.0011(2) 0.0254(13) Uani 1 1 d . . . C38 C 0.1847(4) 0.6472(4) -0.0442(3) 0.0338(14) Uani 1 1 d . . . H38 H 0.1887 0.7009 -0.0385 0.041 Uiso 1 1 calc R . . C39 C 0.1979(5) 0.6166(4) -0.0947(3) 0.0408(16) Uani 1 1 d . . . H39 H 0.2094 0.6489 -0.1240 0.049 Uiso 1 1 calc R . . C40 C 0.1943(5) 0.5380(4) -0.1024(3) 0.0407(16) Uani 1 1 d . . . H40 H 0.2038 0.5162 -0.1370 0.049 Uiso 1 1 calc R . . C41 C 0.1769(4) 0.4918(4) -0.0599(3) 0.0374(15) Uani 1 1 d . . . H41 H 0.1750 0.4380 -0.0650 0.045 Uiso 1 1 calc R . . C42 C 0.1619(4) 0.5232(3) -0.0091(3) 0.0287(13) Uani 1 1 d . . . H42 H 0.1492 0.4909 0.0199 0.034 Uiso 1 1 calc R . . C43 C 0.2370(4) 0.9269(3) 0.0893(3) 0.0362(15) Uani 1 1 d . . . H43A H 0.2025 0.9643 0.0606 0.043 Uiso 1 1 calc R . . H43B H 0.2509 0.9507 0.1289 0.043 Uiso 1 1 calc R . . C44 C 0.3223(4) 0.9115(4) 0.0747(3) 0.0383(16) Uani 1 1 d . . . H44A H 0.3105 0.8807 0.0382 0.046 Uiso 1 1 calc R . . H44B H 0.3491 0.9604 0.0676 0.046 Uiso 1 1 calc R . . C45 C 0.4159(4) 0.7167(3) 0.2227(2) 0.0283(13) Uani 1 1 d . . . H45A H 0.3568 0.7177 0.2299 0.034 Uiso 1 1 calc R . . H45B H 0.4610 0.7178 0.2616 0.034 Uiso 1 1 calc R . . C46 C 0.4256(4) 0.6429(3) 0.1911(2) 0.0268(13) Uani 1 1 d . . . H46A H 0.4006 0.6002 0.2089 0.032 Uiso 1 1 calc R . . H46B H 0.4892 0.6323 0.1967 0.032 Uiso 1 1 calc R . . C47 C 0.4675(4) 0.8910(3) 0.1551(3) 0.0320(14) Uani 1 1 d . . . C48 C 0.5212(4) 0.9536(4) 0.1521(3) 0.0410(16) Uani 1 1 d . . . H48 H 0.5016 0.9937 0.1244 0.049 Uiso 1 1 calc R . . C49 C 0.6025(5) 0.9538(4) 0.1911(3) 0.0489(18) Uani 1 1 d . . . H49 H 0.6417 0.9945 0.1895 0.059 Uiso 1 1 calc R . . C50 C 0.6320(4) 0.8961(4) 0.2341(3) 0.0450(17) Uani 1 1 d . . . H50 H 0.6900 0.8995 0.2604 0.054 Uiso 1 1 calc R . . C51 C 0.5789(4) 0.8349(4) 0.2391(3) 0.0378(15) Uani 1 1 d . . . H51 H 0.5977 0.7963 0.2681 0.045 Uiso 1 1 calc R . . C52 C 0.4954(4) 0.8344(3) 0.1980(3) 0.0297(13) Uani 1 1 d . . . O1 O -0.2014(5) 0.6630(5) 0.1768(3) 0.095(2) Uiso 1 1 d . . . C53 C -0.1218(8) 0.6270(6) 0.2038(5) 0.094(3) Uani 1 1 d . . . H53A H -0.0934 0.6083 0.1739 0.113 Uiso 1 1 calc R . . H53B H -0.1316 0.5832 0.2277 0.113 Uiso 1 1 calc R . . C54 C -0.2163(10) 0.7080(11) 0.2221(6) 0.142(6) Uani 1 1 d . . . H54A H -0.2419 0.6765 0.2480 0.170 Uiso 1 1 calc R . . H54B H -0.2587 0.7493 0.2051 0.170 Uiso 1 1 calc R . . C55 C -0.0661(9) 0.6853(8) 0.2418(6) 0.109(4) Uiso 1 1 d . . . H55A H -0.0283 0.7118 0.2207 0.131 Uiso 1 1 calc R . . H55B H -0.0279 0.6621 0.2783 0.131 Uiso 1 1 calc R . . C56 C -0.1333(10) 0.7401(9) 0.2556(7) 0.130(5) Uiso 1 1 d . . . H56A H -0.1285 0.7408 0.2984 0.156 Uiso 1 1 calc R . . H56B H -0.1255 0.7926 0.2425 0.156 Uiso 1 1 calc R . . O2 O -0.3071(10) 0.9445(8) 0.0486(6) 0.095(2) Uiso 0.50 1 d PD . . C57 C -0.2365(7) 0.9805(6) 0.0298(4) 0.022(2) Uani 0.50 1 d PD . . H57A H -0.2273 0.9543 -0.0053 0.027 Uiso 0.50 1 calc PR . . H57B H -0.2500 1.0348 0.0200 0.027 Uiso 0.50 1 calc PR . . C58 C -0.2563(11) 0.8858(9) 0.0897(8) 0.064(3) Uani 0.50 1 d PD . . H58A H -0.2882 0.8727 0.1191 0.077 Uiso 0.50 1 calc PR . . H58B H -0.2515 0.8390 0.0673 0.077 Uiso 0.50 1 calc PR . . C59 C -0.1765(11) 0.9106(9) 0.1172(8) 0.064(3) Uani 0.50 1 d PD . . H59A H -0.1313 0.8702 0.1207 0.077 Uiso 0.50 1 calc PR . . H59B H -0.1736 0.9307 0.1569 0.077 Uiso 0.50 1 calc PR . . C60 C -0.1658(9) 0.9736(7) 0.0756(6) 0.046(4) Uani 0.50 1 d PD . . H60A H -0.1551 1.0225 0.0974 0.055 Uiso 0.50 1 calc PR . . H60B H -0.1135 0.9625 0.0614 0.055 Uiso 0.50 1 calc PR . . C64 C 0.4021(10) 0.5397(8) -0.1564(6) 0.047(3) Uiso 0.50 1 d P . . H64A H 0.4647 0.5245 -0.1396 0.056 Uiso 0.50 1 calc PR A 2 H64B H 0.3745 0.5460 -0.1237 0.056 Uiso 0.50 1 calc PR A 2 C61 C 0.3958(13) 0.6123(11) -0.1911(6) 0.070 Uiso 0.50 1 d PD C . H61A H 0.3585 0.6501 -0.1779 0.056 Uiso 0.50 1 calc PR B 2 H61B H 0.4554 0.6345 -0.1859 0.056 Uiso 0.50 1 calc PR B 2 C63A C 0.3143(17) 0.5337(14) -0.2469(10) 0.030(5) Uiso 0.25 1 d P C 1 H63A H 0.3070 0.4992 -0.2811 0.036 Uiso 0.25 1 calc PR C 1 H63B H 0.2546 0.5484 -0.2445 0.036 Uiso 0.25 1 calc PR C 1 C63B C 0.3826(18) 0.5143(15) -0.2377(11) 0.034(6) Uiso 0.25 1 d P C 2 H63C H 0.3544 0.4797 -0.2708 0.041 Uiso 0.25 1 calc PR C 2 H63D H 0.4475 0.5106 -0.2307 0.041 Uiso 0.25 1 calc PR C 2 C62 C 0.3626(11) 0.4921(10) -0.1912(7) 0.058(4) Uiso 0.50 1 d P C . H62A H 0.3199 0.4645 -0.1747 0.070 Uiso 0.50 1 calc PR D 1 H62B H 0.4046 0.4547 -0.1996 0.070 Uiso 0.50 1 calc PR D 1 O3 O 0.3550(4) 0.5911(4) -0.2541(3) 0.0107(13) Uiso 0.50 1 d PD . . P4 P 0.65703(13) 0.66339(11) 0.36186(9) 0.0468(5) Uani 1 1 d . . . F1 F 0.5792(3) 0.7214(3) 0.3629(2) 0.0705(14) Uani 1 1 d . E . F2 F 0.6153(3) 0.6548(3) 0.2916(2) 0.0680(14) Uani 1 1 d . E . F3 F 0.7138(3) 0.7335(2) 0.34971(19) 0.0556(11) Uani 1 1 d . E . F4A F 0.5933(7) 0.6018(6) 0.3813(5) 0.063(3) Uiso 0.50 1 d P E 1 F4B F 0.6109(7) 0.5847(6) 0.3643(4) 0.056(3) Uiso 0.50 1 d P E 2 F5 F 0.7000(3) 0.6744(3) 0.43098(19) 0.0711(14) Uani 1 1 d . E . F6 F 0.7365(3) 0.6084(3) 0.3585(2) 0.0763(16) Uani 1 1 d . E . P5A P 0.3039(12) 0.8361(11) -0.1435(7) 0.0550(9) Uani 0.201(10) 1 d PD F 1 F8A F 0.2829(14) 0.7991(14) -0.0869(9) 0.057(7) Uiso 0.201(10) 1 d PD F 1 F7A F 0.3770(14) 0.7799(13) -0.1377(8) 0.056(8) Uani 0.201(10) 1 d PD F 1 F9A F 0.2320(18) 0.8921(17) -0.1474(15) 0.120 Uiso 0.20 1 d PD F 1 F10A F 0.2336(18) 0.7785(16) -0.1835(12) 0.120 Uiso 0.20 1 d PD F 1 F11A F 0.3752(17) 0.8904(12) -0.1042(11) 0.087(14) Uani 0.201(10) 1 d PD F 1 F12A F 0.3225(13) 0.8680(12) -0.2021(7) 0.039(6) Uani 0.201(10) 1 d PD F 1 P5B P 0.2843(3) 0.8353(3) -0.13903(18) 0.0550(9) Uani 0.799(10) 1 d PD F 2 F8B F 0.2953(4) 0.8466(4) -0.0703(2) 0.0625(19) Uani 0.799(10) 1 d PD F 2 F7B F 0.3284(6) 0.7564(3) -0.1270(3) 0.078(2) Uani 0.799(10) 1 d PD F 2 F9B F 0.2383(6) 0.9160(3) -0.1494(3) 0.096(3) Uani 0.799(10) 1 d PD F 2 F10B F 0.1892(5) 0.7986(5) -0.1453(3) 0.099(3) Uani 0.799(10) 1 d PD F 2 F11B F 0.3747(7) 0.8738(6) -0.1333(5) 0.118(4) Uani 0.799(10) 1 d PD F 2 F12B F 0.2671(7) 0.8237(5) -0.2080(3) 0.100(3) Uani 0.799(10) 1 d PD F 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 0.0230(3) 0.0182(2) 0.0229(2) 0.00001(18) -0.00155(17) -0.00063(19) P3 0.0250(8) 0.0202(8) 0.0253(7) -0.0001(6) 0.0021(6) -0.0013(6) P2 0.0273(8) 0.0210(8) 0.0338(8) -0.0003(6) -0.0022(7) 0.0007(6) P1 0.0227(8) 0.0220(8) 0.0211(7) -0.0007(6) -0.0005(6) -0.0020(6) N3 0.024(3) 0.021(3) 0.028(2) -0.002(2) -0.003(2) -0.001(2) N1 0.024(3) 0.021(3) 0.031(3) 0.001(2) 0.000(2) 0.000(2) N2 0.029(3) 0.016(2) 0.039(3) 0.001(2) 0.001(2) -0.003(2) C1 0.030(3) 0.021(3) 0.028(3) -0.003(2) 0.005(3) -0.006(2) C2 0.043(4) 0.041(4) 0.035(3) 0.005(3) 0.009(3) -0.004(3) C3 0.062(5) 0.046(4) 0.039(4) 0.006(3) 0.020(4) -0.006(4) C4 0.051(5) 0.043(4) 0.048(4) -0.002(3) 0.025(4) -0.013(3) C5 0.036(4) 0.045(4) 0.060(5) 0.001(4) 0.018(3) -0.008(3) C6 0.038(4) 0.038(4) 0.040(4) 0.003(3) 0.006(3) -0.004(3) C7 0.021(3) 0.021(3) 0.032(3) -0.005(2) -0.001(2) 0.001(2) C8 0.029(3) 0.031(3) 0.039(3) -0.004(3) 0.006(3) -0.005(3) C9 0.035(4) 0.042(4) 0.050(4) -0.017(3) 0.013(3) -0.004(3) C10 0.033(4) 0.025(3) 0.054(4) -0.014(3) 0.004(3) -0.003(3) C11 0.031(4) 0.028(3) 0.048(4) -0.002(3) 0.005(3) -0.004(3) C12 0.025(3) 0.024(3) 0.039(3) 0.002(3) 0.005(3) 0.002(3) C13 0.032(4) 0.035(4) 0.042(4) -0.011(3) 0.004(3) 0.004(3) C14 0.036(4) 0.056(5) 0.031(3) -0.014(3) -0.004(3) 0.008(3) C15 0.050(5) 0.095(7) 0.033(4) -0.011(4) 0.007(3) 0.009(5) C16 0.046(5) 0.105(8) 0.051(5) -0.042(5) 0.007(4) 0.012(5) C17 0.057(6) 0.072(6) 0.069(6) -0.026(5) 0.000(5) 0.021(5) C18 0.041(4) 0.041(4) 0.067(5) -0.017(4) 0.005(4) 0.009(3) C19 0.036(4) 0.020(3) 0.042(4) 0.001(3) 0.001(3) -0.004(3) C20 0.044(4) 0.033(4) 0.039(4) 0.013(3) 0.001(3) 0.000(3) C21 0.055(5) 0.067(5) 0.040(4) 0.020(4) 0.001(4) -0.008(4) C22 0.057(5) 0.053(5) 0.051(5) 0.024(4) -0.012(4) -0.005(4) C23 0.035(4) 0.040(4) 0.060(5) 0.010(3) -0.011(4) 0.004(3) C24 0.034(4) 0.025(3) 0.051(4) 0.005(3) -0.004(3) 0.004(3) C25 0.028(3) 0.020(3) 0.030(3) -0.001(2) 0.002(3) -0.004(2) C26 0.033(4) 0.028(3) 0.034(3) -0.002(3) -0.006(3) -0.001(3) C27 0.033(4) 0.040(4) 0.051(4) 0.002(3) -0.012(3) -0.001(3) C28 0.027(4) 0.031(4) 0.074(5) 0.004(4) 0.003(4) 0.001(3) C29 0.037(4) 0.033(4) 0.057(4) 0.003(3) 0.013(3) 0.005(3) C30 0.030(4) 0.031(3) 0.033(3) -0.002(3) 0.000(3) 0.001(3) C31 0.027(3) 0.024(3) 0.028(3) 0.000(2) 0.004(2) 0.001(3) C32 0.037(4) 0.039(4) 0.028(3) -0.003(3) 0.003(3) -0.007(3) C33 0.048(4) 0.039(4) 0.036(3) -0.002(3) 0.014(3) -0.017(3) C34 0.046(4) 0.033(4) 0.038(3) 0.005(3) 0.016(3) -0.006(3) C35 0.031(3) 0.032(3) 0.022(3) 0.000(2) 0.001(2) 0.001(3) C36 0.027(3) 0.025(3) 0.028(3) -0.003(2) 0.004(2) -0.002(3) C37 0.023(3) 0.030(3) 0.020(3) -0.004(2) 0.001(2) -0.001(2) C38 0.040(4) 0.027(3) 0.031(3) 0.001(3) 0.004(3) -0.005(3) C39 0.052(4) 0.042(4) 0.027(3) 0.001(3) 0.010(3) -0.007(3) C40 0.046(4) 0.044(4) 0.033(3) -0.011(3) 0.011(3) -0.006(3) C41 0.036(4) 0.031(4) 0.042(4) -0.010(3) 0.005(3) -0.005(3) C42 0.027(3) 0.024(3) 0.031(3) -0.001(2) 0.002(3) -0.005(3) C43 0.029(4) 0.022(3) 0.050(4) 0.005(3) -0.004(3) 0.000(3) C44 0.033(4) 0.028(4) 0.045(4) 0.011(3) -0.004(3) -0.004(3) C45 0.028(3) 0.028(3) 0.023(3) 0.002(2) -0.001(2) -0.001(3) C46 0.021(3) 0.023(3) 0.031(3) 0.006(2) -0.002(2) 0.001(2) C47 0.025(3) 0.025(3) 0.041(3) -0.004(3) 0.001(3) -0.005(3) C48 0.032(4) 0.027(3) 0.058(4) 0.005(3) 0.004(3) -0.006(3) C49 0.038(4) 0.036(4) 0.068(5) 0.000(4) 0.008(4) -0.012(3) C50 0.026(4) 0.041(4) 0.058(4) -0.006(3) -0.005(3) -0.008(3) C51 0.029(4) 0.035(4) 0.042(4) -0.004(3) -0.004(3) -0.002(3) C52 0.028(3) 0.020(3) 0.037(3) -0.004(2) 0.003(3) -0.001(3) C53 0.110(9) 0.083(8) 0.068(6) 0.006(5) -0.011(6) 0.003(7) C54 0.125(12) 0.211(17) 0.095(9) -0.046(11) 0.042(9) 0.038(12) C57 0.037(7) 0.013(5) 0.013(5) 0.006(4) 0.001(5) -0.016(5) C58 0.066(8) 0.048(7) 0.070(8) 0.016(6) 0.007(6) 0.010(6) C59 0.066(8) 0.048(7) 0.070(8) 0.016(6) 0.007(6) 0.010(6) C60 0.054(9) 0.026(7) 0.071(10) 0.015(7) 0.041(8) 0.021(6) P4 0.0391(11) 0.0350(10) 0.0505(11) 0.0024(8) -0.0137(9) -0.0042(8) F1 0.042(3) 0.083(4) 0.081(3) -0.006(3) 0.009(2) 0.007(2) F2 0.063(3) 0.051(3) 0.062(3) -0.013(2) -0.029(2) 0.012(2) F3 0.050(3) 0.047(2) 0.065(3) 0.000(2) 0.007(2) -0.010(2) F5 0.057(3) 0.102(4) 0.043(2) 0.005(2) -0.004(2) -0.008(3) F6 0.065(3) 0.046(3) 0.088(3) -0.013(2) -0.030(3) 0.020(2) P5A 0.084(3) 0.0444(12) 0.0368(12) 0.0103(9) 0.0176(14) 0.0042(16) F7A 0.064(16) 0.078(19) 0.038(11) 0.031(11) 0.033(11) 0.029(13) F11A 0.12(3) 0.021(12) 0.08(2) -0.004(13) -0.051(19) 0.004(13) F12A 0.047(13) 0.040(13) 0.041(11) 0.015(9) 0.029(10) 0.012(10) P5B 0.084(3) 0.0444(12) 0.0368(12) 0.0103(9) 0.0176(14) 0.0042(16) F8B 0.083(4) 0.066(5) 0.038(3) 0.009(3) 0.017(3) -0.004(3) F7B 0.122(7) 0.044(4) 0.060(4) 0.013(3) 0.015(4) 0.014(4) F9B 0.196(9) 0.054(4) 0.037(3) 0.010(3) 0.033(4) 0.042(5) F10B 0.080(5) 0.113(6) 0.087(5) -0.030(5) -0.004(4) -0.008(5) F11B 0.142(9) 0.100(8) 0.146(10) -0.015(6) 0.095(8) -0.064(6) F12B 0.170(9) 0.092(6) 0.039(3) 0.013(4) 0.030(4) 0.051(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.083(5) . ? Rh1 P1 2.2526(15) . ? Rh1 P2 2.2893(16) . ? Rh1 P3 2.3347(16) . ? P3 C7 1.822(6) . ? P3 C1 1.831(6) . ? P3 C46 1.837(6) . ? P2 C13 1.818(7) . ? P2 C19 1.827(6) . ? P2 C43 1.858(6) . ? P1 C37 1.827(6) . ? P1 C25 1.830(6) . ? P1 C31 1.832(6) . ? N3 N1 1.329(6) . ? N3 C52 1.365(7) . ? N3 C45 1.466(7) . ? N1 N2 1.323(7) . ? N2 C47 1.363(8) . ? N2 C44 1.466(8) . ? C1 C2 1.384(9) . ? C1 C6 1.387(9) . ? C2 C3 1.404(10) . ? C2 H2 0.9500 . ? C3 C4 1.380(11) . ? C3 H3 0.9500 . ? C4 C5 1.364(10) . ? C4 H4 0.9500 . ? C5 C6 1.398(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.374(8) . ? C7 C12 1.385(8) . ? C8 C9 1.390(9) . ? C8 H8 0.9500 . ? C9 C10 1.383(10) . ? C9 H9 0.9500 . ? C10 C11 1.371(9) . ? C10 H10 0.9500 . ? C11 C12 1.398(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.379(10) . ? C13 C18 1.384(9) . ? C14 C15 1.407(10) . ? C14 H14 0.9500 . ? C15 C16 1.396(12) . ? C15 H15 0.9500 . ? C16 C17 1.344(13) . ? C16 H16 0.9500 . ? C17 C18 1.376(12) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.383(9) . ? C19 C24 1.394(9) . ? C20 C21 1.394(9) . ? C20 H20 0.9500 . ? C21 C22 1.384(12) . ? C21 H21 0.9500 . ? C22 C23 1.363(11) . ? C22 H22 0.9500 . ? C23 C24 1.397(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.387(8) . ? C25 C26 1.391(8) . ? C26 C27 1.398(9) . ? C26 H26 0.9500 . ? C27 C28 1.357(10) . ? C27 H27 0.9500 . ? C28 C29 1.374(10) . ? C28 H28 0.9500 . ? C29 C30 1.379(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.377(8) . ? C31 C32 1.398(9) . ? C32 C33 1.388(9) . ? C32 H32 0.9500 . ? C33 C34 1.382(9) . ? C33 H33 0.9500 . ? C34 C35 1.391(9) . ? C34 H34 0.9500 . ? C35 C36 1.378(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.383(8) . ? C37 C38 1.392(8) . ? C38 C39 1.374(9) . ? C38 H38 0.9500 . ? C39 C40 1.389(10) . ? C39 H39 0.9500 . ? C40 C41 1.375(9) . ? C40 H40 0.9500 . ? C41 C42 1.397(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.500(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.522(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C52 1.398(9) . ? C47 C48 1.399(9) . ? C48 C49 1.351(10) . ? C48 H48 0.9500 . ? C49 C50 1.417(10) . ? C49 H49 0.9500 . ? C50 C51 1.386(9) . ? C50 H50 0.9500 . ? C51 C52 1.397(8) . ? C51 H51 0.9500 . ? O1 C53 1.388(12) . ? O1 C54 1.399(13) . ? C53 C55 1.475(15) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C56 1.440(18) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.530(17) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O2 C57 1.450(15) . ? O2 C58 1.485(16) . ? C57 C60 1.322(16) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.315(18) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.52(2) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C64 C62 1.21(2) . ? C64 C61 1.50(2) . ? C64 C63B 1.91(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C61 O3 1.494(14) . ? C61 C63B 2.02(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C63A O3 1.23(2) . ? C63A C62 1.51(3) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C63B C62 1.28(3) . ? C63B O3 1.43(3) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? P4 F4B 1.567(10) . ? P4 F3 1.591(5) . ? P4 F5 1.593(5) . ? P4 F1 1.597(5) . ? P4 F6 1.598(5) . ? P4 F2 1.610(5) . ? P4 F4A 1.623(11) . ? P5A F9A 1.480(16) . ? P5A F7A 1.490(15) . ? P5A F11A 1.563(16) . ? P5A F12A 1.594(15) . ? P5A F10A 1.598(17) . ? P5A F8A 1.598(16) . ? P5B F7B 1.538(7) . ? P5B F11B 1.545(8) . ? P5B F9B 1.577(7) . ? P5B F12B 1.587(6) . ? P5B F8B 1.594(6) . ? P5B F10B 1.596(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 N1 Rh1 P1 174.24(13) . . ? N1 Rh1 P2 87.42(13) . . ? P1 Rh1 P2 97.41(6) . . ? N1 Rh1 P3 81.36(14) . . ? P1 Rh1 P3 94.23(5) . . ? P2 Rh1 P3 166.67(6) . . ? C7 P3 C1 102.9(3) . . ? C7 P3 C46 103.5(3) . . ? C1 P3 C46 103.8(3) . . ? C7 P3 Rh1 130.82(19) . . ? C1 P3 Rh1 107.0(2) . . ? C46 P3 Rh1 106.09(19) . . ? C13 P2 C19 107.5(3) . . ? C13 P2 C43 101.5(3) . . ? C19 P2 C43 101.3(3) . . ? C13 P2 Rh1 116.4(2) . . ? C19 P2 Rh1 119.4(2) . . ? C43 P2 Rh1 108.1(2) . . ? C37 P1 C25 103.8(3) . . ? C37 P1 C31 107.4(3) . . ? C25 P1 C31 97.7(3) . . ? C37 P1 Rh1 111.77(19) . . ? C25 P1 Rh1 122.08(19) . . ? C31 P1 Rh1 112.56(19) . . ? N1 N3 C52 110.8(5) . . ? N1 N3 C45 119.5(4) . . ? C52 N3 C45 129.7(5) . . ? N2 N1 N3 107.1(4) . . ? N2 N1 Rh1 127.6(4) . . ? N3 N1 Rh1 123.9(4) . . ? N1 N2 C47 110.8(5) . . ? N1 N2 C44 120.1(5) . . ? C47 N2 C44 129.0(5) . . ? C2 C1 C6 118.9(6) . . ? C2 C1 P3 118.4(5) . . ? C6 C1 P3 122.6(5) . . ? C1 C2 C3 120.6(7) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.1(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.9(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.5(6) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C12 118.8(5) . . ? C8 C7 P3 120.5(5) . . ? C12 C7 P3 120.7(4) . . ? C7 C8 C9 121.4(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 119.0(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 120.7(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C7 C12 C11 120.6(6) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C18 120.2(7) . . ? C14 C13 P2 118.2(5) . . ? C18 C13 P2 121.4(6) . . ? C13 C14 C15 119.8(7) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 118.2(8) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 121.3(8) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.8(8) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 119.8(8) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C20 C19 C24 120.3(6) . . ? C20 C19 P2 117.1(5) . . ? C24 C19 P2 122.6(5) . . ? C19 C20 C21 119.7(7) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 119.5(8) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 121.1(7) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 119.4(7) . . ? C19 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C30 C25 C26 118.6(6) . . ? C30 C25 P1 118.7(4) . . ? C26 C25 P1 122.6(5) . . ? C25 C26 C27 119.5(6) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.1(6) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C30 119.0(7) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C25 121.5(6) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? C36 C31 C32 118.9(5) . . ? C36 C31 P1 120.0(4) . . ? C32 C31 P1 120.8(4) . . ? C33 C32 C31 119.7(6) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 120.8(6) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.1(6) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 120.0(5) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C31 C36 C35 121.4(5) . . ? C31 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C42 C37 C38 118.8(5) . . ? C42 C37 P1 124.6(4) . . ? C38 C37 P1 116.6(4) . . ? C39 C38 C37 121.5(6) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 119.4(6) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 119.8(6) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.6(6) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C37 C42 C41 119.8(6) . . ? C37 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 P2 115.4(4) . . ? C44 C43 H43A 108.4 . . ? P2 C43 H43A 108.4 . . ? C44 C43 H43B 108.4 . . ? P2 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? N2 C44 C43 110.6(5) . . ? N2 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? N3 C45 C46 112.7(5) . . ? N3 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? N3 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C45 C46 P3 112.0(4) . . ? C45 C46 H46A 109.2 . . ? P3 C46 H46A 109.2 . . ? C45 C46 H46B 109.2 . . ? P3 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? N2 C47 C52 105.9(5) . . ? N2 C47 C48 132.7(6) . . ? C52 C47 C48 121.4(6) . . ? C49 C48 C47 116.0(6) . . ? C49 C48 H48 122.0 . . ? C47 C48 H48 122.0 . . ? C48 C49 C50 123.0(6) . . ? C48 C49 H49 118.5 . . ? C50 C49 H49 118.5 . . ? C51 C50 C49 121.9(6) . . ? C51 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? C50 C51 C52 114.7(6) . . ? C50 C51 H51 122.6 . . ? C52 C51 H51 122.6 . . ? N3 C52 C51 131.8(6) . . ? N3 C52 C47 105.4(5) . . ? C51 C52 C47 122.9(6) . . ? C53 O1 C54 103.1(9) . . ? O1 C53 C55 105.7(10) . . ? O1 C53 H53A 110.6 . . ? C55 C53 H53A 110.6 . . ? O1 C53 H53B 110.6 . . ? C55 C53 H53B 110.6 . . ? H53A C53 H53B 108.7 . . ? O1 C54 C56 108.7(12) . . ? O1 C54 H54A 109.9 . . ? C56 C54 H54A 109.9 . . ? O1 C54 H54B 109.9 . . ? C56 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? C53 C55 C56 103.7(11) . . ? C53 C55 H55A 111.0 . . ? C56 C55 H55A 111.0 . . ? C53 C55 H55B 111.0 . . ? C56 C55 H55B 111.0 . . ? H55A C55 H55B 109.0 . . ? C54 C56 C55 102.2(12) . . ? C54 C56 H56A 111.3 . . ? C55 C56 H56A 111.3 . . ? C54 C56 H56B 111.3 . . ? C55 C56 H56B 111.3 . . ? H56A C56 H56B 109.2 . . ? C57 O2 C58 100.5(12) . . ? C60 C57 O2 104.5(10) . . ? C60 C57 H57A 110.9 . . ? O2 C57 H57A 110.9 . . ? C60 C57 H57B 110.9 . . ? O2 C57 H57B 110.9 . . ? H57A C57 H57B 108.9 . . ? C59 C58 O2 111.0(14) . . ? C59 C58 H58A 109.4 . . ? O2 C58 H58A 109.4 . . ? C59 C58 H58B 109.4 . . ? O2 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C58 C59 C60 100.6(13) . . ? C58 C59 H59A 111.7 . . ? C60 C59 H59A 111.7 . . ? C58 C59 H59B 111.7 . . ? C60 C59 H59B 111.7 . . ? H59A C59 H59B 109.4 . . ? C57 C60 C59 112.1(12) . . ? C57 C60 H60A 109.2 . . ? C59 C60 H60A 109.2 . . ? C57 C60 H60B 109.2 . . ? C59 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C62 C64 C61 105.7(14) . . ? C61 C64 C63B 71.5(11) . . ? C62 C64 H64A 110.6 . . ? C61 C64 H64A 110.6 . . ? C63B C64 H64A 101.7 . . ? C62 C64 H64B 110.6 . . ? C61 C64 H64B 110.6 . . ? C63B C64 H64B 145.7 . . ? H64A C64 H64B 108.7 . . ? O3 C61 C64 106.0(12) . . ? O3 C61 C63B 45.2(9) . . ? C64 C61 C63B 63.6(11) . . ? O3 C61 H61A 110.5 . . ? C64 C61 H61A 110.5 . . ? C63B C61 H61A 139.4 . . ? O3 C61 H61B 110.5 . . ? C64 C61 H61B 110.5 . . ? C63B C61 H61B 110.7 . . ? H61A C61 H61B 108.7 . . ? O3 C63A C62 111.2(18) . . ? O3 C63A H63A 109.4 . . ? C62 C63A H63A 109.4 . . ? O3 C63A H63B 109.4 . . ? C62 C63A H63B 109.4 . . ? H63A C63A H63B 108.0 . . ? C62 C63B O3 113(2) . . ? O3 C63B C64 90.3(14) . . ? C62 C63B C61 78.7(15) . . ? O3 C63B C61 47.6(9) . . ? C62 C63B H63C 109.0 . . ? O3 C63B H63C 109.0 . . ? C64 C63B H63C 147.8 . . ? C61 C63B H63C 154.9 . . ? C62 C63B H63D 109.0 . . ? O3 C63B H63D 109.0 . . ? C64 C63B H63D 88.8 . . ? C61 C63B H63D 91.1 . . ? H63C C63B H63D 107.8 . . ? C64 C62 C63B 99.7(18) . . ? C64 C62 C63A 107.2(17) . . ? C63B C62 C63A 45.0(15) . . ? C64 C62 H62A 110.3 . . ? C63B C62 H62A 146.9 . . ? C63A C62 H62A 110.3 . . ? C64 C62 H62B 110.3 . . ? C63B C62 H62B 72.0 . . ? C63A C62 H62B 110.3 . . ? H62A C62 H62B 108.5 . . ? C63A O3 C63B 47.5(14) . . ? C63A O3 C61 99.3(14) . . ? C63B O3 C61 87.2(13) . . ? F4B P4 F3 167.2(5) . . ? F4B P4 F5 97.9(4) . . ? F3 P4 F5 89.5(3) . . ? F4B P4 F1 101.3(4) . . ? F3 P4 F1 89.0(3) . . ? F5 P4 F1 90.8(3) . . ? F4B P4 F6 81.2(4) . . ? F3 P4 F6 88.3(3) . . ? F5 P4 F6 90.5(3) . . ? F1 P4 F6 177.0(3) . . ? F4B P4 F2 84.0(4) . . ? F3 P4 F2 88.6(3) . . ? F5 P4 F2 178.1(3) . . ? F1 P4 F2 89.0(3) . . ? F6 P4 F2 89.6(3) . . ? F3 P4 F4A 170.4(5) . . ? F5 P4 F4A 84.9(4) . . ? F1 P4 F4A 83.3(4) . . ? F6 P4 F4A 99.5(5) . . ? F2 P4 F4A 97.0(4) . . ? F9A P5A F7A 178.5(16) . . ? F9A P5A F11A 92.4(14) . . ? F7A P5A F11A 86.6(12) . . ? F9A P5A F12A 91.9(15) . . ? F7A P5A F12A 89.3(11) . . ? F11A P5A F12A 91.5(13) . . ? F9A P5A F10A 89.5(14) . . ? F7A P5A F10A 91.4(13) . . ? F11A P5A F10A 178.0(16) . . ? F12A P5A F10A 88.4(12) . . ? F9A P5A F8A 89.4(14) . . ? F7A P5A F8A 89.4(11) . . ? F11A P5A F8A 91.9(13) . . ? F12A P5A F8A 176.2(15) . . ? F10A P5A F8A 88.1(13) . . ? F7B P5B F11B 91.1(5) . . ? F7B P5B F9B 178.1(5) . . ? F11B P5B F9B 89.6(5) . . ? F7B P5B F12B 90.7(4) . . ? F11B P5B F12B 92.1(6) . . ? F9B P5B F12B 90.9(4) . . ? F7B P5B F8B 90.5(4) . . ? F11B P5B F8B 91.2(5) . . ? F9B P5B F8B 87.8(4) . . ? F12B P5B F8B 176.5(5) . . ? F7B P5B F10B 91.0(5) . . ? F11B P5B F10B 177.9(6) . . ? F9B P5B F10B 88.2(5) . . ? F12B P5B F10B 88.1(5) . . ? F8B P5B F10B 88.6(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 N1 Rh1 P3 C7 -177.6(3) . . . . ? P1 Rh1 P3 C7 6.1(3) . . . . ? P2 Rh1 P3 C7 -144.7(3) . . . . ? N1 Rh1 P3 C1 -52.7(2) . . . . ? P1 Rh1 P3 C1 131.02(19) . . . . ? P2 Rh1 P3 C1 -19.8(3) . . . . ? N1 Rh1 P3 C46 57.6(2) . . . . ? P1 Rh1 P3 C46 -118.6(2) . . . . ? P2 Rh1 P3 C46 90.6(3) . . . . ? N1 Rh1 P2 C13 -88.4(3) . . . . ? P1 Rh1 P2 C13 88.4(2) . . . . ? P3 Rh1 P2 C13 -121.0(3) . . . . ? N1 Rh1 P2 C19 139.9(3) . . . . ? P1 Rh1 P2 C19 -43.3(3) . . . . ? P3 Rh1 P2 C19 107.3(3) . . . . ? N1 Rh1 P2 C43 25.0(3) . . . . ? P1 Rh1 P2 C43 -158.2(2) . . . . ? P3 Rh1 P2 C43 -7.6(4) . . . . ? P2 Rh1 P1 C37 119.9(2) . . . . ? P3 Rh1 P1 C37 -53.5(2) . . . . ? P2 Rh1 P1 C25 -3.6(2) . . . . ? P3 Rh1 P1 C25 -177.1(2) . . . . ? P2 Rh1 P1 C31 -119.1(2) . . . . ? P3 Rh1 P1 C31 67.4(2) . . . . ? C52 N3 N1 N2 -2.1(6) . . . . ? C45 N3 N1 N2 176.5(5) . . . . ? C52 N3 N1 Rh1 165.4(4) . . . . ? C45 N3 N1 Rh1 -16.0(7) . . . . ? P2 Rh1 N1 N2 -51.7(5) . . . . ? P3 Rh1 N1 N2 121.0(5) . . . . ? P2 Rh1 N1 N3 143.4(4) . . . . ? P3 Rh1 N1 N3 -43.8(4) . . . . ? N3 N1 N2 C47 1.6(6) . . . . ? Rh1 N1 N2 C47 -165.3(4) . . . . ? N3 N1 N2 C44 -175.6(5) . . . . ? Rh1 N1 N2 C44 17.4(8) . . . . ? C7 P3 C1 C2 101.4(5) . . . . ? C46 P3 C1 C2 -151.0(5) . . . . ? Rh1 P3 C1 C2 -39.1(5) . . . . ? C7 P3 C1 C6 -76.2(6) . . . . ? C46 P3 C1 C6 31.5(6) . . . . ? Rh1 P3 C1 C6 143.4(5) . . . . ? C6 C1 C2 C3 -1.6(10) . . . . ? P3 C1 C2 C3 -179.3(5) . . . . ? C1 C2 C3 C4 1.3(11) . . . . ? C2 C3 C4 C5 -1.4(11) . . . . ? C3 C4 C5 C6 1.9(11) . . . . ? C2 C1 C6 C5 2.1(10) . . . . ? P3 C1 C6 C5 179.7(5) . . . . ? C4 C5 C6 C1 -2.3(11) . . . . ? C1 P3 C7 C8 -26.1(5) . . . . ? C46 P3 C7 C8 -134.0(5) . . . . ? Rh1 P3 C7 C8 100.3(5) . . . . ? C1 P3 C7 C12 154.7(5) . . . . ? C46 P3 C7 C12 46.9(5) . . . . ? Rh1 P3 C7 C12 -78.8(5) . . . . ? C12 C7 C8 C9 -2.6(9) . . . . ? P3 C7 C8 C9 178.2(5) . . . . ? C7 C8 C9 C10 1.0(10) . . . . ? C8 C9 C10 C11 1.1(10) . . . . ? C9 C10 C11 C12 -1.4(10) . . . . ? C8 C7 C12 C11 2.3(9) . . . . ? P3 C7 C12 C11 -178.5(5) . . . . ? C10 C11 C12 C7 -0.3(9) . . . . ? C19 P2 C13 C14 130.1(5) . . . . ? C43 P2 C13 C14 -123.9(5) . . . . ? Rh1 P2 C13 C14 -6.8(6) . . . . ? C19 P2 C13 C18 -55.0(6) . . . . ? C43 P2 C13 C18 51.0(6) . . . . ? Rh1 P2 C13 C18 168.1(5) . . . . ? C18 C13 C14 C15 -0.6(10) . . . . ? P2 C13 C14 C15 174.4(6) . . . . ? C13 C14 C15 C16 -0.3(11) . . . . ? C14 C15 C16 C17 1.4(13) . . . . ? C15 C16 C17 C18 -1.5(14) . . . . ? C16 C17 C18 C13 0.5(13) . . . . ? C14 C13 C18 C17 0.5(11) . . . . ? P2 C13 C18 C17 -174.3(6) . . . . ? C13 P2 C19 C20 171.8(5) . . . . ? C43 P2 C19 C20 65.7(5) . . . . ? Rh1 P2 C19 C20 -52.7(5) . . . . ? C13 P2 C19 C24 -8.0(6) . . . . ? C43 P2 C19 C24 -114.2(5) . . . . ? Rh1 P2 C19 C24 127.4(5) . . . . ? C24 C19 C20 C21 -0.1(10) . . . . ? P2 C19 C20 C21 180.0(5) . . . . ? C19 C20 C21 C22 -0.2(11) . . . . ? C20 C21 C22 C23 0.7(12) . . . . ? C21 C22 C23 C24 -0.9(12) . . . . ? C20 C19 C24 C23 0.0(9) . . . . ? P2 C19 C24 C23 179.9(5) . . . . ? C22 C23 C24 C19 0.5(10) . . . . ? C37 P1 C25 C30 160.1(5) . . . . ? C31 P1 C25 C30 50.0(5) . . . . ? Rh1 P1 C25 C30 -72.7(5) . . . . ? C37 P1 C25 C26 -16.3(6) . . . . ? C31 P1 C25 C26 -126.3(5) . . . . ? Rh1 P1 C25 C26 110.9(5) . . . . ? C30 C25 C26 C27 -0.2(9) . . . . ? P1 C25 C26 C27 176.1(5) . . . . ? C25 C26 C27 C28 -0.9(10) . . . . ? C26 C27 C28 C29 1.7(11) . . . . ? C27 C28 C29 C30 -1.2(10) . . . . ? C28 C29 C30 C25 0.0(10) . . . . ? C26 C25 C30 C29 0.7(9) . . . . ? P1 C25 C30 C29 -175.8(5) . . . . ? C37 P1 C31 C36 130.0(5) . . . . ? C25 P1 C31 C36 -122.9(5) . . . . ? Rh1 P1 C31 C36 6.6(5) . . . . ? C37 P1 C31 C32 -56.0(6) . . . . ? C25 P1 C31 C32 51.0(5) . . . . ? Rh1 P1 C31 C32 -179.4(4) . . . . ? C36 C31 C32 C33 -3.7(9) . . . . ? P1 C31 C32 C33 -177.7(5) . . . . ? C31 C32 C33 C34 1.8(10) . . . . ? C32 C33 C34 C35 1.2(10) . . . . ? C33 C34 C35 C36 -2.3(10) . . . . ? C32 C31 C36 C35 2.6(9) . . . . ? P1 C31 C36 C35 176.7(5) . . . . ? C34 C35 C36 C31 0.4(9) . . . . ? C25 P1 C37 C42 -95.7(5) . . . . ? C31 P1 C37 C42 7.0(6) . . . . ? Rh1 P1 C37 C42 130.9(5) . . . . ? C25 P1 C37 C38 84.2(5) . . . . ? C31 P1 C37 C38 -173.0(4) . . . . ? Rh1 P1 C37 C38 -49.1(5) . . . . ? C42 C37 C38 C39 1.5(9) . . . . ? P1 C37 C38 C39 -178.4(5) . . . . ? C37 C38 C39 C40 -1.6(10) . . . . ? C38 C39 C40 C41 0.5(10) . . . . ? C39 C40 C41 C42 0.7(10) . . . . ? C38 C37 C42 C41 -0.4(9) . . . . ? P1 C37 C42 C41 179.6(5) . . . . ? C40 C41 C42 C37 -0.7(9) . . . . ? C13 P2 C43 C44 144.7(5) . . . . ? C19 P2 C43 C44 -104.5(5) . . . . ? Rh1 P2 C43 C44 21.7(5) . . . . ? N1 N2 C44 C43 54.5(7) . . . . ? C47 N2 C44 C43 -122.1(7) . . . . ? P2 C43 C44 N2 -71.2(6) . . . . ? N1 N3 C45 C46 76.4(6) . . . . ? C52 N3 C45 C46 -105.3(6) . . . . ? N3 C45 C46 P3 -41.8(6) . . . . ? C7 P3 C46 C45 -167.1(4) . . . . ? C1 P3 C46 C45 85.7(5) . . . . ? Rh1 P3 C46 C45 -26.9(4) . . . . ? N1 N2 C47 C52 -0.5(7) . . . . ? C44 N2 C47 C52 176.4(6) . . . . ? N1 N2 C47 C48 -178.8(7) . . . . ? C44 N2 C47 C48 -1.9(12) . . . . ? N2 C47 C48 C49 -178.5(7) . . . . ? C52 C47 C48 C49 3.3(10) . . . . ? C47 C48 C49 C50 -2.2(11) . . . . ? C48 C49 C50 C51 0.1(12) . . . . ? C49 C50 C51 C52 0.9(10) . . . . ? N1 N3 C52 C51 -177.9(6) . . . . ? C45 N3 C52 C51 3.7(11) . . . . ? N1 N3 C52 C47 1.8(6) . . . . ? C45 N3 C52 C47 -176.6(6) . . . . ? C50 C51 C52 N3 180.0(6) . . . . ? C50 C51 C52 C47 0.3(9) . . . . ? N2 C47 C52 N3 -0.8(7) . . . . ? C48 C47 C52 N3 177.8(6) . . . . ? N2 C47 C52 C51 179.0(6) . . . . ? C48 C47 C52 C51 -2.4(10) . . . . ? C54 O1 C53 C55 -40.1(14) . . . . ? C53 O1 C54 C56 39.6(16) . . . . ? O1 C53 C55 C56 26.1(14) . . . . ? O1 C54 C56 C55 -22.1(17) . . . . ? C53 C55 C56 C54 -2.5(15) . . . . ? C58 O2 C57 C60 -30.6(15) . . . . ? C57 O2 C58 C59 33.5(19) . . . . ? O2 C58 C59 C60 -21.0(19) . . . . ? O2 C57 C60 C59 20.5(16) . . . . ? C58 C59 C60 C57 0.2(19) . . . . ? C62 C64 C61 O3 -7.6(19) . . . . ? C63B C64 C61 O3 16.2(13) . . . . ? C62 C64 C61 C63B -23.8(15) . . . . ? C61 C64 C63B C62 -144(2) . . . . ? C62 C64 C63B O3 128(2) . . . . ? C61 C64 C63B O3 -16.2(13) . . . . ? C62 C64 C63B C61 144(2) . . . . ? O3 C61 C63B C62 -136(2) . . . . ? C64 C61 C63B C62 22.0(13) . . . . ? C64 C61 C63B O3 157.8(17) . . . . ? O3 C61 C63B C64 -157.8(17) . . . . ? C61 C64 C62 C63B 35(2) . . . . ? C61 C64 C62 C63A -10(2) . . . . ? C63B C64 C62 C63A -45.7(16) . . . . ? O3 C63B C62 C64 -59(2) . . . . ? C61 C63B C62 C64 -25.0(14) . . . . ? O3 C63B C62 C63A 45.7(18) . . . . ? C64 C63B C62 C63A 105(2) . . . . ? C61 C63B C62 C63A 79.7(19) . . . . ? O3 C63A C62 C64 31(2) . . . . ? O3 C63A C62 C63B -56(2) . . . . ? C62 C63A O3 C63B 45.1(18) . . . . ? C62 C63A O3 C61 -32(2) . . . . ? C62 C63B O3 C63A -57(2) . . . . ? C64 C63B O3 C63A -90(2) . . . . ? C61 C63B O3 C63A -105.3(19) . . . . ? C62 C63B O3 C61 48(2) . . . . ? C64 C63B O3 C61 15.5(12) . . . . ? C64 C61 O3 C63A 25.4(18) . . . . ? C63B C61 O3 C63A 46.1(15) . . . . ? C64 C61 O3 C63B -20.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.509 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 961447'