# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1365 data_ccd209 _audit_creation_method SHELXL-97 _chemical_name_common ; tris[3,5-bis(trifluoromethyl)phenyl]borane ; _publ_contact_author ; Gregory J. Kubas CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'kubas@lanl.gov' loop_ _publ_author_name 'Wayde V. Konze' 'Brian L. Scott' 'Gregory J. Kubas' _publ_requested_journal 'Chemical Communications' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H9 B F18' _chemical_formula_weight 650.12 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5433(9) _cell_length_b 11.656(1) _cell_length_c 12.775(1) _cell_angle_alpha 100.544(2) _cell_angle_beta 110.146(1) _cell_angle_gamma 97.299(2) _cell_volume 1283.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_crystal_preparation 'crystallized from benzene' _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4206 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4206 _reflns_number_gt 2437 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4206 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1408(4) 0.3195(3) 0.7592(3) 0.0385(8) Uani 1 1 d . . . C2 C 0.2787(4) 0.3045(3) 0.8363(3) 0.0394(8) Uani 1 1 d . . . H2 H 0.2771 0.2533 0.8840 0.047 Uiso 1 1 calc R . . C3 C 0.4179(4) 0.3647(3) 0.8429(3) 0.0401(9) Uani 1 1 d . . . C4 C 0.4231(4) 0.4433(3) 0.7746(4) 0.0503(10) Uani 1 1 d . . . H4 H 0.5164 0.4838 0.7794 0.060 Uiso 1 1 calc R . . C5 C 0.2876(5) 0.4612(3) 0.6988(3) 0.0488(10) Uani 1 1 d . . . C6 C 0.1488(4) 0.3979(3) 0.6894(3) 0.0434(9) Uani 1 1 d . . . H6 H 0.0592 0.4078 0.6357 0.052 Uiso 1 1 calc R . . C7 C -0.0389(4) 0.2246(3) 0.8593(3) 0.0354(8) Uani 1 1 d . . . C8 C 0.0350(4) 0.3049(3) 0.9663(3) 0.0382(8) Uani 1 1 d . . . H8 H 0.1010 0.3742 0.9731 0.046 Uiso 1 1 calc R . . C9 C 0.0118(4) 0.2831(3) 1.0634(3) 0.0397(8) Uani 1 1 d . . . C10 C -0.0827(4) 0.1783(3) 1.0550(3) 0.0426(9) Uani 1 1 d . . . H10 H -0.0978 0.1634 1.1198 0.051 Uiso 1 1 calc R . . C11 C -0.1542(4) 0.0961(3) 0.9505(3) 0.0372(8) Uani 1 1 d . . . C12 C -0.1346(4) 0.1199(3) 0.8533(3) 0.0347(8) Uani 1 1 d . . . H12 H -0.1860 0.0653 0.7827 0.042 Uiso 1 1 calc R . . C13 C -0.1489(4) 0.2062(3) 0.6296(3) 0.0406(9) Uani 1 1 d . . . C14 C -0.3009(4) 0.2098(3) 0.6152(3) 0.0397(8) Uani 1 1 d . . . H14 H -0.3236 0.2380 0.6792 0.048 Uiso 1 1 calc R . . C15 C -0.4173(4) 0.1725(3) 0.5081(3) 0.0406(9) Uani 1 1 d . . . C16 C -0.3871(4) 0.1256(3) 0.4118(3) 0.0451(9) Uani 1 1 d . . . H16 H -0.4660 0.0985 0.3400 0.054 Uiso 1 1 calc R . . C17 C -0.2400(5) 0.1197(3) 0.4236(3) 0.0442(9) Uani 1 1 d . . . C18 C -0.1223(4) 0.1616(3) 0.5303(3) 0.0424(9) Uani 1 1 d . . . H18 H -0.0227 0.1601 0.5361 0.051 Uiso 1 1 calc R . . C19 C 0.5633(5) 0.3413(4) 0.9215(4) 0.0518(10) Uani 1 1 d . . . C20 C 0.2907(7) 0.5483(5) 0.6250(6) 0.0763(15) Uani 1 1 d . . . C21 C -0.2601(4) -0.0151(3) 0.9414(4) 0.0483(10) Uani 1 1 d . . . C22 C 0.0919(6) 0.3733(4) 1.1759(4) 0.0562(11) Uani 1 1 d . . . C23 C -0.5767(5) 0.1831(3) 0.4935(4) 0.0508(10) Uani 1 1 d . . . C24 C -0.2029(7) 0.0692(4) 0.3222(4) 0.0612(12) Uani 1 1 d . . . B1 B -0.0151(5) 0.2504(3) 0.7496(3) 0.0392(10) Uani 1 1 d . . . F1 F 0.553(2) 0.2850(19) 1.0007(15) 0.111(7) Uani 0.50 1 d P . . F2 F 0.6612(17) 0.4425(11) 0.9814(12) 0.102(5) Uani 0.50 1 d P . . F3 F 0.629(2) 0.2801(16) 0.8690(10) 0.093(5) Uani 0.50 1 d P . . F1' F 0.551(2) 0.3215(19) 1.0143(11) 0.096(6) Uani 0.50 1 d P . . F2' F 0.6830(17) 0.4272(12) 0.9530(14) 0.131(7) Uani 0.50 1 d P . . F3' F 0.599(2) 0.2449(17) 0.8723(16) 0.122(7) Uani 0.50 1 d P . . F4 F 0.4174(11) 0.593(2) 0.629(2) 0.149(9) Uani 0.50 1 d P . . F5 F 0.208(2) 0.4900(8) 0.5089(7) 0.110(3) Uani 0.50 1 d P . . F6 F 0.218(3) 0.6264(18) 0.639(3) 0.155(10) Uani 0.50 1 d P . . F4' F 0.376(3) 0.5301(17) 0.571(2) 0.150(9) Uani 0.50 1 d P . . F5' F 0.1709(17) 0.576(3) 0.577(3) 0.168(13) Uani 0.50 1 d P . . F6' F 0.377(4) 0.6587(10) 0.7015(12) 0.170(8) Uani 0.50 1 d P . . F7 F -0.2094(3) -0.0598(2) 1.0331(2) 0.0735(8) Uani 1 1 d . . . F8 F -0.2765(3) -0.1027(2) 0.8529(2) 0.0870(9) Uani 1 1 d . . . F9 F -0.3959(3) 0.0021(2) 0.9308(3) 0.1083(12) Uani 1 1 d . . . F10 F 0.2289(16) 0.3643(13) 1.2286(14) 0.132(7) Uani 0.50 1 d P . . F11 F 0.103(2) 0.4849(10) 1.1681(10) 0.099(5) Uani 0.50 1 d P . . F12 F 0.020(2) 0.3707(15) 1.2488(15) 0.121(7) Uani 0.50 1 d P . . F10' F 0.2378(11) 0.3926(13) 1.2081(12) 0.113(7) Uani 0.50 1 d P . . F11' F 0.055(2) 0.4734(12) 1.1733(14) 0.165(9) Uani 0.50 1 d P . . F12' F 0.070(2) 0.3351(16) 1.2588(10) 0.120(6) Uani 0.50 1 d P . . F13 F -0.6077(3) 0.1754(3) 0.5861(2) 0.0964(10) Uani 1 1 d . . . F14 F -0.6089(4) 0.2824(3) 0.4735(4) 0.1380(16) Uani 1 1 d . . . F15 F -0.6821(3) 0.0955(3) 0.4143(3) 0.1106(12) Uani 1 1 d . . . F16 F -0.251(2) 0.1244(10) 0.2422(10) 0.100(6) Uani 0.50 1 d P . . F17 F -0.302(2) -0.0390(8) 0.2606(11) 0.118(4) Uani 0.50 1 d P . . F18 F -0.0716(14) 0.058(2) 0.3382(9) 0.165(7) Uani 0.50 1 d P . . F16' F -0.3017(18) 0.062(2) 0.2256(11) 0.153(8) Uani 0.50 1 d P . . F17' F -0.160(2) -0.0324(9) 0.3275(11) 0.094(3) Uani 0.50 1 d P . . F18' F -0.0768(18) 0.1375(9) 0.3234(12) 0.108(5) 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 C1 0.050(2) 0.0324(17) 0.040(2) 0.0119(15) 0.0234(19) 0.0107(16) C2 0.052(2) 0.0313(17) 0.044(2) 0.0111(15) 0.0263(19) 0.0105(16) C3 0.042(2) 0.0313(17) 0.050(2) 0.0055(16) 0.0231(19) 0.0078(15) C4 0.045(2) 0.043(2) 0.073(3) 0.015(2) 0.035(2) 0.0058(17) C5 0.056(3) 0.042(2) 0.063(3) 0.0250(19) 0.033(2) 0.0141(18) C6 0.046(2) 0.0410(19) 0.048(2) 0.0152(17) 0.022(2) 0.0117(16) C7 0.034(2) 0.0400(18) 0.036(2) 0.0114(16) 0.0152(17) 0.0085(15) C8 0.038(2) 0.0387(18) 0.042(2) 0.0115(16) 0.0189(18) 0.0070(15) C9 0.039(2) 0.046(2) 0.035(2) 0.0072(16) 0.0161(18) 0.0083(16) C10 0.042(2) 0.050(2) 0.046(2) 0.0210(18) 0.0237(19) 0.0126(17) C11 0.031(2) 0.0394(18) 0.044(2) 0.0145(17) 0.0155(18) 0.0091(15) C12 0.0316(19) 0.0383(18) 0.035(2) 0.0088(15) 0.0134(17) 0.0093(14) C13 0.049(2) 0.0357(18) 0.043(2) 0.0136(16) 0.0230(19) 0.0073(16) C14 0.048(2) 0.0391(18) 0.036(2) 0.0085(15) 0.0225(19) 0.0058(16) C15 0.049(2) 0.0348(18) 0.042(2) 0.0121(16) 0.019(2) 0.0082(16) C16 0.055(3) 0.0388(19) 0.040(2) 0.0119(16) 0.016(2) 0.0084(17) C17 0.060(3) 0.0360(19) 0.042(2) 0.0146(17) 0.024(2) 0.0109(17) C18 0.047(2) 0.0427(19) 0.045(2) 0.0137(17) 0.025(2) 0.0110(17) C19 0.046(3) 0.053(2) 0.058(3) 0.012(2) 0.022(2) 0.010(2) C20 0.076(4) 0.069(3) 0.109(5) 0.055(3) 0.047(4) 0.020(3) C21 0.047(2) 0.048(2) 0.056(3) 0.022(2) 0.023(2) 0.0067(18) C22 0.065(3) 0.060(3) 0.044(3) 0.009(2) 0.025(3) 0.009(2) C23 0.044(2) 0.054(2) 0.052(3) 0.011(2) 0.017(2) 0.0061(19) C24 0.078(4) 0.063(3) 0.048(3) 0.012(2) 0.029(3) 0.019(3) B1 0.046(3) 0.036(2) 0.044(3) 0.0139(18) 0.024(2) 0.0152(18) F1 0.067(7) 0.153(12) 0.152(15) 0.110(12) 0.047(7) 0.033(7) F2 0.061(8) 0.075(6) 0.104(6) -0.039(5) -0.013(5) -0.001(5) F3 0.091(7) 0.154(14) 0.043(5) -0.005(5) 0.028(5) 0.083(9) F1' 0.069(7) 0.186(15) 0.039(5) 0.037(6) 0.013(4) 0.059(7) F2' 0.036(4) 0.129(12) 0.223(16) 0.111(12) 0.015(8) -0.003(6) F3' 0.108(10) 0.096(7) 0.135(11) 0.015(5) 0.002(7) 0.078(7) F4 0.053(4) 0.169(16) 0.24(2) 0.160(15) 0.032(9) -0.013(8) F5 0.140(11) 0.113(6) 0.081(6) 0.061(5) 0.034(6) 0.008(7) F6 0.23(2) 0.091(9) 0.26(3) 0.124(13) 0.16(2) 0.104(14) F4' 0.25(3) 0.135(11) 0.188(15) 0.107(10) 0.18(2) 0.069(12) F5' 0.071(6) 0.23(3) 0.23(2) 0.21(2) 0.030(11) 0.015(11) F6' 0.26(2) 0.055(5) 0.159(10) 0.061(6) 0.036(12) -0.016(8) F7 0.0818(18) 0.0649(15) 0.0715(17) 0.0415(13) 0.0192(15) -0.0016(13) F8 0.118(2) 0.0555(15) 0.0769(19) 0.0047(14) 0.0446(18) -0.0253(15) F9 0.0468(16) 0.0845(19) 0.214(4) 0.072(2) 0.055(2) 0.0126(14) F10 0.128(13) 0.111(8) 0.087(8) -0.026(6) -0.036(8) 0.072(8) F11 0.170(12) 0.046(5) 0.050(5) 0.008(4) 0.021(6) -0.022(6) F12 0.163(12) 0.097(8) 0.118(12) -0.033(7) 0.117(10) -0.023(6) F10' 0.049(7) 0.156(12) 0.082(7) -0.044(7) 0.026(6) -0.058(7) F11' 0.220(17) 0.100(11) 0.122(10) -0.035(8) 0.009(9) 0.105(12) F12' 0.150(13) 0.134(12) 0.024(4) -0.015(5) 0.025(6) -0.080(9) F13 0.0656(19) 0.151(3) 0.086(2) 0.0332(19) 0.0431(17) 0.0242(18) F14 0.086(2) 0.113(2) 0.284(5) 0.130(3) 0.097(3) 0.0629(19) F15 0.0512(17) 0.130(3) 0.106(2) -0.036(2) 0.0167(17) -0.0037(17) F16 0.194(17) 0.085(5) 0.056(8) 0.025(5) 0.082(10) 0.038(6) F17 0.217(14) 0.052(4) 0.095(7) -0.017(4) 0.100(9) -0.007(6) F18 0.080(9) 0.31(2) 0.080(7) -0.043(14) 0.025(6) 0.089(13) F16' 0.096(8) 0.28(2) 0.053(6) -0.030(12) 0.011(6) 0.093(12) F17' 0.165(10) 0.069(5) 0.094(7) 0.026(5) 0.086(8) 0.064(6) F18' 0.143(12) 0.102(6) 0.092(7) -0.013(5) 0.096(9) -0.027(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 C1 C2 1.401(5) . ? C1 C6 1.402(5) . ? C1 B1 1.552(5) . ? C2 C3 1.389(5) . ? C3 C4 1.383(5) . ? C3 C19 1.498(6) . ? C4 C5 1.390(5) . ? C5 C6 1.387(5) . ? C5 C20 1.510(6) . ? C7 C8 1.393(5) . ? C7 C12 1.402(4) . ? C7 B1 1.569(5) . ? C8 C9 1.393(5) . ? C9 C10 1.387(5) . ? C9 C22 1.497(6) . ? C10 C11 1.380(5) . ? C11 C12 1.389(4) . ? C11 C21 1.499(5) . ? C13 C18 1.400(5) . ? C13 C14 1.404(5) . ? C13 B1 1.563(5) . ? C14 C15 1.381(5) . ? C15 C16 1.390(5) . ? C15 C23 1.492(5) . ? C16 C17 1.372(5) . ? C17 C18 1.386(5) . ? C17 C24 1.496(6) . ? C19 F3 1.258(10) . ? C19 F1' 1.289(14) . ? C19 F2' 1.310(14) . ? C19 F2 1.322(12) . ? C19 F1 1.325(16) . ? C19 F3' 1.329(15) . ? C20 F5' 1.212(15) . ? C20 F4 1.233(11) . ? C20 F6 1.239(14) . ? C20 F4' 1.247(13) . ? C20 F5 1.406(10) . ? C20 F6' 1.416(12) . ? C21 F9 1.301(4) . ? C21 F8 1.326(4) . ? C21 F7 1.332(4) . ? C22 F11' 1.264(13) . ? C22 F10 1.276(13) . ? C22 F10' 1.285(11) . ? C22 F12' 1.291(15) . ? C22 F11 1.317(11) . ? C22 F12 1.334(16) . ? C23 F14 1.283(4) . ? C23 F15 1.318(4) . ? C23 F13 1.329(4) . ? C24 F18 1.227(10) . ? C24 F16' 1.248(12) . ? C24 F16 1.290(13) . ? C24 F17' 1.307(8) . ? C24 F18' 1.350(11) . ? C24 F17 1.389(10) . ? F3 F2' 1.76(2) . ? F4 F4' 0.88(2) . ? F4 F6' 1.280(18) . ? F5 F5' 1.36(3) . ? F5 F4' 1.49(2) . ? F6 F5' 0.83(3) . ? F6 F6' 1.42(2) . ? F10 F12' 1.70(2) . ? F12 F12' 0.66(3) . ? F12 F11' 1.74(3) . ? F16 F16' 0.77(2) . ? F16 F18' 1.600(18) . ? F17 F17' 1.317(13) . ? F17 F16' 1.329(19) . ? F18 F18' 0.99(2) . ? F18 F17' 1.215(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.4(3) . . ? C2 C1 B1 121.5(3) . . ? C6 C1 B1 121.1(3) . . ? C3 C2 C1 121.2(3) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 C19 119.8(3) . . ? C2 C3 C19 119.8(3) . . ? C3 C4 C5 119.5(3) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 C20 119.6(4) . . ? C4 C5 C20 120.3(4) . . ? C5 C6 C1 121.4(4) . . ? C8 C7 C12 117.6(3) . . ? C8 C7 B1 121.2(3) . . ? C12 C7 B1 121.2(3) . . ? C9 C8 C7 121.2(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 C22 121.1(3) . . ? C8 C9 C22 119.0(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 119.9(3) . . ? C10 C11 C21 119.7(3) . . ? C12 C11 C21 120.4(3) . . ? C11 C12 C7 121.4(3) . . ? C18 C13 C14 116.6(3) . . ? C18 C13 B1 121.1(3) . . ? C14 C13 B1 122.3(3) . . ? C15 C14 C13 121.5(3) . . ? C14 C15 C16 120.3(3) . . ? C14 C15 C23 120.7(3) . . ? C16 C15 C23 118.9(4) . . ? C17 C16 C15 119.4(4) . . ? C16 C17 C18 120.2(3) . . ? C16 C17 C24 121.1(4) . . ? C18 C17 C24 118.7(4) . . ? C17 C18 C13 121.9(3) . . ? F3 C19 F1' 121.8(12) . . ? F3 C19 F2' 86.2(12) . . ? F1' C19 F2' 107.0(11) . . ? F3 C19 F2 106.9(12) . . ? F1' C19 F2 90.2(12) . . ? F2' C19 F2 21.7(12) . . ? F3 C19 F1 104.5(12) . . ? F1' C19 F1 19.1(18) . . ? F2' C19 F1 116.5(11) . . ? F2 C19 F1 104.0(12) . . ? F3 C19 F3' 21.4(17) . . ? F1' C19 F3' 106.4(12) . . ? F2' C19 F3' 105.6(13) . . ? F2 C19 F3' 124.6(12) . . ? F1 C19 F3' 87.6(13) . . ? F3 C19 C3 113.2(7) . . ? F1' C19 C3 111.2(9) . . ? F2' C19 C3 114.9(7) . . ? F2 C19 C3 110.7(8) . . ? F1 C19 C3 116.8(8) . . ? F3' C19 C3 111.2(9) . . ? F5' C20 F4 126.4(9) . . ? F5' C20 F6 39.7(14) . . ? F4 C20 F6 110.6(11) . . ? F5' C20 F4' 118.6(13) . . ? F4 C20 F4' 41.5(10) . . ? F6 C20 F4' 134.9(10) . . ? F5' C20 F5 62.3(13) . . ? F4 C20 F5 105.3(11) . . ? F6 C20 F5 101.2(14) . . ? F4' C20 F5 68.2(10) . . ? F5' C20 F6' 101.1(12) . . ? F4 C20 F6' 57.3(9) . . ? F6 C20 F6' 64.1(10) . . ? F4' C20 F6' 98.5(10) . . ? F5 C20 F6' 144.4(6) . . ? F5' C20 C5 116.7(8) . . ? F4 C20 C5 116.4(7) . . ? F6 C20 C5 112.6(9) . . ? F4' C20 C5 112.3(8) . . ? F5 C20 C5 109.4(5) . . ? F6' C20 C5 106.2(7) . . ? F9 C21 F8 107.1(4) . . ? F9 C21 F7 106.7(3) . . ? F8 C21 F7 104.9(3) . . ? F9 C21 C11 112.6(3) . . ? F8 C21 C11 112.7(3) . . ? F7 C21 C11 112.3(3) . . ? F11' C22 F10 121.9(12) . . ? F11' C22 F10' 106.5(12) . . ? F10 C22 F10' 21.3(11) . . ? F11' C22 F12' 110.5(11) . . ? F10 C22 F12' 82.9(11) . . ? F10' C22 F12' 102.5(10) . . ? F11' C22 F11 21.7(14) . . ? F10 C22 F11 104.7(10) . . ? F10' C22 F11 86.6(10) . . ? F12' C22 F11 124.8(9) . . ? F11' C22 F12 83.8(12) . . ? F10 C22 F12 107.3(12) . . ? F10' C22 F12 123.1(11) . . ? F12' C22 F12 29.2(14) . . ? F11 C22 F12 102.1(10) . . ? F11' C22 C9 112.6(9) . . ? F10 C22 C9 113.6(7) . . ? F10' C22 C9 112.9(7) . . ? F12' C22 C9 111.3(7) . . ? F11 C22 C9 114.4(6) . . ? F12 C22 C9 113.6(9) . . ? F14 C23 F15 108.4(4) . . ? F14 C23 F13 104.7(4) . . ? F15 C23 F13 101.4(3) . . ? F14 C23 C15 114.0(3) . . ? F15 C23 C15 114.1(3) . . ? F13 C23 C15 113.1(3) . . ? F18 C24 F16' 123.8(8) . . ? F18 C24 F16 110.7(12) . . ? F16' C24 F16 35.3(10) . . ? F18 C24 F17' 57.2(9) . . ? F16' C24 F17' 110.6(9) . . ? F16 C24 F17' 135.3(7) . . ? F18 C24 F18' 44.7(11) . . ? F16' C24 F18' 104.3(11) . . ? F16 C24 F18' 74.6(8) . . ? F17' C24 F18' 101.3(8) . . ? F18 C24 F17 109.3(9) . . ? F16' C24 F17 60.3(10) . . ? F16 C24 F17 95.3(8) . . ? F17' C24 F17 58.4(6) . . ? F18' C24 F17 139.3(6) . . ? F18 C24 C17 118.7(6) . . ? F16' C24 C17 116.2(6) . . ? F16 C24 C17 110.6(6) . . ? F17' C24 C17 112.3(5) . . ? F18' C24 C17 110.8(6) . . ? F17 C24 C17 109.7(5) . . ? C1 B1 C13 119.6(3) . . ? C1 B1 C7 120.5(3) . . ? C13 B1 C7 119.9(3) . . ? C19 F3 F2' 48.1(8) . . ? C19 F2' F3 45.7(7) . . ? F4' F4 C20 70.1(11) . . ? F4' F4 F6' 138.1(18) . . ? C20 F4 F6' 68.6(9) . . ? F5' F5 C20 51.9(7) . . ? F5' F5 F4' 95.4(10) . . ? C20 F5 F4' 50.9(6) . . ? F5' F6 C20 68.4(16) . . ? F5' F6 F6' 128(2) . . ? C20 F6 F6' 64.1(9) . . ? F4 F4' C20 68.4(13) . . ? F4 F4' F5 123(2) . . ? C20 F4' F5 61.0(9) . . ? F6 F5' C20 71.9(18) . . ? F6 F5' F5 136(3) . . ? C20 F5' F5 65.8(12) . . ? F4 F6' C20 54.2(6) . . ? F4 F6' F6 97.7(11) . . ? C20 F6' F6 51.9(7) . . ? C22 F10 F12' 48.9(7) . . ? F12' F12 C22 72(2) . . ? F12' F12 F11' 114(3) . . ? C22 F12 F11' 46.4(8) . . ? C22 F11' F12 49.8(7) . . ? F12 F12' C22 79(3) . . ? F12 F12' F10 119(3) . . ? C22 F12' F10 48.2(7) . . ? F16' F16 C24 69.4(15) . . ? F16' F16 F18' 115(2) . . ? C24 F16 F18' 54.4(7) . . ? F17' F17 F16' 105.1(10) . . ? F17' F17 C24 57.7(6) . . ? F16' F17 C24 54.6(6) . . ? F18' F18 F17' 137.7(16) . . ? F18' F18 C24 74.2(11) . . ? F17' F18 C24 64.7(8) . . ? F16 F16' C24 75.3(17) . . ? F16 F16' F17 140(2) . . ? C24 F16' F17 65.1(9) . . ? F18 F17' C24 58.1(6) . . ? F18 F17' F17 115.0(11) . . ? C24 F17' F17 63.9(6) . . ? F18 F18' C24 61.1(10) . . ? F18 F18' F16 103.9(14) . . ? C24 F18' F16 51.0(6) . . ? _diffrn_reflns_theta_full 26.40 _refine_diff_density_max 0.446 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.055 data_ccd22 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis(triphenylphosphine)bis[3,5-bis(trifluoromethyl)phenyl]platinum ; _publ_contact_author ; Gregory J. Kubas CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'kubas@lanl.gov' loop_ _publ_author_name 'Wayde V. Konze' 'Brian L. Scott' 'Gregory J. Kubas' _publ_requested_journal 'Chemical Communications' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H48 F12 P2 Pt' _chemical_formula_weight 1302.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3973(6) _cell_length_b 11.4539(5) _cell_length_c 12.8260(6) _cell_angle_alpha 105.6750(10) _cell_angle_beta 111.4660(10) _cell_angle_gamma 103.3930(10) _cell_volume 1394.47(12) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'multifaceted block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_crystal_preparation 'crystallized from benzene' _exptl_absorpt_coefficient_mu 2.654 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5227 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5227 _reflns_number_gt 5227 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5227 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.0000 0.0000 0.01864(4) Uani 1 2 d S . . P1 P 0.20491(5) -0.00020(6) 0.00391(5) 0.02151(11) Uani 1 1 d . . . C1 C 0.2683(2) 0.1169(2) -0.0530(2) 0.0258(4) Uani 1 1 d . . . C2 C 0.1741(2) 0.1293(3) -0.1516(2) 0.0321(5) Uani 1 1 d . . . H2 H 0.0821 0.0816 -0.1833 0.039 Uiso 1 1 calc R . . C3 C 0.2170(3) 0.2124(3) -0.2025(2) 0.0418(6) Uani 1 1 d . . . H3 H 0.1539 0.2196 -0.2688 0.050 Uiso 1 1 calc R . . C4 C 0.3532(3) 0.2844(3) -0.1547(3) 0.0497(7) Uani 1 1 d . . . H4 H 0.3817 0.3405 -0.1885 0.060 Uiso 1 1 calc R . . C5 C 0.4470(3) 0.2734(3) -0.0571(3) 0.0480(7) Uani 1 1 d . . . H5 H 0.5386 0.3227 -0.0249 0.058 Uiso 1 1 calc R . . C6 C 0.4052(2) 0.1887(3) -0.0063(2) 0.0367(6) Uani 1 1 d . . . H6 H 0.4690 0.1803 0.0588 0.044 Uiso 1 1 calc R . . C7 C 0.2033(2) -0.1526(2) -0.09078(19) 0.0256(4) Uani 1 1 d . . . C8 C 0.1540(2) -0.2668(3) -0.0753(2) 0.0304(5) Uani 1 1 d . . . H8 H 0.1228 -0.2640 -0.0174 0.036 Uiso 1 1 calc R . . C9 C 0.1511(3) -0.3843(3) -0.1452(2) 0.0374(6) Uani 1 1 d . . . H9 H 0.1196 -0.4595 -0.1332 0.045 Uiso 1 1 calc R . . C10 C 0.1954(3) -0.3892(3) -0.2328(2) 0.0448(7) Uani 1 1 d . . . H10 H 0.1925 -0.4681 -0.2806 0.054 Uiso 1 1 calc R . . C11 C 0.2438(3) -0.2767(3) -0.2494(2) 0.0441(7) Uani 1 1 d . . . H11 H 0.2737 -0.2801 -0.3082 0.053 Uiso 1 1 calc R . . C12 C 0.2480(2) -0.1591(3) -0.1790(2) 0.0338(5) Uani 1 1 d . . . H12 H 0.2809 -0.0839 -0.1907 0.041 Uiso 1 1 calc R . . C13 C 0.3430(2) 0.0421(2) 0.15473(19) 0.0261(5) Uani 1 1 d . . . C14 C 0.3944(2) 0.1670(3) 0.2438(2) 0.0338(5) Uani 1 1 d . . . H14 H 0.3638 0.2306 0.2243 0.041 Uiso 1 1 calc R . . C15 C 0.4907(3) 0.1979(3) 0.3614(2) 0.0426(6) Uani 1 1 d . . . H15 H 0.5237 0.2817 0.4201 0.051 Uiso 1 1 calc R . . C16 C 0.5380(3) 0.1052(3) 0.3919(2) 0.0479(7) Uani 1 1 d . . . H16 H 0.6011 0.1256 0.4712 0.058 Uiso 1 1 calc R . . C17 C 0.4907(3) -0.0172(3) 0.3038(3) 0.0535(8) Uani 1 1 d . . . H17 H 0.5241 -0.0793 0.3233 0.064 Uiso 1 1 calc R . . C18 C 0.3939(3) -0.0496(3) 0.1861(2) 0.0388(6) Uani 1 1 d . . . H18 H 0.3626 -0.1333 0.1277 0.047 Uiso 1 1 calc R . . C19 C -0.1023(2) -0.1907(2) -0.12996(19) 0.0227(4) Uani 1 1 d . . . C20 C -0.1515(2) -0.2964(2) -0.1020(2) 0.0274(5) Uani 1 1 d . . . H20 H -0.1332 -0.2817 -0.0217 0.033 Uiso 1 1 calc R . . C21 C -0.2266(3) -0.4221(3) -0.1906(2) 0.0339(5) Uani 1 1 d . . . C22 C -0.2552(3) -0.4490(3) -0.3105(2) 0.0378(6) Uani 1 1 d . . . H22 H -0.3069 -0.5329 -0.3699 0.045 Uiso 1 1 calc R . . C23 C -0.2043(3) -0.3469(3) -0.3400(2) 0.0340(5) Uani 1 1 d . . . C24 C -0.1295(2) -0.2215(2) -0.2517(2) 0.0286(5) Uani 1 1 d . . . H24 H -0.0960 -0.1555 -0.2742 0.034 Uiso 1 1 calc R . . C25 C -0.2743(4) -0.5294(3) -0.1533(3) 0.0526(8) Uani 1 1 d . . . C26 C -0.2358(4) -0.3758(3) -0.4699(3) 0.0586(9) Uani 1 1 d . . . C27 C 0.0905(3) -0.2490(4) -0.5577(4) 0.0641(10) Uani 1 1 d . . . H27 H 0.0599 -0.3159 -0.5350 0.077 Uiso 1 1 calc R . . C28 C 0.1131(4) -0.1241(4) -0.4906(3) 0.0641(10) Uani 1 1 d . . . H28 H 0.0958 -0.1061 -0.4237 0.077 Uiso 1 1 calc R . . C29 C 0.1617(4) -0.0247(4) -0.5226(4) 0.0640(9) Uani 1 1 d . . . H29 H 0.1789 0.0610 -0.4765 0.077 Uiso 1 1 calc R . . C30 C 0.1844(3) -0.0528(4) -0.6229(4) 0.0631(10) Uani 1 1 d . . . H30 H 0.2173 0.0142 -0.6446 0.076 Uiso 1 1 calc R . . C31 C 0.1593(3) -0.1780(4) -0.6906(3) 0.0612(9) Uani 1 1 d . . . H31 H 0.1739 -0.1966 -0.7590 0.073 Uiso 1 1 calc R . . C32 C 0.1123(3) -0.2771(4) -0.6578(3) 0.0630(9) Uani 1 1 d . . . H32 H 0.0955 -0.3628 -0.7037 0.076 Uiso 1 1 calc R . . F1 F -0.1722(3) -0.5663(2) -0.0979(2) 0.0835(7) Uani 1 1 d . . . F2 F -0.3184(3) -0.4953(2) -0.0725(2) 0.0891(8) Uani 1 1 d . . . F3 F -0.3684(3) -0.6378(2) -0.2464(2) 0.0893(8) Uani 1 1 d . . . F4 F -0.192(2) -0.2794(9) -0.4931(9) 0.098(4) Uani 0.59(4) 1 d P . . F4' F -0.154(2) -0.297(3) -0.4880(17) 0.114(7) Uani 0.41(4) 1 d P . . F5 F -0.3583(14) -0.4468(14) -0.5456(5) 0.104(6) Uani 0.56(3) 1 d P . . F5' F -0.352(2) -0.349(5) -0.5288(13) 0.155(13) Uani 0.44(3) 1 d P . . F6 F -0.168(3) -0.455(3) -0.5023(14) 0.128(7) Uani 0.63(4) 1 d P . . F6' F -0.274(5) -0.4896(10) -0.5363(16) 0.123(15) Uani 0.37(4) 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 Pt1 0.01704(6) 0.01800(8) 0.01884(6) 0.00636(5) 0.00824(4) 0.00406(4) P1 0.0185(2) 0.0237(3) 0.0212(2) 0.0086(2) 0.0090(2) 0.0063(2) C1 0.0250(10) 0.0278(13) 0.0281(10) 0.0124(10) 0.0148(9) 0.0093(9) C2 0.0261(11) 0.0374(15) 0.0311(11) 0.0149(11) 0.0120(9) 0.0088(10) C3 0.0443(14) 0.0512(19) 0.0406(14) 0.0295(14) 0.0206(12) 0.0197(13) C4 0.0525(17) 0.058(2) 0.0609(18) 0.0415(17) 0.0364(15) 0.0191(15) C5 0.0313(13) 0.054(2) 0.0634(18) 0.0324(16) 0.0258(13) 0.0063(12) C6 0.0250(11) 0.0460(17) 0.0418(13) 0.0234(13) 0.0155(10) 0.0098(11) C7 0.0211(10) 0.0296(14) 0.0226(10) 0.0067(9) 0.0079(8) 0.0109(9) C8 0.0274(11) 0.0339(15) 0.0284(11) 0.0109(10) 0.0117(9) 0.0121(10) C9 0.0393(13) 0.0284(15) 0.0363(13) 0.0081(11) 0.0122(11) 0.0124(11) C10 0.0521(16) 0.0376(18) 0.0352(13) 0.0017(12) 0.0163(12) 0.0216(14) C11 0.0458(15) 0.055(2) 0.0333(13) 0.0093(13) 0.0232(12) 0.0223(14) C12 0.0316(12) 0.0410(16) 0.0298(11) 0.0125(11) 0.0161(10) 0.0134(11) C13 0.0199(10) 0.0321(14) 0.0250(10) 0.0117(10) 0.0099(8) 0.0074(9) C14 0.0247(11) 0.0375(16) 0.0306(12) 0.0089(11) 0.0083(9) 0.0095(10) C15 0.0303(12) 0.0483(19) 0.0292(12) 0.0048(12) 0.0054(10) 0.0074(12) C16 0.0336(13) 0.061(2) 0.0298(13) 0.0172(14) 0.0009(11) 0.0089(13) C17 0.0469(16) 0.053(2) 0.0476(16) 0.0260(16) 0.0025(13) 0.0196(15) C18 0.0345(13) 0.0359(17) 0.0347(13) 0.0131(12) 0.0051(10) 0.0124(11) C19 0.0185(9) 0.0214(12) 0.0238(10) 0.0060(9) 0.0089(8) 0.0047(8) C20 0.0281(11) 0.0248(14) 0.0297(11) 0.0094(10) 0.0156(9) 0.0081(9) C21 0.0369(13) 0.0237(15) 0.0417(13) 0.0124(11) 0.0218(11) 0.0063(10) C22 0.0414(14) 0.0212(15) 0.0381(13) 0.0017(11) 0.0189(11) 0.0009(10) C23 0.0385(13) 0.0261(15) 0.0297(12) 0.0047(10) 0.0170(10) 0.0042(10) C24 0.0295(11) 0.0242(14) 0.0287(11) 0.0088(10) 0.0143(9) 0.0045(9) C25 0.072(2) 0.0311(19) 0.0603(18) 0.0175(15) 0.0425(17) 0.0095(15) C26 0.081(2) 0.040(2) 0.0349(15) 0.0009(14) 0.0298(16) -0.0013(17) C27 0.0412(16) 0.067(3) 0.083(3) 0.043(2) 0.0198(17) 0.0158(16) C28 0.0520(19) 0.091(3) 0.0532(19) 0.029(2) 0.0241(16) 0.032(2) C29 0.0556(19) 0.053(2) 0.075(2) 0.0178(19) 0.0216(18) 0.0270(17) C30 0.0490(18) 0.072(3) 0.083(2) 0.051(2) 0.0257(18) 0.0304(18) C31 0.0478(17) 0.084(3) 0.0498(18) 0.0248(19) 0.0183(15) 0.0288(18) C32 0.0400(16) 0.051(2) 0.067(2) 0.0037(17) 0.0096(15) 0.0118(15) F1 0.121(2) 0.0732(16) 0.0962(17) 0.0630(15) 0.0608(16) 0.0492(15) F2 0.141(2) 0.0477(14) 0.125(2) 0.0387(14) 0.1122(19) 0.0236(13) F3 0.1124(19) 0.0354(13) 0.0826(15) 0.0161(11) 0.0394(14) -0.0186(12) F4 0.187(11) 0.039(5) 0.037(3) 0.015(3) 0.044(5) 0.002(5) F4' 0.097(8) 0.146(17) 0.054(5) 0.021(7) 0.049(5) -0.033(7) F5 0.091(6) 0.107(10) 0.030(2) 0.013(4) -0.009(3) -0.029(5) F5' 0.128(11) 0.33(4) 0.052(5) 0.085(12) 0.043(6) 0.136(18) F6 0.246(16) 0.136(11) 0.084(5) 0.053(6) 0.120(9) 0.124(12) F6' 0.26(4) 0.029(6) 0.062(8) -0.004(4) 0.101(15) 0.011(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C19 2.083(2) . ? Pt1 C19 2.083(2) 2 ? Pt1 P1 2.3180(5) . ? Pt1 P1 2.3180(5) 2 ? P1 C1 1.822(2) . ? P1 C7 1.829(2) . ? P1 C13 1.834(2) . ? C1 C6 1.388(3) . ? C1 C2 1.395(3) . ? C2 C3 1.387(3) . ? C3 C4 1.380(4) . ? C4 C5 1.375(4) . ? C5 C6 1.397(4) . ? C7 C12 1.394(3) . ? C7 C8 1.395(3) . ? C8 C9 1.387(4) . ? C9 C10 1.383(4) . ? C10 C11 1.384(4) . ? C11 C12 1.383(4) . ? C13 C14 1.391(4) . ? C13 C18 1.394(3) . ? C14 C15 1.388(3) . ? C15 C16 1.380(4) . ? C16 C17 1.372(5) . ? C17 C18 1.386(4) . ? C19 C24 1.398(3) . ? C19 C20 1.406(3) . ? C20 C21 1.390(4) . ? C21 C22 1.377(4) . ? C21 C25 1.493(4) . ? C22 C23 1.391(4) . ? C23 C24 1.385(4) . ? C23 C26 1.491(4) . ? C25 F2 1.317(4) . ? C25 F3 1.328(4) . ? C25 F1 1.350(4) . ? C26 F6' 1.216(12) . ? C26 F4 1.259(9) . ? C26 F5 1.268(10) . ? C26 F4' 1.272(14) . ? C26 F6 1.393(8) . ? C26 F5' 1.412(12) . ? C27 C28 1.362(6) . ? C27 C32 1.364(5) . ? C28 C29 1.378(6) . ? C29 C30 1.372(5) . ? C30 C31 1.358(6) . ? C31 C32 1.376(5) . ? F4 F4' 0.51(3) . ? F4 F5' 1.63(3) . ? F4' F6 1.73(4) . ? F5 F5' 1.06(3) . ? F5 F6' 1.16(6) . ? F6 F6' 1.05(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Pt1 C19 180.00(19) . 2 ? C19 Pt1 P1 91.73(6) . . ? C19 Pt1 P1 88.27(6) 2 . ? C19 Pt1 P1 88.27(6) . 2 ? C19 Pt1 P1 91.73(6) 2 2 ? P1 Pt1 P1 180.00(3) . 2 ? C1 P1 C7 103.15(10) . . ? C1 P1 C13 105.47(10) . . ? C7 P1 C13 103.84(10) . . ? C1 P1 Pt1 111.01(7) . . ? C7 P1 Pt1 116.69(7) . . ? C13 P1 Pt1 115.38(7) . . ? C6 C1 C2 119.3(2) . . ? C6 C1 P1 122.92(17) . . ? C2 C1 P1 117.71(17) . . ? C3 C2 C1 120.3(2) . . ? C4 C3 C2 120.0(2) . . ? C5 C4 C3 120.2(2) . . ? C4 C5 C6 120.3(2) . . ? C1 C6 C5 119.9(2) . . ? C12 C7 C8 118.7(2) . . ? C12 C7 P1 122.31(19) . . ? C8 C7 P1 118.97(17) . . ? C9 C8 C7 120.8(2) . . ? C10 C9 C8 119.8(3) . . ? C9 C10 C11 119.9(3) . . ? C12 C11 C10 120.4(2) . . ? C11 C12 C7 120.4(3) . . ? C14 C13 C18 118.1(2) . . ? C14 C13 P1 119.78(17) . . ? C18 C13 P1 121.99(19) . . ? C15 C14 C13 120.7(2) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 119.1(2) . . ? C16 C17 C18 120.9(3) . . ? C17 C18 C13 120.5(3) . . ? C24 C19 C20 115.5(2) . . ? C24 C19 Pt1 122.11(17) . . ? C20 C19 Pt1 122.33(16) . . ? C21 C20 C19 122.0(2) . . ? C22 C21 C20 121.2(2) . . ? C22 C21 C25 120.1(3) . . ? C20 C21 C25 118.8(2) . . ? C21 C22 C23 118.0(2) . . ? C24 C23 C22 120.8(2) . . ? C24 C23 C26 121.1(2) . . ? C22 C23 C26 118.0(2) . . ? C23 C24 C19 122.4(2) . . ? F2 C25 F3 109.0(3) . . ? F2 C25 F1 104.2(3) . . ? F3 C25 F1 104.6(3) . . ? F2 C25 C21 113.5(3) . . ? F3 C25 C21 113.5(3) . . ? F1 C25 C21 111.4(3) . . ? F6' C26 F4 125.3(8) . . ? F6' C26 F5 56(3) . . ? F4 C26 F5 112.1(10) . . ? F6' C26 F4' 114.2(18) . . ? F4 C26 F4' 23.3(13) . . ? F5 C26 F4' 125.8(11) . . ? F6' C26 F6 46.7(14) . . ? F4 C26 F6 102.6(14) . . ? F5 C26 F6 101.4(16) . . ? F4' C26 F6 81.0(19) . . ? F6' C26 F5' 99(3) . . ? F4 C26 F5' 75(2) . . ? F5 C26 F5' 46.2(11) . . ? F4' C26 F5' 97(2) . . ? F6 C26 F5' 137.6(12) . . ? F6' C26 C23 117.1(7) . . ? F4 C26 C23 115.7(5) . . ? F5 C26 C23 114.4(5) . . ? F4' C26 C23 115.7(9) . . ? F6 C26 C23 108.8(5) . . ? F5' C26 C23 110.0(5) . . ? C28 C27 C32 120.8(4) . . ? C27 C28 C29 119.5(4) . . ? C30 C29 C28 119.7(4) . . ? C31 C30 C29 120.4(3) . . ? C30 C31 C32 119.9(3) . . ? C27 C32 C31 119.7(4) . . ? F4' F4 C26 80(3) . . ? F4' F4 F5' 132(4) . . ? C26 F4 F5' 56.7(14) . . ? F4 F4' C26 77(2) . . ? F4 F4' F6 125(3) . . ? C26 F4' F6 52.5(12) . . ? F5' F5 F6' 129(2) . . ? F5' F5 C26 74.1(10) . . ? F6' F5 C26 59.9(12) . . ? F5 F5' C26 59.7(7) . . ? F5 F5' F4 100.0(11) . . ? C26 F5' F4 48.1(7) . . ? F6' F6 C26 57.7(9) . . ? F6' F6 F4' 94.1(17) . . ? C26 F6 F4' 46.4(8) . . ? F6 F6' F5 138.1(18) . . ? F6 F6' C26 75.6(11) . . ? F5 F6' C26 64.5(18) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.606 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.073