# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Andrew Caffyn' _publ_contact_author_email A.CAFFYN@MMU.AC.UK _publ_section_title ; Synthesis and complexation of heptafluoroisopropyldiphenylphosphine ; loop_ _publ_author_name 'Andrew Caffyn' 'Xavier F. Le Goff' 'Lesley C. Lewis-Alleyne' 'Makeba B. Murphy-Jolly' # Attachment 'Dalton_trans_caffyn.cif' data_ll531 _database_code_depnum_ccdc_archive 'CCDC 746473' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H10 F7 P' _chemical_formula_sum 'C15 H10 F7 P' _chemical_formula_weight 354.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/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 8.918(1) _cell_length_b 26.234(1) _cell_length_c 6.377(1) _cell_angle_alpha 90.00 _cell_angle_beta 99.421(1) _cell_angle_gamma 90.00 _cell_volume 1471.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 22637 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9502 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 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 10324 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3775 _reflns_number_gt 3088 _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^)+(0.0902P)^2^+1.5716P] 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 3775 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _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 P1 P 0.81268(7) -0.11021(3) 0.10285(10) 0.03323(19) Uani 1 1 d . . . F1 F 0.58974(17) -0.16070(7) 0.2859(2) 0.0416(4) Uani 1 1 d . . . F2 F 0.6094(2) -0.18128(8) -0.2499(3) 0.0596(5) Uani 1 1 d . . . F3 F 0.7489(2) -0.21983(7) 0.0100(4) 0.0670(6) Uani 1 1 d . . . F4 F 0.5069(2) -0.22358(7) -0.0251(3) 0.0509(4) Uani 1 1 d . . . F5 F 0.5226(2) -0.08293(9) -0.1634(4) 0.0722(7) Uani 1 1 d . . . F6 F 0.4557(2) -0.07774(9) 0.1420(4) 0.0695(6) Uani 1 1 d . . . F7 F 0.36323(17) -0.13572(7) -0.0683(3) 0.0482(4) Uani 1 1 d . . . C1 C 0.9443(3) -0.14939(10) 0.2863(4) 0.0325(5) Uani 1 1 d . . . C2 C 0.9225(3) -0.16848(12) 0.4839(4) 0.0434(6) Uani 1 1 d . . . H2 H 0.8284 -0.1631 0.5319 0.052 Uiso 1 1 calc R . . C3 C 1.0377(3) -0.19532(12) 0.6105(5) 0.0451(6) Uani 1 1 d . . . H3 H 1.0211 -0.2092 0.7422 0.054 Uiso 1 1 calc R . . C4 C 1.1766(3) -0.20173(11) 0.5443(5) 0.0436(6) Uani 1 1 d . . . H4 H 1.2561 -0.2194 0.6325 0.052 Uiso 1 1 calc R . . C5 C 1.2005(3) -0.18269(11) 0.3515(5) 0.0435(6) Uani 1 1 d . . . H5 H 1.2964 -0.1869 0.3074 0.052 Uiso 1 1 calc R . . C6 C 1.0843(3) -0.15731(10) 0.2217(4) 0.0371(5) Uani 1 1 d . . . H6 H 1.1004 -0.1452 0.0868 0.045 Uiso 1 1 calc R . . C7 C 0.7884(3) -0.05374(10) 0.2634(4) 0.0360(5) Uani 1 1 d . . . C8 C 0.8435(3) -0.00897(11) 0.1877(6) 0.0481(7) Uani 1 1 d . . . H8 H 0.8821 -0.0091 0.0574 0.058 Uiso 1 1 calc R . . C9 C 0.8422(4) 0.03647(12) 0.3034(8) 0.0658(11) Uani 1 1 d . . . H9 H 0.8829 0.0668 0.2541 0.079 Uiso 1 1 calc R . . C10 C 0.7815(4) 0.03690(12) 0.4890(7) 0.0619(10) Uani 1 1 d . . . H10 H 0.7784 0.0678 0.5661 0.074 Uiso 1 1 calc R . . C11 C 0.7259(4) -0.00715(13) 0.5620(6) 0.0580(9) Uani 1 1 d . . . H11 H 0.6830 -0.0066 0.6888 0.070 Uiso 1 1 calc R . . C12 C 0.7315(4) -0.05246(11) 0.4532(5) 0.0465(7) Uani 1 1 d . . . H12 H 0.6960 -0.0830 0.5087 0.056 Uiso 1 1 calc R . . C13 C 0.6239(3) -0.14429(9) 0.0916(4) 0.0300(5) Uani 1 1 d . . . C14 C 0.6229(3) -0.19323(11) -0.0423(5) 0.0390(6) Uani 1 1 d . . . C15 C 0.4906(3) -0.10979(11) -0.0050(5) 0.0393(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0263(3) 0.0459(4) 0.0283(3) 0.0050(2) 0.0068(2) -0.0045(2) F1 0.0346(8) 0.0640(10) 0.0274(7) 0.0039(7) 0.0087(6) -0.0132(7) F2 0.0670(12) 0.0784(13) 0.0350(9) -0.0153(9) 0.0136(8) -0.0087(10) F3 0.0451(10) 0.0515(11) 0.0968(17) -0.0231(11) -0.0112(10) 0.0128(8) F4 0.0459(9) 0.0469(9) 0.0571(11) -0.0025(8) -0.0001(8) -0.0118(7) F5 0.0435(10) 0.0917(16) 0.0804(15) 0.0508(13) 0.0066(10) 0.0093(10) F6 0.0471(11) 0.0738(14) 0.0830(15) -0.0318(11) -0.0027(10) 0.0187(10) F7 0.0258(7) 0.0593(10) 0.0565(10) 0.0007(8) -0.0020(7) -0.0027(7) C1 0.0270(11) 0.0382(12) 0.0314(12) -0.0030(9) 0.0021(9) -0.0023(9) C2 0.0311(12) 0.0636(17) 0.0362(14) 0.0032(12) 0.0077(10) 0.0035(12) C3 0.0421(14) 0.0581(17) 0.0329(13) 0.0033(12) -0.0005(11) 0.0017(12) C4 0.0330(12) 0.0402(13) 0.0520(16) -0.0045(12) -0.0093(11) 0.0005(10) C5 0.0288(12) 0.0415(14) 0.0609(18) -0.0066(12) 0.0096(12) -0.0023(10) C6 0.0330(12) 0.0391(12) 0.0411(13) -0.0041(10) 0.0115(10) -0.0064(10) C7 0.0274(11) 0.0356(12) 0.0415(14) 0.0058(10) -0.0044(10) -0.0048(9) C8 0.0308(13) 0.0469(15) 0.0645(19) 0.0191(14) 0.0012(12) -0.0022(11) C9 0.0429(17) 0.0350(15) 0.111(3) 0.0221(18) -0.0126(19) -0.0060(12) C10 0.0515(18) 0.0389(15) 0.084(3) -0.0125(16) -0.0228(18) 0.0050(13) C11 0.066(2) 0.0492(17) 0.0527(19) -0.0125(14) -0.0071(16) 0.0017(15) C12 0.0592(18) 0.0405(14) 0.0385(14) -0.0029(11) 0.0040(13) -0.0098(13) C13 0.0265(10) 0.0395(12) 0.0238(10) 0.0015(9) 0.0039(8) -0.0005(9) C14 0.0348(12) 0.0413(13) 0.0405(14) -0.0042(11) 0.0050(10) -0.0017(10) C15 0.0275(11) 0.0430(13) 0.0459(15) -0.0008(11) 0.0014(10) -0.0002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.831(3) . ? P1 C7 1.834(3) . ? P1 C13 1.897(2) . ? F1 C13 1.392(3) . ? F2 C14 1.346(3) . ? F3 C14 1.319(3) . ? F4 C14 1.324(3) . ? F5 C15 1.301(3) . ? F6 C15 1.333(3) . ? F7 C15 1.329(3) . ? C1 C6 1.393(3) . ? C1 C2 1.399(4) . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.375(4) . ? C4 H4 0.9500 . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.387(4) . ? C7 C8 1.390(4) . ? C8 C9 1.403(5) . ? C8 H8 0.9500 . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 C11 1.369(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.541(3) . ? C13 C14 1.541(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C7 102.63(11) . . ? C1 P1 C13 103.40(11) . . ? C7 P1 C13 102.52(11) . . ? C6 C1 C2 118.5(2) . . ? C6 C1 P1 114.00(19) . . ? C2 C1 P1 127.37(19) . . ? C3 C2 C1 120.4(2) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.9(3) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C12 C7 C8 118.9(3) . . ? C12 C7 P1 126.9(2) . . ? C8 C7 P1 114.1(2) . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 120.5(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? F1 C13 C15 105.70(19) . . ? F1 C13 C14 104.7(2) . . ? C15 C13 C14 109.5(2) . . ? F1 C13 P1 115.75(15) . . ? C15 C13 P1 111.12(17) . . ? C14 C13 P1 109.77(16) . . ? F3 C14 F4 107.8(2) . . ? F3 C14 F2 107.9(2) . . ? F4 C14 F2 106.1(2) . . ? F3 C14 C13 111.9(2) . . ? F4 C14 C13 112.9(2) . . ? F2 C14 C13 110.0(2) . . ? F5 C15 F7 109.1(2) . . ? F5 C15 F6 108.1(3) . . ? F7 C15 F6 104.5(2) . . ? F5 C15 C13 112.1(2) . . ? F7 C15 C13 112.7(2) . . ? F6 C15 C13 110.0(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.230 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.074 #===END #compound 3 data_ll594a _database_code_depnum_ccdc_archive 'CCDC 746474' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 Cl2 F14 P2 Pt' _chemical_formula_sum 'C30 H20 Cl2 F14 P2 Pt' _chemical_formula_weight 974.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/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 10.713(1) _cell_length_b 16.914(1) _cell_length_c 9.180(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.570(1) _cell_angle_gamma 90.00 _cell_volume 1609.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 6466 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 4.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2536 _exptl_absorpt_correction_T_max 0.6493 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 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 15372 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4683 _reflns_number_gt 4012 _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^)+(0.0348P)^2^+0.9171P] 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 4683 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _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 0.01630(5) Uani 1 2 d S . . Cl1 Cl -0.13232(6) -0.09844(5) 0.04969(7) 0.02850(16) Uani 1 1 d . . . P1 P 0.17781(6) -0.02078(5) 0.20028(7) 0.01692(13) Uani 1 1 d . . . F1 F 0.02519(14) -0.08570(11) 0.35786(16) 0.0250(4) Uani 1 1 d . . . F2 F 0.28466(17) -0.20663(12) 0.3384(2) 0.0380(4) Uani 1 1 d . . . F3 F 0.12687(16) -0.18883(11) 0.14417(17) 0.0285(4) Uani 1 1 d . . . F4 F 0.08907(19) -0.23196(11) 0.34785(19) 0.0381(4) Uani 1 1 d . . . F5 F 0.21295(18) -0.15035(12) 0.59307(18) 0.0385(5) Uani 1 1 d . . . F6 F 0.1911(2) -0.02489(14) 0.57645(19) 0.0353(4) Uani 1 1 d . . . F7 F 0.35549(16) -0.07914(13) 0.52455(18) 0.0372(5) Uani 1 1 d . . . C1 C 0.3184(2) -0.05669(16) 0.1439(3) 0.0186(5) Uani 1 1 d . . . C2 C 0.2990(3) -0.08245(18) -0.0050(3) 0.0238(6) Uani 1 1 d . . . H2 H 0.2150 -0.0812 -0.0708 0.029 Uiso 1 1 calc R . . C3 C 0.4021(3) -0.1097(2) -0.0565(3) 0.0282(6) Uani 1 1 d . . . H3 H 0.3881 -0.1278 -0.1573 0.034 Uiso 1 1 calc R . . C4 C 0.5253(3) -0.1108(2) 0.0380(4) 0.0284(6) Uani 1 1 d . . . H4 H 0.5960 -0.1282 0.0012 0.034 Uiso 1 1 calc R . . C5 C 0.5452(3) -0.08659(19) 0.1860(3) 0.0277(6) Uani 1 1 d . . . H5 H 0.6296 -0.0880 0.2510 0.033 Uiso 1 1 calc R . . C6 C 0.4430(2) -0.06037(18) 0.2397(3) 0.0238(6) Uani 1 1 d . . . H6 H 0.4572 -0.0448 0.3420 0.029 Uiso 1 1 calc R . . C7 C 0.2181(2) 0.06906(17) 0.3100(3) 0.0186(5) Uani 1 1 d . . . C8 C 0.3371(3) 0.10671(18) 0.3344(3) 0.0243(6) Uani 1 1 d . . . H8 H 0.4034 0.0844 0.2955 0.029 Uiso 1 1 calc R . . C9 C 0.3590(3) 0.1768(2) 0.4157(4) 0.0337(7) Uani 1 1 d . . . H9 H 0.4406 0.2021 0.4329 0.040 Uiso 1 1 calc R . . C10 C 0.2625(3) 0.20988(19) 0.4718(3) 0.0316(7) Uani 1 1 d . . . H10 H 0.2785 0.2572 0.5293 0.038 Uiso 1 1 calc R . . C11 C 0.1421(3) 0.1739(2) 0.4442(4) 0.0320(7) Uani 1 1 d . . . H11 H 0.0755 0.1972 0.4812 0.038 Uiso 1 1 calc R . . C12 C 0.1192(3) 0.10423(19) 0.3627(3) 0.0279(6) Uani 1 1 d . . . H12 H 0.0364 0.0802 0.3425 0.034 Uiso 1 1 calc R . . C13 C 0.1500(3) -0.09626(18) 0.3464(3) 0.0193(5) Uani 1 1 d . . . C14 C 0.1620(3) -0.18196(18) 0.2933(3) 0.0250(6) Uani 1 1 d . . . C15 C 0.2296(3) -0.08724(19) 0.5119(3) 0.0254(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01078(8) 0.01952(9) 0.01752(8) 0.00253(5) 0.00153(5) -0.00125(5) Cl1 0.0187(3) 0.0342(4) 0.0289(3) 0.0106(3) -0.0010(2) -0.0101(3) P1 0.0124(3) 0.0213(3) 0.0164(3) 0.0006(3) 0.0024(2) -0.0004(3) F1 0.0179(7) 0.0362(11) 0.0217(7) 0.0017(7) 0.0063(6) -0.0024(7) F2 0.0345(10) 0.0299(11) 0.0438(10) 0.0024(8) -0.0009(8) 0.0104(8) F3 0.0345(9) 0.0283(10) 0.0226(7) -0.0030(7) 0.0069(7) -0.0014(7) F4 0.0552(12) 0.0283(11) 0.0331(9) 0.0018(8) 0.0156(8) -0.0124(9) F5 0.0519(11) 0.0387(12) 0.0200(8) 0.0102(7) 0.0001(8) -0.0090(9) F6 0.0429(11) 0.0408(11) 0.0216(8) -0.0067(8) 0.0070(8) -0.0035(10) F7 0.0222(8) 0.0585(14) 0.0258(8) 0.0029(8) -0.0035(7) -0.0046(8) C1 0.0138(11) 0.0202(14) 0.0222(11) 0.0004(10) 0.0054(9) -0.0006(9) C2 0.0179(12) 0.0308(17) 0.0224(12) -0.0022(11) 0.0046(10) 0.0013(11) C3 0.0266(14) 0.0344(18) 0.0254(13) -0.0051(12) 0.0101(11) 0.0009(12) C4 0.0201(13) 0.0308(18) 0.0370(14) 0.0001(14) 0.0121(11) 0.0031(12) C5 0.0139(12) 0.0324(18) 0.0347(14) 0.0019(12) 0.0024(11) 0.0027(11) C6 0.0176(12) 0.0296(17) 0.0229(12) 0.0004(11) 0.0026(10) 0.0028(11) C7 0.0154(11) 0.0198(14) 0.0196(11) 0.0020(10) 0.0025(9) -0.0008(10) C8 0.0175(12) 0.0240(16) 0.0313(14) -0.0030(11) 0.0058(10) -0.0006(10) C9 0.0216(14) 0.0290(18) 0.0480(18) -0.0061(14) 0.0038(13) -0.0058(12) C10 0.0367(16) 0.0214(16) 0.0358(16) -0.0061(12) 0.0075(13) -0.0025(13) C11 0.0301(15) 0.0271(17) 0.0439(17) -0.0046(13) 0.0187(13) 0.0042(13) C12 0.0211(14) 0.0263(17) 0.0391(16) -0.0032(13) 0.0126(12) -0.0011(12) C13 0.0175(12) 0.0221(14) 0.0181(11) 0.0011(10) 0.0043(9) -0.0017(10) C14 0.0300(14) 0.0230(16) 0.0207(12) 0.0023(10) 0.0041(10) 0.0002(11) C15 0.0227(13) 0.0304(17) 0.0208(12) 0.0029(11) 0.0011(10) -0.0026(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.3055(7) 3 ? Pt1 Cl1 2.3055(7) . ? Pt1 P1 2.3174(7) 3 ? Pt1 P1 2.3174(7) . ? P1 C7 1.814(3) . ? P1 C1 1.816(3) . ? P1 C13 1.929(3) . ? F1 C13 1.379(3) . ? F2 C14 1.341(3) . ? F3 C14 1.331(3) . ? F4 C14 1.332(3) . ? F5 C15 1.339(3) . ? F6 C15 1.325(4) . ? F7 C15 1.331(3) . ? C1 C2 1.400(3) . ? C1 C6 1.402(3) . ? C2 C3 1.385(4) . ? C2 H2 0.9500 . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(4) . ? C7 C12 1.403(4) . ? C8 C9 1.389(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.545(4) . ? C13 C15 1.551(4) . ? 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 Cl1 Pt1 Cl1 180.00(4) 3 . ? Cl1 Pt1 P1 99.04(2) 3 3 ? Cl1 Pt1 P1 80.96(2) . 3 ? Cl1 Pt1 P1 80.96(2) 3 . ? Cl1 Pt1 P1 99.04(2) . . ? P1 Pt1 P1 180.00(6) 3 . ? C7 P1 C1 109.87(12) . . ? C7 P1 C13 103.00(12) . . ? C1 P1 C13 105.14(12) . . ? C7 P1 Pt1 110.28(9) . . ? C1 P1 Pt1 113.58(8) . . ? C13 P1 Pt1 114.34(8) . . ? C2 C1 C6 118.9(2) . . ? C2 C1 P1 116.88(18) . . ? C6 C1 P1 124.3(2) . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 119.4(3) . . ? C8 C7 P1 123.6(2) . . ? C12 C7 P1 116.9(2) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.0(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? F1 C13 C14 107.8(2) . . ? F1 C13 C15 102.6(2) . . ? C14 C13 C15 109.4(2) . . ? F1 C13 P1 106.85(17) . . ? C14 C13 P1 111.21(17) . . ? C15 C13 P1 118.2(2) . . ? F3 C14 F4 106.9(2) . . ? F3 C14 F2 107.0(2) . . ? F4 C14 F2 108.0(2) . . ? F3 C14 C13 112.5(2) . . ? F4 C14 C13 112.0(2) . . ? F2 C14 C13 110.4(2) . . ? F6 C15 F7 107.5(2) . . ? F6 C15 F5 106.6(2) . . ? F7 C15 F5 107.9(2) . . ? F6 C15 C13 111.1(2) . . ? F7 C15 C13 113.0(2) . . ? F5 C15 C13 110.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.358 _refine_diff_density_min -1.919 _refine_diff_density_rms 0.140 #===END