Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Gregory Peters' 'Pramesh N. Kapoor' 'Jason D. Palcic' 'D. M. Roddick' _publ_contact_author_name 'Dr Gregory Peters' _publ_contact_author_address ; Department of Chemistry University of Memphis Memphis TN 38152 UNITED STATES OF AMERICA ; _publ_contact_author_email RGPETERS@MEMPHIS.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Perfluoroalkylphosphine Coordination Chemistry of Platinum: Synthesis of (C2F5)2PPh and (C2F5)PPh2 Complexes of Platinum(II) ; data_rpg1 _database_code_depnum_ccdc_archive 'CCDC 229924' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (pentafluoroethyl)diphenylphosphine _chemical_formula_moiety Ph2(C2F5)P _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H10 F5 P' _chemical_formula_weight 304.19 _chemical_melting_point ? _chemical_compound_source ? 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.918(4) _cell_length_b 11.559(2) _cell_length_c 7.9717(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2664.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.84 _cell_measurement_theta_max 12.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3069 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2323 _reflns_number_observed 1927 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL ver. 5.04' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL ver. 5.04' _computing_publication_material 'Siemens SHELXTL ver. 5.04' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+2.9973P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2323 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.1095 _refine_ls_wR_factor_obs 0.1023 _refine_ls_goodness_of_fit_all 1.129 _refine_ls_goodness_of_fit_obs 1.169 _refine_ls_restrained_S_all 1.129 _refine_ls_restrained_S_obs 1.169 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.61911(2) 0.94510(6) 0.10608(8) 0.0287(2) Uani 1 d . . F1 F 0.63555(5) 1.16489(12) 0.2287(2) 0.0373(4) Uani 1 d . . F2 F 0.64845(5) 1.13908(13) -0.0389(2) 0.0415(4) Uani 1 d . . F5 F 0.57610(6) 1.27750(14) 0.0393(2) 0.0563(5) Uani 1 d . . F4 F 0.55672(6) 1.1247(2) -0.0952(2) 0.0625(6) Uani 1 d . . F3 F 0.54221(5) 1.1386(2) 0.1686(2) 0.0541(5) Uani 1 d . . C11 C 0.68171(9) 0.9190(2) 0.1104(3) 0.0293(5) Uani 1 d . . C21 C 0.60030(8) 0.9276(2) 0.3240(3) 0.0273(5) Uani 1 d . . C22 C 0.62799(9) 0.9449(2) 0.4629(3) 0.0346(6) Uani 1 d . . H22 H 0.65922(9) 0.9685(2) 0.4486(3) 0.042 Uiso 1 calc R . C1 C 0.61965(8) 1.1083(2) 0.0897(3) 0.0304(6) Uani 1 d . . C12 C 0.71504(9) 0.9884(2) 0.1868(3) 0.0328(6) Uani 1 d . . H12 H 0.70602(9) 1.0580(2) 0.2412(3) 0.039 Uiso 1 calc R . C16 C 0.69618(10) 0.8185(2) 0.0291(4) 0.0400(7) Uani 1 d . . H16 H 0.67419(10) 0.7709(2) -0.0263(4) 0.048 Uiso 1 calc R . C25 C 0.53782(10) 0.8763(3) 0.5090(4) 0.0501(8) Uani 1 d . . H25 H 0.50652(10) 0.8537(3) 0.5241(4) 0.060 Uiso 1 calc R . C23 C 0.61062(9) 0.9282(3) 0.6225(4) 0.0407(7) Uani 1 d . . H23 H 0.62997(9) 0.9410(3) 0.7170(4) 0.049 Uiso 1 calc R . C15 C 0.74273(11) 0.7877(3) 0.0288(4) 0.0495(8) Uani 1 d . . H15 H 0.75220(11) 0.7184(3) -0.0253(4) 0.059 Uiso 1 calc R . C24 C 0.56575(10) 0.8933(2) 0.6462(4) 0.0418(7) Uani 1 d . . H24 H 0.55411(10) 0.8810(2) 0.7562(4) 0.050 Uiso 1 calc R . C26 C 0.55513(10) 0.8921(3) 0.3489(4) 0.0416(7) Uani 1 d . . H26 H 0.53575(10) 0.8783(3) 0.2548(4) 0.050 Uiso 1 calc R . C2 C 0.57300(10) 1.1634(3) 0.0491(4) 0.0405(7) Uani 1 d . . C13 C 0.76128(9) 0.9567(3) 0.1839(4) 0.0420(7) Uani 1 d . . H13 H 0.78368(9) 1.0047(3) 0.2364(4) 0.050 Uiso 1 calc R . C14 C 0.77502(10) 0.8564(3) 0.1058(4) 0.0479(8) Uani 1 d . . H14 H 0.80672(10) 0.8348(3) 0.1052(4) 0.058 Uiso 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 P1 0.0320(3) 0.0313(3) 0.0227(3) -0.0022(3) -0.0011(3) -0.0039(3) F1 0.0416(8) 0.0324(8) 0.0379(9) -0.0062(7) -0.0037(7) -0.0017(7) F2 0.0403(8) 0.0433(9) 0.0408(9) 0.0116(8) 0.0125(7) 0.0028(7) F5 0.0532(10) 0.0445(10) 0.0711(13) 0.0158(9) 0.0049(9) 0.0166(8) F4 0.0592(11) 0.0781(13) 0.0501(11) -0.0033(10) -0.0228(10) 0.0175(10) F3 0.0336(8) 0.0669(12) 0.0617(12) 0.0143(10) 0.0125(9) 0.0087(8) C11 0.0349(13) 0.0292(12) 0.0238(12) 0.0020(11) 0.0050(11) 0.0032(10) C21 0.0304(12) 0.0266(12) 0.0250(12) 0.0007(10) 0.0037(11) -0.0021(10) C22 0.0275(12) 0.045(2) 0.0311(14) 0.0019(13) 0.0007(11) -0.0036(11) C1 0.0299(12) 0.0347(13) 0.0266(13) 0.0036(11) 0.0020(11) -0.0012(10) C12 0.0324(13) 0.0362(14) 0.0299(13) -0.0016(12) 0.0040(11) 0.0027(11) C16 0.055(2) 0.0310(14) 0.0336(15) -0.0010(12) 0.0082(14) 0.0026(13) C25 0.0368(15) 0.065(2) 0.048(2) -0.005(2) 0.0101(14) -0.0212(14) C23 0.0373(14) 0.057(2) 0.0273(14) -0.0007(13) -0.0006(12) -0.0024(13) C15 0.064(2) 0.039(2) 0.045(2) 0.0052(14) 0.018(2) 0.0202(15) C24 0.047(2) 0.046(2) 0.032(2) 0.0025(13) 0.0135(13) -0.0051(13) C26 0.0377(15) 0.053(2) 0.034(2) -0.0023(13) -0.0020(12) -0.0158(13) C2 0.0378(14) 0.047(2) 0.037(2) 0.0049(14) 0.0000(13) 0.0060(13) C13 0.0311(14) 0.052(2) 0.043(2) 0.0089(14) 0.0044(12) 0.0020(13) C14 0.041(2) 0.053(2) 0.050(2) 0.016(2) 0.0121(15) 0.0170(14) _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 C21 1.832(3) . ? P1 C11 1.835(3) . ? P1 C1 1.891(3) . ? F1 C1 1.366(3) . ? F2 C1 1.368(3) . ? F5 C2 1.324(3) . ? F4 C2 1.321(3) . ? F3 C2 1.335(3) . ? C11 C12 1.394(4) . ? C11 C16 1.394(4) . ? C21 C22 1.381(4) . ? C21 C26 1.383(3) . ? C22 C23 1.382(4) . ? C1 C2 1.526(4) . ? C12 C13 1.387(4) . ? C16 C15 1.393(4) . ? C25 C24 1.374(4) . ? C25 C26 1.383(4) . ? C23 C24 1.372(4) . ? C15 C14 1.371(5) . ? C13 C14 1.374(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 C21 P1 C11 104.88(11) . . ? C21 P1 C1 100.26(11) . . ? C11 P1 C1 99.04(11) . . ? C12 C11 C16 118.4(2) . . ? C12 C11 P1 126.5(2) . . ? C16 C11 P1 115.1(2) . . ? C22 C21 C26 118.4(2) . . ? C22 C21 P1 124.9(2) . . ? C26 C21 P1 116.7(2) . . ? C21 C22 C23 120.5(2) . . ? F1 C1 F2 106.2(2) . . ? F1 C1 C2 105.6(2) . . ? F2 C1 C2 105.7(2) . . ? F1 C1 P1 115.1(2) . . ? F2 C1 P1 108.4(2) . . ? C2 C1 P1 115.0(2) . . ? C13 C12 C11 120.5(3) . . ? C15 C16 C11 120.3(3) . . ? C24 C25 C26 120.2(3) . . ? C24 C23 C22 120.8(3) . . ? C14 C15 C16 120.6(3) . . ? C23 C24 C25 119.3(3) . . ? C25 C26 C21 120.9(3) . . ? F4 C2 F5 108.1(2) . . ? F4 C2 F3 108.1(2) . . ? F5 C2 F3 107.5(2) . . ? F4 C2 C1 111.0(2) . . ? F5 C2 C1 111.6(2) . . ? F3 C2 C1 110.4(2) . . ? C14 C13 C12 120.6(3) . . ? C15 C14 C13 119.6(3) . . ? _refine_diff_density_max 0.308 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.051 #===END data_dmr824 _database_code_depnum_ccdc_archive 'CCDC 229925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-[Ph2P(C2F5)]2PtCl2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cl2 F10 P2 Pt' _chemical_formula_weight 874.37 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0451(13) _cell_length_b 10.2057(12) _cell_length_c 10.9332(15) _cell_angle_alpha 111.426(8) _cell_angle_beta 106.208(12) _cell_angle_gamma 102.847(11) _cell_volume 747.75(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 5.059 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4220 _exptl_absorpt_correction_T_max 0.5710 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1290 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max -3 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 8.51 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1290 _reflns_number_gt 1289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS V. 2.31' _computing_cell_refinement 'Bruker XSCANS V. 2.31' _computing_data_reduction 'Bruker SHELXTL V. 5.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 5.10' _computing_publication_material 'Bruker SHELXTL V. 5.10' _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^)+(0.0320P)^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 1290 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.02704(13) Uani 1 2 d S . . P1 P 0.21910(14) 0.01927(16) 0.19901(14) 0.0282(3) Uani 1 1 d . . . Cl1 Cl 0.20217(15) 0.13899(19) -0.05958(17) 0.0428(4) Uani 1 1 d . . . C1 C 0.4735(6) 0.1389(7) 0.2578(7) 0.0354(13) Uani 1 1 d . . . C2 C 0.5294(8) 0.3093(11) 0.3281(9) 0.052(2) Uani 1 1 d . . . F1 F 0.5830(4) 0.1052(5) 0.3534(5) 0.0512(11) Uani 1 1 d . . . F2 F 0.5199(4) 0.0976(5) 0.1437(5) 0.0500(10) Uani 1 1 d . . . F3 F 0.6871(10) 0.3713(9) 0.3213(11) 0.108(3) Uani 1 1 d . . . F4 F 0.5614(9) 0.3618(9) 0.4671(8) 0.0815(16) Uani 1 1 d . . . F5 F 0.4023(8) 0.3547(8) 0.2753(10) 0.081(2) Uani 1 1 d . . . C11 C 0.2398(6) -0.1628(7) 0.1644(6) 0.0320(12) Uani 1 1 d . . . C12 C 0.2892(10) -0.2285(9) 0.0512(9) 0.0501(17) Uani 1 1 d . . . H12A H 0.3129 -0.1784 -0.0015 0.060 Uiso 1 1 calc R . . C13 C 0.3031(11) -0.3709(11) 0.0169(11) 0.063(2) Uani 1 1 d . . . H13A H 0.3415 -0.4133 -0.0561 0.076 Uiso 1 1 calc R . . C14 C 0.2606(10) -0.4477(10) 0.0897(13) 0.065(2) Uani 1 1 d . . . H14A H 0.2654 -0.5438 0.0638 0.078 Uiso 1 1 calc R . . C15 C 0.2100(10) -0.3828(12) 0.2024(13) 0.064(2) Uani 1 1 d . . . H15A H 0.1837 -0.4342 0.2537 0.076 Uiso 1 1 calc R . . C16 C 0.1990(8) -0.2428(9) 0.2375(8) 0.0476(16) Uani 1 1 d . . . H16A H 0.1633 -0.2003 0.3122 0.057 Uiso 1 1 calc R . . C21 C 0.1905(6) 0.1026(8) 0.3658(6) 0.0343(13) Uani 1 1 d . . . C22 C 0.2922(7) 0.0976(9) 0.4880(8) 0.0466(16) Uani 1 1 d . . . H22A H 0.3722 0.0445 0.4832 0.056 Uiso 1 1 calc R . . C23 C 0.2780(8) 0.1697(12) 0.6174(8) 0.0530(19) Uani 1 1 d . . . H23A H 0.3427 0.1620 0.6979 0.064 Uiso 1 1 calc R . . C24 C 0.1619(9) 0.2551(11) 0.6226(8) 0.062(2) Uani 1 1 d . . . H24A H 0.1533 0.3083 0.7087 0.074 Uiso 1 1 calc R . . C25 C 0.0629(8) 0.2601(9) 0.5030(8) 0.0553(19) Uani 1 1 d . . . H25A H -0.0134 0.3166 0.5083 0.066 Uiso 1 1 calc R . . C26 C 0.0726(7) 0.1829(9) 0.3726(7) 0.0446(16) Uani 1 1 d . . . H26A H 0.0008 0.1850 0.2908 0.054 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 0.03113(16) 0.0279(2) 0.02110(19) 0.01266(13) 0.00584(10) 0.01224(10) P1 0.0316(4) 0.0301(8) 0.0233(8) 0.0140(6) 0.0071(5) 0.0138(5) Cl1 0.0432(5) 0.0467(10) 0.0373(9) 0.0254(8) 0.0117(5) 0.0088(5) C1 0.0360(19) 0.040(4) 0.032(4) 0.022(3) 0.009(2) 0.015(2) C2 0.052(3) 0.047(6) 0.032(4) 0.011(4) 0.000(3) 0.007(3) F1 0.0382(12) 0.060(3) 0.053(3) 0.035(2) 0.0024(14) 0.0180(14) F2 0.0473(14) 0.057(3) 0.048(3) 0.022(2) 0.0255(17) 0.0172(15) F3 0.101(4) 0.056(5) 0.137(9) 0.032(5) 0.056(5) -0.011(3) F4 0.120(3) 0.049(5) 0.038(4) 0.009(4) 0.003(3) 0.020(3) F5 0.111(3) 0.036(4) 0.069(6) 0.017(4) 0.002(3) 0.033(3) C11 0.0342(18) 0.028(3) 0.029(4) 0.014(3) 0.0047(19) 0.0116(18) C12 0.072(3) 0.038(5) 0.042(5) 0.015(4) 0.027(3) 0.022(3) C13 0.084(4) 0.045(5) 0.059(6) 0.017(5) 0.030(4) 0.031(4) C14 0.074(4) 0.025(5) 0.074(8) 0.015(5) 0.007(4) 0.022(3) C15 0.069(3) 0.045(6) 0.066(8) 0.033(6) 0.008(4) 0.013(3) C16 0.053(3) 0.047(5) 0.050(5) 0.031(4) 0.019(3) 0.018(3) C21 0.0353(19) 0.039(4) 0.023(3) 0.012(3) 0.007(2) 0.012(2) C22 0.047(2) 0.057(5) 0.034(4) 0.020(4) 0.011(2) 0.023(3) C23 0.053(3) 0.073(6) 0.031(5) 0.027(4) 0.013(3) 0.021(3) C24 0.051(3) 0.065(6) 0.039(5) -0.001(4) 0.021(3) 0.008(3) C25 0.050(3) 0.059(5) 0.038(5) 0.003(4) 0.014(3) 0.026(3) C26 0.043(2) 0.054(5) 0.031(4) 0.014(3) 0.009(2) 0.023(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 P1 2.2961(13) . ? Pt1 P1 2.2961(13) 2 ? Pt1 Cl1 2.3070(12) 2 ? Pt1 Cl1 2.3070(12) . ? P1 C11 1.812(6) . ? P1 C21 1.813(5) . ? P1 C1 1.917(5) . ? C1 F2 1.348(7) . ? C1 F1 1.368(7) . ? C1 C2 1.517(12) . ? C2 F5 1.292(13) . ? C2 F3 1.321(9) . ? C2 F4 1.338(12) . ? C11 C16 1.384(9) . ? C11 C12 1.388(9) . ? C12 C13 1.401(12) . ? C13 C14 1.361(15) . ? C14 C15 1.388(17) . ? C15 C16 1.368(13) . ? C21 C22 1.384(9) . ? C21 C26 1.385(10) . ? C22 C23 1.386(10) . ? C23 C24 1.411(14) . ? C24 C25 1.353(13) . ? C25 C26 1.389(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 180.0 . 2 ? P1 Pt1 Cl1 82.99(5) . 2 ? P1 Pt1 Cl1 97.01(5) 2 2 ? P1 Pt1 Cl1 97.01(5) . . ? P1 Pt1 Cl1 82.99(5) 2 . ? Cl1 Pt1 Cl1 180.0 2 . ? C11 P1 C21 111.2(3) . . ? C11 P1 C1 99.6(2) . . ? C21 P1 C1 99.9(3) . . ? C11 P1 Pt1 109.89(19) . . ? C21 P1 Pt1 116.25(18) . . ? C1 P1 Pt1 118.52(19) . . ? F2 C1 F1 106.3(4) . . ? F2 C1 C2 108.2(5) . . ? F1 C1 C2 106.6(6) . . ? F2 C1 P1 108.9(4) . . ? F1 C1 P1 108.5(4) . . ? C2 C1 P1 117.7(3) . . ? F5 C2 F3 111.3(10) . . ? F5 C2 F4 105.7(7) . . ? F3 C2 F4 106.6(8) . . ? F5 C2 C1 113.4(6) . . ? F3 C2 C1 109.4(6) . . ? F4 C2 C1 110.2(8) . . ? C16 C11 C12 118.7(6) . . ? C16 C11 P1 124.3(5) . . ? C12 C11 P1 116.9(5) . . ? C11 C12 C13 119.6(7) . . ? C14 C13 C12 120.4(7) . . ? C13 C14 C15 120.2(8) . . ? C16 C15 C14 119.5(8) . . ? C15 C16 C11 121.6(7) . . ? C22 C21 C26 119.4(5) . . ? C22 C21 P1 122.2(4) . . ? C26 C21 P1 118.3(5) . . ? C21 C22 C23 121.8(6) . . ? C22 C23 C24 117.7(7) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 121.5(6) . . ? C21 C26 C25 119.2(6) . . ? _diffrn_measured_fraction_theta_max 0.492 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.492 _refine_diff_density_max 0.448 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.054 #===END data_pk001 _database_code_depnum_ccdc_archive 'CCDC 229926' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common trans-[PhP(C2F5)2]2PtCl2 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H10 Cl2 F20 P2 Pt' _chemical_formula_weight 958.21 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1326(9) _cell_length_b 12.010(2) _cell_length_c 11.5424(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.911(6) _cell_angle_gamma 90.00 _cell_volume 1379.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.48 _cell_measurement_theta_max 12.51 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.307 _exptl_crystal_density_method ? _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 5.546 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2641 _exptl_absorpt_correction_T_max 0.9796 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1% _diffrn_reflns_number 3152 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2418 _reflns_number_observed 2205 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS, v. 2.31' _computing_cell_refinement 'Siemens XSCANS, v. 2.31' _computing_data_reduction 'Siemens SHELXTL, v. 5.03' _computing_structure_solution 'Siemens Shelxtl, v. 5.03' _computing_structure_refinement 'Siemens Shelxtl, v. 5.03' _computing_molecular_graphics 'Siemens SHELXTL, v. 5.03' _computing_publication_material 'Siemens SHELXTL, v. 5.03' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+2.7882P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2417 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_obs 0.0386 _refine_ls_wR_factor_all 0.1098 _refine_ls_wR_factor_obs 0.1058 _refine_ls_goodness_of_fit_all 1.107 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.5000 0.0000 0.0173(2) Uani 1 d S . P1 P 0.06303(12) 0.59142(11) -0.15511(11) 0.0201(3) Uani 1 d . . Cl1 Cl 0.15522(12) 0.36878(11) -0.03053(12) 0.0291(3) Uani 1 d . . C1 C -0.0113(8) 0.5201(6) -0.3013(7) 0.033(2) Uani 1 d . . C2 C -0.1507(7) 0.4680(8) -0.3101(6) 0.043(2) Uani 1 d . . C3 C 0.0070(6) 0.7412(5) -0.1837(5) 0.0343(13) Uani 1 d . . C4 C 0.0725(7) 0.8233(5) -0.0881(7) 0.044(2) Uani 1 d . . C5 C 0.2389(5) 0.6055(4) -0.1598(4) 0.0215(10) Uani 1 d . . C6 C 0.2844(6) 0.6243(5) -0.2651(5) 0.0302(12) Uani 1 d . . H6A H 0.2230(6) 0.6239(5) -0.3384(5) 0.036 Uiso 1 calc R . C7 C 0.4196(6) 0.6433(6) -0.2618(6) 0.0384(14) Uani 1 d . . H7A H 0.4513(6) 0.6550(6) -0.3332(6) 0.046 Uiso 1 calc R . C8 C 0.5085(6) 0.6455(5) -0.1558(6) 0.0355(14) Uani 1 d . . H8A H 0.6010(6) 0.6597(5) -0.1542(6) 0.043 Uiso 1 calc R . C9 C 0.4643(5) 0.6272(5) -0.0525(5) 0.0324(13) Uani 1 d . . H9A H 0.5266(5) 0.6279(5) 0.0202(5) 0.039 Uiso 1 calc R . C10 C 0.3281(5) 0.6075(5) -0.0529(5) 0.0269(11) Uani 1 d . . H10A H 0.2974(5) 0.5958(5) 0.0189(5) 0.032 Uiso 1 calc R . F1 F 0.0723(3) 0.4359(3) -0.3176(3) 0.0433(9) Uani 1 d . . F2 F -0.0207(4) 0.5911(4) -0.3935(3) 0.0507(10) Uani 1 d . . F3 F -0.1908(4) 0.4264(5) -0.4177(3) 0.0620(13) Uani 1 d . . F4 F -0.2367(5) 0.5454(6) -0.2904(5) 0.0694(13) Uani 1 d . . F5 F -0.1466(4) 0.3850(4) -0.2338(3) 0.0569(11) Uani 1 d . . F6 F 0.0390(5) 0.7786(4) -0.2859(4) 0.0578(11) Uani 1 d . . F7 F -0.1279(4) 0.7481(3) -0.1980(3) 0.0475(10) Uani 1 d . . F8 F -0.0064(5) 0.9096(4) -0.0831(6) 0.084(2) Uani 1 d . . F9 F 0.1884(5) 0.8603(4) -0.1101(5) 0.0681(13) Uani 1 d . . F10 F 0.0996(4) 0.7765(3) 0.0178(3) 0.0470(9) Uani 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 0.0147(2) 0.0196(2) 0.0175(2) -0.00037(8) 0.00270(14) -0.00120(8) P1 0.0185(6) 0.0236(7) 0.0180(6) 0.0010(5) 0.0031(5) -0.0003(5) Cl1 0.0238(6) 0.0248(7) 0.0408(7) 0.0006(5) 0.0113(5) 0.0035(5) C1 0.029(4) 0.044(3) 0.024(3) -0.004(3) -0.001(3) -0.004(3) C2 0.029(4) 0.066(4) 0.031(4) -0.009(4) -0.006(3) -0.001(4) C3 0.033(3) 0.036(3) 0.037(3) 0.016(3) 0.013(2) 0.011(2) C4 0.045(4) 0.022(3) 0.074(5) 0.004(3) 0.034(3) -0.002(3) C5 0.023(2) 0.018(2) 0.025(3) -0.001(2) 0.009(2) -0.003(2) C6 0.030(3) 0.035(3) 0.028(3) 0.007(2) 0.011(2) 0.002(2) C7 0.040(3) 0.040(4) 0.042(4) 0.008(3) 0.025(3) 0.001(3) C8 0.022(3) 0.036(3) 0.049(4) 0.001(3) 0.009(3) -0.003(2) C9 0.025(3) 0.038(3) 0.035(3) 0.000(2) 0.004(2) -0.007(2) C10 0.026(3) 0.028(3) 0.027(3) 0.001(2) 0.007(2) -0.003(2) F1 0.032(2) 0.058(3) 0.040(2) -0.020(2) 0.008(2) 0.004(2) F2 0.051(2) 0.076(3) 0.021(2) 0.010(2) -0.002(2) -0.010(2) F3 0.049(2) 0.100(4) 0.031(2) -0.023(2) -0.006(2) -0.023(2) F4 0.030(2) 0.101(4) 0.074(3) -0.023(3) 0.004(2) 0.011(3) F5 0.053(2) 0.072(3) 0.041(2) -0.005(2) -0.003(2) -0.034(2) F6 0.085(3) 0.046(2) 0.052(2) 0.028(2) 0.035(2) 0.018(2) F7 0.035(2) 0.047(2) 0.059(2) 0.014(2) 0.005(2) 0.021(2) F8 0.082(4) 0.037(3) 0.137(5) -0.020(3) 0.034(3) 0.022(2) F9 0.072(3) 0.049(3) 0.096(4) -0.005(2) 0.047(3) -0.027(2) F10 0.056(2) 0.041(2) 0.048(2) -0.012(2) 0.022(2) -0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2916(12) . ? Pt1 P1 2.2917(12) 3_565 ? Pt1 Cl1 2.3002(12) 3_565 ? Pt1 Cl1 2.3002(12) . ? P1 C5 1.801(5) . ? P1 C3 1.897(6) . ? P1 C1 1.915(7) . ? C1 F2 1.353(9) . ? C1 F1 1.355(9) . ? C1 C2 1.531(11) . ? C2 F4 1.323(10) . ? C2 F5 1.325(10) . ? C2 F3 1.328(8) . ? C3 F7 1.348(7) . ? C3 F6 1.357(7) . ? C3 C4 1.533(10) . ? C4 F8 1.318(7) . ? C4 F9 1.324(7) . ? C4 F10 1.326(8) . ? C5 C10 1.385(8) . ? C5 C6 1.398(7) . ? C6 C7 1.382(8) . ? C7 C8 1.376(9) . ? C8 C9 1.368(8) . ? C9 C10 1.399(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 180.0 . 3_565 ? P1 Pt1 Cl1 95.23(5) . 3_565 ? P1 Pt1 Cl1 84.77(5) 3_565 3_565 ? P1 Pt1 Cl1 84.77(5) . . ? P1 Pt1 Cl1 95.23(5) 3_565 . ? Cl1 Pt1 Cl1 180.0 3_565 . ? C5 P1 C3 99.8(2) . . ? C5 P1 C1 104.0(3) . . ? C3 P1 C1 102.5(3) . . ? C5 P1 Pt1 119.5(2) . . ? C3 P1 Pt1 118.2(2) . . ? C1 P1 Pt1 110.7(2) . . ? F2 C1 F1 108.3(6) . . ? F2 C1 C2 106.2(6) . . ? F1 C1 C2 106.2(6) . . ? F2 C1 P1 111.6(5) . . ? F1 C1 P1 107.7(5) . . ? C2 C1 P1 116.4(5) . . ? F4 C2 F5 110.7(7) . . ? F4 C2 F3 109.3(6) . . ? F5 C2 F3 107.7(7) . . ? F4 C2 C1 109.3(8) . . ? F5 C2 C1 110.5(6) . . ? F3 C2 C1 109.3(6) . . ? F7 C3 F6 106.1(5) . . ? F7 C3 C4 109.9(5) . . ? F6 C3 C4 105.7(5) . . ? F7 C3 P1 110.0(4) . . ? F6 C3 P1 110.6(4) . . ? C4 C3 P1 114.2(4) . . ? F8 C4 F9 108.2(5) . . ? F8 C4 F10 108.3(6) . . ? F9 C4 F10 106.4(6) . . ? F8 C4 C3 110.7(6) . . ? F9 C4 C3 110.9(5) . . ? F10 C4 C3 112.2(5) . . ? C10 C5 C6 120.3(5) . . ? C10 C5 P1 117.3(4) . . ? C6 C5 P1 122.2(4) . . ? C7 C6 C5 119.4(6) . . ? C8 C7 C6 120.4(6) . . ? C9 C8 C7 120.3(5) . . ? C8 C9 C10 120.6(5) . . ? C5 C10 C9 118.9(5) . . ? _refine_diff_density_max 1.945 _refine_diff_density_min -2.918 _refine_diff_density_rms 0.226