data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Gregory J. Grant' _publ_contact_author_address ;Univeristy of Tennessee at Chattanooga Chattanooga, TN 37403 ; _publ_contact_author_email Greg-Grant@utc.edu _publ_contact_author_phone 4234254143 loop_ _publ_author_name _publ_author_address G.J.Grant ;Department of Chemistry University of Tennessee at Chattanooga Chattanooga, TN 37403 ; D.E.Janzen ;Department of Chemistry College of St. Catherine St. Paul, MN 55105 ; L.F.Mehne ;Department of Chemistry Convenant College Lookout Mountain, GA 30750 ; 'D.A.da Siva Filho' ;Department of Chemistry and Biochemistry Georgia Institute of Technology Atlanta, Ga 30332 ; J.-L.Bredas ; Department of Chemistry and Biochemistry Georgia Institute of Technology Atlanta, Ga 30332 ; ; D.G.VanDerveer ; ;Department of Chemistry Clemson University Clemson, SC 29638 ; data_pdppy _database_code_depnum_ccdc_archive 'CCDC 666384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 N Pd S3, F6 P' _chemical_formula_sum 'C17 H20 F6 N P Pd S3' _chemical_formula_weight 585.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.958(2) _cell_length_b 12.112(2) _cell_length_c 28.019(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4058.2(14) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 13346 _cell_measurement_theta_min 1.4534 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.6199 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20775 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3686 _reflns_number_gt 3563 _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^)+(0.0355P)^2^+5.2474P] 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 3686 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.313 _refine_ls_restrained_S_all 1.313 _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 Pd1 Pd 0.65163(2) 0.075154(19) 0.633220(8) 0.01554(10) Uani 1 1 d . . . S2 S 0.57258(7) 0.04901(6) 0.55593(3) 0.01917(18) Uani 1 1 d . C . S1 S 0.78138(7) 0.18995(7) 0.59858(3) 0.0244(2) Uani 1 1 d . C . S3 S 0.50625(7) 0.26374(7) 0.63366(3) 0.02202(19) Uani 1 1 d . C . P1 P 0.11671(8) 0.09726(7) 0.56926(3) 0.0227(2) Uani 1 1 d . . . F6 F 0.1834(2) 0.09762(19) 0.51927(8) 0.0386(5) Uani 1 1 d . . . F5 F 0.20125(19) 0.0051(2) 0.58864(8) 0.0435(6) Uani 1 1 d . . . F4 F 0.03446(18) 0.19029(18) 0.54895(9) 0.0393(5) Uani 1 1 d . . . F3 F 0.19905(19) 0.1912(2) 0.58809(9) 0.0427(6) Uani 1 1 d . . . F2 F 0.05178(19) 0.0974(2) 0.61904(8) 0.0404(5) Uani 1 1 d . . . F1 F 0.0351(2) 0.00418(19) 0.55004(9) 0.0451(6) Uani 1 1 d . . . C16 C 0.6266(3) 0.3537(3) 0.62881(12) 0.0251(7) Uani 1 1 d . . . H16A H 0.5994 0.4293 0.6220 0.030 Uiso 1 1 calc R C . H16B H 0.6642 0.3558 0.6603 0.030 Uiso 1 1 calc R . . C12 C 0.7816(3) 0.1397(3) 0.53732(12) 0.0256(7) Uani 1 1 d . . . H12A H 0.8237 0.1927 0.5173 0.031 Uiso 1 1 calc R C . H12B H 0.8220 0.0684 0.5363 0.031 Uiso 1 1 calc R . . C6 C 0.6589(3) 0.0322(3) 0.73435(12) 0.0201(7) Uani 1 1 d . . . C7 C 0.6900(3) 0.0411(3) 0.78211(12) 0.0261(7) Uani 1 1 d . C . H7A H 0.6471 0.0050 0.8060 0.031 Uiso 1 1 calc R . . C17 C 0.7133(3) 0.3241(3) 0.59149(12) 0.0270(8) Uani 1 1 d . C . H17A H 0.7718 0.3819 0.5917 0.032 Uiso 1 1 calc R . . H17B H 0.6769 0.3260 0.5598 0.032 Uiso 1 1 calc R . . C14 C 0.4467(3) 0.1335(3) 0.55507(13) 0.0238(7) Uani 1 1 d . . . H14A H 0.4185 0.1354 0.5219 0.029 Uiso 1 1 calc R C . H14B H 0.3893 0.0959 0.5747 0.029 Uiso 1 1 calc R . . C5 C 0.5651(3) -0.0349(3) 0.71747(11) 0.0206(7) Uani 1 1 d . C . C3 C 0.4120(3) -0.1604(3) 0.72639(14) 0.0317(8) Uani 1 1 d . C . H3A H 0.3633 -0.2020 0.7463 0.038 Uiso 1 1 calc R . . C15 C 0.4567(3) 0.2524(3) 0.57269(12) 0.0223(7) Uani 1 1 d . C . H15A H 0.3825 0.2883 0.5703 0.027 Uiso 1 1 calc R . . H15B H 0.5086 0.2930 0.5515 0.027 Uiso 1 1 calc R . . C2 C 0.4000(3) -0.1638(3) 0.67754(13) 0.0314(8) Uani 1 1 d . C . H2A H 0.3441 -0.2087 0.6633 0.038 Uiso 1 1 calc R . . C9 C 0.8450(3) 0.1537(3) 0.76051(13) 0.0294(8) Uani 1 1 d . C . H9A H 0.9094 0.1948 0.7694 0.035 Uiso 1 1 calc R . . C8 C 0.7826(3) 0.1018(3) 0.79491(12) 0.0290(8) Uani 1 1 d . . . H8A H 0.8033 0.1077 0.8275 0.035 Uiso 1 1 calc R C . C13 C 0.6667(3) 0.1234(3) 0.51558(12) 0.0226(7) Uani 1 1 d . C . H13A H 0.6741 0.0815 0.4854 0.027 Uiso 1 1 calc R . . H13B H 0.6340 0.1964 0.5079 0.027 Uiso 1 1 calc R . . C10 C 0.8143(3) 0.1465(3) 0.71273(12) 0.0255(7) Uani 1 1 d . . . H10A H 0.8580 0.1828 0.6892 0.031 Uiso 1 1 calc R A 1 C4 C 0.4946(3) -0.0965(3) 0.74620(13) 0.0281(8) Uani 1 1 d . . . H4A H 0.5035 -0.0944 0.7799 0.034 Uiso 1 1 calc R C . C1 C 0.47091(16) -0.10069(14) 0.64961(6) 0.0270(8) Uani 1 1 d . . . H1A H 0.4629 -0.1030 0.6159 0.032 Uiso 1 1 calc R B 1 C11 C 0.72111(16) 0.08736(14) 0.69907(6) 0.0193(8) Uani 0.80(3) 1 d PR C 1 N1 N 0.55114(16) -0.03590(14) 0.66884(6) 0.0206(7) Uani 0.80(3) 1 d PR C 1 N1' N 0.72111(16) 0.08736(14) 0.69907(6) 0.0193(8) Uani 0.20(3) 1 d PR C 2 C11' C 0.55114(16) -0.03590(14) 0.66884(6) 0.0206(7) Uani 0.20(3) 1 d PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01715(16) 0.01617(15) 0.01329(15) 0.00107(8) -0.00030(9) 0.00029(9) S2 0.0209(4) 0.0174(4) 0.0192(4) -0.0017(3) 0.0001(3) 0.0001(3) S1 0.0174(4) 0.0368(5) 0.0190(4) -0.0015(3) 0.0009(3) -0.0037(3) S3 0.0245(5) 0.0213(4) 0.0203(4) -0.0019(3) 0.0035(3) 0.0010(3) P1 0.0214(4) 0.0259(4) 0.0208(4) 0.0027(3) -0.0012(4) -0.0035(4) F6 0.0462(13) 0.0444(13) 0.0253(11) 0.0014(9) 0.0098(10) 0.0048(11) F5 0.0375(13) 0.0479(14) 0.0452(14) 0.0146(11) -0.0033(11) 0.0112(11) F4 0.0279(12) 0.0375(12) 0.0524(14) 0.0195(10) 0.0044(10) 0.0031(10) F3 0.0283(12) 0.0484(14) 0.0515(14) -0.0181(11) 0.0057(11) -0.0144(11) F2 0.0309(12) 0.0611(15) 0.0292(12) 0.0022(10) 0.0081(10) -0.0018(11) F1 0.0514(15) 0.0371(13) 0.0468(14) 0.0026(10) -0.0134(12) -0.0198(11) C16 0.033(2) 0.0189(16) 0.0229(18) -0.0059(13) -0.0017(14) -0.0025(15) C12 0.0217(18) 0.0358(19) 0.0193(16) -0.0021(14) 0.0081(14) -0.0018(15) C6 0.0236(17) 0.0176(15) 0.0192(17) 0.0016(12) 0.0013(13) 0.0051(13) C7 0.034(2) 0.0261(17) 0.0186(17) 0.0027(13) 0.0006(15) 0.0045(16) C17 0.032(2) 0.0265(17) 0.0226(17) 0.0010(13) 0.0017(15) -0.0121(15) C14 0.0148(16) 0.0243(17) 0.0323(19) -0.0053(14) -0.0022(14) 0.0009(13) C5 0.0259(18) 0.0169(15) 0.0190(16) 0.0022(12) 0.0009(13) 0.0039(13) C3 0.035(2) 0.0270(18) 0.033(2) 0.0075(15) 0.0061(16) -0.0084(16) C15 0.0183(17) 0.0253(16) 0.0233(17) -0.0029(13) -0.0018(13) 0.0059(14) C2 0.038(2) 0.0235(17) 0.033(2) 0.0003(14) -0.0003(17) -0.0119(16) C9 0.032(2) 0.0300(19) 0.026(2) -0.0049(15) -0.0097(15) -0.0014(15) C8 0.037(2) 0.0327(18) 0.0172(16) -0.0032(14) -0.0075(15) 0.0082(16) C13 0.0289(19) 0.0239(17) 0.0152(16) -0.0003(13) 0.0038(13) 0.0001(14) C10 0.0243(18) 0.0287(18) 0.0234(18) 0.0027(14) -0.0028(14) -0.0015(15) C4 0.034(2) 0.0297(18) 0.0210(17) 0.0057(14) 0.0018(15) 0.0000(15) C1 0.034(2) 0.0241(17) 0.0228(17) -0.0011(13) -0.0022(15) -0.0064(15) C11 0.0217(17) 0.0182(15) 0.0181(16) -0.0011(11) -0.0015(12) 0.0046(12) N1 0.0242(16) 0.0171(13) 0.0205(15) -0.0016(11) -0.0023(12) 0.0016(12) N1' 0.0217(17) 0.0182(15) 0.0181(16) -0.0011(11) -0.0015(12) 0.0046(12) C11' 0.0242(16) 0.0171(13) 0.0205(15) -0.0016(11) -0.0023(12) 0.0016(12) _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 Pd1 N1' 2.0289(18) . ? Pd1 C11 2.0289(18) . ? Pd1 C11' 2.0614(18) . ? Pd1 N1 2.0614(18) . ? Pd1 S1 2.2985(9) . ? Pd1 S2 2.3842(9) . ? Pd1 S3 2.8705(10) . ? S2 C14 1.819(3) . ? S2 C13 1.832(3) . ? S1 C12 1.821(3) . ? S1 C17 1.828(4) . ? S3 C16 1.810(4) . ? S3 C15 1.813(3) . ? P1 F1 1.586(2) . ? P1 F3 1.595(2) . ? P1 F2 1.596(2) . ? P1 F4 1.600(2) . ? P1 F5 1.601(2) . ? P1 F6 1.612(2) . ? C16 C17 1.516(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C12 C13 1.515(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C6 C7 1.393(5) . ? C6 N1' 1.406(4) . ? C6 C11 1.406(4) . ? C6 C5 1.463(5) . ? C7 C8 1.377(5) . ? C7 H7A 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C14 C15 1.527(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C5 C11' 1.373(4) . ? C5 N1 1.373(4) . ? C5 C4 1.384(5) . ? C3 C4 1.373(5) . ? C3 C2 1.377(5) . ? C3 H3A 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C2 C1 1.384(4) . ? C2 H2A 0.9500 . ? C9 C8 1.372(5) . ? C9 C10 1.391(5) . ? C9 H9A 0.9500 . ? C8 H8A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C10 N1' 1.379(4) . ? C10 C11 1.379(4) . ? C10 H10A 0.9500 . ? C4 H4A 0.9500 . ? C1 C11' 1.3515 . ? C1 N1 1.3515 . ? C1 H1A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1' Pd1 C11 0.0 . . ? N1' Pd1 C11' 81.14(7) . . ? C11 Pd1 C11' 81.14(7) . . ? N1' Pd1 N1 81.14(7) . . ? C11 Pd1 N1 81.14(7) . . ? C11' Pd1 N1 0.00(11) . . ? N1' Pd1 S1 93.64(6) . . ? C11 Pd1 S1 93.64(6) . . ? C11' Pd1 S1 173.07(6) . . ? N1 Pd1 S1 173.07(6) . . ? N1' Pd1 S2 176.48(5) . . ? C11 Pd1 S2 176.48(5) . . ? C11' Pd1 S2 97.01(5) . . ? N1 Pd1 S2 97.01(5) . . ? S1 Pd1 S2 87.96(3) . . ? N1' Pd1 S3 100.73(5) . . ? C11 Pd1 S3 100.73(5) . . ? C11' Pd1 S3 99.45(5) . . ? N1 Pd1 S3 99.45(5) . . ? S1 Pd1 S3 85.95(3) . . ? S2 Pd1 S3 82.50(3) . . ? C14 S2 C13 102.92(16) . . ? C14 S2 Pd1 105.38(11) . . ? C13 S2 Pd1 104.56(11) . . ? C12 S1 C17 101.25(16) . . ? C12 S1 Pd1 101.35(11) . . ? C17 S1 Pd1 106.43(11) . . ? C16 S3 C15 103.58(16) . . ? C16 S3 Pd1 89.83(12) . . ? C15 S3 Pd1 97.68(11) . . ? F1 P1 F3 179.48(14) . . ? F1 P1 F2 89.89(14) . . ? F3 P1 F2 90.59(13) . . ? F1 P1 F4 90.08(13) . . ? F3 P1 F4 89.70(14) . . ? F2 P1 F4 90.62(13) . . ? F1 P1 F5 90.48(14) . . ? F3 P1 F5 89.73(14) . . ? F2 P1 F5 90.66(13) . . ? F4 P1 F5 178.60(14) . . ? F1 P1 F6 90.67(14) . . ? F3 P1 F6 88.86(13) . . ? F2 P1 F6 179.39(14) . . ? F4 P1 F6 89.62(12) . . ? F5 P1 F6 89.09(13) . . ? C17 C16 S3 117.0(2) . . ? C17 C16 H16A 108.1 . . ? S3 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? S3 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C13 C12 S1 114.9(2) . . ? C13 C12 H12A 108.5 . . ? S1 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? S1 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C7 C6 N1' 119.8(3) . . ? C7 C6 C11 119.8(3) . . ? C7 C6 C5 123.9(3) . . ? N1' C6 C5 116.2(3) . . ? C11 C6 C5 116.2(3) . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C16 C17 S1 116.1(2) . . ? C16 C17 H17A 108.3 . . ? S1 C17 H17A 108.3 . . ? C16 C17 H17B 108.3 . . ? S1 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C15 C14 S2 117.5(2) . . ? C15 C14 H14A 107.9 . . ? S2 C14 H14A 107.9 . . ? C15 C14 H14B 107.9 . . ? S2 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C11' C5 C4 119.9(3) . . ? N1 C5 C4 119.9(3) . . ? C11' C5 C6 114.8(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 125.3(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C14 C15 S3 113.7(2) . . ? C14 C15 H15A 108.8 . . ? S3 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? S3 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C8 C7 120.0(3) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C12 C13 S2 111.9(2) . . ? C12 C13 H13A 109.2 . . ? S2 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? S2 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N1' C10 C9 120.9(3) . . ? C11 C10 C9 120.9(3) . . ? N1' C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C11' C1 C2 122.02(17) . . ? N1 C1 C2 122.02(17) . . ? C11' C1 H1A 119.0 . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C10 C11 C6 118.6(2) . . ? C10 C11 Pd1 128.41(18) . . ? C6 C11 Pd1 112.82(17) . . ? C1 N1 C5 119.16(16) . . ? C1 N1 Pd1 126.85(5) . . ? C5 N1 Pd1 113.82(18) . . ? C10 N1' C6 118.6(2) . . ? C10 N1' Pd1 128.41(18) . . ? C6 N1' Pd1 112.82(17) . . ? C1 C11' C5 119.16(16) . . ? C1 C11' Pd1 126.85(5) . . ? C5 C11' Pd1 113.82(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11' Pd1 S2 C14 81.51(13) . . . . ? N1 Pd1 S2 C14 81.51(13) . . . . ? S1 Pd1 S2 C14 -103.33(12) . . . . ? S3 Pd1 S2 C14 -17.15(12) . . . . ? C11' Pd1 S2 C13 -170.37(12) . . . . ? N1 Pd1 S2 C13 -170.37(12) . . . . ? S1 Pd1 S2 C13 4.79(12) . . . . ? S3 Pd1 S2 C13 90.97(12) . . . . ? N1' Pd1 S1 C12 152.57(13) . . . . ? C11 Pd1 S1 C12 152.57(13) . . . . ? S2 Pd1 S1 C12 -24.29(12) . . . . ? S3 Pd1 S1 C12 -106.91(12) . . . . ? N1' Pd1 S1 C17 -101.97(13) . . . . ? C11 Pd1 S1 C17 -101.97(13) . . . . ? S2 Pd1 S1 C17 81.17(12) . . . . ? S3 Pd1 S1 C17 -1.45(12) . . . . ? N1' Pd1 S3 C16 72.18(12) . . . . ? C11 Pd1 S3 C16 72.18(12) . . . . ? C11' Pd1 S3 C16 154.86(12) . . . . ? N1 Pd1 S3 C16 154.86(12) . . . . ? S1 Pd1 S3 C16 -20.76(11) . . . . ? S2 Pd1 S3 C16 -109.24(11) . . . . ? N1' Pd1 S3 C15 175.86(13) . . . . ? C11 Pd1 S3 C15 175.86(13) . . . . ? C11' Pd1 S3 C15 -101.45(13) . . . . ? N1 Pd1 S3 C15 -101.45(13) . . . . ? S1 Pd1 S3 C15 82.92(12) . . . . ? S2 Pd1 S3 C15 -5.55(12) . . . . ? C15 S3 C16 C17 -50.5(3) . . . . ? Pd1 S3 C16 C17 47.3(3) . . . . ? C17 S1 C12 C13 -62.3(3) . . . . ? Pd1 S1 C12 C13 47.2(3) . . . . ? N1' C6 C7 C8 -1.2(5) . . . . ? C11 C6 C7 C8 -1.2(5) . . . . ? C5 C6 C7 C8 176.8(3) . . . . ? S3 C16 C17 S1 -61.0(3) . . . . ? C12 S1 C17 C16 137.0(3) . . . . ? Pd1 S1 C17 C16 31.5(3) . . . . ? C13 S2 C14 C15 -61.3(3) . . . . ? Pd1 S2 C14 C15 48.0(3) . . . . ? C7 C6 C5 C11' -177.5(3) . . . . ? N1' C6 C5 C11' 0.6(4) . . . . ? C11 C6 C5 C11' 0.6(4) . . . . ? C7 C6 C5 N1 -177.5(3) . . . . ? N1' C6 C5 N1 0.6(4) . . . . ? C11 C6 C5 N1 0.6(4) . . . . ? C7 C6 C5 C4 1.1(5) . . . . ? N1' C6 C5 C4 179.2(3) . . . . ? C11 C6 C5 C4 179.2(3) . . . . ? S2 C14 C15 S3 -58.4(3) . . . . ? C16 S3 C15 C14 125.0(3) . . . . ? Pd1 S3 C15 C14 33.3(2) . . . . ? C4 C3 C2 C1 -1.2(6) . . . . ? C10 C9 C8 C7 0.8(6) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? S1 C12 C13 S2 -46.9(3) . . . . ? C14 S2 C13 C12 131.4(2) . . . . ? Pd1 S2 C13 C12 21.5(3) . . . . ? C8 C9 C10 N1' 0.0(5) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C11' C5 C4 C3 1.3(5) . . . . ? N1 C5 C4 C3 1.3(5) . . . . ? C6 C5 C4 C3 -177.2(3) . . . . ? C3 C2 C1 C11' -0.1(4) . . . . ? C3 C2 C1 N1 -0.1(4) . . . . ? N1' C10 C11 C6 0(50) . . . . ? C9 C10 C11 C6 -1.4(4) . . . . ? N1' C10 C11 Pd1 0(100) . . . . ? C9 C10 C11 Pd1 174.2(2) . . . . ? C7 C6 C11 C10 2.0(4) . . . . ? N1' C6 C11 C10 0(100) . . . . ? C5 C6 C11 C10 -176.2(3) . . . . ? C7 C6 C11 Pd1 -174.3(2) . . . . ? N1' C6 C11 Pd1 0(26) . . . . ? C5 C6 C11 Pd1 7.5(3) . . . . ? N1' Pd1 C11 C10 0(20) . . . . ? C11' Pd1 C11 C10 175.0(2) . . . . ? N1 Pd1 C11 C10 175.0(2) . . . . ? S3 Pd1 C11 C10 -86.9(2) . . . . ? N1' Pd1 C11 C6 0.0(15) . . . . ? C11' Pd1 C11 C6 -9.2(2) . . . . ? N1 Pd1 C11 C6 -9.2(2) . . . . ? S1 Pd1 C11 C6 175.42(17) . . . . ? S3 Pd1 C11 C6 88.87(17) . . . . ? C11' C1 N1 C5 0(10) . . . . ? C2 C1 N1 C5 1.9(2) . . . . ? C11' C1 N1 Pd1 0(100) . . . . ? C2 C1 N1 Pd1 -172.9(2) . . . . ? C11' C5 N1 C1 0(7) . . . . ? C4 C5 N1 C1 -2.5(4) . . . . ? C6 C5 N1 C1 176.14(18) . . . . ? C11' C5 N1 Pd1 0(100) . . . . ? C4 C5 N1 Pd1 173.0(2) . . . . ? C6 C5 N1 Pd1 -8.4(3) . . . . ? N1' Pd1 N1 C1 -175.194(7) . . . . ? C11 Pd1 N1 C1 -175.194(7) . . . . ? C11' Pd1 N1 C1 0.0(7) . . . . ? S2 Pd1 N1 C1 1.79(5) . . . . ? S3 Pd1 N1 C1 85.30(4) . . . . ? N1' Pd1 N1 C5 9.7(2) . . . . ? C11 Pd1 N1 C5 9.7(2) . . . . ? C11' Pd1 N1 C5 0(21) . . . . ? S2 Pd1 N1 C5 -173.29(18) . . . . ? S3 Pd1 N1 C5 -89.77(18) . . . . ? C11 C10 N1' C6 0(50) . . . . ? C9 C10 N1' C6 -1.4(4) . . . . ? C11 C10 N1' Pd1 0(100) . . . . ? C9 C10 N1' Pd1 174.2(2) . . . . ? C7 C6 N1' C10 2.0(4) . . . . ? C11 C6 N1' C10 0(100) . . . . ? C5 C6 N1' C10 -176.2(3) . . . . ? C7 C6 N1' Pd1 -174.3(2) . . . . ? C11 C6 N1' Pd1 0(26) . . . . ? C5 C6 N1' Pd1 7.5(3) . . . . ? C11 Pd1 N1' C10 0(20) . . . . ? C11' Pd1 N1' C10 175.0(2) . . . . ? N1 Pd1 N1' C10 175.0(2) . . . . ? S1 Pd1 N1' C10 -0.4(2) . . . . ? S3 Pd1 N1' C10 -86.9(2) . . . . ? C11 Pd1 N1' C6 0.0(15) . . . . ? C11' Pd1 N1' C6 -9.2(2) . . . . ? N1 Pd1 N1' C6 -9.2(2) . . . . ? S1 Pd1 N1' C6 175.42(17) . . . . ? S3 Pd1 N1' C6 88.87(17) . . . . ? N1 C1 C11' C5 0(10) . . . . ? C2 C1 C11' C5 1.9(2) . . . . ? N1 C1 C11' Pd1 0(100) . . . . ? C2 C1 C11' Pd1 -172.9(2) . . . . ? N1 C5 C11' C1 0(7) . . . . ? C4 C5 C11' C1 -2.5(4) . . . . ? C6 C5 C11' C1 176.14(18) . . . . ? N1 C5 C11' Pd1 0(100) . . . . ? C4 C5 C11' Pd1 173.0(2) . . . . ? C6 C5 C11' Pd1 -8.4(3) . . . . ? N1' Pd1 C11' C1 -175.194(7) . . . . ? C11 Pd1 C11' C1 -175.194(7) . . . . ? N1 Pd1 C11' C1 0.0(7) . . . . ? S2 Pd1 C11' C1 1.79(5) . . . . ? S3 Pd1 C11' C1 85.30(4) . . . . ? N1' Pd1 C11' C5 9.7(2) . . . . ? C11 Pd1 C11' C5 9.7(2) . . . . ? N1 Pd1 C11' C5 0(21) . . . . ? S2 Pd1 C11' C5 -173.29(18) . . . . ? S3 Pd1 C11' C5 -89.77(18) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.347 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.090 data_pd9s3bqz _database_code_depnum_ccdc_archive 'CCDC 666385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 N Pd S3, F6 P' _chemical_formula_sum 'C19 H20 F6 N P Pd S3' _chemical_formula_weight 609.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7612(14) _cell_length_b 10.211(2) _cell_length_c 15.738(3) _cell_angle_alpha 91.67(3) _cell_angle_beta 101.17(3) _cell_angle_gamma 96.64(3) _cell_volume 1057.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 5164 _cell_measurement_theta_min 2.6417 _cell_measurement_theta_max 26.0212 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6027 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.6199 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9072 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3684 _reflns_number_gt 3422 _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^)+(0.0423P)^2^+1.9070P] 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 3684 _refine_ls_number_parameters 287 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Pd1 Pd 0.84038(3) 0.27954(2) 0.226119(14) 0.01856(10) Uani 1 1 d . A . S1 S 0.88248(14) 0.34223(9) 0.37543(5) 0.0280(2) Uani 1 1 d . . . S2 S 0.89588(12) 0.07227(8) 0.26328(5) 0.02207(18) Uani 1 1 d . . . S3 S 1.29682(13) 0.32407(9) 0.27028(6) 0.0319(2) Uani 1 1 d . . . P1 P 0.46392(14) 0.78606(9) 0.38156(6) 0.0286(2) Uani 1 1 d . . . F5 F 0.3931(4) 0.6907(2) 0.45121(15) 0.0494(6) Uani 1 1 d . . . F4 F 0.5304(4) 0.8834(3) 0.31219(18) 0.0569(7) Uani 1 1 d . . . N1 N 0.7932(4) 0.4631(3) 0.17769(18) 0.0210(5) Uani 1 1 d . . . C4 C 1.3221(5) 0.1507(4) 0.2735(3) 0.0361(9) Uani 1 1 d . A . H4A H 1.4358 0.1342 0.2450 0.043 Uiso 1 1 calc R . . H4B H 1.3610 0.1295 0.3350 0.043 Uiso 1 1 calc R . . C5 C 1.3099(7) 0.3654(5) 0.3880(3) 0.0317(12) Uani 0.832(9) 1 d PD A 1 H5A H 1.3220 0.2834 0.4197 0.038 Uiso 0.832(9) 1 calc PR A 1 H5B H 1.4353 0.4266 0.4100 0.038 Uiso 0.832(9) 1 calc PR A 1 C6 C 1.1321(7) 0.4271(6) 0.4095(3) 0.0319(12) Uani 0.832(9) 1 d PD A 1 H6A H 1.1336 0.5150 0.3844 0.038 Uiso 0.832(9) 1 calc PR A 1 H6B H 1.1565 0.4423 0.4733 0.038 Uiso 0.832(9) 1 calc PR A 1 C5A C 1.326(4) 0.405(3) 0.3578(17) 0.0317(12) Uani 0.168(9) 1 d PD A 2 H5C H 1.4669 0.4001 0.3889 0.038 Uiso 0.168(9) 1 calc PR A 2 H5D H 1.3163 0.4979 0.3442 0.038 Uiso 0.168(9) 1 calc PR A 2 C6A C 1.189(4) 0.371(3) 0.4206(14) 0.0319(12) Uani 0.168(9) 1 d PD A 2 H6C H 1.2179 0.4419 0.4668 0.038 Uiso 0.168(9) 1 calc PR A 2 H6D H 1.2283 0.2890 0.4482 0.038 Uiso 0.168(9) 1 calc PR A 2 F3 F 0.6629(6) 0.7196(4) 0.3855(2) 0.0926(13) Uani 1 1 d . . . F2 F 0.2702(6) 0.8570(5) 0.3809(3) 0.1142(18) Uani 1 1 d . . . F1 F 0.5865(6) 0.8826(3) 0.4595(2) 0.0801(11) Uani 1 1 d . . . F6 F 0.3471(8) 0.6882(4) 0.30603(19) 0.1193(19) Uani 1 1 d . . . C14 C 0.7610(5) 0.5765(3) 0.0433(2) 0.0253(7) Uani 1 1 d . . . C19 C 0.7725(5) 0.4619(3) 0.0896(2) 0.0203(6) Uani 1 1 d . A . C7 C 0.7783(4) 0.2244(3) 0.0983(2) 0.0197(6) Uani 1 1 d . . . C10 C 0.7118(5) 0.1976(4) -0.0843(2) 0.0274(7) Uani 1 1 d . A . H10A H 0.6936 0.1870 -0.1456 0.033 Uiso 1 1 calc R . . C18 C 0.7619(4) 0.3355(3) 0.0467(2) 0.0196(6) Uani 1 1 d . A . C11 C 0.7320(5) 0.3256(3) -0.0440(2) 0.0233(7) Uani 1 1 d . . . C2 C 0.9663(6) 0.0780(4) 0.3817(2) 0.0310(8) Uani 1 1 d . A . H2A H 0.9222 -0.0090 0.4025 0.037 Uiso 1 1 calc R . . H2B H 1.1160 0.0954 0.3994 0.037 Uiso 1 1 calc R . . C8 C 0.7527(5) 0.1022(3) 0.0559(2) 0.0252(7) Uani 1 1 d . A . H8A H 0.7582 0.0253 0.0885 0.030 Uiso 1 1 calc R . . C15 C 0.7705(5) 0.6959(3) 0.0912(3) 0.0316(8) Uani 1 1 d . A . H15A H 0.7656 0.7765 0.0627 0.038 Uiso 1 1 calc R . . C3 C 1.1362(5) 0.0546(4) 0.2314(3) 0.0329(8) Uani 1 1 d . A . H3A H 1.1682 -0.0360 0.2435 0.039 Uiso 1 1 calc R . . H3B H 1.1164 0.0624 0.1678 0.039 Uiso 1 1 calc R . . C13 C 0.7379(5) 0.5628(4) -0.0487(2) 0.0292(8) Uani 1 1 d . A . H13A H 0.7326 0.6396 -0.0813 0.035 Uiso 1 1 calc R . . C9 C 0.7185(5) 0.0899(4) -0.0354(2) 0.0296(7) Uani 1 1 d . . . H9A H 0.6996 0.0044 -0.0634 0.036 Uiso 1 1 calc R A . C12 C 0.7232(5) 0.4441(4) -0.0907(2) 0.0276(7) Uani 1 1 d . A . H12A H 0.7070 0.4388 -0.1521 0.033 Uiso 1 1 calc R . . C1 C 0.8716(6) 0.1837(4) 0.4239(2) 0.0314(8) Uani 1 1 d . A . H1A H 0.9406 0.1970 0.4856 0.038 Uiso 1 1 calc R . . H1B H 0.7274 0.1508 0.4225 0.038 Uiso 1 1 calc R . . C17 C 0.7979(5) 0.5773(3) 0.2209(2) 0.0298(8) Uani 1 1 d . A . H17A H 0.8091 0.5783 0.2820 0.036 Uiso 1 1 calc R . . C16 C 0.7869(6) 0.6956(4) 0.1795(3) 0.0341(8) Uani 1 1 d . . . H16A H 0.7906 0.7759 0.2122 0.041 Uiso 1 1 calc R A . 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 Pd1 0.02047(14) 0.01932(14) 0.01665(14) 0.00095(9) 0.00475(9) 0.00377(9) S1 0.0357(5) 0.0300(4) 0.0203(4) -0.0012(3) 0.0100(3) 0.0047(4) S2 0.0232(4) 0.0211(4) 0.0219(4) 0.0036(3) 0.0046(3) 0.0018(3) S3 0.0231(4) 0.0369(5) 0.0368(5) 0.0155(4) 0.0077(4) 0.0015(4) P1 0.0324(5) 0.0309(5) 0.0224(4) 0.0041(4) 0.0059(4) 0.0016(4) F5 0.0639(16) 0.0477(14) 0.0311(12) 0.0120(10) 0.0062(11) -0.0125(12) F4 0.0549(16) 0.0685(18) 0.0547(16) 0.0325(14) 0.0247(13) 0.0082(13) N1 0.0151(13) 0.0233(14) 0.0250(14) 0.0015(11) 0.0047(10) 0.0029(10) C4 0.0201(17) 0.040(2) 0.052(2) 0.0102(18) 0.0104(16) 0.0101(15) C5 0.026(2) 0.039(3) 0.027(3) 0.007(2) 0.000(2) -0.0022(19) C6 0.029(2) 0.034(3) 0.027(2) -0.001(2) -0.0019(18) -0.004(2) C5A 0.026(2) 0.039(3) 0.027(3) 0.007(2) 0.000(2) -0.0022(19) C6A 0.029(2) 0.034(3) 0.027(2) -0.001(2) -0.0019(18) -0.004(2) F3 0.098(3) 0.133(3) 0.075(2) 0.040(2) 0.043(2) 0.082(3) F2 0.090(3) 0.185(4) 0.112(3) 0.103(3) 0.068(2) 0.093(3) F1 0.120(3) 0.0552(18) 0.0534(17) -0.0140(14) 0.0165(18) -0.0323(18) F6 0.173(4) 0.121(3) 0.0282(15) -0.0116(17) -0.005(2) -0.084(3) C14 0.0146(15) 0.0258(17) 0.0368(19) 0.0078(14) 0.0061(13) 0.0048(12) C19 0.0132(14) 0.0229(16) 0.0256(16) 0.0018(13) 0.0060(12) 0.0017(12) C7 0.0143(14) 0.0224(15) 0.0222(15) 0.0016(12) 0.0035(12) 0.0016(12) C10 0.0277(18) 0.039(2) 0.0177(15) -0.0025(14) 0.0062(13) 0.0089(15) C18 0.0122(14) 0.0254(16) 0.0220(15) 0.0014(13) 0.0035(11) 0.0048(12) C11 0.0147(15) 0.0345(18) 0.0221(16) 0.0037(13) 0.0058(12) 0.0054(13) C2 0.040(2) 0.0297(18) 0.0223(17) 0.0066(14) 0.0047(15) 0.0004(15) C8 0.0273(17) 0.0233(16) 0.0240(16) -0.0007(13) 0.0043(13) 0.0010(13) C15 0.0244(18) 0.0202(17) 0.052(2) 0.0109(15) 0.0096(16) 0.0046(13) C3 0.0273(18) 0.036(2) 0.039(2) 0.0019(16) 0.0099(15) 0.0127(15) C13 0.0217(17) 0.036(2) 0.0323(18) 0.0169(15) 0.0080(14) 0.0062(14) C9 0.0278(18) 0.0325(18) 0.0277(18) -0.0090(14) 0.0057(14) 0.0031(14) C12 0.0187(16) 0.041(2) 0.0246(17) 0.0098(15) 0.0047(13) 0.0073(14) C1 0.036(2) 0.038(2) 0.0209(16) 0.0055(14) 0.0101(14) 0.0007(16) C17 0.0334(19) 0.0241(17) 0.0315(18) -0.0059(14) 0.0044(15) 0.0073(14) C16 0.035(2) 0.0220(17) 0.044(2) -0.0055(15) 0.0070(16) 0.0035(15) _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 Pd1 C7 2.023(3) . ? Pd1 N1 2.080(3) . ? Pd1 S2 2.2657(10) . ? Pd1 S1 2.3714(10) . ? S1 C6 1.781(4) . ? S1 C1 1.809(4) . ? S1 C6A 2.04(3) . ? S2 C3 1.817(4) . ? S2 C2 1.829(3) . ? S3 C5A 1.55(3) . ? S3 C4 1.799(4) . ? S3 C5 1.871(5) . ? P1 F6 1.556(3) . ? P1 F2 1.567(3) . ? P1 F3 1.567(3) . ? P1 F1 1.584(3) . ? P1 F4 1.591(2) . ? P1 F5 1.593(2) . ? N1 C17 1.326(4) . ? N1 C19 1.365(4) . ? C4 C3 1.528(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5A C6A 1.502(18) . ? C5A H5C 0.9900 . ? C5A H5D 0.9900 . ? C6A H6C 0.9900 . ? C6A H6D 0.9900 . ? C14 C19 1.399(5) . ? C14 C15 1.403(5) . ? C14 C13 1.427(5) . ? C19 C18 1.427(4) . ? C7 C8 1.373(5) . ? C7 C18 1.416(5) . ? C10 C9 1.361(5) . ? C10 C11 1.416(5) . ? C10 H10A 0.9500 . ? C18 C11 1.402(4) . ? C11 C12 1.436(5) . ? C2 C1 1.517(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C8 C9 1.410(5) . ? C8 H8A 0.9500 . ? C15 C16 1.372(6) . ? C15 H15A 0.9500 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C13 C12 1.348(5) . ? C13 H13A 0.9500 . ? C9 H9A 0.9500 . ? C12 H12A 0.9500 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C17 C16 1.393(5) . ? C17 H17A 0.9500 . ? C16 H16A 0.9500 . ? 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 C7 Pd1 N1 81.91(12) . . ? C7 Pd1 S2 91.75(10) . . ? N1 Pd1 S2 173.37(8) . . ? C7 Pd1 S1 175.05(9) . . ? N1 Pd1 S1 97.54(8) . . ? S2 Pd1 S1 88.94(4) . . ? C6 S1 C1 108.7(2) . . ? C1 S1 C6A 89.3(8) . . ? C6 S1 Pd1 107.56(15) . . ? C1 S1 Pd1 101.88(12) . . ? C6A S1 Pd1 105.2(7) . . ? C3 S2 C2 102.19(18) . . ? C3 S2 Pd1 103.01(13) . . ? C2 S2 Pd1 106.58(13) . . ? C5A S3 C4 117.9(11) . . ? C4 S3 C5 100.2(2) . . ? F6 P1 F2 90.9(3) . . ? F6 P1 F3 91.6(3) . . ? F2 P1 F3 177.5(3) . . ? F6 P1 F1 178.4(3) . . ? F2 P1 F1 90.4(3) . . ? F3 P1 F1 87.1(2) . . ? F6 P1 F4 89.28(18) . . ? F2 P1 F4 89.93(17) . . ? F3 P1 F4 90.00(18) . . ? F1 P1 F4 91.57(17) . . ? F6 P1 F5 90.92(16) . . ? F2 P1 F5 88.72(17) . . ? F3 P1 F5 91.34(18) . . ? F1 P1 F5 88.26(15) . . ? F4 P1 F5 178.64(16) . . ? C17 N1 C19 118.7(3) . . ? C17 N1 Pd1 128.8(2) . . ? C19 N1 Pd1 112.3(2) . . ? C3 C4 S3 117.1(3) . . ? C3 C4 H4A 108.0 . . ? S3 C4 H4A 108.0 . . ? C3 C4 H4B 108.0 . . ? S3 C4 H4B 108.0 . . ? H4A C4 H4B 107.3 . . ? C6 C5 S3 115.7(3) . . ? C6 C5 H5A 108.4 . . ? S3 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? S3 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C5 C6 S1 119.1(4) . . ? C5 C6 H6A 107.5 . . ? S1 C6 H6A 107.5 . . ? C5 C6 H6B 107.5 . . ? S1 C6 H6B 107.5 . . ? H6A C6 H6B 107.0 . . ? C6A C5A S3 121(2) . . ? C6A C5A H5C 107.2 . . ? S3 C5A H5C 107.2 . . ? C6A C5A H5D 107.2 . . ? S3 C5A H5D 107.2 . . ? H5C C5A H5D 106.8 . . ? C5A C6A S1 118.7(17) . . ? C5A C6A H6C 107.6 . . ? S1 C6A H6C 107.6 . . ? C5A C6A H6D 107.6 . . ? S1 C6A H6D 107.6 . . ? H6C C6A H6D 107.1 . . ? C19 C14 C15 117.1(3) . . ? C19 C14 C13 117.7(3) . . ? C15 C14 C13 125.3(3) . . ? N1 C19 C14 122.7(3) . . ? N1 C19 C18 115.9(3) . . ? C14 C19 C18 121.4(3) . . ? C8 C7 C18 117.5(3) . . ? C8 C7 Pd1 131.4(2) . . ? C18 C7 Pd1 111.1(2) . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C11 C18 C7 122.7(3) . . ? C11 C18 C19 119.2(3) . . ? C7 C18 C19 118.1(3) . . ? C18 C11 C10 117.4(3) . . ? C18 C11 C12 118.9(3) . . ? C10 C11 C12 123.7(3) . . ? C1 C2 S2 112.3(3) . . ? C1 C2 H2A 109.1 . . ? S2 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S2 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C4 C3 S2 118.1(3) . . ? C4 C3 H3A 107.8 . . ? S2 C3 H3A 107.8 . . ? C4 C3 H3B 107.8 . . ? S2 C3 H3B 107.8 . . ? H3A C3 H3B 107.1 . . ? C12 C13 C14 122.0(3) . . ? C12 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C2 C1 S1 115.7(2) . . ? C2 C1 H1A 108.3 . . ? S1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? S1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? N1 C17 C16 122.1(3) . . ? N1 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C6 -77.4(2) . . . . ? S2 Pd1 S1 C6 101.2(2) . . . . ? N1 Pd1 S1 C1 168.43(15) . . . . ? S2 Pd1 S1 C1 -12.96(13) . . . . ? N1 Pd1 S1 C6A -99.0(9) . . . . ? S2 Pd1 S1 C6A 79.6(9) . . . . ? C7 Pd1 S2 C3 71.70(16) . . . . ? S1 Pd1 S2 C3 -113.20(13) . . . . ? C7 Pd1 S2 C2 178.86(15) . . . . ? S1 Pd1 S2 C2 -6.04(13) . . . . ? C7 Pd1 N1 C17 178.1(3) . . . . ? S1 Pd1 N1 C17 3.0(3) . . . . ? C7 Pd1 N1 C19 -8.0(2) . . . . ? S1 Pd1 N1 C19 177.01(19) . . . . ? C5A S3 C4 C3 119.0(10) . . . . ? C5 S3 C4 C3 111.7(3) . . . . ? C5A S3 C5 C6 76(3) . . . . ? C4 S3 C5 C6 -123.8(4) . . . . ? S3 C5 C6 S1 56.4(6) . . . . ? C1 S1 C6 C5 59.8(5) . . . . ? C6A S1 C6 C5 36.9(18) . . . . ? Pd1 S1 C6 C5 -49.7(5) . . . . ? C4 S3 C5A C6A -61(3) . . . . ? C5 S3 C5A C6A -38(2) . . . . ? S3 C5A C6A S1 -48(4) . . . . ? C6 S1 C6A C5A -75(3) . . . . ? C1 S1 C6A C5A 127(2) . . . . ? Pd1 S1 C6A C5A 25(3) . . . . ? C17 N1 C19 C14 1.6(5) . . . . ? Pd1 N1 C19 C14 -173.1(2) . . . . ? C17 N1 C19 C18 -178.0(3) . . . . ? Pd1 N1 C19 C18 7.3(3) . . . . ? C15 C14 C19 N1 -0.4(5) . . . . ? C13 C14 C19 N1 -179.5(3) . . . . ? C15 C14 C19 C18 179.3(3) . . . . ? C13 C14 C19 C18 0.1(5) . . . . ? N1 Pd1 C7 C8 -173.7(3) . . . . ? S2 Pd1 C7 C8 8.2(3) . . . . ? N1 Pd1 C7 C18 6.9(2) . . . . ? S2 Pd1 C7 C18 -171.1(2) . . . . ? C8 C7 C18 C11 -3.5(5) . . . . ? Pd1 C7 C18 C11 176.0(2) . . . . ? C8 C7 C18 C19 175.3(3) . . . . ? Pd1 C7 C18 C19 -5.3(3) . . . . ? N1 C19 C18 C11 177.3(3) . . . . ? C14 C19 C18 C11 -2.3(4) . . . . ? N1 C19 C18 C7 -1.5(4) . . . . ? C14 C19 C18 C7 178.9(3) . . . . ? C7 C18 C11 C10 1.9(5) . . . . ? C19 C18 C11 C10 -176.8(3) . . . . ? C7 C18 C11 C12 -178.1(3) . . . . ? C19 C18 C11 C12 3.1(4) . . . . ? C9 C10 C11 C18 1.0(5) . . . . ? C9 C10 C11 C12 -178.9(3) . . . . ? C3 S2 C2 C1 136.7(3) . . . . ? Pd1 S2 C2 C1 29.0(3) . . . . ? C18 C7 C8 C9 2.1(5) . . . . ? Pd1 C7 C8 C9 -177.2(3) . . . . ? C19 C14 C15 C16 -1.1(5) . . . . ? C13 C14 C15 C16 178.0(3) . . . . ? S3 C4 C3 S2 -52.0(4) . . . . ? C2 S2 C3 C4 -50.4(3) . . . . ? Pd1 S2 C3 C4 60.1(3) . . . . ? C19 C14 C13 C12 1.3(5) . . . . ? C15 C14 C13 C12 -177.8(3) . . . . ? C11 C10 C9 C8 -2.4(5) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C14 C13 C12 C11 -0.5(5) . . . . ? C18 C11 C12 C13 -1.8(5) . . . . ? C10 C11 C12 C13 178.1(3) . . . . ? S2 C2 C1 S1 -44.4(3) . . . . ? C6 S1 C1 C2 -77.6(3) . . . . ? C6A S1 C1 C2 -69.7(8) . . . . ? Pd1 S1 C1 C2 35.7(3) . . . . ? C19 N1 C17 C16 -1.4(5) . . . . ? Pd1 N1 C17 C16 172.2(3) . . . . ? C14 C15 C16 C17 1.3(6) . . . . ? N1 C17 C16 C15 0.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.036 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.085 data_pt9s3bqy _database_code_depnum_ccdc_archive 'CCDC 666386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 N Pt S3, F6 P ' _chemical_formula_sum 'C19 H20 F6 N P Pt S3' _chemical_formula_weight 698.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.793(3) _cell_length_b 11.925(2) _cell_length_c 12.317(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.33(3) _cell_angle_gamma 90.00 _cell_volume 2175.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 9640 _cell_measurement_theta_min 3.1005 _cell_measurement_theta_max 26.0212 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 6.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2386 _exptl_absorpt_correction_T_max 0.4385 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.6199 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18144 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3848 _reflns_number_gt 3432 _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^)+(0.0281P)^2^+24.3395P] 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 3848 _refine_ls_number_parameters 293 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 0.20566(2) 0.06987(2) 0.63453(3) 0.02426(11) Uani 1 1 d . A . S1 S 0.32845(15) 0.1308(2) 0.5861(2) 0.0370(5) Uani 1 1 d D . . S2 S 0.28610(15) -0.08505(18) 0.7158(2) 0.0366(5) Uani 1 1 d D . . P1 P 0.32146(16) 0.9293(2) 0.2350(2) 0.0373(5) Uani 1 1 d . . . F1 F 0.3027(5) 1.0149(6) 0.3240(6) 0.0682(19) Uani 1 1 d . . . F2 F 0.3392(4) 0.8445(5) 0.1456(6) 0.0600(17) Uani 1 1 d . . . F3 F 0.2425(4) 0.8526(6) 0.2432(6) 0.0625(18) Uani 1 1 d . . . F4 F 0.4008(4) 1.0075(5) 0.2259(7) 0.0662(19) Uani 1 1 d . . . F5 F 0.3905(5) 0.8630(7) 0.3387(6) 0.075(2) Uani 1 1 d . . . F6 F 0.2521(4) 0.9964(7) 0.1314(7) 0.075(2) Uani 1 1 d . . . C1 C 0.3901(10) -0.0009(12) 0.5953(10) 0.044(3) Uani 0.841(5) 1 d PD A 1 H1A H 0.3598 -0.0456 0.5247 0.052 Uiso 0.841(5) 1 calc PR A 1 H1B H 0.4519 0.0162 0.5974 0.052 Uiso 0.841(5) 1 calc PR A 1 C2 C 0.3958(12) -0.0683(19) 0.697(3) 0.051(4) Uani 0.841(5) 1 d PD A 1 H2A H 0.4387 -0.0324 0.7667 0.061 Uiso 0.841(5) 1 calc PR A 1 H2B H 0.4199 -0.1434 0.6889 0.061 Uiso 0.841(5) 1 calc PR A 1 S3 S 0.4320(2) 0.1214(3) 0.9234(3) 0.0431(7) Uani 0.841(5) 1 d P A 1 C6 C 0.4052(8) 0.2168(10) 0.7015(9) 0.053(3) Uani 0.841(5) 1 d P A 1 H6A H 0.4669 0.1869 0.7182 0.064 Uiso 0.841(5) 1 calc PR A 1 H6B H 0.4044 0.2934 0.6700 0.064 Uiso 0.841(5) 1 calc PR A 1 C5 C 0.3905(7) 0.2282(8) 0.8149(8) 0.042(2) Uani 0.841(5) 1 d P A 1 H5A H 0.3247 0.2347 0.7978 0.051 Uiso 0.841(5) 1 calc PR A 1 H5B H 0.4179 0.3001 0.8499 0.051 Uiso 0.841(5) 1 calc PR A 1 C4 C 0.3335(8) 0.0454(10) 0.9247(10) 0.041(3) Uani 0.841(5) 1 d P A 1 H4A H 0.3361 0.0395 1.0060 0.050 Uiso 0.841(5) 1 calc PR A 1 H4B H 0.2794 0.0904 0.8823 0.050 Uiso 0.841(5) 1 calc PR A 1 C3 C 0.3203(7) -0.0723(9) 0.8728(9) 0.050(3) Uani 0.841(5) 1 d P A 1 H3A H 0.2745 -0.1109 0.8974 0.059 Uiso 0.841(5) 1 calc PR A 1 H3B H 0.3778 -0.1137 0.9075 0.059 Uiso 0.841(5) 1 calc PR A 1 C1A C 0.397(6) 0.005(5) 0.637(6) 0.044(3) Uani 0.159(5) 1 d PD A 2 H1C H 0.3982 -0.0279 0.5635 0.052 Uiso 0.159(5) 1 calc PR A 2 H1D H 0.4585 0.0373 0.6740 0.052 Uiso 0.159(5) 1 calc PR A 2 C2A C 0.400(6) -0.094(13) 0.708(19) 0.051(4) Uani 0.159(5) 1 d PD A 2 H2C H 0.4477 -0.0879 0.7849 0.061 Uiso 0.159(5) 1 calc PR A 2 H2D H 0.4087 -0.1634 0.6689 0.061 Uiso 0.159(5) 1 calc PR A 2 S3A S 0.3304(10) 0.1465(14) 0.8748(13) 0.0431(7) Uani 0.159(5) 1 d P A 2 C6A C 0.4052(8) 0.2168(10) 0.7015(9) 0.053(3) Uani 0.159(5) 1 d P A 2 H6C H 0.4669 0.1869 0.7182 0.064 Uiso 0.159(5) 1 calc PR A 2 H6D H 0.4044 0.2934 0.6700 0.064 Uiso 0.159(5) 1 calc PR A 2 C5A C 0.3905(7) 0.2282(8) 0.8149(8) 0.042(2) Uani 0.159(5) 1 d P A 2 H5C H 0.3654 0.3044 0.8133 0.051 Uiso 0.159(5) 1 calc PR A 2 H5D H 0.4521 0.2306 0.8737 0.051 Uiso 0.159(5) 1 calc PR A 2 C4A C 0.376(4) 0.018(6) 0.908(6) 0.041(3) Uani 0.159(5) 1 d P A 2 H4C H 0.4246 0.0111 0.8744 0.050 Uiso 0.159(5) 1 calc PR A 2 H4D H 0.4055 0.0140 0.9932 0.050 Uiso 0.159(5) 1 calc PR A 2 C3A C 0.3203(7) -0.0723(9) 0.8728(9) 0.050(3) Uani 0.159(5) 1 d P A 2 H3C H 0.2665 -0.0624 0.8954 0.059 Uiso 0.159(5) 1 calc PR A 2 H3D H 0.3522 -0.1413 0.9103 0.059 Uiso 0.159(5) 1 calc PR A 2 C7 C 0.0933(5) 0.0166(6) 0.6634(6) 0.0210(15) Uani 1 1 d . . . N1 N 0.1219(5) 0.2000(6) 0.5555(6) 0.0331(16) Uani 1 1 d . . . C8 C 0.0758(5) -0.0791(7) 0.7121(7) 0.0265(17) Uani 1 1 d . A . H8A H 0.1225 -0.1331 0.7411 0.032 Uiso 1 1 calc R . . C9 C -0.0084(6) -0.1007(7) 0.7208(7) 0.0313(19) Uani 1 1 d . . . H9A H -0.0179 -0.1695 0.7538 0.038 Uiso 1 1 calc R A . C10 C -0.0777(6) -0.0250(8) 0.6830(7) 0.033(2) Uani 1 1 d . A . H10A H -0.1336 -0.0391 0.6933 0.040 Uiso 1 1 calc R . . C11 C -0.0646(5) 0.0740(7) 0.6287(7) 0.0283(17) Uani 1 1 d . . . C12 C -0.1333(6) 0.1574(8) 0.5793(7) 0.035(2) Uani 1 1 d . A . H12A H -0.1905 0.1488 0.5879 0.041 Uiso 1 1 calc R . . C13 C -0.1194(6) 0.2476(8) 0.5211(8) 0.038(2) Uani 1 1 d . . . H13A H -0.1675 0.2986 0.4872 0.046 Uiso 1 1 calc R A . C14 C -0.0332(5) 0.2678(7) 0.5094(7) 0.0294(18) Uani 1 1 d . A . C15 C -0.0140(6) 0.3581(7) 0.4489(7) 0.036(2) Uani 1 1 d . . . H15A H -0.0592 0.4117 0.4115 0.043 Uiso 1 1 calc R A . C16 C 0.0716(7) 0.3678(8) 0.4447(8) 0.042(2) Uani 1 1 d . A . H16A H 0.0854 0.4288 0.4042 0.051 Uiso 1 1 calc R . . C17 C 0.1391(6) 0.2887(7) 0.4996(8) 0.035(2) Uani 1 1 d . A . H17A H 0.1980 0.2983 0.4968 0.041 Uiso 1 1 calc R . . C18 C 0.0210(5) 0.0922(6) 0.6201(6) 0.0235(16) Uani 1 1 d . A . C19 C 0.0354(5) 0.1902(7) 0.5619(7) 0.0274(18) Uani 1 1 d . A . 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 0.02313(16) 0.02293(16) 0.02515(18) 0.00047(13) 0.00639(12) 0.00130(13) S1 0.0334(11) 0.0443(13) 0.0330(12) 0.0011(10) 0.0112(9) -0.0048(10) S2 0.0288(11) 0.0264(11) 0.0506(14) 0.0011(10) 0.0086(10) 0.0041(9) P1 0.0309(11) 0.0337(12) 0.0448(14) -0.0065(11) 0.0100(10) -0.0027(10) F1 0.074(4) 0.057(4) 0.077(5) -0.031(4) 0.030(4) -0.012(3) F2 0.072(4) 0.046(3) 0.081(5) -0.018(3) 0.049(4) -0.013(3) F3 0.059(4) 0.061(4) 0.084(5) -0.021(4) 0.046(4) -0.022(3) F4 0.042(3) 0.047(4) 0.103(5) -0.003(4) 0.017(3) -0.013(3) F5 0.065(4) 0.093(6) 0.060(4) 0.024(4) 0.013(3) 0.016(4) F6 0.053(4) 0.085(5) 0.080(5) 0.025(4) 0.012(4) 0.019(4) C1 0.024(5) 0.079(8) 0.029(7) -0.009(7) 0.009(6) 0.019(5) C2 0.036(6) 0.036(14) 0.083(11) 0.010(9) 0.024(7) 0.010(6) S3 0.0408(15) 0.0427(16) 0.0359(15) 0.0010(12) 0.0009(12) -0.0063(13) C6 0.067(7) 0.049(6) 0.045(6) -0.004(5) 0.020(5) -0.016(6) C5 0.054(6) 0.027(5) 0.042(6) -0.004(4) 0.013(5) -0.009(4) C4 0.036(6) 0.053(7) 0.037(6) 0.002(5) 0.016(5) -0.005(6) C3 0.045(6) 0.045(6) 0.047(6) 0.012(5) 0.001(5) -0.002(5) C1A 0.024(5) 0.079(8) 0.029(7) -0.009(7) 0.009(6) 0.019(5) C2A 0.036(6) 0.036(14) 0.083(11) 0.010(9) 0.024(7) 0.010(6) S3A 0.0408(15) 0.0427(16) 0.0359(15) 0.0010(12) 0.0009(12) -0.0063(13) C6A 0.067(7) 0.049(6) 0.045(6) -0.004(5) 0.020(5) -0.016(6) C5A 0.054(6) 0.027(5) 0.042(6) -0.004(4) 0.013(5) -0.009(4) C4A 0.036(6) 0.053(7) 0.037(6) 0.002(5) 0.016(5) -0.005(6) C3A 0.045(6) 0.045(6) 0.047(6) 0.012(5) 0.001(5) -0.002(5) C7 0.023(4) 0.020(4) 0.018(4) -0.004(3) 0.005(3) -0.003(3) N1 0.037(4) 0.031(4) 0.029(4) -0.001(3) 0.010(3) -0.002(3) C8 0.026(4) 0.023(4) 0.025(4) -0.003(3) 0.001(3) -0.001(3) C9 0.037(5) 0.032(5) 0.022(4) -0.001(3) 0.006(4) -0.010(4) C10 0.031(4) 0.047(5) 0.022(4) -0.002(4) 0.009(4) -0.013(4) C11 0.028(4) 0.039(5) 0.017(4) -0.001(4) 0.006(3) 0.000(4) C12 0.023(4) 0.044(5) 0.033(5) -0.003(4) 0.005(4) 0.006(4) C13 0.033(5) 0.042(5) 0.035(5) -0.004(4) 0.004(4) 0.010(4) C14 0.030(4) 0.030(4) 0.022(4) -0.003(3) 0.001(3) 0.004(3) C15 0.049(5) 0.023(4) 0.030(5) 0.008(4) 0.005(4) 0.017(4) C16 0.054(6) 0.032(5) 0.037(5) 0.008(4) 0.009(5) -0.003(4) C17 0.042(5) 0.026(4) 0.037(5) 0.011(4) 0.016(4) 0.003(4) C18 0.022(4) 0.027(4) 0.020(4) -0.005(3) 0.004(3) 0.001(3) C19 0.030(4) 0.027(4) 0.019(4) -0.004(3) 0.002(3) 0.001(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 C7 2.030(8) . ? Pt1 N1 2.052(7) . ? Pt1 S2 2.268(2) . ? Pt1 S1 2.334(2) . ? S1 C1A 1.83(2) . ? S1 C6 1.828(11) . ? S1 C1 1.831(11) . ? S2 C3 1.824(11) . ? S2 C2 1.839(11) . ? S2 C2A 1.84(2) . ? P1 F5 1.574(7) . ? P1 F3 1.578(6) . ? P1 F6 1.581(7) . ? P1 F2 1.591(6) . ? P1 F4 1.597(6) . ? P1 F1 1.599(7) . ? C1 C2 1.46(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? S3 C5 1.797(10) . ? S3 C4 1.805(12) . ? C6 C5 1.499(14) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C4 C3 1.526(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C1A C2A 1.46(3) . ? C1A H1C 0.9900 . ? C1A H1D 0.9900 . ? C2A H2C 0.9900 . ? C2A H2D 0.9900 . ? S3A C4A 1.68(7) . ? C4A H4C 0.9900 . ? C4A H4D 0.9900 . ? C7 C8 1.362(11) . ? C7 C18 1.405(11) . ? N1 C17 1.340(11) . ? N1 C19 1.401(11) . ? C8 C9 1.394(12) . ? C8 H8A 0.9500 . ? C9 C10 1.369(13) . ? C9 H9A 0.9500 . ? C10 C11 1.407(12) . ? C10 H10A 0.9500 . ? C11 C18 1.410(11) . ? C11 C12 1.442(12) . ? C12 C13 1.352(13) . ? C12 H12A 0.9500 . ? C13 C14 1.438(13) . ? C13 H13A 0.9500 . ? C14 C19 1.401(11) . ? C14 C15 1.401(12) . ? C15 C16 1.375(14) . ? C15 H15A 0.9500 . ? C16 C17 1.408(13) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.430(11) . ? 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 C7 Pt1 N1 82.0(3) . . ? C7 Pt1 S2 93.3(2) . . ? N1 Pt1 S2 174.4(2) . . ? C7 Pt1 S1 175.6(2) . . ? N1 Pt1 S1 95.7(2) . . ? S2 Pt1 S1 88.79(9) . . ? C1A S1 C6 92(3) . . ? C6 S1 C1 103.8(6) . . ? C1A S1 Pt1 96(3) . . ? C6 S1 Pt1 111.2(4) . . ? C1 S1 Pt1 100.8(5) . . ? C3 S2 C2 100.4(12) . . ? C3 S2 C2A 97(7) . . ? C3 S2 Pt1 108.3(4) . . ? C2 S2 Pt1 105.3(4) . . ? C2A S2 Pt1 115(2) . . ? F5 P1 F3 89.8(4) . . ? F5 P1 F6 179.7(5) . . ? F3 P1 F6 90.2(4) . . ? F5 P1 F2 90.2(4) . . ? F3 P1 F2 90.5(3) . . ? F6 P1 F2 90.1(4) . . ? F5 P1 F4 90.6(4) . . ? F3 P1 F4 179.6(5) . . ? F6 P1 F4 89.4(4) . . ? F2 P1 F4 89.5(4) . . ? F5 P1 F1 90.3(4) . . ? F3 P1 F1 89.3(4) . . ? F6 P1 F1 89.4(4) . . ? F2 P1 F1 179.5(4) . . ? F4 P1 F1 90.7(4) . . ? C2 C1 S1 113.5(11) . . ? C2 C1 H1A 108.9 . . ? S1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? S1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 S2 112.8(13) . . ? C1 C2 H2A 109.0 . . ? S2 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? S2 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C5 S3 C4 105.7(5) . . ? C5 C6 S1 120.0(8) . . ? C5 C6 H6A 107.3 . . ? S1 C6 H6A 107.3 . . ? C5 C6 H6B 107.3 . . ? S1 C6 H6B 107.3 . . ? H6A C6 H6B 106.9 . . ? C6 C5 S3 119.7(8) . . ? C6 C5 H5A 107.4 . . ? S3 C5 H5A 107.4 . . ? C6 C5 H5B 107.4 . . ? S3 C5 H5B 107.4 . . ? H5A C5 H5B 106.9 . . ? C3 C4 S3 116.8(9) . . ? C3 C4 H4A 108.1 . . ? S3 C4 H4A 108.1 . . ? C3 C4 H4B 108.1 . . ? S3 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C3 S2 117.9(7) . . ? C4 C3 H3A 107.8 . . ? S2 C3 H3A 107.8 . . ? C4 C3 H3B 107.8 . . ? S2 C3 H3B 107.8 . . ? H3A C3 H3B 107.2 . . ? C2A C1A S1 139(7) . . ? C2A C1A H1C 102.3 . . ? S1 C1A H1C 102.3 . . ? C2A C1A H1D 102.3 . . ? S1 C1A H1D 102.3 . . ? H1C C1A H1D 104.8 . . ? C1A C2A S2 99(6) . . ? C1A C2A H2C 111.9 . . ? S2 C2A H2C 111.9 . . ? C1A C2A H2D 111.9 . . ? S2 C2A H2D 111.9 . . ? H2C C2A H2D 109.6 . . ? S3A C4A H4C 107.9 . . ? S3A C4A H4D 107.9 . . ? H4C C4A H4D 107.2 . . ? C8 C7 C18 116.3(7) . . ? C8 C7 Pt1 131.5(6) . . ? C18 C7 Pt1 112.2(5) . . ? C17 N1 C19 118.1(7) . . ? C17 N1 Pt1 128.9(6) . . ? C19 N1 Pt1 113.0(5) . . ? C7 C8 C9 122.2(8) . . ? C7 C8 H8A 118.9 . . ? C9 C8 H8A 118.9 . . ? C10 C9 C8 121.6(8) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 118.9(8) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C10 C11 C18 117.9(8) . . ? C10 C11 C12 124.5(8) . . ? C18 C11 C12 117.6(8) . . ? C13 C12 C11 122.3(8) . . ? C13 C12 H12A 118.8 . . ? C11 C12 H12A 118.8 . . ? C12 C13 C14 121.4(8) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C19 C14 C15 118.5(8) . . ? C19 C14 C13 116.7(8) . . ? C15 C14 C13 124.7(8) . . ? C16 C15 C14 118.8(8) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 121.1(8) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? N1 C17 C16 121.3(8) . . ? N1 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C7 C18 C11 123.1(7) . . ? C7 C18 C19 117.7(7) . . ? C11 C18 C19 119.2(7) . . ? N1 C19 C14 122.1(8) . . ? N1 C19 C18 115.1(7) . . ? C14 C19 C18 122.7(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 S1 C1A -172(3) . . . . ? S2 Pt1 S1 C1A 5(3) . . . . ? N1 Pt1 S1 C6 93.2(5) . . . . ? S2 Pt1 S1 C6 -90.2(4) . . . . ? N1 Pt1 S1 C1 -157.2(4) . . . . ? S2 Pt1 S1 C1 19.4(4) . . . . ? C7 Pt1 S2 C3 -76.4(4) . . . . ? S1 Pt1 S2 C3 107.5(4) . . . . ? C7 Pt1 S2 C2 176.8(13) . . . . ? S1 Pt1 S2 C2 0.7(13) . . . . ? C7 Pt1 S2 C2A 176(9) . . . . ? S1 Pt1 S2 C2A 0(9) . . . . ? C1A S1 C1 C2 30(14) . . . . ? C6 S1 C1 C2 71.8(18) . . . . ? Pt1 S1 C1 C2 -43.4(17) . . . . ? S1 C1 C2 S2 49(3) . . . . ? C3 S2 C2 C1 -140(2) . . . . ? Pt1 S2 C2 C1 -28(2) . . . . ? C1A S1 C6 C5 -90(3) . . . . ? C1 S1 C6 C5 -100.3(10) . . . . ? Pt1 S1 C6 C5 7.3(10) . . . . ? S1 C6 C5 S3 82.7(11) . . . . ? C4 S3 C5 C6 -106.8(9) . . . . ? C5 S3 C4 C3 107.4(9) . . . . ? S3 C4 C3 S2 -72.4(10) . . . . ? C2 S2 C3 C4 81.5(11) . . . . ? C2A S2 C3 C4 91(5) . . . . ? Pt1 S2 C3 C4 -28.5(9) . . . . ? C6 S1 C1A C2A 98(19) . . . . ? Pt1 S1 C1A C2A -14(19) . . . . ? C3 S2 C2A C1A -119(12) . . . . ? Pt1 S2 C2A C1A -5(16) . . . . ? N1 Pt1 C7 C8 175.7(8) . . . . ? S2 Pt1 C7 C8 -1.2(7) . . . . ? N1 Pt1 C7 C18 -1.3(5) . . . . ? S2 Pt1 C7 C18 -178.2(5) . . . . ? C7 Pt1 N1 C17 -177.8(8) . . . . ? S1 Pt1 N1 C17 -1.6(8) . . . . ? C7 Pt1 N1 C19 1.1(5) . . . . ? S1 Pt1 N1 C19 177.4(5) . . . . ? C18 C7 C8 C9 -1.2(11) . . . . ? Pt1 C7 C8 C9 -178.2(6) . . . . ? C7 C8 C9 C10 -1.5(13) . . . . ? C8 C9 C10 C11 3.4(12) . . . . ? C9 C10 C11 C18 -2.4(12) . . . . ? C9 C10 C11 C12 176.4(8) . . . . ? C10 C11 C12 C13 -175.4(8) . . . . ? C18 C11 C12 C13 3.3(12) . . . . ? C11 C12 C13 C14 -2.7(14) . . . . ? C12 C13 C14 C19 -0.5(13) . . . . ? C12 C13 C14 C15 178.9(9) . . . . ? C19 C14 C15 C16 -0.8(13) . . . . ? C13 C14 C15 C16 179.8(9) . . . . ? C14 C15 C16 C17 0.2(14) . . . . ? C19 N1 C17 C16 -2.3(13) . . . . ? Pt1 N1 C17 C16 176.6(7) . . . . ? C15 C16 C17 N1 1.4(14) . . . . ? C8 C7 C18 C11 2.1(11) . . . . ? Pt1 C7 C18 C11 179.7(6) . . . . ? C8 C7 C18 C19 -176.1(7) . . . . ? Pt1 C7 C18 C19 1.4(9) . . . . ? C10 C11 C18 C7 -0.3(12) . . . . ? C12 C11 C18 C7 -179.2(7) . . . . ? C10 C11 C18 C19 177.9(7) . . . . ? C12 C11 C18 C19 -0.9(11) . . . . ? C17 N1 C19 C14 1.7(12) . . . . ? Pt1 N1 C19 C14 -177.4(6) . . . . ? C17 N1 C19 C18 178.4(7) . . . . ? Pt1 N1 C19 C18 -0.7(9) . . . . ? C15 C14 C19 N1 -0.1(12) . . . . ? C13 C14 C19 N1 179.3(7) . . . . ? C15 C14 C19 C18 -176.5(8) . . . . ? C13 C14 C19 C18 2.9(12) . . . . ? C7 C18 C19 N1 -0.5(10) . . . . ? C11 C18 C19 N1 -178.8(7) . . . . ? C7 C18 C19 C14 176.2(7) . . . . ? C11 C18 C19 C14 -2.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.594 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.161 data_pdpc9s3 _database_code_depnum_ccdc_archive 'CCDC 666387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H32 P Pd S3), 2(F6 P), C H3 N O2' _chemical_formula_sum 'C55 H67 F12 N O2 P4 Pd2 S6' _chemical_formula_weight 1531.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.830(6) _cell_length_b 11.056(2) _cell_length_c 21.087(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.91(3) _cell_angle_gamma 90.00 _cell_volume 6138(2) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6394 _exptl_absorpt_correction_T_max 0.7065 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18846 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5352 _reflns_number_gt 4752 _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^)+(0.0900P)^2^+56.6081P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5352 _refine_ls_number_parameters 396 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1903 _refine_ls_wR_factor_gt 0.1839 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.100 _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 Pd1 Pd 0.886166(17) 0.19835(4) 0.54858(2) 0.0370(2) Uani 1 1 d . B . P1 P 0.89110(6) 0.00069(15) 0.57690(8) 0.0348(4) Uani 1 1 d D . . S1 S 0.91345(6) 0.19321(16) 0.45216(9) 0.0458(4) Uani 1 1 d . . . S2 S 0.88847(6) 0.41256(15) 0.54427(8) 0.0443(4) Uani 1 1 d . . . S3 S 0.78943(7) 0.22655(19) 0.45355(9) 0.0508(5) Uani 1 1 d . . . C1 C 0.9424(3) 0.3424(8) 0.4601(5) 0.071(2) Uani 1 1 d . B . H1A H 0.9751 0.3399 0.4971 0.085 Uiso 1 1 calc R . . H1B H 0.9500 0.3601 0.4183 0.085 Uiso 1 1 calc R . . C2 C 0.9119(3) 0.4435(8) 0.4728(5) 0.068(2) Uani 1 1 d . B . H2A H 0.8826 0.4583 0.4320 0.082 Uiso 1 1 calc R . . H2B H 0.9329 0.5177 0.4823 0.082 Uiso 1 1 calc R . . C3 C 0.8213(3) 0.4544(7) 0.5081(4) 0.0575(19) Uani 1 1 d . B . H3A H 0.8053 0.4445 0.5435 0.069 Uiso 1 1 calc R . . H3B H 0.8197 0.5415 0.4968 0.069 Uiso 1 1 calc R . . C4 C 0.7892(3) 0.3885(7) 0.4476(4) 0.0524(17) Uani 1 1 d . B . H4A H 0.8007 0.4109 0.4094 0.063 Uiso 1 1 calc R . . H4B H 0.7538 0.4170 0.4370 0.063 Uiso 1 1 calc R . . C5 C 0.8088(3) 0.1736(9) 0.3845(4) 0.065(2) Uani 1 1 d . B . H5A H 0.8090 0.0841 0.3860 0.078 Uiso 1 1 calc R . . H5B H 0.7819 0.1976 0.3426 0.078 Uiso 1 1 calc R . . C6 C 0.8578(3) 0.2125(9) 0.3786(4) 0.061(2) Uani 1 1 d . B . H6A H 0.8551 0.2992 0.3662 0.074 Uiso 1 1 calc R . . H6B H 0.8635 0.1672 0.3411 0.074 Uiso 1 1 calc R . . C7 C 0.8678(3) 0.2119(6) 0.6364(3) 0.0488(17) Uani 1 1 d . . . H7A H 0.8991 0.2334 0.6734 0.059 Uiso 1 1 calc R B . H7B H 0.8436 0.2797 0.6313 0.059 Uiso 1 1 calc R . . C8 C 0.8453(2) 0.1025(6) 0.6569(3) 0.0413(14) Uani 1 1 d . B . C9 C 0.8184(3) 0.1102(7) 0.7025(3) 0.0486(16) Uani 1 1 d . . . H9A H 0.8130 0.1865 0.7197 0.058 Uiso 1 1 calc R B . C10 C 0.8000(3) 0.0067(7) 0.7223(4) 0.0508(17) Uani 1 1 d . B . H10A H 0.7821 0.0120 0.7536 0.061 Uiso 1 1 calc R . . C11 C 0.8070(3) -0.1042(7) 0.6976(3) 0.0506(17) Uani 1 1 d . . . H11A H 0.7932 -0.1743 0.7112 0.061 Uiso 1 1 calc R B . C12 C 0.8341(3) -0.1152(7) 0.6527(3) 0.0479(16) Uani 1 1 d . B . H12A H 0.8397 -0.1923 0.6365 0.057 Uiso 1 1 calc R . . C13 C 0.8528(2) -0.0100(6) 0.6321(3) 0.0367(13) Uani 1 1 d . B . C21 C 0.9432(3) -0.1217(8) 0.4756(5) 0.066(2) Uani 1 1 d . B . H21A H 0.9534 -0.0404 0.4934 0.098 Uiso 1 1 calc R . . H21B H 0.9505 -0.1321 0.4335 0.098 Uiso 1 1 calc R . . H21C H 0.9620 -0.1821 0.5082 0.098 Uiso 1 1 calc R . . C22 C 0.8893(3) -0.1373(7) 0.4634(4) 0.0567(18) Uani 1 1 d . . . C23 C 0.8612(4) -0.2063(8) 0.4037(4) 0.067(2) Uani 1 1 d . B . H23A H 0.8780 -0.2402 0.3751 0.080 Uiso 1 1 calc R . . C24 C 0.8119(4) -0.2200(10) 0.3907(5) 0.080(3) Uani 1 1 d . . . H24A H 0.7939 -0.2620 0.3508 0.096 Uiso 1 1 calc R B . C25 C 0.7841(4) -0.1795(9) 0.4293(5) 0.080(3) Uani 1 1 d . B . H25A H 0.7487 -0.1951 0.4171 0.096 Uiso 1 1 calc R . . C26 C 0.8087(3) -0.1161(8) 0.4860(4) 0.064(2) Uani 1 1 d . . . H26A H 0.7905 -0.0855 0.5135 0.077 Uiso 1 1 calc R B . C27 C 0.8629(3) -0.0957(6) 0.5039(3) 0.0455(15) Uani 1 1 d . B . C28 C 0.9974(9) 0.433(2) 0.7737(10) 0.092(6) Uani 0.50 1 d P A -1 H28A H 1.0169 0.5082 0.7810 0.138 Uiso 0.50 1 calc PR A -1 H28B H 0.9654 0.4438 0.7370 0.138 Uiso 0.50 1 calc PR A -1 H28C H 1.0172 0.3681 0.7620 0.138 Uiso 0.50 1 calc PR A -1 N1 N 0.9857(6) 0.3968(15) 0.8405(16) 0.118(9) Uani 0.50 1 d P A -1 O1 O 0.9716(7) 0.2916(15) 0.8326(10) 0.114(4) Uani 0.50 1 d P A -1 O2 O 0.9885(7) 0.4675(18) 0.8764(10) 0.114(4) Uani 0.50 1 d P A -1 C14 C 0.9302(5) -0.2833(11) 0.6205(7) 0.076(3) Uani 0.772(10) 1 d PD B 3 H14A H 0.9037 -0.2639 0.5782 0.114 Uiso 0.772(10) 1 calc PR B 3 H14B H 0.9146 -0.2987 0.6553 0.114 Uiso 0.772(10) 1 calc PR B 3 H14C H 0.9487 -0.3556 0.6145 0.114 Uiso 0.772(10) 1 calc PR B 3 C15 C 0.9672(4) -0.1769(13) 0.6417(6) 0.063(2) Uani 0.772(10) 1 d PD B 3 C16 C 1.0154(5) -0.2060(15) 0.6801(7) 0.085(4) Uani 0.772(10) 1 d PD B 3 H16A H 1.0247 -0.2883 0.6902 0.102 Uiso 0.772(10) 1 calc PR B 3 C17 C 1.0495(5) -0.1185(15) 0.7035(7) 0.085(4) Uani 0.772(10) 1 d PD B 3 H17A H 1.0824 -0.1413 0.7315 0.102 Uiso 0.772(10) 1 calc PR B 3 C18 C 1.0396(4) 0.0102(17) 0.6891(5) 0.084(5) Uani 0.772(10) 1 d PD B 3 H18A H 1.0644 0.0717 0.7055 0.101 Uiso 0.772(10) 1 calc PR B 3 C19 C 0.9898(4) 0.0328(13) 0.6485(5) 0.063(2) Uani 0.772(10) 1 d PD B 3 H19A H 0.9804 0.1140 0.6354 0.076 Uiso 0.772(10) 1 calc PR B 3 C20 C 0.9537(5) -0.0552(15) 0.6266(9) 0.045(3) Uani 0.772(10) 1 d PD B 3 C14' C 0.9953(15) 0.115(3) 0.666(2) 0.076(3) Uani 0.228(10) 1 d PD B 4 H14D H 0.9758 0.1416 0.6948 0.114 Uiso 0.228(10) 1 calc PR B 4 H14E H 0.9801 0.1492 0.6211 0.114 Uiso 0.228(10) 1 calc PR B 4 H14F H 1.0305 0.1428 0.6851 0.114 Uiso 0.228(10) 1 calc PR B 4 C15' C 0.9943(12) -0.023(3) 0.6617(17) 0.063(2) Uani 0.228(10) 1 d PD B 4 C16' C 1.0368(12) -0.086(3) 0.694(3) 0.085(4) Uani 0.228(10) 1 d PD B 4 H16B H 1.0679 -0.0447 0.7152 0.102 Uiso 0.228(10) 1 calc PR B 4 C17' C 1.0346(11) -0.207(4) 0.694(2) 0.085(4) Uani 0.228(10) 1 d PD B 4 H17B H 1.0640 -0.2501 0.7199 0.102 Uiso 0.228(10) 1 calc PR B 4 C18' C 0.9888(12) -0.276(3) 0.6576(17) 0.084(5) Uani 0.228(10) 1 d PD B 4 H18B H 0.9876 -0.3621 0.6543 0.101 Uiso 0.228(10) 1 calc PR B 4 C19' C 0.9480(11) -0.201(4) 0.629(2) 0.063(2) Uani 0.228(10) 1 d PD B 4 H19B H 0.9152 -0.2374 0.6148 0.076 Uiso 0.228(10) 1 calc PR B 4 C20' C 0.9505(17) -0.080(4) 0.618(4) 0.045(3) Uani 0.228(10) 1 d PD B 4 P2 P 0.84536(10) 0.5082(2) 0.74565(14) 0.0785(8) Uani 1 1 d . . . F1 F 0.8021(2) 0.4158(6) 0.7149(4) 0.110(2) Uani 1 1 d . . . F3 F 0.8045(3) 0.6119(6) 0.7373(5) 0.139(3) Uani 1 1 d . . . F5 F 0.8394(4) 0.4880(6) 0.8164(3) 0.128(3) Uani 1 1 d . . . F2 F 0.8835(3) 0.3997(12) 0.7578(6) 0.215(7) Uani 1 1 d . . . F4 F 0.8511(6) 0.5250(12) 0.6762(6) 0.237(7) Uani 1 1 d . . . F6 F 0.8868(4) 0.6040(11) 0.7757(6) 0.223(7) 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 Pd1 0.0388(3) 0.0430(3) 0.0307(3) 0.00085(19) 0.0133(2) -0.0009(2) P1 0.0263(7) 0.0453(9) 0.0315(8) 0.0021(7) 0.0075(6) 0.0040(6) S1 0.0410(9) 0.0588(11) 0.0397(9) 0.0017(7) 0.0160(7) 0.0048(7) S2 0.0494(9) 0.0414(9) 0.0413(9) -0.0009(7) 0.0137(7) -0.0056(7) S3 0.0403(9) 0.0687(12) 0.0450(10) -0.0075(8) 0.0160(8) -0.0022(8) C1 0.060(5) 0.078(6) 0.089(6) 0.013(5) 0.044(5) -0.007(4) C2 0.062(5) 0.071(5) 0.077(6) 0.024(4) 0.030(4) -0.018(4) C3 0.057(4) 0.051(4) 0.066(5) 0.000(4) 0.021(4) 0.006(3) C4 0.046(4) 0.064(5) 0.045(4) 0.006(3) 0.012(3) 0.011(3) C5 0.049(4) 0.101(7) 0.040(4) -0.017(4) 0.009(3) 0.001(4) C6 0.056(5) 0.095(6) 0.034(4) 0.001(4) 0.017(3) 0.008(4) C7 0.067(5) 0.046(4) 0.036(4) -0.007(3) 0.020(3) 0.002(3) C8 0.043(3) 0.051(4) 0.028(3) 0.006(3) 0.008(3) 0.005(3) C9 0.054(4) 0.058(4) 0.037(4) 0.001(3) 0.020(3) 0.009(3) C10 0.040(4) 0.074(5) 0.042(4) 0.009(3) 0.018(3) 0.005(3) C11 0.040(4) 0.066(5) 0.045(4) 0.013(3) 0.012(3) -0.007(3) C12 0.054(4) 0.048(4) 0.042(4) 0.003(3) 0.016(3) -0.001(3) C13 0.027(3) 0.050(4) 0.031(3) 0.005(3) 0.008(2) 0.004(3) C21 0.057(5) 0.071(5) 0.073(5) -0.002(4) 0.028(4) 0.007(4) C22 0.068(5) 0.059(5) 0.046(4) 0.001(3) 0.021(4) 0.002(4) C23 0.071(6) 0.078(6) 0.049(5) -0.009(4) 0.015(4) -0.005(4) C24 0.078(7) 0.102(8) 0.061(6) -0.020(5) 0.024(5) -0.010(5) C25 0.057(5) 0.094(7) 0.079(7) -0.015(5) 0.008(5) -0.022(5) C26 0.063(5) 0.062(5) 0.057(5) -0.004(4) 0.006(4) -0.013(4) C27 0.050(4) 0.041(4) 0.038(4) 0.000(3) 0.005(3) -0.005(3) C28 0.091(14) 0.111(16) 0.084(16) -0.034(12) 0.044(13) -0.020(13) N1 0.040(8) 0.036(8) 0.26(3) 0.013(12) 0.022(12) 0.007(7) O1 0.092(8) 0.100(9) 0.139(11) 0.001(8) 0.024(7) 0.019(7) O2 0.092(8) 0.100(9) 0.139(11) 0.001(8) 0.024(7) 0.019(7) C14 0.084(8) 0.060(7) 0.089(9) 0.016(6) 0.036(7) 0.023(6) C15 0.052(4) 0.106(8) 0.036(4) 0.009(4) 0.018(4) 0.030(5) C16 0.051(6) 0.167(11) 0.038(5) 0.018(6) 0.018(5) 0.047(6) C17 0.051(6) 0.167(11) 0.038(5) 0.018(6) 0.018(5) 0.047(6) C18 0.040(5) 0.178(15) 0.031(5) -0.011(7) 0.009(4) -0.014(7) C19 0.052(4) 0.106(8) 0.036(4) 0.009(4) 0.018(4) 0.030(5) C20 0.033(4) 0.077(8) 0.023(6) -0.006(5) 0.005(3) 0.009(5) C14' 0.084(8) 0.060(7) 0.089(9) 0.016(6) 0.036(7) 0.023(6) C15' 0.052(4) 0.106(8) 0.036(4) 0.009(4) 0.018(4) 0.030(5) C16' 0.051(6) 0.167(11) 0.038(5) 0.018(6) 0.018(5) 0.047(6) C17' 0.051(6) 0.167(11) 0.038(5) 0.018(6) 0.018(5) 0.047(6) C18' 0.040(5) 0.178(15) 0.031(5) -0.011(7) 0.009(4) -0.014(7) C19' 0.052(4) 0.106(8) 0.036(4) 0.009(4) 0.018(4) 0.030(5) C20' 0.033(4) 0.077(8) 0.023(6) -0.006(5) 0.005(3) 0.009(5) P2 0.0807(16) 0.0862(17) 0.0856(17) -0.0442(14) 0.0504(14) -0.0381(14) F1 0.078(4) 0.084(4) 0.158(6) -0.057(4) 0.023(4) -0.018(3) F3 0.177(8) 0.061(4) 0.179(8) -0.014(4) 0.059(6) 0.009(4) F5 0.206(8) 0.107(5) 0.086(5) -0.020(4) 0.070(5) -0.009(5) F2 0.073(5) 0.281(13) 0.259(12) -0.187(11) 0.010(6) 0.023(6) F4 0.392(18) 0.241(12) 0.161(9) -0.106(9) 0.202(12) -0.182(13) F6 0.175(8) 0.259(12) 0.300(13) -0.213(11) 0.168(9) -0.165(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 Pd1 C7 2.081(7) . ? Pd1 P1 2.2579(17) . ? Pd1 S2 2.3717(18) . ? Pd1 S1 2.3906(18) . ? Pd1 S3 2.804(2) . ? P1 C13 1.819(6) . ? P1 C20 1.825(9) . ? P1 C27 1.827(7) . ? P1 C20' 1.833(18) . ? S1 C6 1.814(8) . ? S1 C1 1.820(9) . ? S2 C3 1.836(8) . ? S2 C2 1.858(8) . ? S3 C4 1.794(8) . ? S3 C5 1.806(8) . ? C1 C2 1.478(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.488(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.474(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.488(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.390(9) . ? C8 C9 1.401(9) . ? C9 C10 1.372(10) . ? C9 H9A 0.9500 . ? C10 C11 1.370(11) . ? C10 H10A 0.9500 . ? C11 C12 1.394(10) . ? C11 H11A 0.9500 . ? C12 C13 1.400(9) . ? C12 H12A 0.9500 . ? C21 C22 1.447(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.373(10) . ? C22 C23 1.463(11) . ? C23 C24 1.319(13) . ? C23 H23A 0.9500 . ? C24 C25 1.367(14) . ? C24 H24A 0.9500 . ? C25 C26 1.362(12) . ? C25 H25A 0.9500 . ? C26 C27 1.449(10) . ? C26 H26A 0.9500 . ? C28 N1 1.60(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N1 O2 1.07(3) . ? N1 O1 1.22(2) . ? C14 C15 1.530(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.363(15) . ? C15 C20 1.406(18) . ? C16 C17 1.332(18) . ? C16 H16A 0.9500 . ? C17 C18 1.46(2) . ? C17 H17A 0.9500 . ? C18 C19 1.396(15) . ? C18 H18A 0.9500 . ? C19 C20 1.37(2) . ? C19 H19A 0.9500 . ? C14' C15' 1.52(2) . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' C16' 1.35(2) . ? C15' C20' 1.42(2) . ? C16' C17' 1.34(2) . ? C16' H16B 0.9500 . ? C17' C18' 1.48(3) . ? C17' H17B 0.9500 . ? C18' C19' 1.38(2) . ? C18' H18B 0.9500 . ? C19' C20' 1.37(3) . ? C19' H19B 0.9500 . ? P2 F4 1.536(9) . ? P2 F6 1.543(7) . ? P2 F1 1.552(6) . ? P2 F2 1.566(10) . ? P2 F5 1.569(7) . ? P2 F3 1.585(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Pd1 P1 81.1(2) . . ? C7 Pd1 S2 88.8(2) . . ? P1 Pd1 S2 167.56(6) . . ? C7 Pd1 S1 175.1(2) . . ? P1 Pd1 S1 101.13(6) . . ? S2 Pd1 S1 88.35(6) . . ? C7 Pd1 S3 99.9(2) . . ? P1 Pd1 S3 104.99(6) . . ? S2 Pd1 S3 83.87(6) . . ? S1 Pd1 S3 83.73(6) . . ? C13 P1 C20 105.0(9) . . ? C13 P1 C27 108.7(3) . . ? C20 P1 C27 110.8(5) . . ? C13 P1 C20' 107(3) . . ? C27 P1 C20' 101.1(17) . . ? C13 P1 Pd1 103.5(2) . . ? C20 P1 Pd1 116.4(7) . . ? C27 P1 Pd1 111.7(2) . . ? C20' P1 Pd1 124(2) . . ? C6 S1 C1 101.6(4) . . ? C6 S1 Pd1 107.8(2) . . ? C1 S1 Pd1 98.8(3) . . ? C3 S2 C2 101.3(4) . . ? C3 S2 Pd1 103.3(3) . . ? C2 S2 Pd1 103.6(3) . . ? C4 S3 C5 105.1(4) . . ? C4 S3 Pd1 98.1(2) . . ? C5 S3 Pd1 94.2(3) . . ? C2 C1 S1 116.0(6) . . ? C2 C1 H1A 108.3 . . ? S1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? S1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C1 C2 S2 112.4(6) . . ? C1 C2 H2A 109.1 . . ? S2 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S2 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S2 118.6(5) . . ? C4 C3 H3A 107.7 . . ? S2 C3 H3A 107.7 . . ? C4 C3 H3B 107.7 . . ? S2 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? C3 C4 S3 116.2(5) . . ? C3 C4 H4A 108.2 . . ? S3 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? S3 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C6 C5 S3 119.9(6) . . ? C6 C5 H5A 107.3 . . ? S3 C5 H5A 107.3 . . ? C6 C5 H5B 107.3 . . ? S3 C5 H5B 107.3 . . ? H5A C5 H5B 106.9 . . ? C5 C6 S1 116.8(6) . . ? C5 C6 H6A 108.1 . . ? S1 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? S1 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 Pd1 116.5(4) . . ? C8 C7 H7A 108.2 . . ? Pd1 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? Pd1 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? C13 C8 C9 119.4(6) . . ? C13 C8 C7 119.4(6) . . ? C9 C8 C7 121.2(6) . . ? C10 C9 C8 119.5(7) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 121.2(6) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C12 120.7(7) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C13 118.4(7) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C8 C13 C12 120.8(6) . . ? C8 C13 P1 111.8(5) . . ? C12 C13 P1 127.3(5) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C21 125.5(7) . . ? C27 C22 C23 117.8(7) . . ? C21 C22 C23 116.7(7) . . ? C24 C23 C22 117.9(8) . . ? C24 C23 H23A 121.1 . . ? C22 C23 H23A 121.1 . . ? C23 C24 C25 126.2(9) . . ? C23 C24 H24A 116.9 . . ? C25 C24 H24A 116.9 . . ? C26 C25 C24 118.0(9) . . ? C26 C25 H25A 121.0 . . ? C24 C25 H25A 121.0 . . ? C25 C26 C27 119.7(8) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? C22 C27 C26 120.4(7) . . ? C22 C27 P1 123.4(6) . . ? C26 C27 P1 115.9(6) . . ? O2 N1 O1 137(3) . . ? O2 N1 C28 117(2) . . ? O1 N1 C28 105(2) . . ? C16 C15 C20 120.0(13) . . ? C16 C15 C14 115.5(13) . . ? C20 C15 C14 124.4(11) . . ? C17 C16 C15 119.6(14) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C18 124.5(11) . . ? C16 C17 H17A 117.8 . . ? C18 C17 H17A 117.8 . . ? C19 C18 C17 112.6(13) . . ? C19 C18 H18A 123.7 . . ? C17 C18 H18A 123.7 . . ? C20 C19 C18 123.7(13) . . ? C20 C19 H19A 118.2 . . ? C18 C19 H19A 118.2 . . ? C19 C20 C15 119.5(9) . . ? C19 C20 P1 114.4(11) . . ? C15 C20 P1 126.1(12) . . ? C16' C15' C20' 121(2) . . ? C16' C15' C14' 119(3) . . ? C20' C15' C14' 119(2) . . ? C17' C16' C15' 119(3) . . ? C17' C16' H16B 120.5 . . ? C15' C16' H16B 120.5 . . ? C16' C17' C18' 123(2) . . ? C16' C17' H17B 118.3 . . ? C18' C17' H17B 118.3 . . ? C19' C18' C17' 112(2) . . ? C19' C18' H18B 124.2 . . ? C17' C18' H18B 124.2 . . ? C20' C19' C18' 126(3) . . ? C20' C19' H19B 117.2 . . ? C18' C19' H19B 117.2 . . ? C19' C20' C15' 115(3) . . ? C19' C20' P1 118(3) . . ? C15' C20' P1 123(2) . . ? F4 P2 F6 90.7(6) . . ? F4 P2 F1 89.3(5) . . ? F6 P2 F1 177.7(6) . . ? F4 P2 F2 88.5(7) . . ? F6 P2 F2 94.7(6) . . ? F1 P2 F2 87.6(4) . . ? F4 P2 F5 178.8(6) . . ? F6 P2 F5 90.1(5) . . ? F1 P2 F5 89.9(4) . . ? F2 P2 F5 90.6(6) . . ? F4 P2 F3 95.7(8) . . ? F6 P2 F3 87.9(6) . . ? F1 P2 F3 89.9(4) . . ? F2 P2 F3 175.0(7) . . ? F5 P2 F3 85.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Pd1 P1 C13 21.7(3) . . . . ? S2 Pd1 P1 C13 58.1(4) . . . . ? S1 Pd1 P1 C13 -162.7(2) . . . . ? S3 Pd1 P1 C13 -76.3(2) . . . . ? C7 Pd1 P1 C20 -92.9(8) . . . . ? S2 Pd1 P1 C20 -56.5(9) . . . . ? S1 Pd1 P1 C20 82.7(8) . . . . ? S3 Pd1 P1 C20 169.1(8) . . . . ? C7 Pd1 P1 C27 138.5(3) . . . . ? S2 Pd1 P1 C27 174.9(3) . . . . ? S1 Pd1 P1 C27 -45.9(3) . . . . ? S3 Pd1 P1 C27 40.5(3) . . . . ? C7 Pd1 P1 C20' -100(3) . . . . ? S2 Pd1 P1 C20' -64(3) . . . . ? S1 Pd1 P1 C20' 76(3) . . . . ? S3 Pd1 P1 C20' 162(3) . . . . ? P1 Pd1 S1 C6 105.1(3) . . . . ? S2 Pd1 S1 C6 -83.1(3) . . . . ? S3 Pd1 S1 C6 1.0(3) . . . . ? P1 Pd1 S1 C1 -149.6(3) . . . . ? S2 Pd1 S1 C1 22.3(3) . . . . ? S3 Pd1 S1 C1 106.3(3) . . . . ? C7 Pd1 S2 C3 -80.9(4) . . . . ? P1 Pd1 S2 C3 -116.8(4) . . . . ? S1 Pd1 S2 C3 103.1(3) . . . . ? S3 Pd1 S2 C3 19.2(3) . . . . ? C7 Pd1 S2 C2 173.8(4) . . . . ? P1 Pd1 S2 C2 137.9(4) . . . . ? S1 Pd1 S2 C2 -2.2(3) . . . . ? S3 Pd1 S2 C2 -86.1(3) . . . . ? C7 Pd1 S3 C4 88.3(3) . . . . ? P1 Pd1 S3 C4 171.6(2) . . . . ? S2 Pd1 S3 C4 0.5(2) . . . . ? S1 Pd1 S3 C4 -88.5(2) . . . . ? C7 Pd1 S3 C5 -165.8(4) . . . . ? P1 Pd1 S3 C5 -82.4(3) . . . . ? S2 Pd1 S3 C5 106.5(3) . . . . ? S1 Pd1 S3 C5 17.5(3) . . . . ? C6 S1 C1 C2 62.8(8) . . . . ? Pd1 S1 C1 C2 -47.6(8) . . . . ? S1 C1 C2 S2 51.1(9) . . . . ? C3 S2 C2 C1 -132.0(7) . . . . ? Pd1 S2 C2 C1 -25.2(7) . . . . ? C2 S2 C3 C4 60.1(7) . . . . ? Pd1 S2 C3 C4 -47.0(7) . . . . ? S2 C3 C4 S3 53.3(8) . . . . ? C5 S3 C4 C3 -123.9(6) . . . . ? Pd1 S3 C4 C3 -27.3(6) . . . . ? C4 S3 C5 C6 57.8(8) . . . . ? Pd1 S3 C5 C6 -41.7(7) . . . . ? S3 C5 C6 S1 51.4(10) . . . . ? C1 S1 C6 C5 -129.8(7) . . . . ? Pd1 S1 C6 C5 -26.5(8) . . . . ? P1 Pd1 C7 C8 -25.3(5) . . . . ? S2 Pd1 C7 C8 162.0(5) . . . . ? S3 Pd1 C7 C8 78.5(5) . . . . ? Pd1 C7 C8 C13 21.1(8) . . . . ? Pd1 C7 C8 C9 -161.4(5) . . . . ? C13 C8 C9 C10 0.2(10) . . . . ? C7 C8 C9 C10 -177.4(6) . . . . ? C8 C9 C10 C11 -0.7(11) . . . . ? C9 C10 C11 C12 1.4(11) . . . . ? C10 C11 C12 C13 -1.7(10) . . . . ? C9 C8 C13 C12 -0.5(10) . . . . ? C7 C8 C13 C12 177.1(6) . . . . ? C9 C8 C13 P1 -177.3(5) . . . . ? C7 C8 C13 P1 0.4(8) . . . . ? C11 C12 C13 C8 1.3(10) . . . . ? C11 C12 C13 P1 177.4(5) . . . . ? C20 P1 C13 C8 104.3(7) . . . . ? C27 P1 C13 C8 -137.1(5) . . . . ? C20' P1 C13 C8 114.6(15) . . . . ? Pd1 P1 C13 C8 -18.2(5) . . . . ? C20 P1 C13 C12 -72.2(8) . . . . ? C27 P1 C13 C12 46.5(7) . . . . ? C20' P1 C13 C12 -61.8(16) . . . . ? Pd1 P1 C13 C12 165.3(5) . . . . ? C27 C22 C23 C24 2.9(13) . . . . ? C21 C22 C23 C24 -178.8(9) . . . . ? C22 C23 C24 C25 -2.6(17) . . . . ? C23 C24 C25 C26 1.8(18) . . . . ? C24 C25 C26 C27 -1.1(14) . . . . ? C21 C22 C27 C26 179.5(8) . . . . ? C23 C22 C27 C26 -2.4(11) . . . . ? C21 C22 C27 P1 6.4(11) . . . . ? C23 C22 C27 P1 -175.5(6) . . . . ? C25 C26 C27 C22 1.6(12) . . . . ? C25 C26 C27 P1 175.2(7) . . . . ? C13 P1 C27 C22 -159.7(6) . . . . ? C20 P1 C27 C22 -44.8(11) . . . . ? C20' P1 C27 C22 -48(3) . . . . ? Pd1 P1 C27 C22 86.7(6) . . . . ? C13 P1 C27 C26 26.9(6) . . . . ? C20 P1 C27 C26 141.8(10) . . . . ? C20' P1 C27 C26 139(3) . . . . ? Pd1 P1 C27 C26 -86.7(6) . . . . ? C20 C15 C16 C17 0(2) . . . . ? C14 C15 C16 C17 -176.8(13) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C16 C17 C18 C19 1.0(18) . . . . ? C17 C18 C19 C20 2.1(18) . . . . ? C18 C19 C20 C15 -4(3) . . . . ? C18 C19 C20 P1 177.8(10) . . . . ? C16 C15 C20 C19 3(3) . . . . ? C14 C15 C20 C19 179.5(14) . . . . ? C16 C15 C20 P1 -179.3(14) . . . . ? C14 C15 C20 P1 -2(3) . . . . ? C13 P1 C20 C19 -106.0(16) . . . . ? C27 P1 C20 C19 136.8(13) . . . . ? Pd1 P1 C20 C19 7.8(19) . . . . ? C13 P1 C20 C15 75.9(18) . . . . ? C27 P1 C20 C15 -41(2) . . . . ? Pd1 P1 C20 C15 -170.3(15) . . . . ? C20' C15' C16' C17' -13(9) . . . . ? C14' C15' C16' C17' 174(5) . . . . ? C15' C16' C17' C18' 5(10) . . . . ? C16' C17' C18' C19' -6(8) . . . . ? C17' C18' C19' C20' 17(7) . . . . ? C18' C19' C20' C15' -24(10) . . . . ? C18' C19' C20' P1 178(4) . . . . ? C16' C15' C20' C19' 21(10) . . . . ? C14' C15' C20' C19' -166(5) . . . . ? C16' C15' C20' P1 177(5) . . . . ? C14' C15' C20' P1 -10(9) . . . . ? C13 P1 C20' C19' 64(6) . . . . ? C27 P1 C20' C19' -50(7) . . . . ? Pd1 P1 C20' C19' -176(4) . . . . ? C13 P1 C20' C15' -91(7) . . . . ? C20 P1 C20' C15' -10(16) . . . . ? C27 P1 C20' C15' 155(6) . . . . ? Pd1 P1 C20' C15' 29(9) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.288 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.116 data_ptpc9s3 _database_code_depnum_ccdc_archive 'CCDC 666388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H32 P Pt S3), 2(F6 P), C H3 N O2' _chemical_formula_sum 'C55 H67 F12 N O2 P4 Pt2 S6' _chemical_formula_weight 1708.52 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.874(6) _cell_length_b 11.047(2) _cell_length_c 21.054(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.81(3) _cell_angle_gamma 90.00 _cell_volume 6137(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19164 _cell_measurement_theta_min 1.9984 _cell_measurement_theta_max 26.3714 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 4.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.474 _exptl_absorpt_correction_T_max 0.710 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28143 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6262 _reflns_number_gt 5212 _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^)+(0.0345P)^2^+74.4382P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6262 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 0.387060(10) 0.69817(3) 0.548529(12) 0.02750(9) Uani 1 1 d . . . S1 S 0.41245(7) 0.6901(2) 0.45242(9) 0.0356(4) Uani 1 1 d . . . S2 S 0.38777(7) 0.90922(18) 0.54215(9) 0.0329(4) Uani 1 1 d . . . S3 S 0.28682(8) 0.7276(2) 0.45079(10) 0.0427(5) Uani 1 1 d . . . P1 P 0.39116(6) 0.50143(18) 0.57551(8) 0.0254(4) Uani 1 1 d . . . P2 P 0.65549(11) 1.0142(3) 0.75598(15) 0.0642(8) Uani 1 1 d . . . F1 F 0.6518(7) 1.0348(14) 0.8261(6) 0.231(9) Uani 1 1 d . . . F2 F 0.6157(3) 0.9142(15) 0.7464(8) 0.234(10) Uani 1 1 d . . . F3 F 0.6161(4) 1.1169(11) 0.7283(6) 0.169(6) Uani 1 1 d . . . F4 F 0.6980(4) 1.1120(7) 0.7633(6) 0.129(3) Uani 1 1 d . . . F5 F 0.6602(4) 0.9916(8) 0.6848(4) 0.120(3) Uani 1 1 d . . . F6 F 0.6969(3) 0.9179(7) 0.7861(4) 0.096(3) Uani 1 1 d . . . C7 C 0.3679(3) 0.7144(8) 0.6364(4) 0.0385(18) Uani 1 1 d . . . H7A H 0.3986 0.7381 0.6735 0.046 Uiso 1 1 calc R . . H7B H 0.3430 0.7809 0.6303 0.046 Uiso 1 1 calc R . . C8 C 0.3462(3) 0.6033(7) 0.6571(3) 0.0291(15) Uani 1 1 d . . . C9 C 0.3201(3) 0.6090(8) 0.7034(4) 0.0379(18) Uani 1 1 d . . . H9A H 0.3160 0.6847 0.7224 0.046 Uiso 1 1 calc R . . C10 C 0.3002(3) 0.5060(9) 0.7218(4) 0.043(2) Uani 1 1 d . . . H10A H 0.2815 0.5116 0.7522 0.052 Uiso 1 1 calc R . . C11 C 0.3071(3) 0.3947(9) 0.6965(4) 0.043(2) Uani 1 1 d . . . H11A H 0.2938 0.3238 0.7102 0.052 Uiso 1 1 calc R . . C12 C 0.3336(3) 0.3864(8) 0.6508(4) 0.0377(18) Uani 1 1 d . . . H12A H 0.3384 0.3100 0.6331 0.045 Uiso 1 1 calc R . . C13 C 0.3529(2) 0.4915(7) 0.6312(3) 0.0281(15) Uani 1 1 d . . . C14 C 0.4306(5) 0.2200(12) 0.6205(6) 0.080(4) Uani 1 1 d . . . H14A H 0.4021 0.2423 0.5809 0.120 Uiso 1 1 calc R . . H14B H 0.4180 0.1994 0.6575 0.120 Uiso 1 1 calc R . . H14C H 0.4483 0.1501 0.6099 0.120 Uiso 1 1 calc R . . C15 C 0.4656(4) 0.3218(10) 0.6402(4) 0.053(3) Uani 1 1 d . . . C16 C 0.5161(4) 0.2938(14) 0.6808(5) 0.073(4) Uani 1 1 d . . . H16A H 0.5260 0.2120 0.6912 0.088 Uiso 1 1 calc R . . C17 C 0.5497(5) 0.3833(16) 0.7042(5) 0.078(4) Uani 1 1 d . . . H17A H 0.5828 0.3620 0.7323 0.094 Uiso 1 1 calc R . . C18 C 0.5393(4) 0.5048(16) 0.6899(5) 0.080(4) Uani 1 1 d . . . H18A H 0.5642 0.5658 0.7064 0.096 Uiso 1 1 calc R . . C19 C 0.4907(3) 0.5316(12) 0.6507(4) 0.062(3) Uani 1 1 d . . . H19A H 0.4816 0.6140 0.6406 0.074 Uiso 1 1 calc R . . C20 C 0.4539(3) 0.4420(8) 0.6247(3) 0.0360(19) Uani 1 1 d . . . C21 C 0.4446(3) 0.3791(10) 0.4758(5) 0.051(2) Uani 1 1 d . . . H21A H 0.4527 0.4650 0.4848 0.077 Uiso 1 1 calc R . . H21B H 0.4539 0.3537 0.4367 0.077 Uiso 1 1 calc R . . H21C H 0.4637 0.3311 0.5149 0.077 Uiso 1 1 calc R . . C22 C 0.3898(4) 0.3601(9) 0.4622(4) 0.046(2) Uani 1 1 d . . . C23 C 0.3627(4) 0.2922(10) 0.4038(4) 0.058(3) Uani 1 1 d . . . H23A H 0.3800 0.2605 0.3753 0.070 Uiso 1 1 calc R . . C24 C 0.3119(4) 0.2733(11) 0.3893(5) 0.066(3) Uani 1 1 d . . . H24A H 0.2945 0.2279 0.3504 0.079 Uiso 1 1 calc R . . C25 C 0.2849(4) 0.3175(10) 0.4288(5) 0.063(3) Uani 1 1 d . . . H25A H 0.2495 0.3033 0.4170 0.076 Uiso 1 1 calc R . . C26 C 0.3097(3) 0.3818(8) 0.4850(4) 0.046(2) Uani 1 1 d . . . H26A H 0.2915 0.4126 0.5126 0.055 Uiso 1 1 calc R . . C27 C 0.3636(3) 0.4034(7) 0.5030(4) 0.0354(17) Uani 1 1 d . . . C1 C 0.4394(4) 0.8397(10) 0.4562(6) 0.066(3) Uani 1 1 d . . . H1A H 0.4733 0.8391 0.4910 0.079 Uiso 1 1 calc R . . H1B H 0.4446 0.8562 0.4127 0.079 Uiso 1 1 calc R . . C2 C 0.4098(4) 0.9413(9) 0.4710(5) 0.059(3) Uani 1 1 d . . . H2A H 0.3802 0.9578 0.4309 0.071 Uiso 1 1 calc R . . H2B H 0.4312 1.0149 0.4808 0.071 Uiso 1 1 calc R . . C3 C 0.3211(3) 0.9538(8) 0.5092(4) 0.043(2) Uani 1 1 d . . . H3A H 0.3059 0.9415 0.5452 0.052 Uiso 1 1 calc R . . H3B H 0.3198 1.0416 0.4995 0.052 Uiso 1 1 calc R . . C4 C 0.2881(3) 0.8899(9) 0.4470(5) 0.050(2) Uani 1 1 d . . . H4A H 0.2998 0.9132 0.4090 0.060 Uiso 1 1 calc R . . H4B H 0.2530 0.9201 0.4369 0.060 Uiso 1 1 calc R . . C5 C 0.3075(4) 0.6738(13) 0.3820(5) 0.072(4) Uani 1 1 d . . . H5A H 0.3053 0.5843 0.3818 0.086 Uiso 1 1 calc R . . H5B H 0.2823 0.7023 0.3398 0.086 Uiso 1 1 calc R . . C6 C 0.3567(3) 0.7046(12) 0.3788(4) 0.061(3) Uani 1 1 d . . . H6A H 0.3551 0.7898 0.3636 0.073 Uiso 1 1 calc R . . H6B H 0.3625 0.6543 0.3430 0.073 Uiso 1 1 calc R . . O2 O 0.5106(7) 0.962(2) 0.6210(12) 0.104(5) Uani 0.50 1 d P A -1 N1 N 0.5152(6) 0.8873(18) 0.6648(14) 0.081(7) Uani 0.50 1 d P A -1 O1 O 0.5331(7) 0.793(2) 0.6629(12) 0.104(5) Uani 0.50 1 d P A -1 C28 C 0.5024(11) 0.921(3) 0.7242(13) 0.087(8) Uani 0.50 1 d P A -1 H28A H 0.5034 0.8486 0.7517 0.130 Uiso 0.50 1 calc PR A -1 H28B H 0.4682 0.9556 0.7106 0.130 Uiso 0.50 1 calc PR A -1 H28C H 0.5268 0.9805 0.7503 0.130 Uiso 0.50 1 calc PR A -1 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 0.02921(14) 0.03150(16) 0.02285(13) -0.00034(13) 0.00987(10) -0.00120(14) S1 0.0342(9) 0.0451(12) 0.0311(9) 0.0011(9) 0.0158(7) 0.0022(9) S2 0.0369(9) 0.0284(10) 0.0340(9) -0.0009(8) 0.0123(8) -0.0055(8) S3 0.0337(10) 0.0568(15) 0.0397(10) -0.0108(9) 0.0147(8) -0.0042(9) P1 0.0220(8) 0.0307(10) 0.0223(8) 0.0022(7) 0.0055(7) 0.0017(7) P2 0.0711(17) 0.0683(19) 0.0677(17) 0.0382(15) 0.0426(15) 0.0331(15) F1 0.38(2) 0.256(16) 0.123(8) 0.110(9) 0.179(12) 0.211(16) F2 0.070(6) 0.285(17) 0.304(17) 0.229(15) -0.001(8) -0.033(8) F3 0.145(8) 0.200(11) 0.204(10) 0.152(9) 0.115(8) 0.128(8) F4 0.154(8) 0.054(5) 0.184(10) 0.013(6) 0.061(7) -0.008(5) F5 0.213(10) 0.089(6) 0.070(5) 0.014(4) 0.063(6) 0.022(6) F6 0.075(4) 0.070(5) 0.141(7) 0.058(5) 0.031(4) 0.026(4) C7 0.057(5) 0.031(5) 0.030(4) -0.005(3) 0.019(4) 0.000(4) C8 0.029(3) 0.035(4) 0.022(3) 0.005(3) 0.007(3) 0.003(3) C9 0.043(4) 0.041(5) 0.034(4) 0.008(3) 0.018(3) 0.008(4) C10 0.040(4) 0.060(6) 0.036(4) 0.004(4) 0.019(4) 0.010(4) C11 0.033(4) 0.055(6) 0.038(4) 0.020(4) 0.008(3) -0.006(4) C12 0.039(4) 0.033(4) 0.040(4) 0.007(3) 0.012(3) -0.003(3) C13 0.023(3) 0.034(4) 0.026(3) 0.007(3) 0.007(3) 0.002(3) C14 0.085(8) 0.078(9) 0.084(8) 0.027(7) 0.038(7) 0.044(7) C15 0.055(5) 0.076(8) 0.037(4) 0.021(5) 0.026(4) 0.033(5) C16 0.073(7) 0.123(11) 0.038(5) 0.029(7) 0.038(5) 0.052(8) C17 0.055(6) 0.150(14) 0.034(5) 0.023(7) 0.020(5) 0.031(8) C18 0.039(5) 0.175(15) 0.029(5) -0.006(7) 0.013(4) -0.002(7) C19 0.035(4) 0.117(10) 0.034(4) -0.022(5) 0.012(4) -0.009(5) C20 0.023(3) 0.065(6) 0.018(3) -0.001(3) 0.004(3) 0.011(3) C21 0.046(5) 0.063(7) 0.047(5) -0.003(4) 0.018(4) 0.003(4) C22 0.057(5) 0.044(5) 0.039(4) 0.006(4) 0.018(4) 0.003(4) C23 0.062(6) 0.072(7) 0.040(5) -0.009(5) 0.014(4) -0.008(5) C24 0.062(6) 0.085(9) 0.051(6) -0.015(5) 0.020(5) -0.010(6) C25 0.047(5) 0.071(8) 0.062(6) -0.013(5) 0.005(5) -0.021(5) C26 0.049(5) 0.037(5) 0.045(5) -0.003(4) 0.005(4) -0.013(4) C27 0.043(4) 0.034(4) 0.026(3) 0.003(3) 0.006(3) 0.000(3) C1 0.074(7) 0.057(7) 0.091(8) 0.007(6) 0.061(6) -0.006(5) C2 0.074(7) 0.038(5) 0.073(7) 0.008(5) 0.036(6) -0.021(5) C3 0.046(5) 0.041(5) 0.040(4) -0.003(4) 0.011(4) 0.008(4) C4 0.046(5) 0.052(6) 0.050(5) 0.009(4) 0.012(4) -0.001(4) C5 0.043(5) 0.125(11) 0.048(5) -0.037(6) 0.015(4) -0.001(6) C6 0.047(5) 0.107(9) 0.030(4) -0.003(5) 0.013(4) 0.012(6) O2 0.073(8) 0.092(11) 0.144(13) -0.016(10) 0.033(8) -0.021(8) N1 0.038(9) 0.037(10) 0.15(2) 0.006(12) 0.012(11) -0.007(8) O1 0.073(8) 0.092(11) 0.144(13) -0.016(10) 0.033(8) -0.021(8) C28 0.090(17) 0.10(2) 0.086(17) 0.030(16) 0.056(15) 0.004(17) _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 C7 2.093(7) . ? Pt1 P1 2.240(2) . ? Pt1 S2 2.336(2) . ? Pt1 S1 2.3509(18) . ? S1 C1 1.806(11) . ? S1 C6 1.814(9) . ? S2 C2 1.828(10) . ? S2 C3 1.828(8) . ? S3 C4 1.795(10) . ? S3 C5 1.824(9) . ? P1 C13 1.825(7) . ? P1 C27 1.827(8) . ? P1 C20 1.843(7) . ? P2 F1 1.529(10) . ? P2 F2 1.532(12) . ? P2 F6 1.547(6) . ? P2 F3 1.555(8) . ? P2 F5 1.567(8) . ? P2 F4 1.574(10) . ? C7 C8 1.493(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.387(11) . ? C8 C9 1.394(10) . ? C9 C10 1.374(12) . ? C9 H9A 0.9500 . ? C10 C11 1.378(13) . ? C10 H10A 0.9500 . ? C11 C12 1.390(11) . ? C11 H11A 0.9500 . ? C12 C13 1.397(11) . ? C12 H12A 0.9500 . ? C14 C15 1.458(17) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.381(13) . ? C15 C16 1.425(14) . ? C16 C17 1.342(19) . ? C16 H16A 0.9500 . ? C17 C18 1.39(2) . ? C17 H17A 0.9500 . ? C18 C19 1.372(14) . ? C18 H18A 0.9500 . ? C19 C20 1.403(13) . ? C19 H19A 0.9500 . ? C21 C22 1.475(12) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.380(12) . ? C22 C23 1.431(13) . ? C23 C24 1.365(14) . ? C23 H23A 0.9500 . ? C24 C25 1.378(15) . ? C24 H24A 0.9500 . ? C25 C26 1.362(12) . ? C25 H25A 0.9500 . ? C26 C27 1.445(12) . ? C26 H26A 0.9500 . ? C1 C2 1.484(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.436(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O2 N1 1.21(3) . ? N1 O1 1.16(3) . ? N1 C28 1.45(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 C7 Pt1 P1 82.3(2) . . ? C7 Pt1 S2 88.5(2) . . ? P1 Pt1 S2 169.23(7) . . ? C7 Pt1 S1 176.3(2) . . ? P1 Pt1 S1 100.17(7) . . ? S2 Pt1 S1 88.73(7) . . ? C1 S1 C6 100.8(6) . . ? C1 S1 Pt1 99.4(4) . . ? C6 S1 Pt1 108.7(3) . . ? C2 S2 C3 101.9(5) . . ? C2 S2 Pt1 104.6(3) . . ? C3 S2 Pt1 105.3(3) . . ? C4 S3 C5 105.9(6) . . ? C13 P1 C27 109.0(4) . . ? C13 P1 C20 105.2(3) . . ? C27 P1 C20 109.0(4) . . ? C13 P1 Pt1 103.2(3) . . ? C27 P1 Pt1 112.9(3) . . ? C20 P1 Pt1 116.7(3) . . ? F1 P2 F2 87.9(9) . . ? F1 P2 F6 88.9(5) . . ? F2 P2 F6 88.3(5) . . ? F1 P2 F3 89.7(6) . . ? F2 P2 F3 94.8(7) . . ? F6 P2 F3 176.6(7) . . ? F1 P2 F5 178.9(6) . . ? F2 P2 F5 92.2(9) . . ? F6 P2 F5 90.0(5) . . ? F3 P2 F5 91.4(6) . . ? F1 P2 F4 95.0(9) . . ? F2 P2 F4 176.4(9) . . ? F6 P2 F4 89.6(5) . . ? F3 P2 F4 87.4(6) . . ? F5 P2 F4 84.8(6) . . ? C8 C7 Pt1 115.5(5) . . ? C8 C7 H7A 108.4 . . ? Pt1 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? Pt1 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C13 C8 C9 118.8(7) . . ? C13 C8 C7 120.0(6) . . ? C9 C8 C7 121.3(7) . . ? C10 C9 C8 120.6(8) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 120.7(7) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C12 119.8(8) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C13 119.4(8) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C8 C13 C12 120.7(7) . . ? C8 C13 P1 112.3(5) . . ? C12 C13 P1 127.0(6) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 117.6(11) . . ? C20 C15 C14 126.0(8) . . ? C16 C15 C14 116.4(11) . . ? C17 C16 C15 119.9(13) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 124.1(11) . . ? C16 C17 H17A 117.9 . . ? C18 C17 H17A 117.9 . . ? C19 C18 C17 115.9(13) . . ? C19 C18 H18A 122.0 . . ? C17 C18 H18A 122.0 . . ? C18 C19 C20 122.5(13) . . ? C18 C19 H19A 118.7 . . ? C20 C19 H19A 118.7 . . ? C15 C20 C19 119.9(8) . . ? C15 C20 P1 125.8(7) . . ? C19 C20 P1 114.2(7) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.5(9) . . ? C27 C22 C21 123.6(8) . . ? C23 C22 C21 117.9(8) . . ? C24 C23 C22 119.6(10) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 122.7(10) . . ? C23 C24 H24A 118.7 . . ? C25 C24 H24A 118.7 . . ? C26 C25 C24 119.0(9) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C27 120.5(9) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C22 C27 C26 119.6(8) . . ? C22 C27 P1 124.1(6) . . ? C26 C27 P1 116.0(6) . . ? C2 C1 S1 116.7(7) . . ? C2 C1 H1A 108.1 . . ? S1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? S1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C1 C2 S2 112.5(7) . . ? C1 C2 H2A 109.1 . . ? S2 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S2 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 S2 117.6(6) . . ? C4 C3 H3A 107.9 . . ? S2 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? S2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 C4 S3 116.3(6) . . ? C3 C4 H4A 108.2 . . ? S3 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? S3 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C6 C5 S3 120.8(7) . . ? C6 C5 H5A 107.1 . . ? S3 C5 H5A 107.1 . . ? C6 C5 H5B 107.1 . . ? S3 C5 H5B 107.1 . . ? H5A C5 H5B 106.8 . . ? C5 C6 S1 120.4(7) . . ? C5 C6 H6A 107.2 . . ? S1 C6 H6A 107.2 . . ? C5 C6 H6B 107.2 . . ? S1 C6 H6B 107.2 . . ? H6A C6 H6B 106.9 . . ? O1 N1 O2 122(3) . . ? O1 N1 C28 119(3) . . ? O2 N1 C28 119(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 S1 C1 -152.4(4) . . . . ? S2 Pt1 S1 C1 21.5(4) . . . . ? P1 Pt1 S1 C6 102.7(5) . . . . ? S2 Pt1 S1 C6 -83.4(5) . . . . ? C7 Pt1 S2 C2 174.9(4) . . . . ? P1 Pt1 S2 C2 143.4(5) . . . . ? S1 Pt1 S2 C2 -2.6(4) . . . . ? C7 Pt1 S2 C3 -78.1(4) . . . . ? P1 Pt1 S2 C3 -109.6(4) . . . . ? S1 Pt1 S2 C3 104.4(3) . . . . ? C7 Pt1 P1 C13 20.9(3) . . . . ? S2 Pt1 P1 C13 52.7(4) . . . . ? S1 Pt1 P1 C13 -161.9(2) . . . . ? C7 Pt1 P1 C27 138.5(4) . . . . ? S2 Pt1 P1 C27 170.3(4) . . . . ? S1 Pt1 P1 C27 -44.3(3) . . . . ? C7 Pt1 P1 C20 -93.9(3) . . . . ? S2 Pt1 P1 C20 -62.1(4) . . . . ? S1 Pt1 P1 C20 83.2(3) . . . . ? P1 Pt1 C7 C8 -23.4(5) . . . . ? S2 Pt1 C7 C8 162.3(6) . . . . ? Pt1 C7 C8 C13 18.2(9) . . . . ? Pt1 C7 C8 C9 -163.3(6) . . . . ? C13 C8 C9 C10 -1.7(11) . . . . ? C7 C8 C9 C10 179.8(7) . . . . ? C8 C9 C10 C11 2.1(12) . . . . ? C9 C10 C11 C12 -1.3(12) . . . . ? C10 C11 C12 C13 0.1(11) . . . . ? C9 C8 C13 C12 0.5(10) . . . . ? C7 C8 C13 C12 179.0(7) . . . . ? C9 C8 C13 P1 -176.6(5) . . . . ? C7 C8 C13 P1 2.0(8) . . . . ? C11 C12 C13 C8 0.3(11) . . . . ? C11 C12 C13 P1 176.9(6) . . . . ? C27 P1 C13 C8 -138.8(5) . . . . ? C20 P1 C13 C8 104.3(6) . . . . ? Pt1 P1 C13 C8 -18.5(5) . . . . ? C27 P1 C13 C12 44.4(7) . . . . ? C20 P1 C13 C12 -72.5(7) . . . . ? Pt1 P1 C13 C12 164.7(6) . . . . ? C20 C15 C16 C17 2.2(12) . . . . ? C14 C15 C16 C17 -176.1(9) . . . . ? C15 C16 C17 C18 -2.0(15) . . . . ? C16 C17 C18 C19 1.7(15) . . . . ? C17 C18 C19 C20 -1.6(13) . . . . ? C16 C15 C20 C19 -2.1(11) . . . . ? C14 C15 C20 C19 176.0(9) . . . . ? C16 C15 C20 P1 -178.1(6) . . . . ? C14 C15 C20 P1 0.0(13) . . . . ? C18 C19 C20 C15 2.0(12) . . . . ? C18 C19 C20 P1 178.4(7) . . . . ? C13 P1 C20 C15 73.7(7) . . . . ? C27 P1 C20 C15 -43.2(8) . . . . ? Pt1 P1 C20 C15 -172.6(6) . . . . ? C13 P1 C20 C19 -102.5(6) . . . . ? C27 P1 C20 C19 140.7(6) . . . . ? Pt1 P1 C20 C19 11.2(6) . . . . ? C27 C22 C23 C24 0.9(15) . . . . ? C21 C22 C23 C24 -179.6(10) . . . . ? C22 C23 C24 C25 0.2(18) . . . . ? C23 C24 C25 C26 -0.6(19) . . . . ? C24 C25 C26 C27 0.0(16) . . . . ? C23 C22 C27 C26 -1.4(13) . . . . ? C21 C22 C27 C26 179.1(9) . . . . ? C23 C22 C27 P1 -174.9(7) . . . . ? C21 C22 C27 P1 5.5(13) . . . . ? C25 C26 C27 C22 1.0(13) . . . . ? C25 C26 C27 P1 175.1(8) . . . . ? C13 P1 C27 C22 -159.3(7) . . . . ? C20 P1 C27 C22 -45.0(8) . . . . ? Pt1 P1 C27 C22 86.6(7) . . . . ? C13 P1 C27 C26 26.9(7) . . . . ? C20 P1 C27 C26 141.3(6) . . . . ? Pt1 P1 C27 C26 -87.2(6) . . . . ? C6 S1 C1 C2 66.4(10) . . . . ? Pt1 S1 C1 C2 -44.8(10) . . . . ? S1 C1 C2 S2 47.5(11) . . . . ? C3 S2 C2 C1 -132.5(8) . . . . ? Pt1 S2 C2 C1 -23.0(9) . . . . ? C2 S2 C3 C4 59.2(8) . . . . ? Pt1 S2 C3 C4 -49.7(7) . . . . ? S2 C3 C4 S3 54.8(9) . . . . ? C5 S3 C4 C3 -122.2(7) . . . . ? C4 S3 C5 C6 60.0(12) . . . . ? S3 C5 C6 S1 46.8(15) . . . . ? C1 S1 C6 C5 -127.1(11) . . . . ? Pt1 S1 C6 C5 -23.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.508 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.139 data_pdpc9s3a _database_code_depnum_ccdc_archive 'CCDC 666389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H33 Cl P Pd S3, 0.5(F6 P), 0.5(F6 P)' _chemical_formula_sum 'C27 H33 Cl F6 P2 Pd S3' _chemical_formula_weight 771.50 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1919(16) _cell_length_b 18.529(4) _cell_length_c 22.595(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.63(3) _cell_angle_gamma 90.00 _cell_volume 3428.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15495 _cell_measurement_theta_min 2.7049 _cell_measurement_theta_max 26.0212 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7396 _exptl_absorpt_correction_T_max 0.8410 _exptl_absorpt_process_details 'REQAB, subroutine of CrystalClear, Rigaku/MSC, The Woodlands, TX, 1999.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.6199 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26510 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6056 _reflns_number_gt 5552 _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^)+(0.0099P)^2^+30.4001P] 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 6056 _refine_ls_number_parameters 391 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.206 _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 Pd1 Pd 0.47069(6) 0.19584(3) 0.31444(2) 0.02244(14) Uani 1 1 d . . . Cl1 Cl 0.74915(19) 0.18736(11) 0.29963(8) 0.0383(4) Uani 1 1 d . . . P1 P 0.41192(18) 0.24171(9) 0.22134(7) 0.0206(3) Uani 1 1 d . . . S1 S 0.5222(2) 0.18390(11) 0.41771(8) 0.0386(4) Uani 1 1 d . . . S2 S 0.19766(18) 0.19918(10) 0.33340(7) 0.0285(4) Uani 1 1 d . . . S3 S 0.4336(2) 0.04093(10) 0.32384(9) 0.0367(4) Uani 1 1 d . . . C1 C 0.3220(10) 0.1895(6) 0.4496(3) 0.057(2) Uani 1 1 d . . . H1A H 0.2810 0.1401 0.4570 0.069 Uiso 1 1 calc R . . H1B H 0.3313 0.2148 0.4882 0.069 Uiso 1 1 calc R . . C2 C 0.2028(12) 0.2286(6) 0.4103(4) 0.064(3) Uani 1 1 d . . . H2A H 0.2292 0.2807 0.4115 0.077 Uiso 1 1 calc R . . H2B H 0.0923 0.2225 0.4263 0.077 Uiso 1 1 calc R . . C3 C 0.1286(10) 0.1069(4) 0.3433(5) 0.054(2) Uani 1 1 d . . . H3A H 0.1294 0.0973 0.3865 0.065 Uiso 1 1 calc R . . H3B H 0.0132 0.1046 0.3291 0.065 Uiso 1 1 calc R . . C4 C 0.2135(9) 0.0486(5) 0.3160(4) 0.052(2) Uani 1 1 d . . . H4A H 0.1862 0.0505 0.2731 0.063 Uiso 1 1 calc R . . H4B H 0.1666 0.0031 0.3311 0.063 Uiso 1 1 calc R . . C5 C 0.4693(11) 0.0329(5) 0.4028(4) 0.052(2) Uani 1 1 d . . . H5A H 0.3629 0.0352 0.4225 0.063 Uiso 1 1 calc R . . H5B H 0.5176 -0.0151 0.4114 0.063 Uiso 1 1 calc R . . C6 C 0.5796(10) 0.0898(5) 0.4290(4) 0.050(2) Uani 1 1 d . . . H6A H 0.6895 0.0828 0.4128 0.060 Uiso 1 1 calc R . . H6B H 0.5893 0.0811 0.4722 0.060 Uiso 1 1 calc R . . C7 C 0.4954(9) 0.0812(4) 0.1761(3) 0.0403(18) Uani 1 1 d . . . H7A H 0.4965 0.0326 0.1932 0.060 Uiso 1 1 calc R . . H7B H 0.5588 0.1139 0.2020 0.060 Uiso 1 1 calc R . . H7C H 0.5439 0.0798 0.1370 0.060 Uiso 1 1 calc R . . C8 C 0.3208(8) 0.1080(4) 0.1701(3) 0.0293(15) Uani 1 1 d . . . C9 C 0.2027(10) 0.0602(4) 0.1477(3) 0.0371(17) Uani 1 1 d . . . H9A H 0.2352 0.0137 0.1349 0.045 Uiso 1 1 calc R . . C10 C 0.0390(10) 0.0791(4) 0.1438(3) 0.0413(18) Uani 1 1 d . . . H10A H -0.0390 0.0457 0.1282 0.050 Uiso 1 1 calc R . . C11 C -0.0100(8) 0.1454(4) 0.1621(3) 0.0369(17) Uani 1 1 d . . . H11A H -0.1225 0.1578 0.1601 0.044 Uiso 1 1 calc R . . C12 C 0.1037(7) 0.1947(4) 0.1838(3) 0.0287(14) Uani 1 1 d . . . H12A H 0.0685 0.2408 0.1966 0.034 Uiso 1 1 calc R . . C13 C 0.2709(7) 0.1773(4) 0.1869(3) 0.0246(14) Uani 1 1 d . . . C14 C 0.2576(9) 0.3429(4) 0.1141(3) 0.0338(16) Uani 1 1 d . . . H14A H 0.1771 0.3691 0.0895 0.051 Uiso 1 1 calc R . . H14B H 0.2332 0.2912 0.1127 0.051 Uiso 1 1 calc R . . H14C H 0.3671 0.3514 0.0992 0.051 Uiso 1 1 calc R . . C15 C 0.2506(7) 0.3693(3) 0.1774(3) 0.0262(14) Uani 1 1 d . . . C16 C 0.1879(8) 0.4377(4) 0.1870(3) 0.0309(15) Uani 1 1 d . . . H16A H 0.1482 0.4650 0.1540 0.037 Uiso 1 1 calc R . . C17 C 0.1811(8) 0.4675(4) 0.2429(3) 0.0358(16) Uani 1 1 d . . . H17A H 0.1386 0.5147 0.2480 0.043 Uiso 1 1 calc R . . C18 C 0.2360(8) 0.4285(4) 0.2908(3) 0.0344(16) Uani 1 1 d . . . H18A H 0.2295 0.4481 0.3296 0.041 Uiso 1 1 calc R . . C19 C 0.3010(8) 0.3606(4) 0.2825(3) 0.0292(14) Uani 1 1 d . . . H19A H 0.3418 0.3344 0.3159 0.035 Uiso 1 1 calc R . . C20 C 0.3082(7) 0.3294(3) 0.2265(3) 0.0217(13) Uani 1 1 d . . . C21 C 0.7044(9) 0.3552(4) 0.2402(3) 0.0381(17) Uani 1 1 d . . . H21A H 0.8178 0.3702 0.2476 0.057 Uiso 1 1 calc R . . H21B H 0.6701 0.3235 0.2722 0.057 Uiso 1 1 calc R . . H21C H 0.6339 0.3980 0.2384 0.057 Uiso 1 1 calc R . . C22 C 0.6911(7) 0.3153(4) 0.1822(3) 0.0311(15) Uani 1 1 d . . . C23 C 0.7975(8) 0.3340(4) 0.1381(3) 0.0359(17) Uani 1 1 d . . . H23A H 0.8783 0.3697 0.1462 0.043 Uiso 1 1 calc R . . C24 C 0.7902(9) 0.3028(5) 0.0830(3) 0.0439(19) Uani 1 1 d . . . H24A H 0.8648 0.3170 0.0538 0.053 Uiso 1 1 calc R . . C25 C 0.6737(9) 0.2502(4) 0.0700(3) 0.0356(16) Uani 1 1 d . . . H25A H 0.6685 0.2285 0.0319 0.043 Uiso 1 1 calc R . . C26 C 0.5647(8) 0.2297(4) 0.1130(3) 0.0291(14) Uani 1 1 d . . . H26A H 0.4851 0.1936 0.1042 0.035 Uiso 1 1 calc R . . C27 C 0.5716(7) 0.2616(3) 0.1689(3) 0.0233(13) Uani 1 1 d . . . P2 P 0.0000 0.0000 0.5000 0.0211(5) Uani 1 2 d S . . F1 F 0.0477(6) -0.0241(3) 0.43489(17) 0.0465(11) Uani 1 1 d . . . F2 F -0.0330(5) 0.0800(2) 0.4765(2) 0.0443(11) Uani 1 1 d . . . F3 F -0.1863(5) -0.0215(2) 0.48610(19) 0.0400(10) Uani 1 1 d . . . P3 P 0.4115(9) 0.0801(4) -0.0251(2) 0.0820(19) Uani 0.50 1 d PD A -1 F8 F 0.317(2) 0.1375(8) 0.0093(6) 0.115(6) Uani 0.50 1 d PD A -1 F7 F 0.4679(19) 0.1339(9) -0.0709(7) 0.116(5) Uani 0.50 1 d PD A -1 F6 F 0.568(2) 0.0899(14) 0.0138(8) 0.180(7) Uani 0.50 1 d PD A -1 F5 F 0.243(2) 0.0765(14) -0.0604(8) 0.180(7) Uani 0.50 1 d PD A -1 F4 F 0.501(3) 0.0207(12) -0.0602(10) 0.175(9) Uani 0.50 1 d PD A -1 F9 F 0.354(4) 0.0265(9) 0.0222(8) 0.189(12) Uani 0.50 1 d PD A -1 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 Pd1 0.0187(2) 0.0269(3) 0.0218(2) 0.0078(2) 0.00046(17) 0.00275(19) Cl1 0.0180(8) 0.0508(11) 0.0462(10) 0.0170(9) 0.0025(7) 0.0048(7) P1 0.0185(7) 0.0234(8) 0.0200(8) 0.0049(6) 0.0011(6) 0.0006(6) S1 0.0386(10) 0.0536(12) 0.0235(8) 0.0117(8) -0.0046(7) -0.0033(9) S2 0.0211(8) 0.0340(9) 0.0306(8) 0.0125(7) 0.0055(6) 0.0081(7) S3 0.0297(9) 0.0316(9) 0.0491(11) 0.0047(8) 0.0090(8) 0.0025(7) C1 0.052(5) 0.093(7) 0.027(4) 0.012(4) 0.014(4) 0.003(5) C2 0.064(6) 0.091(8) 0.040(5) 0.014(5) 0.026(4) 0.028(5) C3 0.032(4) 0.038(5) 0.093(7) 0.021(5) 0.012(4) -0.002(3) C4 0.032(4) 0.050(5) 0.075(6) -0.001(4) 0.005(4) -0.010(4) C5 0.065(6) 0.038(5) 0.055(5) 0.027(4) 0.013(4) 0.012(4) C6 0.049(5) 0.058(6) 0.043(5) 0.025(4) -0.009(4) 0.018(4) C7 0.049(5) 0.036(4) 0.036(4) -0.001(3) 0.002(3) 0.016(3) C8 0.038(4) 0.026(3) 0.024(3) 0.002(3) 0.006(3) 0.001(3) C9 0.055(5) 0.028(4) 0.029(4) -0.003(3) 0.005(3) -0.009(3) C10 0.046(5) 0.044(5) 0.033(4) -0.007(3) -0.004(3) -0.018(4) C11 0.025(4) 0.048(5) 0.037(4) 0.006(3) -0.002(3) -0.012(3) C12 0.024(3) 0.033(4) 0.030(3) 0.007(3) -0.002(3) -0.001(3) C13 0.024(3) 0.034(4) 0.016(3) 0.000(3) -0.002(2) -0.006(3) C14 0.036(4) 0.041(4) 0.024(3) 0.009(3) -0.004(3) 0.002(3) C15 0.021(3) 0.026(3) 0.031(3) 0.003(3) 0.000(3) -0.001(3) C16 0.025(3) 0.029(4) 0.038(4) 0.007(3) -0.005(3) 0.004(3) C17 0.033(4) 0.029(4) 0.046(4) -0.004(3) -0.002(3) 0.005(3) C18 0.033(4) 0.032(4) 0.038(4) -0.007(3) 0.002(3) 0.000(3) C19 0.030(3) 0.032(4) 0.025(3) 0.002(3) -0.002(3) 0.004(3) C20 0.019(3) 0.021(3) 0.026(3) 0.001(2) 0.001(2) 0.001(2) C21 0.031(4) 0.035(4) 0.048(4) 0.004(3) -0.008(3) -0.009(3) C22 0.019(3) 0.031(4) 0.044(4) 0.012(3) 0.000(3) 0.000(3) C23 0.025(3) 0.033(4) 0.050(5) 0.010(3) 0.005(3) -0.004(3) C24 0.033(4) 0.054(5) 0.045(4) 0.022(4) 0.013(3) 0.002(4) C25 0.036(4) 0.045(4) 0.026(3) -0.001(3) 0.005(3) 0.002(3) C26 0.022(3) 0.038(4) 0.028(3) 0.004(3) 0.000(3) 0.006(3) C27 0.023(3) 0.023(3) 0.024(3) 0.007(3) 0.000(2) -0.002(3) P2 0.0238(11) 0.0242(12) 0.0151(10) 0.0005(9) -0.0007(8) 0.0002(9) F1 0.062(3) 0.053(3) 0.024(2) -0.0120(19) 0.0077(19) 0.000(2) F2 0.046(3) 0.030(2) 0.057(3) 0.017(2) 0.005(2) 0.0044(19) F3 0.025(2) 0.048(3) 0.047(2) -0.001(2) -0.0037(17) -0.0023(18) P3 0.113(5) 0.103(5) 0.029(2) -0.016(3) -0.003(3) -0.003(4) F8 0.169(15) 0.105(12) 0.072(9) 0.028(8) 0.020(9) 0.066(11) F7 0.104(11) 0.130(14) 0.114(12) 0.046(11) 0.009(9) 0.008(10) F6 0.182(14) 0.259(19) 0.099(9) -0.049(11) -0.006(9) -0.107(14) F5 0.182(14) 0.259(19) 0.099(9) -0.049(11) -0.006(9) -0.107(14) F4 0.23(3) 0.16(2) 0.138(17) -0.085(16) 0.044(17) 0.015(18) F9 0.37(4) 0.096(13) 0.103(13) 0.005(11) 0.125(19) 0.026(18) _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 Pd1 S2 2.2900(17) . ? Pd1 P1 2.3068(16) . ? Pd1 Cl1 2.3202(17) . ? Pd1 S1 2.3700(18) . ? Pd1 S3 2.895(2) . ? P1 C13 1.820(6) . ? P1 C27 1.827(6) . ? P1 C20 1.838(6) . ? S1 C1 1.814(8) . ? S1 C6 1.823(8) . ? S2 C3 1.817(8) . ? S2 C2 1.820(9) . ? S3 C5 1.805(9) . ? S3 C4 1.812(8) . ? C1 C2 1.489(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.435(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.396(10) . ? C8 C13 1.403(9) . ? C9 C10 1.386(11) . ? C9 H9A 0.9500 . ? C10 C11 1.360(11) . ? C10 H10A 0.9500 . ? C11 C12 1.385(10) . ? C11 H11A 0.9500 . ? C12 C13 1.407(9) . ? C12 H12A 0.9500 . ? C14 C15 1.513(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.387(9) . ? C15 C20 1.406(9) . ? C16 C17 1.381(10) . ? C16 H16A 0.9500 . ? C17 C18 1.367(10) . ? C17 H17A 0.9500 . ? C18 C19 1.382(10) . ? C18 H18A 0.9500 . ? C19 C20 1.394(9) . ? C19 H19A 0.9500 . ? C21 C22 1.505(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.387(9) . ? C22 C27 1.422(9) . ? C23 C24 1.371(11) . ? C23 H23A 0.9500 . ? C24 C25 1.388(11) . ? C24 H24A 0.9500 . ? C25 C26 1.390(9) . ? C25 H25A 0.9500 . ? C26 C27 1.397(9) . ? C26 H26A 0.9500 . ? P2 F2 1.595(4) . ? P2 F2 1.595(4) 3_556 ? P2 F1 1.596(4) . ? P2 F1 1.596(4) 3_556 ? P2 F3 1.600(4) 3_556 ? P2 F3 1.600(4) . ? P3 F7 1.519(12) . ? P3 F8 1.537(11) . ? P3 F9 1.541(12) . ? P3 F6 1.542(13) . ? P3 F4 1.552(13) . ? P3 F5 1.577(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 P1 88.91(6) . . ? S2 Pd1 Cl1 176.60(6) . . ? P1 Pd1 Cl1 94.24(6) . . ? S2 Pd1 S1 88.05(7) . . ? P1 Pd1 S1 163.53(7) . . ? Cl1 Pd1 S1 89.27(7) . . ? S2 Pd1 S3 84.72(6) . . ? P1 Pd1 S3 114.37(6) . . ? Cl1 Pd1 S3 92.82(6) . . ? S1 Pd1 S3 81.45(7) . . ? C13 P1 C27 108.2(3) . . ? C13 P1 C20 108.5(3) . . ? C27 P1 C20 101.7(3) . . ? C13 P1 Pd1 105.2(2) . . ? C27 P1 Pd1 122.1(2) . . ? C20 P1 Pd1 110.6(2) . . ? C1 S1 C6 103.4(5) . . ? C1 S1 Pd1 104.4(3) . . ? C6 S1 Pd1 105.4(3) . . ? C3 S2 C2 99.3(5) . . ? C3 S2 Pd1 107.9(3) . . ? C2 S2 Pd1 101.0(3) . . ? C5 S3 C4 103.6(4) . . ? C5 S3 Pd1 98.0(3) . . ? C4 S3 Pd1 91.3(3) . . ? C2 C1 S1 112.1(6) . . ? C2 C1 H1A 109.2 . . ? S1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? S1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 S2 114.9(7) . . ? C1 C2 H2A 108.5 . . ? S2 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? S2 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C4 C3 S2 119.9(6) . . ? C4 C3 H3A 107.3 . . ? S2 C3 H3A 107.3 . . ? C4 C3 H3B 107.3 . . ? S2 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C3 C4 S3 120.7(6) . . ? C3 C4 H4A 107.2 . . ? S3 C4 H4A 107.2 . . ? C3 C4 H4B 107.2 . . ? S3 C4 H4B 107.2 . . ? H4A C4 H4B 106.8 . . ? C6 C5 S3 114.3(6) . . ? C6 C5 H5A 108.7 . . ? S3 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? S3 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 S1 117.8(5) . . ? C5 C6 H6A 107.8 . . ? S1 C6 H6A 107.8 . . ? C5 C6 H6B 107.8 . . ? S1 C6 H6B 107.8 . . ? H6A C6 H6B 107.2 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.3(6) . . ? C9 C8 C7 117.9(6) . . ? C13 C8 C7 123.8(6) . . ? C10 C9 C8 121.5(7) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 120.2(7) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 120.1(7) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C13 120.7(7) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C8 C13 C12 119.1(6) . . ? C8 C13 P1 122.0(5) . . ? C12 C13 P1 118.4(5) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.4(6) . . ? C16 C15 C14 117.9(6) . . ? C20 C15 C14 123.7(6) . . ? C17 C16 C15 122.2(6) . . ? C17 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C18 C17 C16 119.6(7) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 119.5(7) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 121.9(6) . . ? C18 C19 H19A 119.1 . . ? C20 C19 H19A 119.1 . . ? C19 C20 C15 118.5(6) . . ? C19 C20 P1 117.1(5) . . ? C15 C20 P1 124.1(5) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 117.7(7) . . ? C23 C22 C21 118.2(6) . . ? C27 C22 C21 124.0(6) . . ? C24 C23 C22 122.4(7) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C25 120.0(7) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 119.7(7) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C22 119.9(6) . . ? C26 C27 P1 119.4(5) . . ? C22 C27 P1 120.4(5) . . ? F2 P2 F2 180.0(3) . 3_556 ? F2 P2 F1 89.8(2) . . ? F2 P2 F1 90.2(2) 3_556 . ? F2 P2 F1 90.2(2) . 3_556 ? F2 P2 F1 89.8(2) 3_556 3_556 ? F1 P2 F1 180.00(10) . 3_556 ? F2 P2 F3 89.2(2) . 3_556 ? F2 P2 F3 90.8(2) 3_556 3_556 ? F1 P2 F3 89.6(2) . 3_556 ? F1 P2 F3 90.4(2) 3_556 3_556 ? F2 P2 F3 90.8(2) . . ? F2 P2 F3 89.2(2) 3_556 . ? F1 P2 F3 90.4(2) . . ? F1 P2 F3 89.6(2) 3_556 . ? F3 P2 F3 180.0 3_556 . ? F7 P3 F8 93.3(10) . . ? F7 P3 F9 179.0(11) . . ? F8 P3 F9 85.9(10) . . ? F7 P3 F6 92.8(11) . . ? F8 P3 F6 92.9(12) . . ? F9 P3 F6 86.8(15) . . ? F7 P3 F4 87.7(12) . . ? F8 P3 F4 178.0(13) . . ? F9 P3 F4 93.1(12) . . ? F6 P3 F4 88.7(13) . . ? F7 P3 F5 87.8(11) . . ? F8 P3 F5 80.8(11) . . ? F9 P3 F5 92.6(15) . . ? F6 P3 F5 173.7(13) . . ? F4 P3 F5 97.5(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Pd1 P1 C13 -58.2(2) . . . . ? Cl1 Pd1 P1 C13 120.5(2) . . . . ? S1 Pd1 P1 C13 -137.6(3) . . . . ? S3 Pd1 P1 C13 25.5(2) . . . . ? S2 Pd1 P1 C27 178.3(3) . . . . ? Cl1 Pd1 P1 C27 -3.0(3) . . . . ? S1 Pd1 P1 C27 98.9(3) . . . . ? S3 Pd1 P1 C27 -98.0(3) . . . . ? S2 Pd1 P1 C20 58.8(2) . . . . ? Cl1 Pd1 P1 C20 -122.5(2) . . . . ? S1 Pd1 P1 C20 -20.6(3) . . . . ? S3 Pd1 P1 C20 142.5(2) . . . . ? S2 Pd1 S1 C1 -3.0(4) . . . . ? P1 Pd1 S1 C1 76.4(4) . . . . ? Cl1 Pd1 S1 C1 179.0(4) . . . . ? S3 Pd1 S1 C1 -88.0(4) . . . . ? S2 Pd1 S1 C6 105.5(3) . . . . ? P1 Pd1 S1 C6 -175.0(3) . . . . ? Cl1 Pd1 S1 C6 -72.4(3) . . . . ? S3 Pd1 S1 C6 20.6(3) . . . . ? P1 Pd1 S2 C3 115.4(4) . . . . ? S1 Pd1 S2 C3 -80.8(4) . . . . ? S3 Pd1 S2 C3 0.8(4) . . . . ? P1 Pd1 S2 C2 -141.0(4) . . . . ? S1 Pd1 S2 C2 22.8(4) . . . . ? S3 Pd1 S2 C2 104.4(4) . . . . ? S2 Pd1 S3 C5 -87.8(3) . . . . ? P1 Pd1 S3 C5 -174.2(3) . . . . ? Cl1 Pd1 S3 C5 89.9(3) . . . . ? S1 Pd1 S3 C5 1.0(3) . . . . ? S2 Pd1 S3 C4 16.2(3) . . . . ? P1 Pd1 S3 C4 -70.2(3) . . . . ? Cl1 Pd1 S3 C4 -166.2(3) . . . . ? S1 Pd1 S3 C4 105.0(3) . . . . ? C6 S1 C1 C2 -133.8(8) . . . . ? Pd1 S1 C1 C2 -23.7(9) . . . . ? S1 C1 C2 S2 48.4(10) . . . . ? C3 S2 C2 C1 63.6(8) . . . . ? Pd1 S2 C2 C1 -46.8(8) . . . . ? C2 S2 C3 C4 -130.7(8) . . . . ? Pd1 S2 C3 C4 -25.8(9) . . . . ? S2 C3 C4 S3 49.7(11) . . . . ? C5 S3 C4 C3 60.1(8) . . . . ? Pd1 S3 C4 C3 -38.5(8) . . . . ? C4 S3 C5 C6 -122.3(7) . . . . ? Pd1 S3 C5 C6 -29.1(6) . . . . ? S3 C5 C6 S1 56.6(8) . . . . ? C1 S1 C6 C5 58.3(7) . . . . ? Pd1 S1 C6 C5 -51.0(7) . . . . ? C13 C8 C9 C10 -2.2(10) . . . . ? C7 C8 C9 C10 176.5(7) . . . . ? C8 C9 C10 C11 -0.2(11) . . . . ? C9 C10 C11 C12 1.2(11) . . . . ? C10 C11 C12 C13 0.2(10) . . . . ? C9 C8 C13 C12 3.5(9) . . . . ? C7 C8 C13 C12 -175.1(6) . . . . ? C9 C8 C13 P1 175.7(5) . . . . ? C7 C8 C13 P1 -2.9(9) . . . . ? C11 C12 C13 C8 -2.6(9) . . . . ? C11 C12 C13 P1 -175.1(5) . . . . ? C27 P1 C13 C8 62.2(6) . . . . ? C20 P1 C13 C8 171.9(5) . . . . ? Pd1 P1 C13 C8 -69.7(5) . . . . ? C27 P1 C13 C12 -125.5(5) . . . . ? C20 P1 C13 C12 -15.9(6) . . . . ? Pd1 P1 C13 C12 102.5(5) . . . . ? C20 C15 C16 C17 0.3(10) . . . . ? C14 C15 C16 C17 -177.9(6) . . . . ? C15 C16 C17 C18 -0.8(11) . . . . ? C16 C17 C18 C19 1.5(11) . . . . ? C17 C18 C19 C20 -1.8(10) . . . . ? C18 C19 C20 C15 1.4(10) . . . . ? C18 C19 C20 P1 175.4(5) . . . . ? C16 C15 C20 C19 -0.6(9) . . . . ? C14 C15 C20 C19 177.5(6) . . . . ? C16 C15 C20 P1 -174.2(5) . . . . ? C14 C15 C20 P1 3.9(9) . . . . ? C13 P1 C20 C19 124.0(5) . . . . ? C27 P1 C20 C19 -122.0(5) . . . . ? Pd1 P1 C20 C19 9.1(5) . . . . ? C13 P1 C20 C15 -62.3(6) . . . . ? C27 P1 C20 C15 51.7(6) . . . . ? Pd1 P1 C20 C15 -177.2(5) . . . . ? C27 C22 C23 C24 0.2(10) . . . . ? C21 C22 C23 C24 -177.2(7) . . . . ? C22 C23 C24 C25 -0.3(11) . . . . ? C23 C24 C25 C26 0.1(11) . . . . ? C24 C25 C26 C27 0.2(10) . . . . ? C25 C26 C27 C22 -0.3(9) . . . . ? C25 C26 C27 P1 172.6(5) . . . . ? C23 C22 C27 C26 0.1(9) . . . . ? C21 C22 C27 C26 177.3(6) . . . . ? C23 C22 C27 P1 -172.7(5) . . . . ? C21 C22 C27 P1 4.6(9) . . . . ? C13 P1 C27 C26 1.8(6) . . . . ? C20 P1 C27 C26 -112.5(5) . . . . ? Pd1 P1 C27 C26 123.8(5) . . . . ? C13 P1 C27 C22 174.6(5) . . . . ? C20 P1 C27 C22 60.3(5) . . . . ? Pd1 P1 C27 C22 -63.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.573 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.119