Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mary F. Mahon' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email M.F.MAHON@BATH.AC.UK _publ_section_title ; Structure and reactivity of new phosphine ligands containing the hemi-labile sulfone moiety ; loop_ _publ_author_name 'M. Mahon' 'Christopher Chapman' 'Christopher Frost' data_k01cgf1 _database_code_depnum_ccdc_archive 'CCDC 232453' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H25 F3 N O5 P Pd S2' _chemical_formula_weight 713.98 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4590(1) _cell_length_b 12.1110(1) _cell_length_c 25.6990(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.0270(3) _cell_angle_gamma 90.00 _cell_volume 2899.06(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52542 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour v_pale_yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.43 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56679 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8465 _reflns_number_gt 7497 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0985P)^2^+6.5828P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8465 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 0.577 _refine_ls_restrained_S_all 0.577 _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 -0.066552(12) 0.284445(10) 0.678423(5) 0.01606(5) Uani 1 1 d . . . P1 P 0.02122(4) 0.18740(3) 0.616484(16) 0.01552(8) Uani 1 1 d . . . S1 S -0.26622(4) 0.04265(3) 0.590894(16) 0.01925(9) Uani 1 1 d . . . S2 S -0.14311(5) 0.50241(3) 0.611871(17) 0.02122(9) Uani 1 1 d . . . N1 N -0.16938(17) 0.34377(13) 0.74089(6) 0.0248(3) Uani 1 1 d . . . F1 F -0.40089(15) 0.54973(14) 0.56121(6) 0.0484(4) Uani 1 1 d . . . F2 F -0.23220(19) 0.65380(12) 0.54276(6) 0.0511(4) Uani 1 1 d . . . F3 F -0.2592(2) 0.48970(14) 0.51160(5) 0.0527(4) Uani 1 1 d . . . O1 O -0.29997(14) 0.11136(11) 0.63298(5) 0.0241(3) Uani 1 1 d . . . O2 O -0.37040(14) -0.03770(12) 0.56754(6) 0.0290(3) Uani 1 1 d . . . O3 O -0.16642(18) 0.57867(12) 0.65257(6) 0.0335(3) Uani 1 1 d . . . O4 O -0.19726(14) 0.39062(10) 0.61876(5) 0.0226(2) Uani 1 1 d . . . O5 O -0.00381(16) 0.50554(14) 0.59689(7) 0.0369(3) Uani 1 1 d . . . C11 C 0.19442(18) 0.22061(13) 0.60044(7) 0.0183(3) Uani 1 1 d . . . C12 C 0.26914(19) 0.31253(15) 0.62358(7) 0.0223(3) Uani 1 1 d . . . H12 H 0.2328 0.3537 0.6488 0.027 Uiso 1 1 calc R . . C13 C 0.39847(19) 0.34229(16) 0.60863(8) 0.0276(4) Uani 1 1 d . . . H13 H 0.4482 0.4038 0.6239 0.033 Uiso 1 1 calc R . . C14 C 0.4538(2) 0.28117(15) 0.57128(9) 0.0286(4) Uani 1 1 d . . . H14 H 0.5408 0.3011 0.5618 0.034 Uiso 1 1 calc R . . C15 C 0.3789(2) 0.18988(17) 0.54796(8) 0.0265(4) Uani 1 1 d . . . H15 H 0.4156 0.1493 0.5226 0.032 Uiso 1 1 calc R . . C16 C 0.24994(19) 0.15923(15) 0.56234(7) 0.0229(3) Uani 1 1 d . . . H16 H 0.2003 0.0980 0.5467 0.028 Uiso 1 1 calc R . . C21 C -0.09881(17) 0.19661(14) 0.55279(6) 0.0176(3) Uani 1 1 d . . . C22 C -0.0705(2) 0.27031(15) 0.51426(7) 0.0220(3) Uani 1 1 d . . . H22 H 0.0093 0.3163 0.5212 0.026 Uiso 1 1 calc R . . C23 C -0.1613(2) 0.27541(16) 0.46522(8) 0.0277(4) Uani 1 1 d . . . H23 H -0.1428 0.3257 0.4399 0.033 Uiso 1 1 calc R . . C24 C -0.2792(2) 0.20570(17) 0.45422(7) 0.0283(4) Uani 1 1 d . . . H24 H -0.3385 0.2091 0.4214 0.034 Uiso 1 1 calc R . . C25 C -0.30936(18) 0.13117(16) 0.49167(7) 0.0236(3) Uani 1 1 d . . . H25 H -0.3871 0.0834 0.4840 0.028 Uiso 1 1 calc R . . C26 C -0.22107(17) 0.12914(14) 0.54107(6) 0.0186(3) Uani 1 1 d . . . C31 C 0.02451(17) 0.03773(13) 0.62700(6) 0.0172(3) Uani 1 1 d . . . C32 C 0.15043(18) -0.01818(14) 0.64781(7) 0.0209(3) Uani 1 1 d . . . H32 H 0.2368 0.0202 0.6548 0.025 Uiso 1 1 calc R . . C33 C 0.1483(2) -0.13087(15) 0.65821(7) 0.0250(3) Uani 1 1 d . . . H33 H 0.2323 -0.1664 0.6736 0.030 Uiso 1 1 calc R . . C34 C 0.0216(2) -0.19063(15) 0.64569(8) 0.0266(4) Uani 1 1 d . . . H34 H 0.0210 -0.2660 0.6526 0.032 Uiso 1 1 calc R . . C35 C -0.1041(2) -0.13779(14) 0.62293(7) 0.0231(3) Uani 1 1 d . . . H35 H -0.1885 -0.1777 0.6132 0.028 Uiso 1 1 calc R . . C36 C -0.10217(18) -0.02476(14) 0.61495(6) 0.0186(3) Uani 1 1 d . . . C41 C 0.04955(19) 0.20179(13) 0.73738(7) 0.0198(3) Uani 1 1 d . . . C42 C 0.1888(2) 0.16084(15) 0.74187(7) 0.0239(3) Uani 1 1 d . . . H42 H 0.2386 0.1694 0.7139 0.029 Uiso 1 1 calc R . . C43 C 0.2546(2) 0.10716(15) 0.78778(8) 0.0280(4) Uani 1 1 d . . . H43 H 0.3466 0.0785 0.7898 0.034 Uiso 1 1 calc R . . C44 C 0.1835(2) 0.09623(15) 0.83039(8) 0.0291(4) Uani 1 1 d . . . H44 H 0.2272 0.0597 0.8608 0.035 Uiso 1 1 calc R . . C45 C 0.0463(2) 0.14024(16) 0.82740(7) 0.0286(4) Uani 1 1 d . . . H45 H -0.0009 0.1348 0.8562 0.034 Uiso 1 1 calc R . . C46 C -0.0203(2) 0.19255(15) 0.78108(7) 0.0236(3) Uani 1 1 d . . . C47 C -0.1662(2) 0.24390(18) 0.77568(8) 0.0300(4) Uani 1 1 d . . . H47A H -0.1856 0.2651 0.8101 0.036 Uiso 1 1 calc R . . H47B H -0.2390 0.1915 0.7601 0.036 Uiso 1 1 calc R . . C48 C -0.3199(2) 0.3780(2) 0.72289(9) 0.0384(5) Uani 1 1 d . . . H48A H -0.3633 0.3954 0.7530 0.058 Uiso 1 1 calc R . . H48B H -0.3720 0.3189 0.7033 0.058 Uiso 1 1 calc R . . H48C H -0.3222 0.4419 0.7007 0.058 Uiso 1 1 calc R . . C49 C -0.0886(3) 0.43540(17) 0.77056(8) 0.0343(4) Uani 1 1 d . . . H49A H -0.0862 0.4974 0.7474 0.051 Uiso 1 1 calc R . . H49B H 0.0076 0.4117 0.7840 0.051 Uiso 1 1 calc R . . H49C H -0.1350 0.4565 0.7994 0.051 Uiso 1 1 calc R . . C50 C -0.2660(2) 0.55057(16) 0.55337(8) 0.0280(4) 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 0.01861(8) 0.01419(7) 0.01516(7) -0.00016(4) 0.00229(5) 0.00107(4) P1 0.01642(18) 0.01368(17) 0.01596(18) -0.00107(14) 0.00144(14) -0.00027(13) S1 0.01658(17) 0.02071(19) 0.02056(18) -0.00048(14) 0.00352(14) -0.00249(14) S2 0.02310(19) 0.01793(18) 0.02187(19) 0.00231(14) 0.00181(15) -0.00082(14) N1 0.0273(7) 0.0262(7) 0.0219(7) 0.0029(6) 0.0070(6) 0.0070(6) F1 0.0285(6) 0.0632(10) 0.0509(9) 0.0114(7) -0.0002(6) 0.0108(6) F2 0.0697(10) 0.0295(7) 0.0487(8) 0.0202(6) -0.0045(7) -0.0027(7) F3 0.0765(11) 0.0525(9) 0.0242(6) -0.0045(6) -0.0051(6) 0.0249(8) O1 0.0239(6) 0.0271(6) 0.0233(6) 0.0000(5) 0.0093(5) 0.0018(5) O2 0.0224(6) 0.0285(7) 0.0350(7) -0.0026(6) 0.0015(5) -0.0091(5) O3 0.0515(9) 0.0217(6) 0.0267(7) -0.0030(5) 0.0050(6) -0.0035(6) O4 0.0246(6) 0.0179(5) 0.0237(6) 0.0026(5) -0.0003(5) 0.0001(4) O5 0.0230(7) 0.0412(9) 0.0466(9) 0.0097(7) 0.0068(6) -0.0016(6) C11 0.0166(7) 0.0167(7) 0.0213(7) -0.0004(5) 0.0022(6) -0.0012(5) C12 0.0211(7) 0.0179(7) 0.0266(8) -0.0022(6) 0.0011(6) -0.0012(6) C13 0.0205(8) 0.0215(8) 0.0396(10) -0.0020(7) 0.0017(7) -0.0047(6) C14 0.0177(8) 0.0263(9) 0.0425(11) 0.0040(7) 0.0070(7) -0.0009(6) C15 0.0213(8) 0.0284(9) 0.0311(9) -0.0014(7) 0.0081(7) 0.0029(7) C16 0.0211(8) 0.0206(8) 0.0272(8) -0.0041(6) 0.0044(6) -0.0005(6) C21 0.0186(7) 0.0184(7) 0.0159(7) -0.0013(6) 0.0036(5) 0.0011(5) C22 0.0247(8) 0.0216(7) 0.0207(8) 0.0018(6) 0.0065(6) 0.0010(6) C23 0.0342(10) 0.0298(9) 0.0192(8) 0.0056(7) 0.0050(7) 0.0041(7) C24 0.0279(9) 0.0388(11) 0.0159(8) 0.0001(7) -0.0024(7) 0.0055(7) C25 0.0191(7) 0.0298(9) 0.0211(8) -0.0048(7) 0.0011(6) 0.0010(6) C26 0.0194(7) 0.0194(7) 0.0172(7) -0.0015(6) 0.0036(6) 0.0006(6) C31 0.0199(7) 0.0141(7) 0.0170(7) -0.0015(5) 0.0018(5) -0.0004(5) C32 0.0217(7) 0.0177(7) 0.0221(8) -0.0007(6) 0.0004(6) 0.0007(6) C33 0.0275(8) 0.0189(8) 0.0282(9) 0.0015(6) 0.0036(7) 0.0048(6) C34 0.0326(9) 0.0157(7) 0.0320(9) 0.0026(7) 0.0074(7) 0.0003(7) C35 0.0256(8) 0.0181(7) 0.0263(8) -0.0015(6) 0.0063(6) -0.0040(6) C36 0.0193(7) 0.0180(7) 0.0186(7) -0.0004(6) 0.0037(6) -0.0003(6) C41 0.0247(8) 0.0163(7) 0.0166(7) -0.0007(5) -0.0016(6) 0.0004(6) C42 0.0282(8) 0.0204(8) 0.0212(8) -0.0033(6) -0.0011(6) 0.0026(6) C43 0.0315(9) 0.0208(8) 0.0271(9) -0.0036(7) -0.0078(7) 0.0043(7) C44 0.0421(11) 0.0176(8) 0.0224(8) 0.0033(6) -0.0082(7) -0.0031(7) C45 0.0413(10) 0.0229(8) 0.0200(8) 0.0052(6) 0.0009(7) -0.0046(7) C46 0.0296(9) 0.0205(7) 0.0201(8) 0.0023(6) 0.0028(6) -0.0019(7) C47 0.0327(9) 0.0332(10) 0.0266(9) 0.0086(8) 0.0125(7) 0.0028(8) C48 0.0313(10) 0.0502(13) 0.0371(11) 0.0120(10) 0.0150(9) 0.0151(9) C49 0.0510(12) 0.0269(9) 0.0258(9) -0.0070(7) 0.0092(8) 0.0073(9) C50 0.0354(10) 0.0222(8) 0.0249(8) 0.0039(7) 0.0014(7) 0.0056(7) _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 C41 1.9810(17) . ? Pd1 N1 2.1408(15) . ? Pd1 O4 2.2075(12) . ? Pd1 P1 2.2504(4) . ? Pd1 O1 3.1200(14) . ? P1 C11 1.8030(17) . ? P1 C21 1.8259(17) . ? P1 C31 1.8321(16) . ? S1 O2 1.4397(14) . ? S1 O1 1.4439(13) . ? S1 C26 1.7634(17) . ? S1 C36 1.7671(17) . ? S2 O5 1.4362(15) . ? S2 O3 1.4409(15) . ? S2 O4 1.4691(13) . ? S2 C50 1.8285(19) . ? N1 C48 1.478(3) . ? N1 C49 1.481(3) . ? N1 C47 1.501(2) . ? F1 C50 1.326(2) . ? F2 C50 1.330(2) . ? F3 C50 1.313(2) . ? C11 C12 1.395(2) . ? C11 C16 1.402(2) . ? C12 C13 1.392(3) . ? C13 C14 1.385(3) . ? C14 C15 1.391(3) . ? C15 C16 1.385(2) . ? C21 C22 1.393(2) . ? C21 C26 1.405(2) . ? C22 C23 1.398(3) . ? C23 C24 1.388(3) . ? C24 C25 1.385(3) . ? C25 C26 1.393(2) . ? C31 C32 1.393(2) . ? C31 C36 1.405(2) . ? C32 C33 1.392(2) . ? C33 C34 1.389(3) . ? C34 C35 1.387(3) . ? C35 C36 1.385(2) . ? C41 C42 1.394(2) . ? C41 C46 1.403(3) . ? C42 C43 1.395(3) . ? C43 C44 1.387(3) . ? C44 C45 1.392(3) . ? C45 C46 1.398(2) . ? C46 C47 1.498(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Pd1 N1 81.94(7) . . ? C41 Pd1 O4 173.97(6) . . ? N1 Pd1 O4 93.02(5) . . ? C41 Pd1 P1 93.06(5) . . ? N1 Pd1 P1 167.79(5) . . ? O4 Pd1 P1 92.52(4) . . ? C41 Pd1 O1 102.05(6) . . ? N1 Pd1 O1 97.00(5) . . ? O4 Pd1 O1 81.79(4) . . ? P1 Pd1 O1 73.06(3) . . ? C11 P1 C21 103.26(8) . . ? C11 P1 C31 105.17(7) . . ? C21 P1 C31 100.64(8) . . ? C11 P1 Pd1 120.46(6) . . ? C21 P1 Pd1 110.72(5) . . ? C31 P1 Pd1 114.28(5) . . ? O2 S1 O1 118.51(8) . . ? O2 S1 C26 109.48(8) . . ? O1 S1 C26 108.34(8) . . ? O2 S1 C36 109.22(8) . . ? O1 S1 C36 107.42(8) . . ? C26 S1 C36 102.69(8) . . ? O5 S2 O3 116.18(10) . . ? O5 S2 O4 114.33(9) . . ? O3 S2 O4 113.74(8) . . ? O5 S2 C50 104.64(10) . . ? O3 S2 C50 103.70(9) . . ? O4 S2 C50 102.01(8) . . ? C48 N1 C49 109.47(17) . . ? C48 N1 C47 109.32(16) . . ? C49 N1 C47 110.00(16) . . ? C48 N1 Pd1 113.46(13) . . ? C49 N1 Pd1 112.12(12) . . ? C47 N1 Pd1 102.21(11) . . ? S1 O1 Pd1 115.67(7) . . ? S2 O4 Pd1 117.11(7) . . ? C12 C11 C16 119.81(16) . . ? C12 C11 P1 119.58(13) . . ? C16 C11 P1 120.47(12) . . ? C13 C12 C11 119.56(17) . . ? C14 C13 C12 120.61(17) . . ? C13 C14 C15 119.87(17) . . ? C16 C15 C14 120.25(18) . . ? C15 C16 C11 119.90(16) . . ? C22 C21 C26 118.24(15) . . ? C22 C21 P1 120.64(13) . . ? C26 C21 P1 121.11(12) . . ? C21 C22 C23 120.32(17) . . ? C24 C23 C22 120.18(17) . . ? C25 C24 C23 120.70(17) . . ? C24 C25 C26 118.77(17) . . ? C25 C26 C21 121.70(16) . . ? C25 C26 S1 119.32(13) . . ? C21 C26 S1 118.95(12) . . ? C32 C31 C36 117.51(15) . . ? C32 C31 P1 121.93(12) . . ? C36 C31 P1 120.55(12) . . ? C33 C32 C31 120.69(16) . . ? C34 C33 C32 120.48(17) . . ? C35 C34 C33 119.94(17) . . ? C36 C35 C34 119.10(17) . . ? C35 C36 C31 122.17(16) . . ? C35 C36 S1 118.37(13) . . ? C31 C36 S1 119.43(12) . . ? C42 C41 C46 118.38(16) . . ? C42 C41 Pd1 129.30(14) . . ? C46 C41 Pd1 112.15(13) . . ? C41 C42 C43 120.76(18) . . ? C44 C43 C42 120.41(18) . . ? C43 C44 C45 119.67(17) . . ? C44 C45 C46 119.86(19) . . ? C45 C46 C41 120.84(18) . . ? C45 C46 C47 122.57(18) . . ? C41 C46 C47 116.57(16) . . ? C46 C47 N1 108.20(15) . . ? F3 C50 F1 107.77(18) . . ? F3 C50 F2 108.21(18) . . ? F1 C50 F2 108.08(17) . . ? F3 C50 S2 112.25(14) . . ? F1 C50 S2 111.31(14) . . ? F2 C50 S2 109.10(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.473 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.071 data_c:\backup\helix\h01cgf4\maxus\h01cgf4 _database_code_depnum_ccdc_archive 'CCDC 232454' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 F6 N O3 P Pd S Sb' _chemical_formula_weight 818.68 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7950(1) _cell_length_b 14.2050(1) _cell_length_c 15.4340(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.108(1) _cell_angle_gamma 90.00 _cell_volume 2933.19(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34173 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 33.142 _exptl_crystal_description Tabloid _exptl_crystal_colour v_pale_yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59819 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 33.14 _reflns_number_total 11173 _reflns_number_gt 9319 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.4902*P+(0.0256P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00140(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11173 _refine_ls_number_parameters 381 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _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 Sb1 Sb 0.536856(8) 0.476027(8) 0.736969(8) 0.02259(3) Uani 1 1 d . . . Pd1 Pd 0.973998(8) 0.316936(8) 0.814925(8) 0.01833(3) Uani 1 1 d . . . S1 S 0.87748(3) 0.55726(3) 0.73268(3) 0.01929(7) Uani 1 1 d . . . P1 P 0.99915(3) 0.37977(3) 0.68864(3) 0.01702(7) Uani 1 1 d . . . F1 F 0.53997(10) 0.47151(9) 0.61655(8) 0.0408(3) Uani 1 1 d . . . F2 F 0.62727(9) 0.57644(9) 0.75458(10) 0.0462(3) Uani 1 1 d . . . F3 F 0.53172(12) 0.48157(11) 0.85662(9) 0.0517(4) Uani 1 1 d . . . F4 F 0.44541(11) 0.37699(9) 0.71647(11) 0.0541(4) Uani 1 1 d . . . F5 F 0.43112(8) 0.56213(9) 0.70704(8) 0.0383(3) Uani 1 1 d . . . F6 F 0.64310(10) 0.39014(10) 0.76664(11) 0.0557(4) Uani 1 1 d . . . O1 O 0.87227(9) 0.50003(9) 0.80844(8) 0.0244(2) Uani 1 1 d . . . O2 O 0.83118(9) 0.64898(8) 0.72487(9) 0.0275(2) Uani 1 1 d . . . O3 O 0.81731(10) 0.28308(10) 0.74988(10) 0.0309(3) Uani 1 1 d D . . N1 N 0.95863(11) 0.29328(10) 0.94755(10) 0.0234(3) Uani 1 1 d . . . C1 C 1.11410(12) 0.34216(11) 0.87947(11) 0.0214(3) Uani 1 1 d . . . C2 C 1.20063(12) 0.33661(13) 0.84858(11) 0.0253(3) Uani 1 1 d . . . H2 H 1.1963 0.3175 0.7888 0.030 Uiso 1 1 calc R . . C3 C 1.29412(13) 0.35890(14) 0.90450(13) 0.0306(4) Uani 1 1 d . . . H3 H 1.3527 0.3556 0.8827 0.037 Uiso 1 1 calc R . . C4 C 1.30011(14) 0.38584(15) 0.99195(13) 0.0349(4) Uani 1 1 d . . . H4 H 1.3628 0.4035 1.0295 0.042 Uiso 1 1 calc R . . C5 C 1.21549(15) 0.38723(14) 1.02493(13) 0.0341(4) Uani 1 1 d . . . H5 H 1.2208 0.4030 1.0857 0.041 Uiso 1 1 calc R . . C6 C 1.12276(13) 0.36560(12) 0.96948(12) 0.0265(3) Uani 1 1 d . . . C7 C 1.02780(15) 0.36417(14) 1.00077(13) 0.0327(4) Uani 1 1 d . . . H7A H 1.0427 0.3477 1.0650 0.039 Uiso 1 1 calc R . . H7B H 0.9962 0.4272 0.9929 0.039 Uiso 1 1 calc R . . C8 C 0.99037(15) 0.19758(13) 0.98028(14) 0.0327(4) Uani 1 1 d . . . H8A H 1.0607 0.1883 0.9801 0.049 Uiso 1 1 calc R . . H8B H 0.9492 0.1509 0.9412 0.049 Uiso 1 1 calc R . . H8C H 0.9822 0.1901 1.0412 0.049 Uiso 1 1 calc R . . C9 C 0.85569(14) 0.31024(15) 0.95755(14) 0.0346(4) Uani 1 1 d . . . H9A H 0.8111 0.2608 0.9263 0.052 Uiso 1 1 calc R . . H9B H 0.8322 0.3717 0.9319 0.052 Uiso 1 1 calc R . . H9C H 0.8558 0.3095 1.0211 0.052 Uiso 1 1 calc R . . C10 C 1.05864(11) 0.31146(11) 0.61757(11) 0.0199(3) Uani 1 1 d . . . C11 C 1.06400(13) 0.21457(12) 0.63296(12) 0.0241(3) Uani 1 1 d . . . H11 H 1.0467 0.1894 0.6842 0.029 Uiso 1 1 calc R . . C12 C 1.09456(14) 0.15476(13) 0.57337(13) 0.0296(4) Uani 1 1 d . . . H12 H 1.0977 0.0888 0.5837 0.036 Uiso 1 1 calc R . . C13 C 1.12024(14) 0.19133(13) 0.49933(13) 0.0299(4) Uani 1 1 d . . . H13 H 1.1407 0.1504 0.4584 0.036 Uiso 1 1 calc R . . C14 C 1.11632(14) 0.28766(14) 0.48440(13) 0.0307(4) Uani 1 1 d . . . H14 H 1.1348 0.3124 0.4335 0.037 Uiso 1 1 calc R . . C15 C 1.08573(14) 0.34821(13) 0.54299(12) 0.0270(3) Uani 1 1 d . . . H15 H 1.0832 0.4142 0.5325 0.032 Uiso 1 1 calc R . . C16 C 0.88061(11) 0.41441(11) 0.61385(10) 0.0185(3) Uani 1 1 d . . . C17 C 0.83822(13) 0.36358(12) 0.53673(11) 0.0246(3) Uani 1 1 d . . . H17 H 0.8711 0.3093 0.5219 0.030 Uiso 1 1 calc R . . C18 C 0.74740(13) 0.39236(14) 0.48118(12) 0.0297(4) Uani 1 1 d . . . H18 H 0.7188 0.3572 0.4289 0.036 Uiso 1 1 calc R . . C19 C 0.69867(13) 0.47107(14) 0.50112(13) 0.0306(4) Uani 1 1 d . . . H19 H 0.6374 0.4904 0.4622 0.037 Uiso 1 1 calc R . . C20 C 0.73917(12) 0.52225(12) 0.57827(12) 0.0262(3) Uani 1 1 d . . . H20 H 0.7058 0.5764 0.5927 0.031 Uiso 1 1 calc R . . C21 C 0.82883(11) 0.49319(11) 0.63378(11) 0.0194(3) Uani 1 1 d . . . C22 C 1.05892(11) 0.49502(11) 0.70927(10) 0.0188(3) Uani 1 1 d . . . C23 C 1.15892(12) 0.51042(12) 0.70979(12) 0.0244(3) Uani 1 1 d . . . H23 H 1.1975 0.4609 0.6938 0.029 Uiso 1 1 calc R . . C24 C 1.20253(13) 0.59817(14) 0.73363(13) 0.0295(4) Uani 1 1 d . . . H24 H 1.2711 0.6074 0.7349 0.035 Uiso 1 1 calc R . . C25 C 1.14771(14) 0.67166(13) 0.75543(14) 0.0315(4) Uani 1 1 d . . . H25 H 1.1787 0.7308 0.7724 0.038 Uiso 1 1 calc R . . C26 C 1.04658(13) 0.65922(12) 0.75250(12) 0.0267(3) Uani 1 1 d . . . H26 H 1.0075 0.7100 0.7653 0.032 Uiso 1 1 calc R . . C27 C 1.00440(11) 0.57121(11) 0.73061(10) 0.0198(3) Uani 1 1 d . . . H3A H 0.801(2) 0.2255(14) 0.753(2) 0.073(10) Uiso 1 1 d D . . H3B H 0.769(2) 0.314(3) 0.765(3) 0.106(14) Uiso 1 1 d 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 Sb1 0.02090(5) 0.01902(5) 0.02702(6) -0.00097(4) 0.00421(4) 0.00137(4) Pd1 0.01648(5) 0.01859(6) 0.02101(6) 0.00211(4) 0.00664(4) 0.00107(4) S1 0.01791(16) 0.01737(16) 0.02390(18) -0.00187(13) 0.00759(13) 0.00050(13) P1 0.01627(16) 0.01646(17) 0.01871(17) 0.00078(13) 0.00502(13) 0.00109(13) F1 0.0433(7) 0.0500(8) 0.0309(6) -0.0087(5) 0.0128(5) 0.0015(6) F2 0.0367(6) 0.0382(7) 0.0592(8) -0.0068(6) 0.0032(6) -0.0162(5) F3 0.0640(9) 0.0636(9) 0.0277(6) 0.0065(6) 0.0116(6) 0.0089(7) F4 0.0516(8) 0.0321(7) 0.0797(10) -0.0039(7) 0.0181(7) -0.0189(6) F5 0.0312(6) 0.0398(6) 0.0399(6) -0.0079(5) 0.0011(5) 0.0161(5) F6 0.0431(7) 0.0456(8) 0.0737(10) 0.0058(7) 0.0054(7) 0.0253(6) O1 0.0259(6) 0.0254(6) 0.0244(6) 0.0000(4) 0.0110(5) -0.0003(5) O2 0.0259(6) 0.0195(6) 0.0396(7) -0.0016(5) 0.0129(5) 0.0030(5) O3 0.0224(6) 0.0282(7) 0.0421(8) 0.0056(6) 0.0077(5) -0.0045(5) N1 0.0251(7) 0.0234(7) 0.0244(7) 0.0018(5) 0.0115(5) 0.0005(5) C1 0.0206(7) 0.0204(7) 0.0228(7) 0.0022(6) 0.0048(5) 0.0005(6) C2 0.0215(7) 0.0306(8) 0.0237(8) 0.0030(6) 0.0051(6) 0.0018(6) C3 0.0208(7) 0.0354(10) 0.0348(9) 0.0055(8) 0.0049(7) 0.0007(7) C4 0.0264(8) 0.0378(10) 0.0350(10) -0.0009(8) -0.0028(7) -0.0053(8) C5 0.0382(10) 0.0352(10) 0.0271(9) -0.0062(7) 0.0047(7) -0.0072(8) C6 0.0295(8) 0.0252(8) 0.0259(8) -0.0033(6) 0.0088(6) -0.0026(6) C7 0.0373(10) 0.0342(9) 0.0305(9) -0.0094(7) 0.0159(7) -0.0080(8) C8 0.0340(9) 0.0273(8) 0.0385(10) 0.0122(7) 0.0120(8) 0.0019(7) C9 0.0294(9) 0.0425(11) 0.0384(10) 0.0040(8) 0.0205(8) 0.0035(8) C10 0.0186(6) 0.0207(7) 0.0212(7) 0.0003(5) 0.0062(5) 0.0030(5) C11 0.0266(8) 0.0210(7) 0.0265(8) 0.0023(6) 0.0098(6) 0.0026(6) C12 0.0324(9) 0.0212(8) 0.0380(10) -0.0033(7) 0.0139(7) 0.0021(7) C13 0.0282(8) 0.0315(9) 0.0327(9) -0.0098(7) 0.0126(7) -0.0004(7) C14 0.0337(9) 0.0347(9) 0.0281(9) -0.0012(7) 0.0159(7) 0.0002(7) C15 0.0322(9) 0.0251(8) 0.0272(8) 0.0030(6) 0.0139(7) 0.0029(7) C16 0.0176(6) 0.0190(7) 0.0189(7) 0.0013(5) 0.0043(5) -0.0007(5) C17 0.0245(7) 0.0245(8) 0.0247(8) -0.0034(6) 0.0059(6) -0.0033(6) C18 0.0262(8) 0.0388(10) 0.0222(8) -0.0041(7) 0.0024(6) -0.0070(7) C19 0.0197(7) 0.0391(10) 0.0292(9) 0.0040(7) -0.0009(6) -0.0003(7) C20 0.0184(7) 0.0266(8) 0.0324(9) 0.0046(6) 0.0040(6) 0.0020(6) C21 0.0181(6) 0.0175(7) 0.0224(7) 0.0006(5) 0.0047(5) -0.0009(5) C22 0.0175(6) 0.0199(7) 0.0189(7) 0.0008(5) 0.0045(5) -0.0011(5) C23 0.0197(7) 0.0270(8) 0.0277(8) -0.0008(6) 0.0080(6) -0.0008(6) C24 0.0210(7) 0.0349(9) 0.0337(9) -0.0022(7) 0.0089(7) -0.0090(7) C25 0.0298(9) 0.0279(9) 0.0385(10) -0.0065(7) 0.0118(7) -0.0126(7) C26 0.0275(8) 0.0222(8) 0.0321(9) -0.0052(6) 0.0105(7) -0.0040(6) C27 0.0178(6) 0.0202(7) 0.0220(7) -0.0008(5) 0.0061(5) -0.0024(5) _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 Sb1 F4 1.8644(12) . ? Sb1 F3 1.8669(13) . ? Sb1 F2 1.8705(12) . ? Sb1 F1 1.8705(12) . ? Sb1 F5 1.8731(11) . ? Sb1 F6 1.8760(12) . ? Pd1 C1 1.9793(16) . ? Pd1 N1 2.1352(14) . ? Pd1 O3 2.2031(13) . ? Pd1 P1 2.2462(4) . ? Pd1 O1 2.9454(12) . ? S1 O1 1.4402(13) . ? S1 O2 1.4430(12) . ? S1 C21 1.7633(16) . ? S1 C27 1.7701(16) . ? P1 C10 1.8047(16) . ? P1 C16 1.8245(15) . ? P1 C22 1.8258(16) . ? N1 C8 1.479(2) . ? N1 C9 1.485(2) . ? N1 C7 1.489(2) . ? C1 C2 1.391(2) . ? C1 C6 1.405(2) . ? C2 C3 1.402(2) . ? C3 C4 1.386(3) . ? C4 C5 1.383(3) . ? C5 C6 1.389(3) . ? C6 C7 1.503(3) . ? C10 C15 1.395(2) . ? C10 C11 1.396(2) . ? C11 C12 1.391(2) . ? C12 C13 1.378(3) . ? C13 C14 1.387(3) . ? C14 C15 1.386(2) . ? C16 C17 1.393(2) . ? C16 C21 1.402(2) . ? C17 C18 1.396(2) . ? C18 C19 1.377(3) . ? C19 C20 1.391(3) . ? C20 C21 1.385(2) . ? C22 C23 1.395(2) . ? C22 C27 1.402(2) . ? C23 C24 1.394(2) . ? C24 C25 1.378(3) . ? C25 C26 1.396(2) . ? C26 C27 1.386(2) . ? 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 F4 Sb1 F3 90.71(7) . . ? F4 Sb1 F2 178.55(7) . . ? F3 Sb1 F2 90.51(7) . . ? F4 Sb1 F1 89.08(7) . . ? F3 Sb1 F1 179.05(6) . . ? F2 Sb1 F1 89.69(6) . . ? F4 Sb1 F5 89.82(6) . . ? F3 Sb1 F5 90.08(6) . . ? F2 Sb1 F5 89.40(6) . . ? F1 Sb1 F5 88.99(6) . . ? F4 Sb1 F6 90.39(7) . . ? F3 Sb1 F6 90.10(7) . . ? F2 Sb1 F6 90.40(7) . . ? F1 Sb1 F6 90.83(6) . . ? F5 Sb1 F6 179.73(7) . . ? C1 Pd1 N1 81.89(6) . . ? C1 Pd1 O3 176.47(6) . . ? N1 Pd1 O3 94.98(5) . . ? C1 Pd1 P1 91.51(5) . . ? N1 Pd1 P1 165.19(4) . . ? O3 Pd1 P1 91.91(4) . . ? C1 Pd1 O1 104.83(5) . . ? N1 Pd1 O1 90.79(5) . . ? O3 Pd1 O1 76.75(4) . . ? P1 Pd1 O1 78.04(3) . . ? O1 S1 O2 117.95(8) . . ? O1 S1 C21 109.13(7) . . ? O2 S1 C21 109.05(8) . . ? O1 S1 C27 108.86(7) . . ? O2 S1 C27 108.48(7) . . ? C21 S1 C27 102.22(7) . . ? C10 P1 C16 103.34(7) . . ? C10 P1 C22 109.58(7) . . ? C16 P1 C22 99.53(7) . . ? C10 P1 Pd1 120.20(5) . . ? C16 P1 Pd1 110.61(5) . . ? C22 P1 Pd1 111.33(5) . . ? S1 O1 Pd1 114.10(6) . . ? C8 N1 C9 108.94(14) . . ? C8 N1 C7 109.67(15) . . ? C9 N1 C7 109.47(15) . . ? C8 N1 Pd1 112.45(11) . . ? C9 N1 Pd1 113.27(11) . . ? C7 N1 Pd1 102.85(10) . . ? C2 C1 C6 118.62(15) . . ? C2 C1 Pd1 129.15(12) . . ? C6 C1 Pd1 112.19(12) . . ? C1 C2 C3 120.91(16) . . ? C4 C3 C2 119.30(17) . . ? C5 C4 C3 120.48(17) . . ? C4 C5 C6 120.23(18) . . ? C5 C6 C1 120.34(17) . . ? C5 C6 C7 123.30(17) . . ? C1 C6 C7 116.36(15) . . ? N1 C7 C6 108.87(14) . . ? C15 C10 C11 119.71(15) . . ? C15 C10 P1 123.58(12) . . ? C11 C10 P1 116.10(12) . . ? C12 C11 C10 120.13(16) . . ? C13 C12 C11 119.91(17) . . ? C12 C13 C14 120.17(17) . . ? C15 C14 C13 120.63(17) . . ? C14 C15 C10 119.43(16) . . ? C17 C16 C21 118.11(14) . . ? C17 C16 P1 121.71(12) . . ? C21 C16 P1 120.17(12) . . ? C16 C17 C18 120.00(16) . . ? C19 C18 C17 120.95(16) . . ? C18 C19 C20 119.97(16) . . ? C21 C20 C19 119.06(16) . . ? C20 C21 C16 121.89(15) . . ? C20 C21 S1 118.41(13) . . ? C16 C21 S1 119.69(11) . . ? C23 C22 C27 117.64(15) . . ? C23 C22 P1 123.07(12) . . ? C27 C22 P1 119.19(11) . . ? C24 C23 C22 120.29(16) . . ? C25 C24 C23 120.98(16) . . ? C24 C25 C26 119.98(16) . . ? C27 C26 C25 118.62(16) . . ? C26 C27 C22 122.43(15) . . ? C26 C27 S1 117.07(12) . . ? C22 C27 S1 120.49(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.740 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.088 # Attachment 'cpd16_h01cgf5.cif' data_c:\backup\helix\h01cgf5\maxus\k01cgf5 _database_code_depnum_ccdc_archive 'CCDC 232455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.25 H50 Cl3 N2 O2 P Pd S' _chemical_formula_weight 881.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6200(1) _cell_length_b 15.3270(1) _cell_length_c 15.3980(1) _cell_angle_alpha 108.523(1) _cell_angle_beta 100.290(1) _cell_angle_gamma 108.962(1) _cell_volume 2133.66(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39265 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 911 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.7701 _exptl_absorpt_correction_T_max 0.8357 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43431 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 30.09 _reflns_number_total 12423 _reflns_number_gt 10845 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.1573*P+(0.0452P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0065(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12423 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.391148(12) 0.241485(9) 0.297030(8) 0.01846(5) Uani 1 1 d . . . Cl1 Cl 0.30969(4) 0.15696(3) 0.12259(3) 0.02591(9) Uani 1 1 d . . . Cl2 Cl -0.01502(8) 0.17688(6) -0.05646(6) 0.06387(19) Uani 1 1 d . . . Cl3 Cl 0.05564(9) 0.03907(7) -0.19760(6) 0.0690(2) Uani 1 1 d . . . S1 S 0.74311(4) 0.33985(3) 0.21754(3) 0.01934(8) Uani 1 1 d . . . P1 P 0.55591(4) 0.18017(3) 0.30915(3) 0.01704(8) Uani 1 1 d . . . O1 O 0.88687(13) 0.38595(9) 0.27784(9) 0.0262(3) Uani 1 1 d . . . O2 O 0.64107(14) 0.35949(9) 0.26150(9) 0.0255(3) Uani 1 1 d . . . N1 N 0.25686(15) 0.31842(11) 0.29448(11) 0.0240(3) Uani 1 1 d . . . N2 N 0.73782(15) 0.36814(10) 0.12401(10) 0.0213(3) Uani 1 1 d . . . C1 C 0.40943(17) 0.29053(13) 0.43804(12) 0.0225(3) Uani 1 1 d . . . C2 C 0.4567(2) 0.25751(15) 0.50690(14) 0.0302(4) Uani 1 1 d . . . H2 H 0.4919 0.2070 0.4892 0.036 Uiso 1 1 calc R . . C3 C 0.4535(2) 0.29705(17) 0.60133(14) 0.0363(4) Uani 1 1 d . . . H3 H 0.4864 0.2733 0.6468 0.044 Uiso 1 1 calc R . . C4 C 0.4026(2) 0.37068(17) 0.62894(14) 0.0369(5) Uani 1 1 d . . . H4 H 0.4019 0.3983 0.6934 0.044 Uiso 1 1 calc R . . C5 C 0.35317(19) 0.40351(15) 0.56198(14) 0.0318(4) Uani 1 1 d . . . H5 H 0.3177 0.4537 0.5805 0.038 Uiso 1 1 calc R . . C6 C 0.35462(17) 0.36355(13) 0.46696(13) 0.0254(3) Uani 1 1 d . . . C7 C 0.3037(2) 0.39898(14) 0.39375(14) 0.0292(4) Uani 1 1 d . . . H7A H 0.3800 0.4604 0.3992 0.035 Uiso 1 1 calc R . . H7B H 0.2246 0.4163 0.4058 0.035 Uiso 1 1 calc R . . C8 C 0.2678(2) 0.36696(17) 0.22516(16) 0.0364(4) Uani 1 1 d . . . H8A H 0.2291 0.3149 0.1592 0.055 Uiso 1 1 calc R . . H8B H 0.3666 0.4088 0.2376 0.055 Uiso 1 1 calc R . . H8C H 0.2151 0.4093 0.2329 0.055 Uiso 1 1 calc R . . C9 C 0.11018(19) 0.24676(16) 0.26905(15) 0.0335(4) Uani 1 1 d . . . H9A H 0.0490 0.2829 0.2708 0.050 Uiso 1 1 calc R . . H9B H 0.1027 0.2155 0.3155 0.050 Uiso 1 1 calc R . . H9C H 0.0816 0.1944 0.2041 0.050 Uiso 1 1 calc R . . C10 C 0.49188(18) 0.06508(12) 0.33021(12) 0.0218(3) Uani 1 1 d . . . C11 C 0.5757(2) 0.03411(15) 0.38251(15) 0.0317(4) Uani 1 1 d . . . H11 H 0.6738 0.0740 0.4101 0.038 Uiso 1 1 calc R . . C12 C 0.5173(3) -0.05479(16) 0.39489(17) 0.0409(5) Uani 1 1 d . . . H12 H 0.5758 -0.0751 0.4309 0.049 Uiso 1 1 calc R . . C13 C 0.3755(3) -0.11342(16) 0.35531(17) 0.0424(5) Uani 1 1 d . . . H13 H 0.3360 -0.1742 0.3638 0.051 Uiso 1 1 calc R . . C14 C 0.2910(3) -0.08361(17) 0.3033(2) 0.0488(6) Uani 1 1 d . . . H14 H 0.1931 -0.1241 0.2757 0.059 Uiso 1 1 calc R . . C15 C 0.3484(2) 0.00551(15) 0.29103(17) 0.0372(5) Uani 1 1 d . . . H15 H 0.2892 0.0258 0.2556 0.045 Uiso 1 1 calc R . . C16 C 0.72766(16) 0.26031(12) 0.39995(11) 0.0196(3) Uani 1 1 d . . . C17 C 0.83852(18) 0.23001(14) 0.39835(12) 0.0245(3) Uani 1 1 d . . . H17 H 0.8237 0.1670 0.3510 0.029 Uiso 1 1 calc R . . C18 C 0.97021(19) 0.29204(16) 0.46593(13) 0.0292(4) Uani 1 1 d . . . H18 H 1.0447 0.2706 0.4656 0.035 Uiso 1 1 calc R . . C19 C 0.99310(19) 0.38468(16) 0.53355(13) 0.0312(4) Uani 1 1 d . . . H19 H 1.0836 0.4273 0.5791 0.037 Uiso 1 1 calc R . . C20 C 0.88436(19) 0.41563(15) 0.53505(13) 0.0299(4) Uani 1 1 d . . . H20 H 0.9005 0.4794 0.5818 0.036 Uiso 1 1 calc R . . C21 C 0.75194(18) 0.35400(13) 0.46864(12) 0.0240(3) Uani 1 1 d . . . H21 H 0.6778 0.3757 0.4700 0.029 Uiso 1 1 calc R . . C22 C 0.61106(16) 0.13989(12) 0.20110(11) 0.0179(3) Uani 1 1 d . . . C23 C 0.58163(18) 0.03761(12) 0.15444(12) 0.0228(3) Uani 1 1 d . . . H23 H 0.5262 -0.0094 0.1751 0.027 Uiso 1 1 calc R . . C24 C 0.6313(2) 0.00294(13) 0.07871(13) 0.0261(3) Uani 1 1 d . . . H24 H 0.6077 -0.0672 0.0474 0.031 Uiso 1 1 calc R . . C25 C 0.7148(2) 0.06979(14) 0.04869(13) 0.0268(4) Uani 1 1 d . . . H25 H 0.7515 0.0464 -0.0016 0.032 Uiso 1 1 calc R . . C26 C 0.74437(18) 0.17141(13) 0.09280(12) 0.0232(3) Uani 1 1 d . . . H26 H 0.8015 0.2178 0.0723 0.028 Uiso 1 1 calc R . . C27 C 0.69143(16) 0.20638(12) 0.16665(11) 0.0186(3) Uani 1 1 d . . . C28 C 0.85329(19) 0.45668(13) 0.12576(13) 0.0261(3) Uani 1 1 d . . . H28 H 0.8183 0.4655 0.0657 0.031 Uiso 1 1 calc R . . C29 C 0.9829(2) 0.43524(18) 0.11858(16) 0.0370(5) Uani 1 1 d . . . H29A H 1.0125 0.4155 0.1714 0.044 Uiso 1 1 calc R . . H29B H 0.9576 0.3776 0.0567 0.044 Uiso 1 1 calc R . . C30 C 1.1061(2) 0.5255(2) 0.12443(18) 0.0538(7) Uani 1 1 d . . . H30A H 1.1903 0.5105 0.1294 0.065 Uiso 1 1 calc R . . H30B H 1.0843 0.5361 0.0643 0.065 Uiso 1 1 calc R . . C31 C 1.1379(3) 0.6211(2) 0.20971(19) 0.0714(10) Uani 1 1 d . . . H31A H 1.1706 0.6138 0.2703 0.086 Uiso 1 1 calc R . . H31B H 1.2139 0.6782 0.2081 0.086 Uiso 1 1 calc R . . C32 C 1.0092(4) 0.64267(18) 0.2075(2) 0.0663(9) Uani 1 1 d . . . H32A H 0.9795 0.6530 0.1482 0.080 Uiso 1 1 calc R . . H32B H 1.0321 0.7056 0.2636 0.080 Uiso 1 1 calc R . . C33 C 0.8872(3) 0.55567(15) 0.20990(16) 0.0407(5) Uani 1 1 d . . . H33A H 0.9134 0.5489 0.2717 0.049 Uiso 1 1 calc R . . H33B H 0.8032 0.5710 0.2056 0.049 Uiso 1 1 calc R . . C34 C 0.59640(18) 0.32654(13) 0.05275(12) 0.0234(3) Uani 1 1 d . . . H34 H 0.5348 0.2686 0.0635 0.028 Uiso 1 1 calc R . . C35 C 0.5294(2) 0.40238(15) 0.06602(15) 0.0306(4) Uani 1 1 d . . . H35A H 0.5896 0.4623 0.0584 0.037 Uiso 1 1 calc R . . H35B H 0.5219 0.4247 0.1320 0.037 Uiso 1 1 calc R . . C36 C 0.3835(2) 0.35521(19) -0.00799(18) 0.0424(5) Uani 1 1 d . . . H36A H 0.3212 0.2985 0.0030 0.051 Uiso 1 1 calc R . . H36B H 0.3432 0.4061 0.0005 0.051 Uiso 1 1 calc R . . C37 C 0.3902(3) 0.31695(19) -0.11035(18) 0.0451(5) Uani 1 1 d . . . H37A H 0.4464 0.3744 -0.1230 0.054 Uiso 1 1 calc R . . H37B H 0.2943 0.2849 -0.1568 0.054 Uiso 1 1 calc R . . C38 C 0.4558(2) 0.24074(16) -0.12488(16) 0.0397(5) Uani 1 1 d . . . H38A H 0.4644 0.2200 -0.1906 0.048 Uiso 1 1 calc R . . H38B H 0.3939 0.1800 -0.1193 0.048 Uiso 1 1 calc R . . C39 C 0.6011(2) 0.28478(15) -0.05043(13) 0.0311(4) Uani 1 1 d . . . H39A H 0.6369 0.2316 -0.0584 0.037 Uiso 1 1 calc R . . H39B H 0.6666 0.3395 -0.0621 0.037 Uiso 1 1 calc R . . C40 C 0.0171(3) 0.0665(2) -0.08860(19) 0.0533(6) Uani 1 1 d . . . H40A H 0.0967 0.0758 -0.0369 0.064 Uiso 1 1 calc R . . H40B H -0.0666 0.0091 -0.0949 0.064 Uiso 1 1 calc R . . C91 C -0.0808(11) -0.1557(8) 0.3762(8) 0.108(3) Uiso 0.50 1 d PU . . C92 C -0.1428(18) -0.0974(13) 0.4027(12) 0.119(5) Uiso 0.35 1 d PU . . C93 C 0.0000 0.0000 0.5000 0.074(6) Uiso 0.20 2 d SPU . . C92A C 0.0483(19) -0.0842(14) 0.4501(13) 0.052(4) Uiso 0.15 1 d PU . . C93B C 0.093(2) 0.0689(18) 0.4503(17) 0.041(5) Uiso 0.10 1 d P . . C93A C -0.054(2) 0.0337(18) 0.4474(17) 0.040(5) Uiso 0.10 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01742(7) 0.01862(7) 0.01988(7) 0.00666(5) 0.00728(5) 0.00836(5) Cl1 0.02505(19) 0.0278(2) 0.02078(18) 0.00480(15) 0.00517(15) 0.01188(16) Cl2 0.0541(4) 0.0620(4) 0.0670(4) 0.0224(4) 0.0248(3) 0.0141(3) Cl3 0.0611(4) 0.0738(5) 0.0705(5) 0.0268(4) 0.0262(4) 0.0250(4) S1 0.02217(18) 0.01465(17) 0.01875(18) 0.00605(14) 0.00716(14) 0.00489(14) P1 0.01721(18) 0.01549(18) 0.01793(18) 0.00618(15) 0.00612(14) 0.00634(15) O1 0.0253(6) 0.0219(6) 0.0218(6) 0.0078(5) 0.0027(5) 0.0017(5) O2 0.0339(7) 0.0190(6) 0.0276(6) 0.0097(5) 0.0171(5) 0.0114(5) N1 0.0218(7) 0.0245(7) 0.0269(7) 0.0080(6) 0.0083(6) 0.0130(6) N2 0.0211(7) 0.0179(6) 0.0229(7) 0.0100(5) 0.0071(5) 0.0039(5) C1 0.0200(7) 0.0228(8) 0.0227(8) 0.0067(6) 0.0105(6) 0.0068(6) C2 0.0343(10) 0.0339(10) 0.0275(9) 0.0133(8) 0.0150(7) 0.0161(8) C3 0.0430(11) 0.0418(11) 0.0257(9) 0.0149(8) 0.0156(8) 0.0156(9) C4 0.0348(10) 0.0414(11) 0.0248(9) 0.0047(8) 0.0144(8) 0.0098(9) C5 0.0235(8) 0.0308(9) 0.0302(9) -0.0004(7) 0.0105(7) 0.0092(7) C6 0.0179(7) 0.0238(8) 0.0271(8) 0.0036(7) 0.0077(6) 0.0059(6) C7 0.0267(9) 0.0240(8) 0.0325(9) 0.0037(7) 0.0076(7) 0.0136(7) C8 0.0435(11) 0.0391(11) 0.0400(11) 0.0202(9) 0.0154(9) 0.0274(10) C9 0.0195(8) 0.0367(10) 0.0346(10) 0.0047(8) 0.0065(7) 0.0105(8) C10 0.0256(8) 0.0184(7) 0.0222(7) 0.0088(6) 0.0100(6) 0.0079(6) C11 0.0327(10) 0.0282(9) 0.0355(10) 0.0182(8) 0.0087(8) 0.0098(8) C12 0.0538(13) 0.0311(10) 0.0402(11) 0.0227(9) 0.0095(10) 0.0149(10) C13 0.0545(14) 0.0248(9) 0.0443(12) 0.0207(9) 0.0136(10) 0.0064(9) C14 0.0364(11) 0.0321(11) 0.0677(16) 0.0279(11) 0.0075(11) -0.0010(9) C15 0.0262(9) 0.0293(10) 0.0523(13) 0.0231(9) 0.0052(8) 0.0043(8) C16 0.0184(7) 0.0207(7) 0.0182(7) 0.0078(6) 0.0057(6) 0.0064(6) C17 0.0226(8) 0.0277(8) 0.0223(8) 0.0077(7) 0.0082(6) 0.0111(7) C18 0.0212(8) 0.0412(10) 0.0248(8) 0.0119(8) 0.0079(7) 0.0135(8) C19 0.0211(8) 0.0400(10) 0.0215(8) 0.0060(7) 0.0046(6) 0.0069(8) C20 0.0255(9) 0.0279(9) 0.0235(8) 0.0011(7) 0.0055(7) 0.0061(7) C21 0.0230(8) 0.0222(8) 0.0240(8) 0.0069(6) 0.0077(6) 0.0082(6) C22 0.0176(7) 0.0168(7) 0.0187(7) 0.0062(6) 0.0054(5) 0.0075(6) C23 0.0262(8) 0.0172(7) 0.0239(8) 0.0075(6) 0.0084(6) 0.0082(6) C24 0.0333(9) 0.0178(7) 0.0262(8) 0.0056(6) 0.0102(7) 0.0121(7) C25 0.0315(9) 0.0256(8) 0.0260(8) 0.0079(7) 0.0140(7) 0.0148(7) C26 0.0248(8) 0.0225(8) 0.0235(8) 0.0089(6) 0.0105(6) 0.0100(7) C27 0.0181(7) 0.0158(7) 0.0193(7) 0.0055(6) 0.0047(6) 0.0061(6) C28 0.0270(8) 0.0213(8) 0.0251(8) 0.0119(7) 0.0083(7) 0.0015(7) C29 0.0238(9) 0.0478(12) 0.0409(11) 0.0266(10) 0.0111(8) 0.0071(8) C30 0.0280(11) 0.0749(18) 0.0415(12) 0.0332(13) 0.0066(9) -0.0065(11) C31 0.0507(16) 0.0699(19) 0.0398(13) 0.0215(13) 0.0002(11) -0.0318(14) C32 0.092(2) 0.0254(11) 0.0456(14) 0.0123(10) 0.0170(14) -0.0150(13) C33 0.0570(14) 0.0194(9) 0.0328(10) 0.0081(8) 0.0148(9) 0.0021(9) C34 0.0221(8) 0.0206(8) 0.0259(8) 0.0115(6) 0.0064(6) 0.0052(6) C35 0.0324(9) 0.0294(9) 0.0378(10) 0.0185(8) 0.0139(8) 0.0154(8) C36 0.0331(11) 0.0485(13) 0.0582(14) 0.0344(12) 0.0130(10) 0.0199(10) C37 0.0419(12) 0.0446(12) 0.0471(13) 0.0283(11) -0.0011(10) 0.0140(10) C38 0.0432(12) 0.0319(10) 0.0323(10) 0.0143(8) -0.0026(9) 0.0077(9) C39 0.0354(10) 0.0277(9) 0.0252(9) 0.0094(7) 0.0065(7) 0.0099(8) C40 0.0416(13) 0.0560(15) 0.0498(14) 0.0288(12) 0.0008(11) 0.0050(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.0086(17) . ? Pd1 N1 2.1279(14) . ? Pd1 P1 2.2456(4) . ? Pd1 Cl1 2.4233(4) . ? Pd1 O2 2.9399(12) . ? Cl2 C40 1.768(3) . ? Cl3 C40 1.752(3) . ? S1 O2 1.4379(13) . ? S1 O1 1.4380(13) . ? S1 N2 1.6276(14) . ? S1 C27 1.7884(16) . ? P1 C16 1.8254(16) . ? P1 C10 1.8281(17) . ? P1 C22 1.8500(16) . ? P1 O2 2.9687(13) . ? N1 C9 1.478(2) . ? N1 C8 1.483(3) . ? N1 C7 1.496(2) . ? N2 C34 1.487(2) . ? N2 C28 1.493(2) . ? C1 C2 1.396(3) . ? C1 C6 1.410(2) . ? C2 C3 1.398(3) . ? C3 C4 1.385(3) . ? C4 C5 1.379(3) . ? C5 C6 1.400(3) . ? C6 C7 1.490(3) . ? C10 C11 1.388(3) . ? C10 C15 1.392(3) . ? C11 C12 1.391(3) . ? C12 C13 1.376(3) . ? C13 C14 1.377(3) . ? C14 C15 1.392(3) . ? C16 C21 1.394(2) . ? C16 C17 1.400(2) . ? C17 C18 1.389(2) . ? C18 C19 1.380(3) . ? C19 C20 1.385(3) . ? C20 C21 1.387(2) . ? C22 C23 1.399(2) . ? C22 C27 1.410(2) . ? C23 C24 1.389(2) . ? C24 C25 1.381(3) . ? C25 C26 1.385(2) . ? C26 C27 1.391(2) . ? C28 C29 1.529(3) . ? C28 C33 1.530(3) . ? C29 C30 1.529(3) . ? C30 C31 1.511(4) . ? C31 C32 1.505(5) . ? C32 C33 1.544(3) . ? C34 C35 1.529(3) . ? C34 C39 1.529(3) . ? C35 C36 1.530(3) . ? C36 C37 1.521(4) . ? C37 C38 1.523(3) . ? C38 C39 1.532(3) . ? C91 C92 1.282(18) . ? C91 C92A 1.43(2) . ? C92 C93A 1.75(3) . ? C92 C93 1.752(17) . ? C92 C92A 1.95(2) . ? C93 C93A 1.24(2) 2_556 ? C93 C93A 1.24(2) . ? C93 C92A 1.568(19) . ? C93 C92A 1.568(19) 2_556 ? C93 C93B 1.67(2) 2_556 ? C93 C93B 1.67(2) . ? C93 C92 1.752(17) 2_556 ? C92A C93A 1.50(3) 2_556 ? C93B C93A 1.47(3) . ? C93A C92A 1.50(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 82.62(6) . . ? C1 Pd1 P1 95.23(5) . . ? N1 Pd1 P1 172.58(4) . . ? C1 Pd1 Cl1 165.73(5) . . ? N1 Pd1 Cl1 91.75(4) . . ? P1 Pd1 Cl1 91.914(15) . . ? C1 Pd1 O2 111.90(5) . . ? N1 Pd1 O2 105.80(5) . . ? P1 Pd1 O2 68.34(3) . . ? Cl1 Pd1 O2 82.23(3) . . ? O2 S1 O1 117.65(8) . . ? O2 S1 N2 111.38(8) . . ? O1 S1 N2 107.95(7) . . ? O2 S1 C27 107.86(7) . . ? O1 S1 C27 107.79(7) . . ? N2 S1 C27 103.20(7) . . ? C16 P1 C10 105.93(8) . . ? C16 P1 C22 99.62(7) . . ? C10 P1 C22 102.88(7) . . ? C16 P1 Pd1 119.26(5) . . ? C10 P1 Pd1 110.63(6) . . ? C22 P1 Pd1 116.67(5) . . ? C16 P1 O2 78.41(6) . . ? C10 P1 O2 175.63(6) . . ? C22 P1 O2 75.59(6) . . ? Pd1 P1 O2 66.99(3) . . ? S1 O2 Pd1 136.93(7) . . ? S1 O2 P1 97.30(6) . . ? Pd1 O2 P1 44.672(19) . . ? C9 N1 C8 109.50(16) . . ? C9 N1 C7 110.68(14) . . ? C8 N1 C7 108.43(15) . . ? C9 N1 Pd1 109.55(12) . . ? C8 N1 Pd1 112.17(11) . . ? C7 N1 Pd1 106.48(10) . . ? C34 N2 C28 119.53(13) . . ? C34 N2 S1 115.72(11) . . ? C28 N2 S1 121.38(11) . . ? C2 C1 C6 117.21(16) . . ? C2 C1 Pd1 129.75(13) . . ? C6 C1 Pd1 112.83(13) . . ? C1 C2 C3 121.48(18) . . ? C4 C3 C2 120.4(2) . . ? C5 C4 C3 119.36(18) . . ? C4 C5 C6 120.65(18) . . ? C5 C6 C1 120.89(18) . . ? C5 C6 C7 121.60(17) . . ? C1 C6 C7 117.46(16) . . ? C6 C7 N1 110.11(14) . . ? C11 C10 C15 118.50(17) . . ? C11 C10 P1 124.70(14) . . ? C15 C10 P1 116.79(14) . . ? C10 C11 C12 120.59(19) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C14 119.64(19) . . ? C13 C14 C15 120.3(2) . . ? C10 C15 C14 120.5(2) . . ? C21 C16 C17 119.24(15) . . ? C21 C16 P1 120.70(13) . . ? C17 C16 P1 120.00(12) . . ? C18 C17 C16 120.08(16) . . ? C19 C18 C17 120.17(17) . . ? C18 C19 C20 120.10(17) . . ? C19 C20 C21 120.34(17) . . ? C20 C21 C16 120.04(16) . . ? C23 C22 C27 117.03(14) . . ? C23 C22 P1 118.34(12) . . ? C27 C22 P1 124.41(12) . . ? C24 C23 C22 121.71(16) . . ? C25 C24 C23 120.38(16) . . ? C24 C25 C26 119.19(16) . . ? C25 C26 C27 120.80(16) . . ? C26 C27 C22 120.79(15) . . ? C26 C27 S1 115.03(12) . . ? C22 C27 S1 124.05(12) . . ? N2 C28 C29 111.33(15) . . ? N2 C28 C33 113.62(15) . . ? C29 C28 C33 112.87(17) . . ? C30 C29 C28 113.2(2) . . ? C31 C30 C29 112.4(2) . . ? C32 C31 C30 110.4(2) . . ? C31 C32 C33 111.7(2) . . ? C28 C33 C32 110.27(19) . . ? N2 C34 C35 112.92(14) . . ? N2 C34 C39 110.96(14) . . ? C35 C34 C39 111.21(15) . . ? C34 C35 C36 110.71(17) . . ? C37 C36 C35 111.04(18) . . ? C36 C37 C38 110.72(18) . . ? C37 C38 C39 111.49(18) . . ? C34 C39 C38 111.68(17) . . ? Cl3 C40 Cl2 111.27(15) . . ? C92 C91 C92A 91.7(13) . . ? C91 C92 C93A 121.5(15) . . ? C91 C92 C93 97.0(11) . . ? C93A C92 C93 41.6(9) . . ? C91 C92 C92A 47.2(9) . . ? C93A C92 C92A 80.8(12) . . ? C93 C92 C92A 49.8(7) . . ? C93A C93 C93A 180.0(17) 2_556 . ? C93A C93 C92A 63.2(12) 2_556 . ? C93A C93 C92A 116.8(12) . . ? C93A C93 C92A 116.8(12) 2_556 2_556 ? C93A C93 C92A 63.2(12) . 2_556 ? C92A C93 C92A 180.0(14) . 2_556 ? C93A C93 C93B 58.3(13) 2_556 2_556 ? C93A C93 C93B 121.7(13) . 2_556 ? C92A C93 C93B 92.6(11) . 2_556 ? C92A C93 C93B 87.4(11) 2_556 2_556 ? C93A C93 C93B 121.7(13) 2_556 . ? C93A C93 C93B 58.3(13) . . ? C92A C93 C93B 87.4(11) . . ? C92A C93 C93B 92.6(11) 2_556 . ? C93B C93 C93B 180.000(4) 2_556 . ? C93A C93 C92 111.0(12) 2_556 . ? C93A C93 C92 69.0(12) . . ? C92A C93 C92 71.7(9) . . ? C92A C93 C92 108.3(9) 2_556 . ? C93B C93 C92 75.6(10) 2_556 . ? C93B C93 C92 104.4(10) . . ? C93A C93 C92 69.0(12) 2_556 2_556 ? C93A C93 C92 111.0(12) . 2_556 ? C92A C93 C92 108.3(9) . 2_556 ? C92A C93 C92 71.7(9) 2_556 2_556 ? C93B C93 C92 104.4(10) 2_556 2_556 ? C93B C93 C92 75.6(10) . 2_556 ? C92 C93 C92 180.000(2) . 2_556 ? C91 C92A C93A 122.0(16) . 2_556 ? C91 C92A C93 99.6(12) . . ? C93A C92A C93 47.8(10) 2_556 . ? C91 C92A C92 41.1(8) . . ? C93A C92A C92 91.3(14) 2_556 . ? C93 C92A C92 58.6(8) . . ? C93A C93B C93 46.3(11) . . ? C93 C93A C93B 75.4(15) . . ? C93 C93A C92A 69.0(13) . 2_556 ? C93B C93A C92A 104.2(18) . 2_556 ? C93 C93A C92 69.3(12) . . ? C93B C93A C92 114.2(18) . . ? C92A C93A C92 111.9(16) 2_556 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.790 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.078 data_c:\backup\kappa\k02cgf2\maxus\k02cgf2 _database_code_depnum_ccdc_archive 'CCDC 232456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H48 F6 N2 O2 P Pd S Sb' _chemical_formula_weight 981.97 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.4920(2) _cell_length_b 12.2630(10) _cell_length_c 18.5860(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.396(1) _cell_angle_gamma 90.00 _cell_volume 4116.44(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39265 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80179 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 30.04 _reflns_number_total 12008 _reflns_number_gt 10667 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.8881*P+(0.0316P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00086(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12008 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Sb1 Sb 0.343963(6) -0.168726(9) 0.128148(6) 0.02394(4) Uani 1 1 d . . . Pd1 Pd 0.164150(6) 0.214153(9) -0.140633(6) 0.01714(4) Uani 1 1 d . . . S1 S -0.00188(2) 0.12047(3) -0.14440(2) 0.01972(7) Uani 1 1 d . . . P1 P 0.09065(2) 0.35364(3) -0.18897(2) 0.01791(8) Uani 1 1 d . . . F1 F 0.38654(17) -0.27110(17) 0.07623(15) 0.0638(6) Uani 0.72 1 d P A 1 F2 F 0.32479(7) -0.28116(11) 0.18956(7) 0.0496(3) Uani 1 1 d . A . F3 F 0.30250(18) -0.0691(2) 0.18153(16) 0.0764(7) Uani 0.72 1 d P A 1 F4 F 0.36254(7) -0.05834(11) 0.06526(8) 0.0497(3) Uani 1 1 d . A . F5 F 0.43686(12) -0.1433(2) 0.18849(14) 0.0610(7) Uani 0.72 1 d P A 1 F6 F 0.25165(12) -0.1938(2) 0.06776(13) 0.0550(6) Uani 0.72 1 d P A 1 O1 O 0.06373(6) 0.12274(9) -0.17727(7) 0.0230(2) Uani 1 1 d . . . O2 O 0.01027(7) 0.08505(10) -0.06942(6) 0.0287(3) Uani 1 1 d . . . N1 N 0.22712(7) 0.07349(11) -0.10183(7) 0.0221(3) Uani 1 1 d . . . N2 N -0.06486(7) 0.04849(10) -0.19543(7) 0.0203(2) Uani 1 1 d . . . C1 C 0.26343(8) 0.28381(13) -0.12713(9) 0.0214(3) Uani 1 1 d . . . C2 C 0.28363(9) 0.38137(14) -0.15619(9) 0.0256(3) Uani 1 1 d . . . H2 H 0.2462 0.4296 -0.1808 0.031 Uiso 1 1 calc R . . C3 C 0.35771(10) 0.40924(15) -0.14977(11) 0.0319(4) Uani 1 1 d . . . H3 H 0.3701 0.4772 -0.1685 0.038 Uiso 1 1 calc R . . C4 C 0.41329(10) 0.33918(18) -0.11643(13) 0.0426(5) Uani 1 1 d . . . H4 H 0.4638 0.3581 -0.1126 0.051 Uiso 1 1 calc R . . C5 C 0.39449(10) 0.2407(2) -0.08851(14) 0.0483(6) Uani 1 1 d . . . H5 H 0.4323 0.1909 -0.0669 0.058 Uiso 1 1 calc R . . C6 C 0.32062(10) 0.21437(15) -0.09197(11) 0.0318(4) Uani 1 1 d . . . C7 C 0.29921(10) 0.11211(16) -0.05761(11) 0.0366(4) Uani 1 1 d . . . H7A H 0.3376 0.0555 -0.0566 0.044 Uiso 1 1 calc R . . H7B H 0.2948 0.1268 -0.0063 0.044 Uiso 1 1 calc R . . C8 C 0.23866(12) 0.01332(16) -0.16759(11) 0.0378(4) Uani 1 1 d . . . H8A H 0.2695 -0.0510 -0.1519 0.057 Uiso 1 1 calc R . . H8B H 0.2635 0.0609 -0.1971 0.057 Uiso 1 1 calc R . . H8C H 0.1907 -0.0097 -0.1972 0.057 Uiso 1 1 calc R . . C9 C 0.19131(10) -0.00066(14) -0.05723(10) 0.0282(3) Uani 1 1 d . . . H9A H 0.2248 -0.0613 -0.0391 0.042 Uiso 1 1 calc R . . H9B H 0.1453 -0.0293 -0.0877 0.042 Uiso 1 1 calc R . . H9C H 0.1801 0.0394 -0.0153 0.042 Uiso 1 1 calc R . . C10 C -0.07974(9) -0.06633(12) -0.17375(9) 0.0219(3) Uani 1 1 d . . . H10 H -0.1104 -0.1010 -0.2188 0.026 Uiso 1 1 calc R . . C11 C -0.12670(11) -0.06889(15) -0.11570(11) 0.0349(4) Uani 1 1 d . . . H11A H -0.1724 -0.0259 -0.1329 0.042 Uiso 1 1 calc R . . H11B H -0.0988 -0.0359 -0.0694 0.042 Uiso 1 1 calc R . . C12 C -0.14687(15) -0.18745(17) -0.10147(13) 0.0487(6) Uani 1 1 d . . . H12A H -0.1757 -0.1888 -0.0623 0.058 Uiso 1 1 calc R . . H12B H -0.1784 -0.2180 -0.1469 0.058 Uiso 1 1 calc R . . C13 C -0.07811(15) -0.25763(16) -0.07825(12) 0.0484(6) Uani 1 1 d . . . H13A H -0.0485 -0.2308 -0.0308 0.058 Uiso 1 1 calc R . . H13B H -0.0929 -0.3338 -0.0712 0.058 Uiso 1 1 calc R . . C14 C -0.03160(12) -0.25435(14) -0.13620(11) 0.0374(4) Uani 1 1 d . . . H14A H -0.0597 -0.2876 -0.1823 0.045 Uiso 1 1 calc R . . H14B H 0.0140 -0.2978 -0.1191 0.045 Uiso 1 1 calc R . . C15 C -0.01052(10) -0.13698(14) -0.15159(11) 0.0303(4) Uani 1 1 d . . . H15A H 0.0221 -0.1062 -0.1069 0.036 Uiso 1 1 calc R . . H15B H 0.0171 -0.1369 -0.1917 0.036 Uiso 1 1 calc R . . C16 C -0.08700(8) 0.08209(12) -0.27416(8) 0.0208(3) Uani 1 1 d . . . H16 H -0.0711 0.1597 -0.2769 0.025 Uiso 1 1 calc R . . C17 C -0.04856(9) 0.01614(14) -0.32476(9) 0.0252(3) Uani 1 1 d . . . H17A H -0.0619 -0.0618 -0.3228 0.030 Uiso 1 1 calc R . . H17B H 0.0058 0.0227 -0.3078 0.030 Uiso 1 1 calc R . . C18 C -0.07179(11) 0.05771(17) -0.40435(10) 0.0343(4) Uani 1 1 d . . . H18A H -0.0542 0.1336 -0.4070 0.041 Uiso 1 1 calc R . . H18B H -0.0483 0.0121 -0.4369 0.041 Uiso 1 1 calc R . . C19 C -0.15565(11) 0.05413(17) -0.43115(11) 0.0378(4) Uani 1 1 d . . . H19A H -0.1727 -0.0225 -0.4330 0.045 Uiso 1 1 calc R . . H19B H -0.1693 0.0845 -0.4816 0.045 Uiso 1 1 calc R . . C20 C -0.19373(11) 0.11953(17) -0.38005(11) 0.0376(4) Uani 1 1 d . . . H20A H -0.2481 0.1130 -0.3971 0.045 Uiso 1 1 calc R . . H20B H -0.1805 0.1975 -0.3823 0.045 Uiso 1 1 calc R . . C21 C -0.17134(9) 0.07982(15) -0.30028(10) 0.0285(3) Uani 1 1 d . . . H21A H -0.1896 0.0046 -0.2968 0.034 Uiso 1 1 calc R . . H21B H -0.1942 0.1272 -0.2682 0.034 Uiso 1 1 calc R . . C22 C 0.12056(8) 0.49246(12) -0.16501(9) 0.0219(3) Uani 1 1 d . . . C23 C 0.12055(10) 0.57389(14) -0.21731(11) 0.0297(4) Uani 1 1 d . . . H23 H 0.1002 0.5599 -0.2679 0.036 Uiso 1 1 calc R . . C24 C 0.15054(12) 0.67605(15) -0.19523(14) 0.0413(5) Uani 1 1 d . . . H24 H 0.1508 0.7316 -0.2308 0.050 Uiso 1 1 calc R . . C25 C 0.17972(12) 0.69627(16) -0.12190(15) 0.0464(6) Uani 1 1 d . . . H25 H 0.2007 0.7656 -0.1072 0.056 Uiso 1 1 calc R . . C26 C 0.17874(12) 0.61651(17) -0.06912(13) 0.0432(5) Uani 1 1 d . . . H26 H 0.1980 0.6317 -0.0185 0.052 Uiso 1 1 calc R . . C27 C 0.14950(10) 0.51453(15) -0.09077(11) 0.0324(4) Uani 1 1 d . . . H27 H 0.1492 0.4595 -0.0549 0.039 Uiso 1 1 calc R . . C28 C 0.07296(9) 0.34296(13) -0.28879(9) 0.0219(3) Uani 1 1 d . . . C29 C 0.01389(10) 0.39654(17) -0.33466(10) 0.0343(4) Uani 1 1 d . . . H29 H -0.0201 0.4378 -0.3140 0.041 Uiso 1 1 calc R . . C30 C 0.00527(11) 0.3892(2) -0.41036(11) 0.0452(5) Uani 1 1 d . . . H30 H -0.0343 0.4268 -0.4416 0.054 Uiso 1 1 calc R . . C31 C 0.05365(11) 0.3276(2) -0.44108(11) 0.0429(5) Uani 1 1 d . . . H31 H 0.0471 0.3230 -0.4931 0.051 Uiso 1 1 calc R . . C32 C 0.11159(10) 0.27260(18) -0.39597(10) 0.0349(4) Uani 1 1 d . . . H32 H 0.1444 0.2294 -0.4170 0.042 Uiso 1 1 calc R . . C33 C 0.12153(9) 0.28095(14) -0.32020(10) 0.0264(3) Uani 1 1 d . . . H33 H 0.1617 0.2442 -0.2893 0.032 Uiso 1 1 calc R . . C34 C -0.00224(8) 0.34884(12) -0.16737(9) 0.0204(3) Uani 1 1 d . . . C35 C -0.04044(9) 0.44793(13) -0.17000(10) 0.0260(3) Uani 1 1 d . . . H35 H -0.0169 0.5131 -0.1804 0.031 Uiso 1 1 calc R . . C36 C -0.11189(10) 0.45334(14) -0.15786(11) 0.0313(4) Uani 1 1 d . . . H36 H -0.1370 0.5214 -0.1616 0.038 Uiso 1 1 calc R . . C37 C -0.14672(10) 0.36015(15) -0.14032(11) 0.0332(4) Uani 1 1 d . . . H37 H -0.1953 0.3640 -0.1312 0.040 Uiso 1 1 calc R . . C38 C -0.10985(10) 0.26089(14) -0.13627(10) 0.0288(4) Uani 1 1 d . . . H38 H -0.1329 0.1968 -0.1232 0.035 Uiso 1 1 calc R . . C39 C -0.03929(9) 0.25480(12) -0.15129(9) 0.0215(3) Uani 1 1 d . . . F1A F 0.4386(4) -0.2159(9) 0.1391(8) 0.131(5) Uani 0.28 1 d P A 2 F6A F 0.3110(9) -0.2499(9) 0.0447(4) 0.154(6) Uani 0.28 1 d P A 2 F3A F 0.2482(4) -0.1194(9) 0.1164(8) 0.133(5) Uani 0.28 1 d P A 2 F5A F 0.3739(9) -0.0858(7) 0.2092(4) 0.144(5) Uani 0.28 1 d P A 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 Sb1 0.02204(6) 0.02390(6) 0.02466(6) 0.00645(4) 0.00229(4) -0.00092(4) Pd1 0.01688(6) 0.01412(6) 0.02008(6) 0.00066(4) 0.00318(4) -0.00195(4) S1 0.02119(17) 0.01492(16) 0.02246(17) -0.00201(13) 0.00335(13) -0.00496(13) P1 0.01806(17) 0.01395(16) 0.02199(18) -0.00012(13) 0.00490(14) -0.00149(13) F1 0.0978(18) 0.0378(10) 0.0707(16) 0.0018(10) 0.0510(14) 0.0132(12) F2 0.0410(6) 0.0575(8) 0.0481(7) 0.0315(6) 0.0050(5) -0.0065(6) F3 0.0911(19) 0.0710(16) 0.0753(17) -0.0189(14) 0.0362(15) 0.0223(15) F4 0.0473(7) 0.0423(7) 0.0570(8) 0.0289(6) 0.0053(6) -0.0091(6) F5 0.0357(10) 0.0779(17) 0.0573(14) 0.0285(12) -0.0171(9) -0.0219(11) F6 0.0361(10) 0.0706(15) 0.0467(12) 0.0302(10) -0.0169(8) -0.0242(10) O1 0.0188(5) 0.0170(5) 0.0329(6) -0.0025(4) 0.0047(4) -0.0031(4) O2 0.0390(7) 0.0217(6) 0.0229(6) -0.0012(4) 0.0013(5) -0.0092(5) N1 0.0217(6) 0.0200(6) 0.0241(6) 0.0032(5) 0.0044(5) -0.0003(5) N2 0.0219(6) 0.0162(6) 0.0220(6) -0.0021(5) 0.0029(5) -0.0057(5) C1 0.0186(7) 0.0232(7) 0.0215(7) 0.0003(6) 0.0020(5) -0.0053(6) C2 0.0226(7) 0.0241(8) 0.0304(8) 0.0037(6) 0.0062(6) -0.0019(6) C3 0.0270(8) 0.0297(9) 0.0388(10) 0.0065(7) 0.0064(7) -0.0085(7) C4 0.0197(8) 0.0478(12) 0.0559(13) 0.0178(10) -0.0016(8) -0.0100(8) C5 0.0207(8) 0.0503(12) 0.0662(15) 0.0290(11) -0.0075(9) -0.0051(8) C6 0.0228(8) 0.0328(9) 0.0357(10) 0.0120(7) -0.0030(7) -0.0064(7) C7 0.0257(8) 0.0358(10) 0.0414(10) 0.0183(8) -0.0083(7) -0.0061(7) C8 0.0509(11) 0.0286(9) 0.0386(10) 0.0019(8) 0.0206(9) 0.0128(8) C9 0.0314(8) 0.0227(8) 0.0306(8) 0.0054(7) 0.0069(7) -0.0043(7) C10 0.0251(7) 0.0156(6) 0.0254(7) -0.0026(6) 0.0061(6) -0.0073(6) C11 0.0418(10) 0.0258(8) 0.0432(10) -0.0080(8) 0.0230(8) -0.0148(8) C12 0.0735(16) 0.0330(10) 0.0498(13) -0.0126(9) 0.0356(12) -0.0306(11) C13 0.0926(18) 0.0214(9) 0.0308(10) -0.0027(7) 0.0120(11) -0.0218(10) C14 0.0547(12) 0.0170(8) 0.0354(10) -0.0001(7) -0.0013(8) -0.0042(8) C15 0.0331(9) 0.0195(8) 0.0364(9) 0.0011(7) 0.0031(7) -0.0017(7) C16 0.0215(7) 0.0181(7) 0.0222(7) -0.0015(5) 0.0033(5) -0.0004(5) C17 0.0242(7) 0.0268(8) 0.0247(8) -0.0012(6) 0.0054(6) 0.0045(6) C18 0.0419(10) 0.0376(10) 0.0244(8) 0.0020(7) 0.0093(7) 0.0077(8) C19 0.0430(11) 0.0378(10) 0.0274(9) -0.0005(8) -0.0039(8) 0.0084(8) C20 0.0316(9) 0.0375(10) 0.0389(10) -0.0006(8) -0.0030(8) 0.0097(8) C21 0.0206(7) 0.0301(8) 0.0336(9) -0.0038(7) 0.0033(6) 0.0039(6) C22 0.0203(7) 0.0146(6) 0.0320(8) -0.0018(6) 0.0082(6) -0.0018(5) C23 0.0332(9) 0.0190(7) 0.0404(10) 0.0034(7) 0.0156(7) -0.0004(7) C24 0.0449(11) 0.0190(8) 0.0655(14) 0.0054(9) 0.0241(10) -0.0044(8) C25 0.0411(11) 0.0202(8) 0.0790(17) -0.0135(10) 0.0152(11) -0.0107(8) C26 0.0423(11) 0.0320(10) 0.0512(12) -0.0179(9) 0.0009(9) -0.0063(8) C27 0.0354(9) 0.0251(8) 0.0347(9) -0.0051(7) 0.0032(7) -0.0040(7) C28 0.0208(7) 0.0221(7) 0.0226(7) 0.0001(6) 0.0043(6) -0.0016(6) C29 0.0287(8) 0.0436(11) 0.0292(9) -0.0006(8) 0.0032(7) 0.0127(8) C30 0.0343(10) 0.0711(15) 0.0271(9) 0.0050(9) -0.0006(7) 0.0183(10) C31 0.0310(9) 0.0742(16) 0.0229(9) -0.0009(9) 0.0044(7) 0.0041(9) C32 0.0246(8) 0.0524(12) 0.0289(9) -0.0077(8) 0.0086(7) 0.0033(8) C33 0.0214(7) 0.0306(8) 0.0267(8) 0.0001(6) 0.0041(6) 0.0033(6) C34 0.0192(7) 0.0181(7) 0.0247(7) -0.0041(6) 0.0066(6) -0.0014(5) C35 0.0255(8) 0.0166(7) 0.0374(9) -0.0044(6) 0.0103(7) -0.0019(6) C36 0.0272(8) 0.0214(8) 0.0477(11) -0.0094(7) 0.0133(7) 0.0013(6) C37 0.0253(8) 0.0309(9) 0.0476(11) -0.0121(8) 0.0174(8) -0.0031(7) C38 0.0278(8) 0.0236(8) 0.0384(10) -0.0059(7) 0.0146(7) -0.0075(6) C39 0.0239(7) 0.0160(7) 0.0259(7) -0.0039(6) 0.0085(6) -0.0024(6) F1A 0.044(4) 0.135(8) 0.230(13) 0.118(9) 0.062(6) 0.051(5) F6A 0.298(16) 0.113(7) 0.043(4) -0.028(4) 0.021(6) -0.130(10) F3A 0.049(4) 0.126(7) 0.244(13) 0.131(9) 0.077(6) 0.054(5) F5A 0.295(16) 0.076(6) 0.050(4) -0.022(4) 0.014(7) -0.065(8) _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 Sb1 F5A 1.804(7) . ? Sb1 F1A 1.813(6) . ? Sb1 F6A 1.834(6) . ? Sb1 F3A 1.840(5) . ? Sb1 F3 1.842(2) . ? Sb1 F6 1.8564(16) . ? Sb1 F1 1.8583(19) . ? Sb1 F5 1.8651(18) . ? Sb1 F4 1.8679(11) . ? Sb1 F2 1.8717(11) . ? Pd1 C1 1.9913(15) . ? Pd1 N1 2.1191(13) . ? Pd1 O1 2.1508(11) . ? Pd1 P1 2.2486(4) . ? S1 O2 1.4307(12) . ? S1 O1 1.4711(12) . ? S1 N2 1.6003(13) . ? S1 C39 1.7806(16) . ? P1 C22 1.8157(15) . ? P1 C28 1.8181(16) . ? P1 C34 1.8469(16) . ? N1 C9 1.479(2) . ? N1 C8 1.482(2) . ? N1 C7 1.486(2) . ? N2 C16 1.490(2) . ? N2 C10 1.5060(19) . ? C1 C2 1.396(2) . ? C1 C6 1.405(2) . ? C2 C3 1.392(2) . ? C3 C4 1.380(3) . ? C4 C5 1.388(3) . ? C5 C6 1.392(3) . ? C6 C7 1.498(2) . ? C10 C11 1.524(2) . ? C10 C15 1.527(2) . ? C11 C12 1.538(3) . ? C12 C13 1.519(4) . ? C13 C14 1.516(3) . ? C14 C15 1.534(2) . ? C16 C17 1.527(2) . ? C16 C21 1.531(2) . ? C17 C18 1.536(2) . ? C18 C19 1.524(3) . ? C19 C20 1.526(3) . ? C20 C21 1.531(3) . ? C22 C23 1.393(2) . ? C22 C27 1.395(2) . ? C23 C24 1.396(3) . ? C24 C25 1.376(3) . ? C25 C26 1.388(3) . ? C26 C27 1.387(3) . ? C28 C33 1.397(2) . ? C28 C29 1.397(2) . ? C29 C30 1.385(3) . ? C30 C31 1.384(3) . ? C31 C32 1.385(3) . ? C32 C33 1.384(3) . ? C34 C35 1.401(2) . ? C34 C39 1.406(2) . ? C35 C36 1.389(2) . ? C36 C37 1.385(3) . ? C37 C38 1.389(3) . ? C38 C39 1.394(2) . ? 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 F5A Sb1 F1A 88.3(7) . . ? F5A Sb1 F6A 178.1(7) . . ? F1A Sb1 F6A 93.4(8) . . ? F5A Sb1 F3A 91.6(7) . . ? F1A Sb1 F3A 179.3(3) . . ? F6A Sb1 F3A 86.7(7) . . ? F5A Sb1 F3 42.6(5) . . ? F1A Sb1 F3 130.9(5) . . ? F6A Sb1 F3 135.6(6) . . ? F3A Sb1 F3 49.0(5) . . ? F5A Sb1 F6 132.5(6) . . ? F1A Sb1 F6 139.1(5) . . ? F6A Sb1 F6 45.8(5) . . ? F3A Sb1 F6 41.0(5) . . ? F3 Sb1 F6 90.03(15) . . ? F5A Sb1 F1 136.6(6) . . ? F1A Sb1 F1 48.4(5) . . ? F6A Sb1 F1 45.1(5) . . ? F3A Sb1 F1 131.7(5) . . ? F3 Sb1 F1 178.70(13) . . ? F6 Sb1 F1 90.64(15) . . ? F5A Sb1 F5 47.6(5) . . ? F1A Sb1 F5 40.8(5) . . ? F6A Sb1 F5 134.0(6) . . ? F3A Sb1 F5 139.1(5) . . ? F3 Sb1 F5 90.07(15) . . ? F6 Sb1 F5 179.77(10) . . ? F1 Sb1 F5 89.26(15) . . ? F5A Sb1 F4 92.8(3) . . ? F1A Sb1 F4 89.9(2) . . ? F6A Sb1 F4 86.3(3) . . ? F3A Sb1 F4 89.4(2) . . ? F3 Sb1 F4 90.57(11) . . ? F6 Sb1 F4 90.60(7) . . ? F1 Sb1 F4 90.53(8) . . ? F5 Sb1 F4 89.18(8) . . ? F5A Sb1 F2 88.3(3) . . ? F1A Sb1 F2 90.1(2) . . ? F6A Sb1 F2 92.5(3) . . ? F3A Sb1 F2 90.6(2) . . ? F3 Sb1 F2 90.29(10) . . ? F6 Sb1 F2 88.66(7) . . ? F1 Sb1 F2 88.62(8) . . ? F5 Sb1 F2 91.55(8) . . ? F4 Sb1 F2 178.87(7) . . ? C1 Pd1 N1 83.22(6) . . ? C1 Pd1 O1 166.77(6) . . ? N1 Pd1 O1 93.29(5) . . ? C1 Pd1 P1 100.71(5) . . ? N1 Pd1 P1 174.88(4) . . ? O1 Pd1 P1 82.14(3) . . ? O2 S1 O1 116.05(7) . . ? O2 S1 N2 110.61(7) . . ? O1 S1 N2 108.93(7) . . ? O2 S1 C39 109.16(8) . . ? O1 S1 C39 107.16(7) . . ? N2 S1 C39 104.21(7) . . ? C22 P1 C28 107.24(7) . . ? C22 P1 C34 103.01(7) . . ? C28 P1 C34 104.33(7) . . ? C22 P1 Pd1 119.28(5) . . ? C28 P1 Pd1 108.29(5) . . ? C34 P1 Pd1 113.55(5) . . ? S1 O1 Pd1 127.68(7) . . ? C9 N1 C8 108.50(14) . . ? C9 N1 C7 110.03(13) . . ? C8 N1 C7 110.12(15) . . ? C9 N1 Pd1 114.32(10) . . ? C8 N1 Pd1 106.89(10) . . ? C7 N1 Pd1 106.92(10) . . ? C16 N2 C10 119.58(12) . . ? C16 N2 S1 116.16(10) . . ? C10 N2 S1 120.57(10) . . ? C2 C1 C6 117.53(14) . . ? C2 C1 Pd1 129.41(12) . . ? C6 C1 Pd1 112.34(11) . . ? C3 C2 C1 121.16(16) . . ? C4 C3 C2 120.65(17) . . ? C3 C4 C5 119.17(17) . . ? C4 C5 C6 120.45(18) . . ? C5 C6 C1 120.95(16) . . ? C5 C6 C7 121.39(17) . . ? C1 C6 C7 117.66(15) . . ? N1 C7 C6 108.59(14) . . ? N2 C10 C11 111.92(13) . . ? N2 C10 C15 114.32(13) . . ? C11 C10 C15 111.68(15) . . ? C10 C11 C12 109.72(15) . . ? C13 C12 C11 111.42(18) . . ? C14 C13 C12 110.55(17) . . ? C13 C14 C15 111.28(16) . . ? C10 C15 C14 110.54(15) . . ? N2 C16 C17 113.10(12) . . ? N2 C16 C21 110.65(13) . . ? C17 C16 C21 111.86(13) . . ? C16 C17 C18 110.27(14) . . ? C19 C18 C17 111.09(16) . . ? C18 C19 C20 110.76(16) . . ? C19 C20 C21 111.75(15) . . ? C20 C21 C16 110.28(15) . . ? C23 C22 C27 119.57(15) . . ? C23 C22 P1 123.12(13) . . ? C27 C22 P1 117.15(13) . . ? C22 C23 C24 119.84(19) . . ? C25 C24 C23 119.96(19) . . ? C24 C25 C26 120.73(18) . . ? C25 C26 C27 119.6(2) . . ? C26 C27 C22 120.30(19) . . ? C33 C28 C29 119.31(16) . . ? C33 C28 P1 118.35(12) . . ? C29 C28 P1 122.32(13) . . ? C30 C29 C28 119.59(17) . . ? C31 C30 C29 120.74(18) . . ? C30 C31 C32 120.02(18) . . ? C33 C32 C31 119.75(17) . . ? C32 C33 C28 120.58(16) . . ? C35 C34 C39 116.98(14) . . ? C35 C34 P1 116.76(12) . . ? C39 C34 P1 126.22(12) . . ? C36 C35 C34 121.73(15) . . ? C37 C36 C35 120.37(16) . . ? C36 C37 C38 119.22(16) . . ? C37 C38 C39 120.39(16) . . ? C38 C39 C34 121.24(15) . . ? C38 C39 S1 113.66(12) . . ? C34 C39 S1 125.06(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.884 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.074