# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew10901 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 N2 P2 Pd S2' _chemical_formula_sum 'C46 H38 N2 P2 Pd S2' _chemical_formula_weight 851.24 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.9959(8) _cell_length_b 15.2833(11) _cell_length_c 12.9857(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.233(7) _cell_angle_gamma 90.00 _cell_volume 1968.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10047 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.21 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8486 _exptl_absorpt_correction_T_max 0.9431 _exptl_absorpt_process_details xshape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _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 18390 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4298 _reflns_number_gt 2984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _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^)+(0.0318P)^2^+0.0238P] 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 4298 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.0000 0.0000 0.5000 0.02172(9) Uani 1 2 d S . . S1 S -0.17232(8) 0.10424(5) 0.49092(5) 0.02765(17) Uani 1 1 d . . . P1 P 0.09730(8) 0.04207(5) 0.66556(5) 0.02284(17) Uani 1 1 d . . . N1 N 0.0380(3) 0.2138(2) 0.49096(19) 0.0360(7) Uani 1 1 d . . . C1 C -0.0938(3) 0.2071(2) 0.5009(2) 0.0301(7) Uani 1 1 d . . . C2 C -0.1726(4) 0.2814(2) 0.5181(2) 0.0438(9) Uani 1 1 d . . . H2 H -0.2658 0.2755 0.5246 0.053 Uiso 1 1 calc R . . C3 C -0.1122(5) 0.3623(3) 0.5253(3) 0.0539(11) Uani 1 1 d . . . H3 H -0.1636 0.4128 0.5370 0.065 Uiso 1 1 calc R . . C4 C 0.0235(5) 0.3702(3) 0.5156(3) 0.0521(11) Uani 1 1 d . . . H4 H 0.0674 0.4254 0.5204 0.063 Uiso 1 1 calc R . . C5 C 0.0923(4) 0.2947(3) 0.4988(2) 0.0475(10) Uani 1 1 d . . . H5 H 0.1855 0.3000 0.4921 0.057 Uiso 1 1 calc R . . C6 C 0.0400(3) 0.1410(2) 0.7258(2) 0.0284(7) Uani 1 1 d . . . C7 C 0.1185(4) 0.2160(2) 0.7435(2) 0.0373(8) Uani 1 1 d . . . H7 H 0.2082 0.2168 0.7264 0.045 Uiso 1 1 calc R . . C8 C 0.0653(5) 0.2898(3) 0.7861(3) 0.0510(11) Uani 1 1 d . . . H8 H 0.1193 0.3407 0.7994 0.061 Uiso 1 1 calc R . . C9 C -0.0662(5) 0.2894(3) 0.8094(2) 0.0542(12) Uani 1 1 d . . . H9 H -0.1029 0.3404 0.8369 0.065 Uiso 1 1 calc R . . C10 C -0.1437(4) 0.2152(3) 0.7927(2) 0.0476(10) Uani 1 1 d . . . H10 H -0.2335 0.2150 0.8094 0.057 Uiso 1 1 calc R . . C11 C -0.0915(3) 0.1410(2) 0.7518(2) 0.0351(8) Uani 1 1 d . . . H11 H -0.1452 0.0897 0.7413 0.042 Uiso 1 1 calc R . . C12 C 0.0748(3) -0.0386(2) 0.7659(2) 0.0269(6) Uani 1 1 d . . . C13 C 0.1087(3) -0.0176(2) 0.8712(2) 0.0311(8) Uani 1 1 d . . . H13 H 0.1431 0.0388 0.8905 0.037 Uiso 1 1 calc R . . C14 C 0.0923(4) -0.0789(2) 0.9469(2) 0.0354(8) Uani 1 1 d . . . H14 H 0.1163 -0.0644 1.0180 0.042 Uiso 1 1 calc R . . C15 C 0.0414(4) -0.1606(3) 0.9203(2) 0.0409(9) Uani 1 1 d . . . H15 H 0.0308 -0.2025 0.9728 0.049 Uiso 1 1 calc R . . C16 C 0.0056(4) -0.1818(3) 0.8165(3) 0.0458(9) Uani 1 1 d . . . H16 H -0.0301 -0.2380 0.7978 0.055 Uiso 1 1 calc R . . C17 C 0.0220(4) -0.1206(2) 0.7399(2) 0.0350(8) Uani 1 1 d . . . H17 H -0.0033 -0.1351 0.6690 0.042 Uiso 1 1 calc R . . C18 C 0.2788(3) 0.0562(2) 0.66592(19) 0.0250(6) Uani 1 1 d . . . C19 C 0.3249(3) 0.0891(2) 0.5766(2) 0.0331(7) Uani 1 1 d . . . H19 H 0.2618 0.1069 0.5196 0.040 Uiso 1 1 calc R . . C20 C 0.4614(4) 0.0959(2) 0.5702(2) 0.0352(8) Uani 1 1 d . . . H20 H 0.4912 0.1183 0.5088 0.042 Uiso 1 1 calc R . . C21 C 0.5541(4) 0.0708(2) 0.6514(2) 0.0379(8) Uani 1 1 d . . . H21 H 0.6479 0.0755 0.6466 0.045 Uiso 1 1 calc R . . C22 C 0.5092(4) 0.0387(3) 0.7403(2) 0.0494(10) Uani 1 1 d . . . H22 H 0.5729 0.0217 0.7974 0.059 Uiso 1 1 calc R . . C23 C 0.3732(3) 0.0309(3) 0.7475(2) 0.0413(9) Uani 1 1 d . . . H23 H 0.3442 0.0080 0.8090 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01907(16) 0.02903(17) 0.01673(12) -0.00027(14) 0.00094(9) -0.00164(17) S1 0.0214(4) 0.0330(4) 0.0283(3) -0.0016(3) 0.0020(3) -0.0004(3) P1 0.0209(4) 0.0303(4) 0.0170(3) 0.0004(3) 0.0009(3) -0.0026(3) N1 0.0340(18) 0.0417(18) 0.0322(13) -0.0036(12) 0.0040(12) -0.0088(14) C1 0.032(2) 0.034(2) 0.0222(14) 0.0016(12) -0.0025(12) 0.0016(15) C2 0.046(2) 0.041(2) 0.0417(18) 0.0007(16) -0.0052(16) 0.0084(19) C3 0.076(3) 0.034(2) 0.047(2) 0.0006(16) -0.0123(19) 0.009(2) C4 0.074(4) 0.040(2) 0.039(2) 0.0045(16) -0.0063(19) -0.017(2) C5 0.055(3) 0.051(3) 0.0360(18) -0.0026(16) 0.0056(16) -0.021(2) C6 0.0300(18) 0.0364(19) 0.0175(12) -0.0003(12) -0.0015(11) 0.0022(15) C7 0.043(2) 0.0362(19) 0.0298(15) -0.0060(14) -0.0054(13) -0.0045(17) C8 0.073(3) 0.038(2) 0.0366(18) -0.0090(15) -0.0137(18) 0.000(2) C9 0.079(3) 0.054(3) 0.0268(16) -0.0114(16) -0.0042(17) 0.026(2) C10 0.049(2) 0.069(3) 0.0252(15) 0.0010(16) 0.0038(14) 0.026(2) C11 0.034(2) 0.049(2) 0.0222(13) -0.0023(13) 0.0019(12) 0.0089(17) C12 0.0245(17) 0.0330(16) 0.0234(13) 0.0004(12) 0.0038(11) -0.0027(14) C13 0.0339(17) 0.036(2) 0.0232(12) 0.0008(12) 0.0039(11) 0.0042(14) C14 0.039(2) 0.047(2) 0.0211(13) 0.0050(13) 0.0064(13) 0.0096(17) C15 0.036(2) 0.049(2) 0.0376(17) 0.0180(15) 0.0074(14) 0.0009(18) C16 0.049(2) 0.043(2) 0.0448(19) 0.0094(16) 0.0020(16) -0.0128(19) C17 0.036(2) 0.043(2) 0.0254(14) 0.0028(14) 0.0045(13) -0.0067(17) C18 0.0245(17) 0.0292(17) 0.0212(12) -0.0026(11) 0.0020(11) -0.0035(14) C19 0.0291(19) 0.041(2) 0.0289(14) 0.0046(13) 0.0038(12) -0.0050(15) C20 0.0296(19) 0.045(2) 0.0325(15) 0.0022(14) 0.0103(13) -0.0070(16) C21 0.0229(18) 0.053(2) 0.0384(16) -0.0044(15) 0.0056(13) -0.0051(16) C22 0.0251(19) 0.087(3) 0.0341(16) 0.0096(17) -0.0042(13) 0.0008(19) C23 0.0298(19) 0.070(3) 0.0230(13) 0.0094(14) -0.0017(12) -0.0052(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 Pd1 P1 2.3355(7) 3_556 ? Pd1 P1 2.3355(7) . ? Pd1 S1 2.3384(8) 3_556 ? Pd1 S1 2.3384(8) . ? S1 C1 1.754(3) . ? P1 C18 1.826(3) . ? P1 C6 1.828(3) . ? P1 C12 1.828(3) . ? N1 C1 1.344(4) . ? N1 C5 1.349(5) . ? C1 C2 1.417(5) . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.374(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.391(5) . ? C6 C11 1.398(5) . ? C7 C8 1.392(5) . ? C7 H7 0.9500 . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.383(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.385(5) . ? C12 C13 1.405(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.377(5) . ? C14 H14 0.9500 . ? C15 C16 1.389(5) . ? C15 H15 0.9500 . ? C16 C17 1.390(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.382(4) . ? C18 C19 1.394(4) . ? C19 C20 1.381(5) . ? C19 H19 0.9500 . ? C20 C21 1.368(5) . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 H23 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 P1 Pd1 P1 180.0 3_556 . ? P1 Pd1 S1 94.45(3) 3_556 3_556 ? P1 Pd1 S1 85.55(3) . 3_556 ? P1 Pd1 S1 85.55(3) 3_556 . ? P1 Pd1 S1 94.45(3) . . ? S1 Pd1 S1 180.0 3_556 . ? C1 S1 Pd1 106.67(12) . . ? C18 P1 C6 105.38(15) . . ? C18 P1 C12 106.82(14) . . ? C6 P1 C12 100.36(13) . . ? C18 P1 Pd1 109.47(8) . . ? C6 P1 Pd1 120.36(10) . . ? C12 P1 Pd1 113.33(10) . . ? C1 N1 C5 117.0(3) . . ? N1 C1 C2 121.6(3) . . ? N1 C1 S1 119.8(3) . . ? C2 C1 S1 118.6(3) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.2(4) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? N1 C5 C4 125.2(4) . . ? N1 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? C7 C6 C11 119.3(3) . . ? C7 C6 P1 123.5(3) . . ? C11 C6 P1 117.2(3) . . ? C6 C7 C8 119.8(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.3(4) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? C17 C12 C13 118.8(3) . . ? C17 C12 P1 120.9(2) . . ? C13 C12 P1 120.3(2) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.7(3) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C23 C18 C19 118.2(3) . . ? C23 C18 P1 123.4(2) . . ? C19 C18 P1 118.2(2) . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 118.9(3) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C18 120.5(3) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? 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 Pd1 S1 C1 -119.28(10) 3_556 . . . ? P1 Pd1 S1 C1 60.72(10) . . . . ? S1 Pd1 P1 C18 48.84(11) 3_556 . . . ? S1 Pd1 P1 C18 -131.16(11) . . . . ? S1 Pd1 P1 C6 171.06(13) 3_556 . . . ? S1 Pd1 P1 C6 -8.94(13) . . . . ? S1 Pd1 P1 C12 -70.29(11) 3_556 . . . ? S1 Pd1 P1 C12 109.71(11) . . . . ? C5 N1 C1 C2 0.3(4) . . . . ? C5 N1 C1 S1 179.6(2) . . . . ? Pd1 S1 C1 N1 13.0(2) . . . . ? Pd1 S1 C1 C2 -167.7(2) . . . . ? N1 C1 C2 C3 -0.3(4) . . . . ? S1 C1 C2 C3 -179.6(2) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C1 N1 C5 C4 -0.2(5) . . . . ? C3 C4 C5 N1 0.0(5) . . . . ? C18 P1 C6 C7 13.0(3) . . . . ? C12 P1 C6 C7 123.8(3) . . . . ? Pd1 P1 C6 C7 -111.2(2) . . . . ? C18 P1 C6 C11 -169.2(2) . . . . ? C12 P1 C6 C11 -58.4(2) . . . . ? Pd1 P1 C6 C11 66.6(2) . . . . ? C11 C6 C7 C8 -0.3(4) . . . . ? P1 C6 C7 C8 177.5(2) . . . . ? C6 C7 C8 C9 -1.1(5) . . . . ? C7 C8 C9 C10 1.6(5) . . . . ? C8 C9 C10 C11 -0.6(5) . . . . ? C9 C10 C11 C6 -0.8(5) . . . . ? C7 C6 C11 C10 1.2(4) . . . . ? P1 C6 C11 C10 -176.7(2) . . . . ? C18 P1 C12 C17 -112.0(3) . . . . ? C6 P1 C12 C17 138.3(3) . . . . ? Pd1 P1 C12 C17 8.7(3) . . . . ? C18 P1 C12 C13 69.2(3) . . . . ? C6 P1 C12 C13 -40.5(3) . . . . ? Pd1 P1 C12 C13 -170.1(2) . . . . ? C17 C12 C13 C14 1.5(5) . . . . ? P1 C12 C13 C14 -179.7(2) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 0.4(6) . . . . ? C13 C12 C17 C16 -1.4(5) . . . . ? P1 C12 C17 C16 179.8(3) . . . . ? C15 C16 C17 C12 0.5(6) . . . . ? C6 P1 C18 C23 88.4(3) . . . . ? C12 P1 C18 C23 -17.7(3) . . . . ? Pd1 P1 C18 C23 -140.8(3) . . . . ? C6 P1 C18 C19 -95.9(3) . . . . ? C12 P1 C18 C19 158.0(2) . . . . ? Pd1 P1 C18 C19 34.9(3) . . . . ? C23 C18 C19 C20 0.0(5) . . . . ? P1 C18 C19 C20 -175.9(3) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C19 C20 C21 C22 -0.2(5) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C21 C22 C23 C18 -0.8(6) . . . . ? C19 C18 C23 C22 0.4(5) . . . . ? P1 C18 C23 C22 176.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.613 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 963362' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew07701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 Cl2 N2 P Pd S2 Sn' _chemical_formula_sum 'C28 H23 Cl2 N2 P Pd S2 Sn' _chemical_formula_weight 778.56 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 8.7479(4) _cell_length_b 11.8756(5) _cell_length_c 15.2144(6) _cell_angle_alpha 96.721(3) _cell_angle_beta 93.528(3) _cell_angle_gamma 107.858(3) _cell_volume 1486.12(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 47346 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 32.30 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.840 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5826 _exptl_absorpt_correction_T_max 0.8466 _exptl_absorpt_process_details xshape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _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 29645 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0120 _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 -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 32.00 _reflns_number_total 10254 _reflns_number_gt 9754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _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^)+(0.0133P)^2^+1.2628P] 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 10254 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.286 _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 Pd1 Pd 0.176506(15) 0.756772(11) 0.251482(8) 0.01997(3) Uani 1 1 d . . . Sn1 Sn 0.223145(15) 0.558835(10) 0.250894(8) 0.02302(3) Uani 1 1 d . . . Cl1 Cl 0.47502(7) 0.51959(6) 0.26175(4) 0.04048(11) Uani 1 1 d . . . Cl2 Cl 0.02475(8) 0.36695(4) 0.23971(4) 0.04266(12) Uani 1 1 d . . . S1 S 0.12984(7) 0.75399(4) 0.39859(3) 0.03061(9) Uani 1 1 d . . . S2 S 0.21032(6) 0.74592(4) 0.10242(3) 0.02962(9) Uani 1 1 d . . . N2 N 0.2246(2) 0.51917(15) 0.10027(11) 0.0302(3) Uani 1 1 d . . . N1 N 0.2303(2) 0.55885(15) 0.40173(11) 0.0284(3) Uani 1 1 d . . . P1 P 0.14665(5) 0.94975(4) 0.25940(3) 0.02152(8) Uani 1 1 d . . . C1 C 0.1799(2) 0.64194(17) 0.44744(12) 0.0266(3) Uani 1 1 d . . . C2 C 0.1689(3) 0.6428(2) 0.53966(14) 0.0368(4) Uani 1 1 d . . . H2 H 0.1304 0.7000 0.5722 0.044 Uiso 1 1 calc R . . C3 C 0.2143(3) 0.5602(2) 0.58227(15) 0.0424(5) Uani 1 1 d . . . H3 H 0.2087 0.5611 0.6445 0.051 Uiso 1 1 calc R . . C4 C 0.2683(3) 0.4760(2) 0.53420(16) 0.0438(5) Uani 1 1 d . . . H4 H 0.3014 0.4192 0.5629 0.053 Uiso 1 1 calc R . . C5 C 0.2729(3) 0.4765(2) 0.44448(15) 0.0387(5) Uani 1 1 d . . . H5 H 0.3069 0.4176 0.4109 0.046 Uiso 1 1 calc R . . C6 C 0.2152(2) 0.60635(17) 0.05361(12) 0.0264(3) Uani 1 1 d . . . C7 C 0.2103(3) 0.5878(2) -0.03983(14) 0.0361(4) Uani 1 1 d . . . H7 H 0.1995 0.6480 -0.0734 0.043 Uiso 1 1 calc R . . C8 C 0.2211(3) 0.4824(2) -0.08199(15) 0.0447(5) Uani 1 1 d . . . H8 H 0.2196 0.4697 -0.1449 0.054 Uiso 1 1 calc R . . C9 C 0.2344(4) 0.3939(3) -0.03218(17) 0.0491(6) Uani 1 1 d . . . H9 H 0.2428 0.3206 -0.0604 0.059 Uiso 1 1 calc R . . C10 C 0.2351(3) 0.4150(2) 0.05859(16) 0.0429(5) Uani 1 1 d . . . H10 H 0.2432 0.3549 0.0930 0.051 Uiso 1 1 calc R . . C11 C 0.2447(2) 1.04451(16) 0.17918(13) 0.0253(3) Uani 1 1 d . . . C12 C 0.1870(3) 1.0091(2) 0.08945(15) 0.0355(4) Uani 1 1 d . . . H12 H 0.0939 0.9412 0.0723 0.043 Uiso 1 1 calc R . . C13 C 0.2650(3) 1.0727(2) 0.02490(17) 0.0453(5) Uani 1 1 d . . . H13 H 0.2256 1.0477 -0.0361 0.054 Uiso 1 1 calc R . . C14 C 0.3999(3) 1.1723(2) 0.04954(18) 0.0463(6) Uani 1 1 d . . . H14 H 0.4549 1.2141 0.0053 0.056 Uiso 1 1 calc R . . C15 C 0.4544(3) 1.2107(2) 0.13838(18) 0.0413(5) Uani 1 1 d . . . H15 H 0.5451 1.2804 0.1553 0.050 Uiso 1 1 calc R . . C16 C 0.3771(2) 1.14758(17) 0.20350(15) 0.0318(4) Uani 1 1 d . . . H16 H 0.4146 1.1749 0.2646 0.038 Uiso 1 1 calc R . . C17 C 0.2271(2) 1.03856(15) 0.36753(12) 0.0250(3) Uani 1 1 d . . . C18 C 0.3882(2) 1.05413(18) 0.39641(14) 0.0313(4) Uani 1 1 d . . . H18 H 0.4499 1.0180 0.3601 0.038 Uiso 1 1 calc R . . C19 C 0.4586(3) 1.1219(2) 0.47761(16) 0.0391(5) Uani 1 1 d . . . H19 H 0.5691 1.1345 0.4959 0.047 Uiso 1 1 calc R . . C20 C 0.3673(3) 1.1712(2) 0.53200(17) 0.0479(6) Uani 1 1 d . . . H20 H 0.4153 1.2177 0.5876 0.057 Uiso 1 1 calc R . . C21 C 0.2075(4) 1.1531(3) 0.50567(18) 0.0515(6) Uani 1 1 d . . . H21 H 0.1449 1.1856 0.5439 0.062 Uiso 1 1 calc R . . C22 C 0.1365(3) 1.0875(2) 0.42327(16) 0.0379(4) Uani 1 1 d . . . H22 H 0.0263 1.0763 0.4052 0.046 Uiso 1 1 calc R . . C23 C -0.0616(2) 0.94741(15) 0.24077(13) 0.0245(3) Uani 1 1 d . . . C24 C -0.1875(2) 0.84070(16) 0.23326(13) 0.0280(3) Uani 1 1 d . . . H24 H -0.1657 0.7686 0.2409 0.034 Uiso 1 1 calc R . . C25 C -0.3461(2) 0.8397(2) 0.21449(16) 0.0355(4) Uani 1 1 d . . . H25 H -0.4321 0.7664 0.2080 0.043 Uiso 1 1 calc R . . C26 C -0.3786(2) 0.9444(2) 0.20534(17) 0.0386(5) Uani 1 1 d . . . H26 H -0.4870 0.9429 0.1928 0.046 Uiso 1 1 calc R . . C27 C -0.2541(3) 1.0516(2) 0.2143(2) 0.0441(6) Uani 1 1 d . . . H27 H -0.2770 1.1238 0.2086 0.053 Uiso 1 1 calc R . . C28 C -0.0956(2) 1.05308(18) 0.23153(18) 0.0384(5) Uani 1 1 d . . . H28 H -0.0098 1.1264 0.2371 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02045(5) 0.01809(5) 0.02268(6) 0.00423(4) 0.00242(4) 0.00749(4) Sn1 0.02808(6) 0.01913(5) 0.02378(5) 0.00355(4) 0.00160(4) 0.01032(4) Cl1 0.0391(3) 0.0531(3) 0.0386(3) 0.0058(2) 0.0025(2) 0.0289(2) Cl2 0.0534(3) 0.0231(2) 0.0431(3) 0.00526(19) 0.0006(2) 0.0006(2) S1 0.0419(3) 0.0301(2) 0.0262(2) 0.00698(16) 0.00930(18) 0.01845(19) S2 0.0380(2) 0.0270(2) 0.0251(2) 0.00685(16) 0.00491(17) 0.01070(18) N2 0.0374(8) 0.0285(7) 0.0264(7) -0.0008(6) 0.0018(6) 0.0147(6) N1 0.0327(8) 0.0281(7) 0.0270(7) 0.0078(6) 0.0014(6) 0.0124(6) P1 0.01900(17) 0.01841(17) 0.0281(2) 0.00439(15) 0.00212(15) 0.00699(14) C1 0.0268(8) 0.0281(8) 0.0241(8) 0.0066(6) 0.0019(6) 0.0065(6) C2 0.0442(11) 0.0415(11) 0.0251(9) 0.0073(8) 0.0065(8) 0.0127(9) C3 0.0471(12) 0.0513(13) 0.0288(10) 0.0154(9) 0.0021(9) 0.0127(10) C4 0.0517(13) 0.0497(13) 0.0366(11) 0.0215(10) 0.0008(10) 0.0206(11) C5 0.0483(12) 0.0390(11) 0.0365(10) 0.0147(9) 0.0040(9) 0.0218(10) C6 0.0234(7) 0.0297(8) 0.0244(8) 0.0015(6) 0.0025(6) 0.0068(6) C7 0.0378(10) 0.0426(11) 0.0246(8) 0.0042(8) 0.0046(7) 0.0079(9) C8 0.0501(13) 0.0533(14) 0.0264(9) -0.0049(9) 0.0055(9) 0.0140(11) C9 0.0644(16) 0.0488(14) 0.0355(11) -0.0116(10) 0.0041(11) 0.0267(12) C10 0.0615(15) 0.0384(11) 0.0338(10) -0.0039(8) 0.0028(10) 0.0268(11) C11 0.0237(7) 0.0233(7) 0.0324(9) 0.0090(6) 0.0050(6) 0.0105(6) C12 0.0355(10) 0.0360(10) 0.0354(10) 0.0115(8) 0.0006(8) 0.0101(8) C13 0.0526(14) 0.0515(14) 0.0358(11) 0.0175(10) 0.0057(10) 0.0180(11) C14 0.0477(13) 0.0500(13) 0.0513(14) 0.0287(11) 0.0206(11) 0.0195(11) C15 0.0350(10) 0.0343(10) 0.0569(14) 0.0182(10) 0.0146(10) 0.0080(8) C16 0.0295(9) 0.0259(8) 0.0405(10) 0.0099(7) 0.0061(8) 0.0072(7) C17 0.0246(7) 0.0194(7) 0.0303(8) 0.0023(6) 0.0031(6) 0.0063(6) C18 0.0287(9) 0.0300(9) 0.0350(10) 0.0012(7) -0.0016(7) 0.0110(7) C19 0.0372(11) 0.0348(10) 0.0393(11) 0.0015(8) -0.0071(9) 0.0061(8) C20 0.0564(15) 0.0404(12) 0.0363(11) -0.0086(9) -0.0017(10) 0.0063(11) C21 0.0525(15) 0.0515(14) 0.0445(13) -0.0131(11) 0.0124(11) 0.0138(12) C22 0.0312(9) 0.0383(11) 0.0419(11) -0.0045(9) 0.0082(8) 0.0104(8) C23 0.0187(7) 0.0217(7) 0.0332(8) 0.0027(6) 0.0025(6) 0.0069(6) C24 0.0239(8) 0.0240(8) 0.0339(9) 0.0033(7) 0.0040(7) 0.0046(6) C25 0.0218(8) 0.0345(10) 0.0460(12) 0.0031(8) 0.0045(8) 0.0034(7) C26 0.0211(8) 0.0430(11) 0.0521(13) 0.0011(9) 0.0026(8) 0.0132(8) C27 0.0290(10) 0.0335(10) 0.0736(17) 0.0050(10) -0.0006(10) 0.0175(8) C28 0.0235(8) 0.0226(8) 0.0694(15) 0.0064(9) 0.0003(9) 0.0084(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 S2 2.2989(5) . ? Pd1 S1 2.3019(5) . ? Pd1 P1 2.3751(4) . ? Pd1 Sn1 2.50514(19) . ? Sn1 N2 2.2865(17) . ? Sn1 N1 2.2919(16) . ? Sn1 Cl2 2.3835(5) . ? Sn1 Cl1 2.3879(5) . ? S1 C1 1.7502(19) . ? S2 C6 1.749(2) . ? N2 C6 1.342(3) . ? N2 C10 1.355(3) . ? N1 C1 1.340(3) . ? N1 C5 1.364(3) . ? P1 C23 1.8179(17) . ? P1 C17 1.8195(19) . ? P1 C11 1.8304(18) . ? C1 C2 1.411(3) . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(4) . ? C3 H3 0.9500 . ? C4 C5 1.369(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.409(3) . ? C7 C8 1.371(3) . ? C7 H7 0.9500 . ? C8 C9 1.394(4) . ? C8 H8 0.9500 . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 C16 1.395(3) . ? C12 C13 1.393(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.395(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.391(3) . ? C17 C18 1.399(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 C21 1.373(4) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.388(2) . ? C23 C28 1.395(3) . ? C24 C25 1.395(3) . ? C24 H24 0.9500 . ? C25 C26 1.378(3) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 C28 1.390(3) . ? C27 H27 0.9500 . ? C28 H28 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 S2 Pd1 S1 175.903(19) . . ? S2 Pd1 P1 93.072(17) . . ? S1 Pd1 P1 89.751(17) . . ? S2 Pd1 Sn1 88.941(13) . . ? S1 Pd1 Sn1 88.407(13) . . ? P1 Pd1 Sn1 176.258(12) . . ? N2 Sn1 N1 167.48(6) . . ? N2 Sn1 Cl2 86.48(5) . . ? N1 Sn1 Cl2 85.78(5) . . ? N2 Sn1 Cl1 85.97(5) . . ? N1 Sn1 Cl1 86.45(4) . . ? Cl2 Sn1 Cl1 104.48(2) . . ? N2 Sn1 Pd1 96.29(4) . . ? N1 Sn1 Pd1 96.23(4) . . ? Cl2 Sn1 Pd1 127.539(17) . . ? Cl1 Sn1 Pd1 127.983(17) . . ? C1 S1 Pd1 114.59(7) . . ? C6 S2 Pd1 113.93(7) . . ? C6 N2 C10 120.55(18) . . ? C6 N2 Sn1 116.11(12) . . ? C10 N2 Sn1 123.34(15) . . ? C1 N1 C5 120.07(18) . . ? C1 N1 Sn1 115.96(12) . . ? C5 N1 Sn1 123.85(14) . . ? C23 P1 C17 106.62(8) . . ? C23 P1 C11 102.17(8) . . ? C17 P1 C11 104.56(9) . . ? C23 P1 Pd1 113.79(6) . . ? C17 P1 Pd1 111.53(6) . . ? C11 P1 Pd1 117.10(6) . . ? N1 C1 C2 119.72(18) . . ? N1 C1 S1 123.01(14) . . ? C2 C1 S1 117.25(16) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.5(2) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.2(2) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N2 C6 C7 119.74(18) . . ? N2 C6 S2 123.56(14) . . ? C7 C6 S2 116.70(16) . . ? C8 C7 C6 119.7(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 118.5(2) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 121.8(2) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C12 C11 C16 118.99(18) . . ? C12 C11 P1 117.97(14) . . ? C16 C11 P1 123.00(15) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.2(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C22 C17 C18 118.99(18) . . ? C22 C17 P1 123.80(15) . . ? C18 C17 P1 117.17(14) . . ? C19 C18 C17 120.5(2) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.5(2) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C17 C22 C21 120.0(2) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C28 119.55(17) . . ? C24 C23 P1 120.53(14) . . ? C28 C23 P1 119.90(14) . . ? C23 C24 C25 119.74(18) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 120.36(19) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.34(19) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 119.6(2) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C23 120.37(19) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? 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 S2 Pd1 Sn1 N2 -7.60(5) . . . . ? S1 Pd1 Sn1 N2 169.28(5) . . . . ? P1 Pd1 Sn1 N2 -130.2(2) . . . . ? S2 Pd1 Sn1 N1 172.55(5) . . . . ? S1 Pd1 Sn1 N1 -10.57(5) . . . . ? P1 Pd1 Sn1 N1 50.0(2) . . . . ? S2 Pd1 Sn1 Cl2 -97.99(2) . . . . ? S1 Pd1 Sn1 Cl2 78.89(2) . . . . ? P1 Pd1 Sn1 Cl2 139.41(19) . . . . ? S2 Pd1 Sn1 Cl1 82.19(2) . . . . ? S1 Pd1 Sn1 Cl1 -100.93(2) . . . . ? P1 Pd1 Sn1 Cl1 -40.40(19) . . . . ? S2 Pd1 S1 C1 60.4(3) . . . . ? P1 Pd1 S1 C1 -166.01(7) . . . . ? Sn1 Pd1 S1 C1 10.73(7) . . . . ? S1 Pd1 S2 C6 -39.2(3) . . . . ? P1 Pd1 S2 C6 -172.68(7) . . . . ? Sn1 Pd1 S2 C6 10.48(7) . . . . ? N1 Sn1 N2 C6 -175.7(2) . . . . ? Cl2 Sn1 N2 C6 132.44(14) . . . . ? Cl1 Sn1 N2 C6 -122.76(14) . . . . ? Pd1 Sn1 N2 C6 5.04(14) . . . . ? N1 Sn1 N2 C10 3.9(4) . . . . ? Cl2 Sn1 N2 C10 -47.95(19) . . . . ? Cl1 Sn1 N2 C10 56.85(19) . . . . ? Pd1 Sn1 N2 C10 -175.35(18) . . . . ? N2 Sn1 N1 C1 -167.0(2) . . . . ? Cl2 Sn1 N1 C1 -115.06(14) . . . . ? Cl1 Sn1 N1 C1 140.12(14) . . . . ? Pd1 Sn1 N1 C1 12.28(14) . . . . ? N2 Sn1 N1 C5 9.1(4) . . . . ? Cl2 Sn1 N1 C5 61.02(17) . . . . ? Cl1 Sn1 N1 C5 -43.80(17) . . . . ? Pd1 Sn1 N1 C5 -171.64(17) . . . . ? S2 Pd1 P1 C23 91.99(7) . . . . ? S1 Pd1 P1 C23 -85.04(7) . . . . ? Sn1 Pd1 P1 C23 -145.53(19) . . . . ? S2 Pd1 P1 C17 -147.35(6) . . . . ? S1 Pd1 P1 C17 35.62(7) . . . . ? Sn1 Pd1 P1 C17 -24.9(2) . . . . ? S2 Pd1 P1 C11 -26.98(7) . . . . ? S1 Pd1 P1 C11 155.99(7) . . . . ? Sn1 Pd1 P1 C11 95.5(2) . . . . ? C5 N1 C1 C2 -0.9(3) . . . . ? Sn1 N1 C1 C2 175.32(15) . . . . ? C5 N1 C1 S1 177.67(17) . . . . ? Sn1 N1 C1 S1 -6.1(2) . . . . ? Pd1 S1 C1 N1 -4.62(19) . . . . ? Pd1 S1 C1 C2 174.00(14) . . . . ? N1 C1 C2 C3 1.8(3) . . . . ? S1 C1 C2 C3 -176.86(19) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C1 N1 C5 C4 -0.9(3) . . . . ? Sn1 N1 C5 C4 -176.81(19) . . . . ? C3 C4 C5 N1 1.8(4) . . . . ? C10 N2 C6 C7 2.4(3) . . . . ? Sn1 N2 C6 C7 -178.03(14) . . . . ? C10 N2 C6 S2 -177.04(18) . . . . ? Sn1 N2 C6 S2 2.6(2) . . . . ? Pd1 S2 C6 N2 -10.19(19) . . . . ? Pd1 S2 C6 C7 170.41(13) . . . . ? N2 C6 C7 C8 -2.4(3) . . . . ? S2 C6 C7 C8 177.03(18) . . . . ? C6 C7 C8 C9 1.0(4) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? C6 N2 C10 C9 -0.9(4) . . . . ? Sn1 N2 C10 C9 179.5(2) . . . . ? C8 C9 C10 N2 -0.5(4) . . . . ? C23 P1 C11 C12 -58.30(17) . . . . ? C17 P1 C11 C12 -169.30(15) . . . . ? Pd1 P1 C11 C12 66.72(16) . . . . ? C23 P1 C11 C16 123.89(16) . . . . ? C17 P1 C11 C16 12.89(18) . . . . ? Pd1 P1 C11 C16 -111.09(15) . . . . ? C16 C11 C12 C13 2.9(3) . . . . ? P1 C11 C12 C13 -174.99(18) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C12 C13 C14 C15 -1.9(4) . . . . ? C13 C14 C15 C16 1.9(4) . . . . ? C14 C15 C16 C11 0.6(3) . . . . ? C12 C11 C16 C15 -2.9(3) . . . . ? P1 C11 C16 C15 174.86(16) . . . . ? C23 P1 C17 C22 2.7(2) . . . . ? C11 P1 C17 C22 110.49(18) . . . . ? Pd1 P1 C17 C22 -122.03(17) . . . . ? C23 P1 C17 C18 -179.48(15) . . . . ? C11 P1 C17 C18 -71.73(16) . . . . ? Pd1 P1 C17 C18 55.75(16) . . . . ? C22 C17 C18 C19 -2.9(3) . . . . ? P1 C17 C18 C19 179.21(17) . . . . ? C17 C18 C19 C20 2.2(3) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 C22 -1.5(4) . . . . ? C18 C17 C22 C21 1.4(3) . . . . ? P1 C17 C22 C21 179.1(2) . . . . ? C20 C21 C22 C17 0.8(4) . . . . ? C17 P1 C23 C24 -116.46(16) . . . . ? C11 P1 C23 C24 134.11(16) . . . . ? Pd1 P1 C23 C24 6.92(18) . . . . ? C17 P1 C23 C28 65.3(2) . . . . ? C11 P1 C23 C28 -44.2(2) . . . . ? Pd1 P1 C23 C28 -171.35(16) . . . . ? C28 C23 C24 C25 1.5(3) . . . . ? P1 C23 C24 C25 -176.76(16) . . . . ? C23 C24 C25 C26 -1.4(3) . . . . ? C24 C25 C26 C27 0.3(4) . . . . ? C25 C26 C27 C28 0.7(4) . . . . ? C26 C27 C28 C23 -0.7(4) . . . . ? C24 C23 C28 C27 -0.5(4) . . . . ? P1 C23 C28 C27 177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.485 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 963363' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew117_01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 Cl2 N2 P Pd S2 Sn' _chemical_formula_sum 'C28 H23 Cl2 N2 P Pd S2 Sn' _chemical_formula_weight 778.56 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' S S 0.1246 0.1234 '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' Sn Sn -0.6537 1.4246 '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' P P 0.1023 0.0942 '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 11.9426(4) _cell_length_b 11.9476(4) _cell_length_c 12.0757(4) _cell_angle_alpha 82.183(3) _cell_angle_beta 75.922(3) _cell_angle_gamma 60.174(3) _cell_volume 1449.67(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 24097 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 32.39 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6371 _exptl_absorpt_correction_T_max 0.8473 _exptl_absorpt_process_details xshape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _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 32803 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 32.00 _reflns_number_total 10015 _reflns_number_gt 8529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _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^)+(0.0393P)^2^+1.5059P] 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 SHELXL _refine_ls_extinction_coef 0.0048(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10015 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _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 0.167488(15) 0.240456(16) 0.706695(13) 0.01996(5) Uani 1 1 d . . . Sn1 Sn -0.033441(14) 0.240590(15) 0.685821(13) 0.02112(5) Uani 1 1 d . . . S1 S 0.12443(7) 0.19229(7) 0.90118(5) 0.02967(13) Uani 1 1 d . . . S2 S 0.20121(7) 0.29414(8) 0.51482(5) 0.03429(15) Uani 1 1 d . . . P1 P 0.36687(5) 0.22336(6) 0.72127(5) 0.02012(10) Uani 1 1 d . . . Cl1 Cl -0.05842(9) 0.06704(8) 0.64543(7) 0.04397(17) Uani 1 1 d . . . Cl2 Cl -0.24831(6) 0.41852(7) 0.71252(6) 0.03778(15) Uani 1 1 d . . . N1 N -0.0921(2) 0.1907(2) 0.87695(18) 0.0243(4) Uani 1 1 d . . . N2 N -0.0186(2) 0.2938(2) 0.49455(18) 0.0281(4) Uani 1 1 d . . . C1 C -0.0158(2) 0.1767(2) 0.94809(19) 0.0237(4) Uani 1 1 d . . . C2 C -0.0456(3) 0.1452(2) 1.0657(2) 0.0308(5) Uani 1 1 d . . . H2 H 0.0079 0.1377 1.1160 0.037 Uiso 1 1 calc R . . C3 C -0.1523(3) 0.1260(3) 1.1051(2) 0.0367(6) Uani 1 1 d . . . H3 H -0.1727 0.1030 1.1829 0.044 Uiso 1 1 calc R . . C4 C -0.2301(3) 0.1404(3) 1.0305(3) 0.0368(6) Uani 1 1 d . . . H4 H -0.3050 0.1281 1.0564 0.044 Uiso 1 1 calc R . . C5 C -0.1970(3) 0.1731(3) 0.9173(2) 0.0314(5) Uani 1 1 d . . . H5 H -0.2511 0.1835 0.8664 0.038 Uiso 1 1 calc R . . C6 C 0.0800(2) 0.3181(3) 0.4449(2) 0.0258(4) Uani 1 1 d . . . C7 C 0.0903(3) 0.3624(3) 0.3298(2) 0.0352(6) Uani 1 1 d . . . H7 H 0.1593 0.3819 0.2956 0.042 Uiso 1 1 calc R . . C8 C 0.0020(3) 0.3775(3) 0.2674(2) 0.0398(7) Uani 1 1 d . . . H8 H 0.0093 0.4065 0.1901 0.048 Uiso 1 1 calc R . . C9 C -0.0980(3) 0.3495(3) 0.3195(2) 0.0398(7) Uani 1 1 d . . . H9 H -0.1602 0.3576 0.2784 0.048 Uiso 1 1 calc R . . C10 C -0.1056(3) 0.3095(3) 0.4328(2) 0.0374(6) Uani 1 1 d . . . H10 H -0.1757 0.2923 0.4689 0.045 Uiso 1 1 calc R . . C11 C 0.3519(2) 0.3419(2) 0.8133(2) 0.0232(4) Uani 1 1 d . . . C12 C 0.2382(2) 0.4048(2) 0.8965(2) 0.0265(4) Uani 1 1 d . . . H12 H 0.1671 0.3876 0.9034 0.032 Uiso 1 1 calc R . . C13 C 0.2266(3) 0.4925(2) 0.9700(2) 0.0316(5) Uani 1 1 d . . . H13 H 0.1486 0.5337 1.0265 0.038 Uiso 1 1 calc R . . C14 C 0.3272(3) 0.5192(3) 0.9607(3) 0.0365(6) Uani 1 1 d . . . H14 H 0.3204 0.5775 1.0114 0.044 Uiso 1 1 calc R . . C15 C 0.4394(3) 0.4599(3) 0.8765(3) 0.0404(7) Uani 1 1 d . . . H15 H 0.5088 0.4796 0.8687 0.048 Uiso 1 1 calc R . . C16 C 0.4522(3) 0.3720(3) 0.8030(2) 0.0339(6) Uani 1 1 d . . . H16 H 0.5299 0.3326 0.7458 0.041 Uiso 1 1 calc R . . C17 C 0.4727(2) 0.2366(2) 0.58839(19) 0.0227(4) Uani 1 1 d . . . C18 C 0.5926(3) 0.1323(3) 0.5444(2) 0.0342(6) Uani 1 1 d . . . H18 H 0.6217 0.0506 0.5825 0.041 Uiso 1 1 calc R . . C19 C 0.6705(3) 0.1487(3) 0.4427(3) 0.0463(8) Uani 1 1 d . . . H19 H 0.7532 0.0778 0.4124 0.056 Uiso 1 1 calc R . . C20 C 0.6282(3) 0.2668(3) 0.3860(3) 0.0405(7) Uani 1 1 d . . . H20 H 0.6817 0.2764 0.3170 0.049 Uiso 1 1 calc R . . C21 C 0.5094(3) 0.3703(3) 0.4291(2) 0.0339(5) Uani 1 1 d . . . H21 H 0.4805 0.4517 0.3906 0.041 Uiso 1 1 calc R . . C22 C 0.4313(2) 0.3547(3) 0.5301(2) 0.0282(5) Uani 1 1 d . . . H22 H 0.3485 0.4259 0.5595 0.034 Uiso 1 1 calc R . . C23 C 0.4688(2) 0.0661(2) 0.7803(2) 0.0270(5) Uani 1 1 d . . . C24 C 0.4626(3) -0.0386(3) 0.7501(3) 0.0408(7) Uani 1 1 d . . . H24 H 0.4034 -0.0257 0.7034 0.049 Uiso 1 1 calc R . . C25 C 0.5430(4) -0.1623(3) 0.7882(4) 0.0575(10) Uani 1 1 d . . . H25 H 0.5399 -0.2341 0.7665 0.069 Uiso 1 1 calc R . . C26 C 0.6260(4) -0.1799(4) 0.8566(3) 0.0646(13) Uani 1 1 d . . . H26 H 0.6792 -0.2641 0.8842 0.077 Uiso 1 1 calc R . . C27 C 0.6337(4) -0.0776(4) 0.8860(4) 0.0682(13) Uani 1 1 d . . . H27 H 0.6932 -0.0915 0.9327 0.082 Uiso 1 1 calc R . . C28 C 0.5550(3) 0.0464(4) 0.8479(3) 0.0467(8) Uani 1 1 d . . . H28 H 0.5606 0.1172 0.8684 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01480(8) 0.02765(9) 0.01820(8) 0.00139(6) -0.00403(6) -0.01095(6) Sn1 0.01562(7) 0.02904(8) 0.02011(7) 0.00064(5) -0.00337(5) -0.01220(6) S1 0.0329(3) 0.0437(3) 0.0226(3) 0.0096(2) -0.0113(2) -0.0261(3) S2 0.0241(3) 0.0656(5) 0.0200(2) 0.0056(3) -0.0049(2) -0.0281(3) P1 0.0145(2) 0.0250(3) 0.0207(2) -0.00077(19) -0.00439(19) -0.0090(2) Cl1 0.0589(5) 0.0469(4) 0.0403(4) -0.0080(3) -0.0065(3) -0.0359(4) Cl2 0.0201(3) 0.0403(3) 0.0383(3) 0.0070(3) -0.0030(2) -0.0069(2) N1 0.0201(8) 0.0258(9) 0.0263(9) 0.0014(7) -0.0023(7) -0.0121(7) N2 0.0203(9) 0.0433(12) 0.0246(9) 0.0014(8) -0.0075(7) -0.0174(9) C1 0.0271(10) 0.0204(9) 0.0201(9) 0.0010(7) -0.0002(8) -0.0113(8) C2 0.0400(14) 0.0265(11) 0.0198(10) 0.0010(8) 0.0010(9) -0.0149(10) C3 0.0446(15) 0.0271(12) 0.0283(12) 0.0005(9) 0.0092(11) -0.0174(11) C4 0.0308(13) 0.0317(13) 0.0394(14) 0.0011(11) 0.0095(11) -0.0164(11) C5 0.0230(11) 0.0325(12) 0.0357(13) 0.0029(10) 0.0022(9) -0.0155(10) C6 0.0208(10) 0.0361(12) 0.0187(9) 0.0006(8) -0.0040(8) -0.0127(9) C7 0.0299(12) 0.0542(17) 0.0214(11) 0.0061(11) -0.0063(9) -0.0214(12) C8 0.0350(14) 0.0582(19) 0.0229(11) 0.0061(12) -0.0104(10) -0.0198(13) C9 0.0344(14) 0.0615(19) 0.0279(12) 0.0033(12) -0.0162(11) -0.0232(14) C10 0.0298(13) 0.0602(18) 0.0296(12) 0.0037(12) -0.0127(10) -0.0254(13) C11 0.0190(9) 0.0279(10) 0.0223(10) -0.0014(8) -0.0054(8) -0.0103(8) C12 0.0208(10) 0.0251(10) 0.0289(11) 0.0002(8) -0.0019(8) -0.0093(8) C13 0.0321(12) 0.0232(10) 0.0313(12) -0.0051(9) -0.0004(10) -0.0089(9) C14 0.0447(16) 0.0347(13) 0.0357(14) -0.0066(11) -0.0077(12) -0.0222(12) C15 0.0386(15) 0.0533(18) 0.0428(15) -0.0112(13) -0.0055(12) -0.0310(14) C16 0.0281(12) 0.0497(16) 0.0309(12) -0.0111(11) 0.0010(10) -0.0246(12) C17 0.0164(9) 0.0307(11) 0.0215(9) -0.0032(8) -0.0021(7) -0.0118(8) C18 0.0222(11) 0.0331(13) 0.0356(13) -0.0039(10) 0.0027(10) -0.0077(10) C19 0.0281(13) 0.0499(18) 0.0437(17) -0.0108(14) 0.0122(12) -0.0123(13) C20 0.0358(14) 0.0598(19) 0.0293(13) -0.0070(12) 0.0074(11) -0.0302(14) C21 0.0339(13) 0.0439(15) 0.0302(12) 0.0042(11) -0.0048(10) -0.0255(12) C22 0.0213(10) 0.0314(12) 0.0291(11) 0.0009(9) -0.0030(9) -0.0119(9) C23 0.0192(10) 0.0291(11) 0.0251(10) 0.0032(9) -0.0037(8) -0.0072(9) C24 0.0300(13) 0.0296(13) 0.0560(19) 0.0027(12) -0.0069(12) -0.0110(11) C25 0.0437(18) 0.0301(15) 0.073(3) 0.0079(16) 0.0027(18) -0.0077(13) C26 0.051(2) 0.0426(18) 0.0467(19) 0.0166(15) -0.0006(16) 0.0090(16) C27 0.050(2) 0.066(3) 0.048(2) 0.0053(18) -0.0262(17) 0.0075(19) C28 0.0360(15) 0.0508(18) 0.0423(16) 0.0000(14) -0.0218(13) -0.0070(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.3110(6) . ? Pd1 S1 2.3347(6) . ? Pd1 P1 2.3351(6) . ? Pd1 Sn1 2.4722(2) . ? Sn1 N2 2.299(2) . ? Sn1 N1 2.330(2) . ? Sn1 Cl2 2.3591(7) . ? Sn1 Cl1 2.3638(7) . ? S1 C1 1.727(2) . ? S2 C6 1.734(3) . ? P1 C23 1.817(2) . ? P1 C17 1.828(2) . ? P1 C11 1.831(2) . ? N1 C5 1.336(3) . ? N1 C1 1.337(3) . ? N2 C6 1.334(3) . ? N2 C10 1.348(3) . ? C1 C2 1.423(3) . ? C2 C3 1.367(4) . ? C2 H2 0.9500 . ? C3 C4 1.382(5) . ? C3 H3 0.9500 . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.418(3) . ? C7 C8 1.368(4) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C8 H8 0.9500 . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.387(3) . ? C11 C12 1.394(3) . ? C12 C13 1.399(4) . ? C12 H12 0.9500 . ? C13 C14 1.364(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 C22 1.391(4) . ? C18 C19 1.405(4) . ? C18 H18 0.9500 . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 C21 1.373(4) . ? C20 H20 0.9500 . ? C21 C22 1.396(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.377(4) . ? C23 C24 1.391(4) . ? C24 C25 1.391(4) . ? C24 H24 0.9500 . ? C25 C26 1.362(7) . ? C25 H25 0.9500 . ? C26 C27 1.369(7) . ? C26 H26 0.9500 . ? C27 C28 1.389(5) . ? C27 H27 0.9500 . ? C28 H28 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 S2 Pd1 S1 177.69(3) . . ? S2 Pd1 P1 91.13(2) . . ? S1 Pd1 P1 90.67(2) . . ? S2 Pd1 Sn1 88.409(17) . . ? S1 Pd1 Sn1 89.917(17) . . ? P1 Pd1 Sn1 175.411(16) . . ? N2 Sn1 N1 167.48(7) . . ? N2 Sn1 Cl2 86.37(6) . . ? N1 Sn1 Cl2 85.40(5) . . ? N2 Sn1 Cl1 87.53(6) . . ? N1 Sn1 Cl1 85.46(6) . . ? Cl2 Sn1 Cl1 104.75(3) . . ? N2 Sn1 Pd1 97.22(5) . . ? N1 Sn1 Pd1 95.26(5) . . ? Cl2 Sn1 Pd1 126.10(2) . . ? Cl1 Sn1 Pd1 129.08(2) . . ? C1 S1 Pd1 114.85(9) . . ? C6 S2 Pd1 115.44(8) . . ? C23 P1 C17 104.26(11) . . ? C23 P1 C11 105.90(12) . . ? C17 P1 C11 103.50(11) . . ? C23 P1 Pd1 110.12(9) . . ? C17 P1 Pd1 116.85(8) . . ? C11 P1 Pd1 115.11(8) . . ? C5 N1 C1 119.1(2) . . ? C5 N1 Sn1 122.65(19) . . ? C1 N1 Sn1 118.25(15) . . ? C6 N2 C10 118.9(2) . . ? C6 N2 Sn1 116.03(16) . . ? C10 N2 Sn1 124.93(18) . . ? N1 C1 C2 121.1(2) . . ? N1 C1 S1 121.71(17) . . ? C2 C1 S1 117.2(2) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.6(3) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 120.0(2) . . ? N2 C6 S2 122.54(18) . . ? C7 C6 S2 117.41(19) . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 118.5(3) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C8 C9 C10 118.6(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 123.3(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C16 C11 C12 118.0(2) . . ? C16 C11 P1 121.55(18) . . ? C12 C11 P1 120.48(18) . . ? C11 C12 C13 121.3(2) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 121.2(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C11 C16 C15 120.2(2) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C22 119.3(2) . . ? C18 C17 P1 121.7(2) . . ? C22 C17 P1 118.92(17) . . ? C17 C18 C19 119.2(3) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C17 C22 C21 121.2(2) . . ? C17 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C28 C23 C24 119.6(3) . . ? C28 C23 P1 123.0(2) . . ? C24 C23 P1 117.4(2) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 119.7(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 119.6(4) . . ? C23 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? 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 S2 Pd1 Sn1 N2 -0.05(6) . . . . ? S1 Pd1 Sn1 N2 178.36(6) . . . . ? S2 Pd1 Sn1 N1 -178.95(5) . . . . ? S1 Pd1 Sn1 N1 -0.54(5) . . . . ? S2 Pd1 Sn1 Cl2 -90.82(3) . . . . ? S1 Pd1 Sn1 Cl2 87.59(3) . . . . ? S2 Pd1 Sn1 Cl1 92.63(3) . . . . ? S1 Pd1 Sn1 Cl1 -88.96(3) . . . . ? P1 Pd1 S1 C1 -175.16(9) . . . . ? Sn1 Pd1 S1 C1 0.29(9) . . . . ? P1 Pd1 S2 C6 178.38(11) . . . . ? Sn1 Pd1 S2 C6 2.95(10) . . . . ? S2 Pd1 P1 C23 -125.47(9) . . . . ? S1 Pd1 P1 C23 55.98(9) . . . . ? S2 Pd1 P1 C17 -6.82(9) . . . . ? S1 Pd1 P1 C17 174.63(9) . . . . ? S2 Pd1 P1 C11 114.93(9) . . . . ? S1 Pd1 P1 C11 -63.62(9) . . . . ? N2 Sn1 N1 C5 7.4(5) . . . . ? Cl2 Sn1 N1 C5 56.46(19) . . . . ? Cl1 Sn1 N1 C5 -48.77(19) . . . . ? Pd1 Sn1 N1 C5 -177.65(19) . . . . ? N2 Sn1 N1 C1 -174.0(3) . . . . ? Cl2 Sn1 N1 C1 -124.87(17) . . . . ? Cl1 Sn1 N1 C1 129.91(17) . . . . ? Pd1 Sn1 N1 C1 1.03(17) . . . . ? N1 Sn1 N2 C6 171.2(3) . . . . ? Cl2 Sn1 N2 C6 122.22(19) . . . . ? Cl1 Sn1 N2 C6 -132.82(19) . . . . ? Pd1 Sn1 N2 C6 -3.7(2) . . . . ? N1 Sn1 N2 C10 -4.4(5) . . . . ? Cl2 Sn1 N2 C10 -53.5(2) . . . . ? Cl1 Sn1 N2 C10 51.5(2) . . . . ? Pd1 Sn1 N2 C10 -179.4(2) . . . . ? C5 N1 C1 C2 -0.8(3) . . . . ? Sn1 N1 C1 C2 -179.50(17) . . . . ? C5 N1 C1 S1 177.72(18) . . . . ? Sn1 N1 C1 S1 -1.0(3) . . . . ? Pd1 S1 C1 N1 0.4(2) . . . . ? Pd1 S1 C1 C2 178.98(16) . . . . ? N1 C1 C2 C3 1.6(4) . . . . ? S1 C1 C2 C3 -176.9(2) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C1 N1 C5 C4 -0.2(4) . . . . ? Sn1 N1 C5 C4 178.4(2) . . . . ? C3 C4 C5 N1 0.4(4) . . . . ? C10 N2 C6 C7 1.4(4) . . . . ? Sn1 N2 C6 C7 -174.6(2) . . . . ? C10 N2 C6 S2 -177.1(2) . . . . ? Sn1 N2 C6 S2 6.9(3) . . . . ? Pd1 S2 C6 N2 -7.0(3) . . . . ? Pd1 S2 C6 C7 174.48(19) . . . . ? N2 C6 C7 C8 -1.8(4) . . . . ? S2 C6 C7 C8 176.8(3) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C7 C8 C9 C10 1.0(5) . . . . ? C6 N2 C10 C9 0.2(5) . . . . ? Sn1 N2 C10 C9 175.8(3) . . . . ? C8 C9 C10 N2 -1.4(5) . . . . ? C23 P1 C11 C16 79.0(2) . . . . ? C17 P1 C11 C16 -30.3(3) . . . . ? Pd1 P1 C11 C16 -159.1(2) . . . . ? C23 P1 C11 C12 -100.8(2) . . . . ? C17 P1 C11 C12 149.8(2) . . . . ? Pd1 P1 C11 C12 21.1(2) . . . . ? C16 C11 C12 C13 -1.9(4) . . . . ? P1 C11 C12 C13 177.9(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 1.2(5) . . . . ? C13 C14 C15 C16 -1.4(5) . . . . ? C12 C11 C16 C15 1.7(4) . . . . ? P1 C11 C16 C15 -178.1(2) . . . . ? C14 C15 C16 C11 -0.1(5) . . . . ? C23 P1 C17 C18 9.8(2) . . . . ? C11 P1 C17 C18 120.4(2) . . . . ? Pd1 P1 C17 C18 -111.9(2) . . . . ? C23 P1 C17 C22 -170.3(2) . . . . ? C11 P1 C17 C22 -59.7(2) . . . . ? Pd1 P1 C17 C22 67.9(2) . . . . ? C22 C17 C18 C19 1.0(4) . . . . ? P1 C17 C18 C19 -179.2(3) . . . . ? C17 C18 C19 C20 -0.7(5) . . . . ? C18 C19 C20 C21 0.4(5) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C18 C17 C22 C21 -1.0(4) . . . . ? P1 C17 C22 C21 179.1(2) . . . . ? C20 C21 C22 C17 0.8(4) . . . . ? C17 P1 C23 C28 86.0(3) . . . . ? C11 P1 C23 C28 -22.8(3) . . . . ? Pd1 P1 C23 C28 -147.9(2) . . . . ? C17 P1 C23 C24 -90.8(2) . . . . ? C11 P1 C23 C24 160.4(2) . . . . ? Pd1 P1 C23 C24 35.3(2) . . . . ? C28 C23 C24 C25 0.0(5) . . . . ? P1 C23 C24 C25 176.9(3) . . . . ? C23 C24 C25 C26 1.1(5) . . . . ? C24 C25 C26 C27 -1.7(6) . . . . ? C25 C26 C27 C28 1.1(7) . . . . ? C24 C23 C28 C27 -0.6(5) . . . . ? P1 C23 C28 C27 -177.3(3) . . . . ? C26 C27 C28 C23 0.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.041 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 963364' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew09701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 Cl2 N2 P Pd S2 Sn, 2(C H Cl3)' _chemical_formula_sum 'C30 H25 Cl8 N2 P Pd S2 Sn' _chemical_formula_weight 1017.30 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' S S 0.1246 0.1234 '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' Sn Sn -0.6537 1.4246 '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 '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 36.1869(14) _cell_length_b 10.7163(5) _cell_length_c 22.1382(9) _cell_angle_alpha 90.00 _cell_angle_beta 119.940(3) _cell_angle_gamma 90.00 _cell_volume 7439.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 60851 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 32.43 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 1.911 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6830 _exptl_absorpt_correction_T_max 0.8243 _exptl_absorpt_process_details xshape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _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 62249 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 32.00 _reflns_number_total 12857 _reflns_number_gt 11518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; The asymmetric unit contains two molecules of solvent of crystallization (chloroform) one of which is disordered over two sites (with site occupancies of 0.565(5) and 0.435(5)). For the refinement of this disorder the following restraints were used: All C-Cl bonds were constrained to the same length and all Cl-Cl separations within each part of the molecule were also restrained to the same distance. Furthermore, the C atoms C29, C29a and the Cl atoms Cl3, Cl3a and Cl4, Cl4a were refined with the same anisotropic displacement parameters. eadp c29a c29b eadp cl3a cl3b eadp cl4a cl4b sadi 0.001 c29a cl3a c29a cl4a c29a cl5a c29b cl3b c29b cl4b c29b cl5b sadi 0.001 cl3a cl4a cl4a cl5a cl5a cl3a cl3b cl4b cl4b cl5b cl5b cl3b Site occupancies were refined with one free variable (21, -21) which in total yields full occupancy of this solvent site. 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^)+(0.0438P)^2^+14.2491P] 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 SHELXL _refine_ls_extinction_coef 0.00089(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12857 _refine_ls_number_parameters 426 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.082 _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 Cl1 Cl 0.416103(16) 0.81747(5) 0.44109(3) 0.02742(10) Uani 1 1 d . . . Cl2 Cl 0.329121(17) 0.59801(6) 0.41174(3) 0.02861(10) Uani 1 1 d . . . N1 N 0.41702(6) 0.51857(17) 0.42005(8) 0.0216(3) Uani 1 1 d . . . N2 N 0.31856(5) 0.82958(16) 0.31581(9) 0.0215(3) Uani 1 1 d . . . P1 P 0.353933(16) 0.57889(5) 0.13306(2) 0.01773(9) Uani 1 1 d . . . Pd1 Pd 0.362162(4) 0.619307(13) 0.243234(7) 0.01624(4) Uani 1 1 d . . . S1 S 0.419183(17) 0.48554(5) 0.29945(3) 0.02368(10) Uani 1 1 d . . . S2 S 0.303964(17) 0.74919(5) 0.18901(3) 0.02515(10) Uani 1 1 d . . . Sn1 Sn 0.367924(4) 0.671151(12) 0.357865(6) 0.01669(4) Uani 1 1 d . . . C1 C 0.43321(6) 0.45528(19) 0.38618(10) 0.0212(3) Uani 1 1 d . . . C2 C 0.46325(8) 0.3597(2) 0.42090(13) 0.0307(5) Uani 1 1 d . . . H2 H 0.4746 0.3141 0.3971 0.037 Uiso 1 1 calc R . . C3 C 0.47602(8) 0.3326(2) 0.48924(14) 0.0350(5) Uani 1 1 d . . . H3 H 0.4962 0.2682 0.5129 0.042 Uiso 1 1 calc R . . C4 C 0.45919(8) 0.3999(3) 0.52362(12) 0.0341(5) Uani 1 1 d . . . H4 H 0.4677 0.3827 0.5709 0.041 Uiso 1 1 calc R . . C5 C 0.42989(8) 0.4921(2) 0.48742(11) 0.0288(4) Uani 1 1 d . . . H5 H 0.4183 0.5388 0.5106 0.035 Uiso 1 1 calc R . . C6 C 0.29629(6) 0.84335(18) 0.24637(10) 0.0197(3) Uani 1 1 d . . . C7 C 0.26469(7) 0.9368(2) 0.21702(12) 0.0277(4) Uani 1 1 d . . . H7 H 0.2486 0.9470 0.1679 0.033 Uiso 1 1 calc R . . C8 C 0.25733(7) 1.0129(2) 0.25971(13) 0.0314(5) Uani 1 1 d . . . H8 H 0.2364 1.0767 0.2401 0.038 Uiso 1 1 calc R . . C9 C 0.28049(8) 0.9970(2) 0.33166(13) 0.0305(4) Uani 1 1 d . . . H9 H 0.2757 1.0488 0.3619 0.037 Uiso 1 1 calc R . . C10 C 0.31052(7) 0.9039(2) 0.35739(12) 0.0278(4) Uani 1 1 d . . . H10 H 0.3263 0.8910 0.4064 0.033 Uiso 1 1 calc R . . C11 C 0.36345(7) 0.71108(19) 0.09142(10) 0.0220(3) Uani 1 1 d . . . C12 C 0.37844(8) 0.8236(2) 0.12720(12) 0.0281(4) Uani 1 1 d . . . H12 H 0.3817 0.8332 0.1722 0.034 Uiso 1 1 calc R . . C13 C 0.38867(9) 0.9215(3) 0.09718(14) 0.0382(6) Uani 1 1 d . . . H13 H 0.3991 0.9978 0.1219 0.046 Uiso 1 1 calc R . . C14 C 0.38373(9) 0.9083(3) 0.03091(15) 0.0389(6) Uani 1 1 d . . . H14 H 0.3907 0.9755 0.0104 0.047 Uiso 1 1 calc R . . C15 C 0.36864(11) 0.7970(3) -0.00502(15) 0.0418(6) Uani 1 1 d . . . H15 H 0.3649 0.7883 -0.0505 0.050 Uiso 1 1 calc R . . C16 C 0.35901(9) 0.6982(2) 0.02523(12) 0.0336(5) Uani 1 1 d . . . H16 H 0.3494 0.6214 0.0009 0.040 Uiso 1 1 calc R . . C17 C 0.30009(6) 0.52391(19) 0.07487(10) 0.0210(3) Uani 1 1 d . . . C18 C 0.28701(7) 0.4167(2) 0.09490(12) 0.0287(4) Uani 1 1 d . . . H18 H 0.3062 0.3765 0.1374 0.034 Uiso 1 1 calc R . . C19 C 0.24664(8) 0.3682(2) 0.05396(14) 0.0333(5) Uani 1 1 d . . . H19 H 0.2384 0.2940 0.0675 0.040 Uiso 1 1 calc R . . C20 C 0.21823(8) 0.4291(3) -0.00734(14) 0.0377(5) Uani 1 1 d . . . H20 H 0.1903 0.3966 -0.0358 0.045 Uiso 1 1 calc R . . C21 C 0.23049(9) 0.5365(3) -0.02689(14) 0.0417(6) Uani 1 1 d . . . H21 H 0.2107 0.5782 -0.0685 0.050 Uiso 1 1 calc R . . C22 C 0.27132(8) 0.5844(2) 0.01333(12) 0.0308(5) Uani 1 1 d . . . H22 H 0.2796 0.6578 -0.0009 0.037 Uiso 1 1 calc R . . C23 C 0.38897(7) 0.4612(2) 0.12883(10) 0.0218(3) Uani 1 1 d . . . C24 C 0.43266(7) 0.4875(3) 0.16305(12) 0.0333(5) Uani 1 1 d . . . H24 H 0.4429 0.5641 0.1874 0.040 Uiso 1 1 calc R . . C25 C 0.46106(9) 0.4022(3) 0.16162(14) 0.0441(7) Uani 1 1 d . . . H25 H 0.4907 0.4204 0.1849 0.053 Uiso 1 1 calc R . . C26 C 0.44612(11) 0.2900(3) 0.12610(16) 0.0462(7) Uani 1 1 d . . . H26 H 0.4656 0.2309 0.1258 0.055 Uiso 1 1 calc R . . C27 C 0.40338(11) 0.2646(2) 0.09152(17) 0.0421(6) Uani 1 1 d . . . H27 H 0.3933 0.1886 0.0664 0.051 Uiso 1 1 calc R . . C28 C 0.37444(8) 0.3489(2) 0.09276(13) 0.0293(4) Uani 1 1 d . . . H28 H 0.3448 0.3299 0.0691 0.035 Uiso 1 1 calc R . . C30 C 0.36080(10) 0.2005(3) 0.27550(15) 0.0375(5) Uani 1 1 d . . . H30 H 0.3838 0.2571 0.2793 0.045 Uiso 1 1 calc R . . Cl6 Cl 0.32244(3) 0.29117(8) 0.28206(5) 0.0569(2) Uani 1 1 d . . . Cl7 Cl 0.38364(3) 0.09109(9) 0.34361(4) 0.05185(18) Uani 1 1 d . . . Cl8 Cl 0.33814(3) 0.12321(8) 0.19455(4) 0.0541(2) Uani 1 1 d . . . C29A C 0.53355(13) -0.0488(2) 0.1638(2) 0.0420(8) Uani 0.565(5) 1 d PD A 1 H29A H 0.5608 -0.0680 0.1646 0.050 Uiso 0.565(5) 1 calc PR A 1 Cl3A Cl 0.4942(3) -0.0019(5) 0.0790(2) 0.0567(3) Uani 0.565(5) 1 d PD A 1 Cl4A Cl 0.5417(3) 0.0732(3) 0.2232(3) 0.0546(5) Uani 0.565(5) 1 d PD A 1 Cl5A Cl 0.51523(13) -0.1828(3) 0.18782(15) 0.0928(12) Uani 0.565(5) 1 d PD A 1 C29B C 0.50869(14) -0.0532(3) 0.1655(3) 0.0420(8) Uani 0.435(5) 1 d PD A 2 H29B H 0.4820 -0.0610 0.1680 0.050 Uiso 0.435(5) 1 calc PR A 2 Cl3B Cl 0.4964(4) -0.0016(6) 0.0815(3) 0.0567(3) Uani 0.435(5) 1 d PD A 2 Cl4B Cl 0.5436(4) 0.0558(3) 0.2282(4) 0.0546(5) Uani 0.435(5) 1 d PD A 2 Cl5B Cl 0.53464(10) -0.1997(2) 0.18212(12) 0.0533(7) Uani 0.435(5) 1 d PD 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 Cl1 0.0236(2) 0.0236(2) 0.0271(2) -0.00515(17) 0.00666(18) -0.00150(17) Cl2 0.0276(2) 0.0356(3) 0.0249(2) 0.00528(19) 0.01482(19) -0.00287(19) N1 0.0236(7) 0.0218(7) 0.0167(7) 0.0020(6) 0.0081(6) 0.0026(6) N2 0.0201(7) 0.0242(8) 0.0199(7) 0.0000(6) 0.0098(6) 0.0029(6) P1 0.0214(2) 0.0174(2) 0.01501(18) 0.00029(15) 0.00953(16) 0.00119(16) Pd1 0.01922(7) 0.01628(7) 0.01364(6) 0.00094(4) 0.00851(5) 0.00180(4) S1 0.0271(2) 0.0250(2) 0.0224(2) 0.00520(17) 0.01499(18) 0.00866(18) S2 0.0271(2) 0.0301(2) 0.01673(19) 0.00399(17) 0.00982(18) 0.01081(19) Sn1 0.01846(6) 0.01778(6) 0.01310(6) 0.00065(4) 0.00731(4) 0.00176(4) C1 0.0201(8) 0.0204(8) 0.0217(8) 0.0040(7) 0.0094(7) 0.0020(6) C2 0.0304(10) 0.0291(10) 0.0340(11) 0.0117(9) 0.0170(9) 0.0148(9) C3 0.0317(11) 0.0359(12) 0.0329(11) 0.0169(10) 0.0127(9) 0.0126(9) C4 0.0355(12) 0.0376(12) 0.0238(9) 0.0128(9) 0.0108(9) 0.0114(10) C5 0.0334(11) 0.0312(10) 0.0180(8) 0.0066(7) 0.0099(8) 0.0102(9) C6 0.0197(8) 0.0196(8) 0.0209(8) 0.0029(6) 0.0110(7) 0.0022(6) C7 0.0258(9) 0.0293(10) 0.0264(9) 0.0063(8) 0.0119(8) 0.0110(8) C8 0.0278(10) 0.0298(11) 0.0382(12) 0.0040(9) 0.0177(9) 0.0108(8) C9 0.0294(10) 0.0295(10) 0.0365(11) -0.0024(9) 0.0193(9) 0.0076(8) C10 0.0286(10) 0.0305(10) 0.0252(9) -0.0028(8) 0.0142(8) 0.0068(8) C11 0.0268(9) 0.0205(8) 0.0208(8) 0.0026(7) 0.0134(7) 0.0020(7) C12 0.0311(10) 0.0261(10) 0.0234(9) 0.0001(7) 0.0108(8) -0.0059(8) C13 0.0427(13) 0.0287(11) 0.0385(12) 0.0040(10) 0.0167(11) -0.0096(10) C14 0.0441(14) 0.0336(12) 0.0436(14) 0.0146(11) 0.0253(12) -0.0013(10) C15 0.0624(18) 0.0421(14) 0.0359(12) 0.0109(11) 0.0359(13) 0.0047(13) C16 0.0541(15) 0.0290(11) 0.0277(10) 0.0006(8) 0.0279(11) 0.0009(10) C17 0.0217(8) 0.0211(8) 0.0187(8) -0.0014(6) 0.0091(7) 0.0009(7) C18 0.0281(10) 0.0325(11) 0.0275(10) 0.0050(8) 0.0154(8) -0.0018(8) C19 0.0318(11) 0.0330(11) 0.0392(12) -0.0036(10) 0.0208(10) -0.0071(9) C20 0.0266(10) 0.0428(14) 0.0356(12) -0.0094(11) 0.0093(9) -0.0070(10) C21 0.0304(12) 0.0443(14) 0.0318(11) 0.0025(11) 0.0015(10) 0.0003(10) C22 0.0293(10) 0.0264(10) 0.0260(10) 0.0039(8) 0.0059(8) 0.0013(8) C23 0.0267(9) 0.0237(9) 0.0177(7) 0.0026(7) 0.0131(7) 0.0057(7) C24 0.0258(10) 0.0514(15) 0.0219(9) -0.0050(9) 0.0114(8) 0.0056(10) C25 0.0314(12) 0.075(2) 0.0281(11) 0.0072(12) 0.0168(10) 0.0205(13) C26 0.0587(17) 0.0485(16) 0.0481(15) 0.0188(13) 0.0393(14) 0.0320(14) C27 0.0657(18) 0.0236(11) 0.0571(16) 0.0073(11) 0.0458(16) 0.0135(11) C28 0.0412(12) 0.0201(9) 0.0359(11) 0.0012(8) 0.0263(10) 0.0023(8) C30 0.0470(14) 0.0295(11) 0.0430(13) 0.0012(10) 0.0277(12) -0.0049(10) Cl6 0.0706(5) 0.0404(4) 0.0784(6) 0.0078(4) 0.0514(5) 0.0095(4) Cl7 0.0585(4) 0.0581(5) 0.0455(4) 0.0167(3) 0.0308(4) 0.0095(4) Cl8 0.0704(5) 0.0497(4) 0.0420(4) -0.0039(3) 0.0279(4) -0.0070(4) C29A 0.0323(17) 0.047(2) 0.0416(19) -0.0004(16) 0.0144(16) 0.0068(17) Cl3A 0.0582(9) 0.0618(5) 0.0351(4) 0.0025(4) 0.0121(5) 0.0130(4) Cl4A 0.0554(8) 0.0618(9) 0.0393(8) -0.0064(9) 0.0181(7) 0.0070(13) Cl5A 0.110(3) 0.0662(15) 0.0825(16) 0.0119(12) 0.0333(16) -0.0228(16) C29B 0.0323(17) 0.047(2) 0.0416(19) -0.0004(16) 0.0144(16) 0.0068(17) Cl3B 0.0582(9) 0.0618(5) 0.0351(4) 0.0025(4) 0.0121(5) 0.0130(4) Cl4B 0.0554(8) 0.0618(9) 0.0393(8) -0.0064(9) 0.0181(7) 0.0070(13) Cl5B 0.0639(15) 0.0496(10) 0.0396(9) 0.0078(7) 0.0206(9) 0.0201(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Sn1 2.3846(5) . ? Cl2 Sn1 2.3834(5) . ? N1 C1 1.343(3) . ? N1 C5 1.352(3) . ? N1 Sn1 2.2987(17) . ? N2 C6 1.341(3) . ? N2 C10 1.354(3) . ? N2 Sn1 2.2978(17) . ? P1 C11 1.814(2) . ? P1 C17 1.816(2) . ? P1 C23 1.824(2) . ? P1 Pd1 2.3452(5) . ? Pd1 S2 2.3000(5) . ? Pd1 S1 2.3018(5) . ? Pd1 Sn1 2.5028(2) . ? S1 C1 1.754(2) . ? S2 C6 1.749(2) . ? C1 C2 1.410(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.411(3) . ? C7 C8 1.371(3) . ? C7 H7 0.9500 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.373(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 C16 1.399(3) . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C14 1.394(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.395(3) . ? C17 C18 1.396(3) . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.390(4) . ? C19 H19 0.9500 . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.393(3) . ? C23 C24 1.399(3) . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C27 1.368(5) . ? C26 H26 0.9500 . ? C27 C28 1.394(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 Cl7 1.757(3) . ? C30 Cl6 1.759(3) . ? C30 Cl8 1.762(3) . ? C30 H30 1.0000 . ? C29A Cl5A 1.771(3) . ? C29A Cl3A 1.771(3) . ? C29A Cl4A 1.771(3) . ? C29A H29A 1.0000 . ? C29B Cl5B 1.771(3) . ? C29B Cl3B 1.771(3) . ? C29B Cl4B 1.771(3) . ? C29B H29B 1.0000 . ? 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 N1 C5 120.27(18) . . ? C1 N1 Sn1 116.55(13) . . ? C5 N1 Sn1 123.18(15) . . ? C6 N2 C10 120.30(18) . . ? C6 N2 Sn1 116.54(13) . . ? C10 N2 Sn1 123.11(14) . . ? C11 P1 C17 107.54(9) . . ? C11 P1 C23 101.59(10) . . ? C17 P1 C23 105.45(10) . . ? C11 P1 Pd1 115.24(7) . . ? C17 P1 Pd1 109.40(7) . . ? C23 P1 Pd1 116.78(6) . . ? S2 Pd1 S1 177.86(2) . . ? S2 Pd1 P1 87.768(18) . . ? S1 Pd1 P1 93.528(18) . . ? S2 Pd1 Sn1 89.203(14) . . ? S1 Pd1 Sn1 89.511(14) . . ? P1 Pd1 Sn1 176.946(14) . . ? C1 S1 Pd1 113.49(7) . . ? C6 S2 Pd1 113.95(7) . . ? N2 Sn1 N1 168.64(6) . . ? N2 Sn1 Cl2 85.00(5) . . ? N1 Sn1 Cl2 86.48(5) . . ? N2 Sn1 Cl1 87.02(5) . . ? N1 Sn1 Cl1 87.50(5) . . ? Cl2 Sn1 Cl1 102.46(2) . . ? N2 Sn1 Pd1 95.66(4) . . ? N1 Sn1 Pd1 95.61(4) . . ? Cl2 Sn1 Pd1 131.505(15) . . ? Cl1 Sn1 Pd1 126.029(16) . . ? N1 C1 C2 119.68(19) . . ? N1 C1 S1 123.32(15) . . ? C2 C1 S1 117.00(17) . . ? C3 C2 C1 119.8(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 118.3(2) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.3(2) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N2 C6 C7 119.43(19) . . ? N2 C6 S2 123.12(15) . . ? C7 C6 S2 117.45(15) . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 117.6(2) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? N2 C10 C9 122.7(2) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C12 C11 C16 119.2(2) . . ? C12 C11 P1 120.33(16) . . ? C16 C11 P1 120.24(17) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.2(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.4(2) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C22 C17 C18 119.1(2) . . ? C22 C17 P1 123.76(17) . . ? C18 C17 P1 117.09(15) . . ? C19 C18 C17 121.1(2) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 119.4(2) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.3 . . ? C28 C23 C24 119.1(2) . . ? C28 C23 P1 123.58(17) . . ? C24 C23 P1 117.36(17) . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.9(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.7(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 119.9(3) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? Cl7 C30 Cl6 110.52(16) . . ? Cl7 C30 Cl8 109.86(15) . . ? Cl6 C30 Cl8 110.98(17) . . ? Cl7 C30 H30 108.5 . . ? Cl6 C30 H30 108.5 . . ? Cl8 C30 H30 108.5 . . ? Cl5A C29A Cl3A 109.0(3) . . ? Cl5A C29A Cl4A 109.0(3) . . ? Cl3A C29A Cl4A 108.9(3) . . ? Cl5A C29A H29A 110.0 . . ? Cl3A C29A H29A 110.0 . . ? Cl4A C29A H29A 110.0 . . ? Cl5B C29B Cl3B 109.0(3) . . ? Cl5B C29B Cl4B 109.0(3) . . ? Cl3B C29B Cl4B 108.9(3) . . ? Cl5B C29B H29B 110.0 . . ? Cl3B C29B H29B 110.0 . . ? Cl4B C29B H29B 110.0 . . ? 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 P1 Pd1 S2 66.21(8) . . . . ? C17 P1 Pd1 S2 -55.06(7) . . . . ? C23 P1 Pd1 S2 -174.67(8) . . . . ? C11 P1 Pd1 S1 -115.49(8) . . . . ? C17 P1 Pd1 S1 123.24(7) . . . . ? C23 P1 Pd1 S1 3.63(8) . . . . ? P1 Pd1 S1 C1 -168.47(8) . . . . ? Sn1 Pd1 S1 C1 11.83(8) . . . . ? P1 Pd1 S2 C6 -168.10(8) . . . . ? Sn1 Pd1 S2 C6 11.51(8) . . . . ? C6 N2 Sn1 N1 -164.2(3) . . . . ? C10 N2 Sn1 N1 13.4(4) . . . . ? C6 N2 Sn1 Cl2 -122.72(15) . . . . ? C10 N2 Sn1 Cl2 54.93(18) . . . . ? C6 N2 Sn1 Cl1 134.49(15) . . . . ? C10 N2 Sn1 Cl1 -47.86(18) . . . . ? C6 N2 Sn1 Pd1 8.57(15) . . . . ? C10 N2 Sn1 Pd1 -173.79(17) . . . . ? C5 N1 Sn1 N2 -0.4(4) . . . . ? C1 N1 Sn1 Cl2 138.70(15) . . . . ? C5 N1 Sn1 Cl2 -41.80(18) . . . . ? C1 N1 Sn1 Cl1 -118.65(15) . . . . ? C5 N1 Sn1 Cl1 60.85(18) . . . . ? C1 N1 Sn1 Pd1 7.32(15) . . . . ? C5 N1 Sn1 Pd1 -173.18(18) . . . . ? S2 Pd1 Sn1 N2 -9.50(5) . . . . ? S1 Pd1 Sn1 N2 172.20(5) . . . . ? S2 Pd1 Sn1 N1 169.08(5) . . . . ? S1 Pd1 Sn1 N1 -9.22(5) . . . . ? S2 Pd1 Sn1 Cl2 78.82(3) . . . . ? S1 Pd1 Sn1 Cl2 -99.48(2) . . . . ? S2 Pd1 Sn1 Cl1 -99.93(2) . . . . ? S1 Pd1 Sn1 Cl1 81.78(2) . . . . ? C5 N1 C1 C2 1.0(3) . . . . ? Sn1 N1 C1 C2 -179.51(17) . . . . ? C5 N1 C1 S1 -178.64(17) . . . . ? Sn1 N1 C1 S1 0.9(2) . . . . ? Pd1 S1 C1 N1 -10.1(2) . . . . ? Pd1 S1 C1 C2 170.30(16) . . . . ? N1 C1 C2 C3 -0.5(4) . . . . ? S1 C1 C2 C3 179.1(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C1 N1 C5 C4 -0.8(4) . . . . ? Sn1 N1 C5 C4 179.7(2) . . . . ? C3 C4 C5 N1 0.2(4) . . . . ? C10 N2 C6 C7 0.7(3) . . . . ? Sn1 N2 C6 C7 178.37(16) . . . . ? C10 N2 C6 S2 -178.66(17) . . . . ? Sn1 N2 C6 S2 -0.9(2) . . . . ? Pd1 S2 C6 N2 -8.6(2) . . . . ? Pd1 S2 C6 C7 172.04(15) . . . . ? N2 C6 C7 C8 0.5(3) . . . . ? S2 C6 C7 C8 179.82(19) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C6 N2 C10 C9 -1.4(4) . . . . ? Sn1 N2 C10 C9 -178.94(19) . . . . ? C8 C9 C10 N2 0.9(4) . . . . ? C17 P1 C11 C12 127.99(19) . . . . ? C23 P1 C11 C12 -121.52(19) . . . . ? Pd1 P1 C11 C12 5.7(2) . . . . ? C17 P1 C11 C16 -57.0(2) . . . . ? C23 P1 C11 C16 53.5(2) . . . . ? Pd1 P1 C11 C16 -179.30(17) . . . . ? C16 C11 C12 C13 0.2(4) . . . . ? P1 C11 C12 C13 175.2(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 -0.9(5) . . . . ? C14 C15 C16 C11 1.6(5) . . . . ? C12 C11 C16 C15 -1.2(4) . . . . ? P1 C11 C16 C15 -176.3(2) . . . . ? C11 P1 C17 C22 -5.9(2) . . . . ? C23 P1 C17 C22 -113.7(2) . . . . ? Pd1 P1 C17 C22 119.90(19) . . . . ? C11 P1 C17 C18 175.96(17) . . . . ? C23 P1 C17 C18 68.15(19) . . . . ? Pd1 P1 C17 C18 -58.21(18) . . . . ? C22 C17 C18 C19 1.8(4) . . . . ? P1 C17 C18 C19 179.97(19) . . . . ? C17 C18 C19 C20 -1.7(4) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C19 C20 C21 C22 1.0(5) . . . . ? C20 C21 C22 C17 -0.9(4) . . . . ? C18 C17 C22 C21 -0.5(4) . . . . ? P1 C17 C22 C21 -178.5(2) . . . . ? C11 P1 C23 C28 -118.13(19) . . . . ? C17 P1 C23 C28 -6.1(2) . . . . ? Pd1 P1 C23 C28 115.64(17) . . . . ? C11 P1 C23 C24 60.82(18) . . . . ? C17 P1 C23 C24 172.90(17) . . . . ? Pd1 P1 C23 C24 -65.41(18) . . . . ? C28 C23 C24 C25 -0.7(3) . . . . ? P1 C23 C24 C25 -179.7(2) . . . . ? C23 C24 C25 C26 0.0(4) . . . . ? C24 C25 C26 C27 1.2(4) . . . . ? C25 C26 C27 C28 -1.5(4) . . . . ? C24 C23 C28 C27 0.3(3) . . . . ? P1 C23 C28 C27 179.28(19) . . . . ? C26 C27 C28 C23 0.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.796 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.116 _database_code_depnum_ccdc_archive 'CCDC 963365' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew07301 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Cl4 P2 Pd Sn, 2(C H Cl3) ' _chemical_formula_sum 'C38 H32 Cl10 P2 Pd Sn' _chemical_formula_weight 1130.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.8853(2) _cell_length_b 16.0997(2) _cell_length_c 22.9151(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.421(2) _cell_angle_gamma 90.00 _cell_volume 4376.99(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 85206 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 30.39 _exptl_crystal_description piece _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.693 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6531 _exptl_absorpt_correction_T_max 0.8098 _exptl_absorpt_process_details xshape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _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 79190 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12735 _reflns_number_gt 11757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; The asymmetric unit contains two molecules of solvent of crystallization (chloroform) which are disordered over two sites each (with site occupancies of 0.643(8) and 0.357(8) for molecule 1 and 0.888(4) and 0.112(4) for molecule 2). For the refinement of this disorder the following restraints were used: For the low occupancy part of molecule 1 the C-Cl bonds were constrained to the same length and the Cl-Cl separations within this part of the molecule were also restrained to the same distance. Furthermore, the C atoms C37, C37a and the Cl atoms Cl6, Cl6a of the two alternative molecules, which are in very close proximity to each other, were refined with the same anisotropic displacement parameters. eadp c37 c37a eadp cl6 cl6a sadi 0.001 c37a cl5a c37a cl6a c37a cl7a sadi 0.001 cl5a cl6a cl6a cl7a cl7a cl5a For the low occupancy part of molecule 2 the C-Cl bonds were constrained to the same length and the Cl-Cl separations within this part of the molecule were also restrained to the same distance. Furthermore, the C and Cl atoms were refined with the same anisotropic displacement parameters as their parent atoms in the high occupancy part of the molecule. eadp c38 c38a eadp cl8 cl11 eadp cl9 cl12 eadp cl10 cl13 sadi 0.001 c38a cl11 c38a cl12 c38a cl13 sadi 0.001 cl11 cl12 cl12 cl13 cl13 cl11 Site occupancies were refined with free variables (21, -21; 31, -31) which in total yield full occupancy of each solvent site. 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^)+(0.0318P)^2^+3.4324P] 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 SHELXL _refine_ls_extinction_coef 0.00194(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12735 _refine_ls_number_parameters 508 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.002 _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 0.121884(10) 0.183128(8) 0.227994(5) 0.01630(4) Uani 1 1 d . . . Sn1 Sn -0.087585(9) 0.183931(7) 0.192281(5) 0.01881(4) Uani 1 1 d . . . Cl1 Cl 0.02131(4) 0.18899(3) 0.313144(19) 0.02649(9) Uani 1 1 d . . . Cl2 Cl -0.19638(5) 0.07457(4) 0.22778(3) 0.04461(14) Uani 1 1 d . . . Cl3 Cl -0.19547(5) 0.29739(4) 0.21914(3) 0.04039(13) Uani 1 1 d . . . Cl4 Cl -0.16230(4) 0.17200(5) 0.09424(2) 0.04146(14) Uani 1 1 d . . . P1 P 0.29555(4) 0.16461(3) 0.283137(19) 0.01846(8) Uani 1 1 d . . . P2 P 0.18126(4) 0.18290(3) 0.134938(19) 0.01822(8) Uani 1 1 d . . . C1 C 0.40255(15) 0.24472(12) 0.28491(8) 0.0231(3) Uani 1 1 d . . . C2 C 0.39378(19) 0.31133(12) 0.24624(10) 0.0308(4) Uani 1 1 d . . . H2 H 0.3297 0.3165 0.2197 0.037 Uiso 1 1 calc R . . C3 C 0.4797(2) 0.37074(15) 0.24660(12) 0.0427(6) Uani 1 1 d . . . H3 H 0.4736 0.4165 0.2204 0.051 Uiso 1 1 calc R . . C4 C 0.5729(2) 0.36311(16) 0.28480(13) 0.0468(6) Uani 1 1 d . . . H4 H 0.6317 0.4031 0.2843 0.056 Uiso 1 1 calc R . . C5 C 0.58179(19) 0.29767(17) 0.32384(13) 0.0428(6) Uani 1 1 d . . . H5 H 0.6464 0.2929 0.3501 0.051 Uiso 1 1 calc R . . C6 C 0.49674(17) 0.23920(14) 0.32474(10) 0.0312(4) Uani 1 1 d . . . H6 H 0.5020 0.1952 0.3524 0.037 Uiso 1 1 calc R . . C7 C 0.36151(15) 0.06881(11) 0.26088(8) 0.0214(3) Uani 1 1 d . . . C8 C 0.29128(16) 0.00565(12) 0.23876(9) 0.0270(4) Uani 1 1 d . . . H8 H 0.2120 0.0139 0.2356 0.032 Uiso 1 1 calc R . . C9 C 0.33606(19) -0.06918(13) 0.22122(10) 0.0329(4) Uani 1 1 d . . . H9 H 0.2877 -0.1116 0.2055 0.040 Uiso 1 1 calc R . . C10 C 0.4513(2) -0.08199(13) 0.22671(10) 0.0339(4) Uani 1 1 d . . . H10 H 0.4819 -0.1338 0.2157 0.041 Uiso 1 1 calc R . . C11 C 0.52193(18) -0.01956(14) 0.24814(10) 0.0336(4) Uani 1 1 d . . . H11 H 0.6011 -0.0284 0.2515 0.040 Uiso 1 1 calc R . . C12 C 0.47797(16) 0.05598(13) 0.26473(9) 0.0283(4) Uani 1 1 d . . . H12 H 0.5271 0.0991 0.2787 0.034 Uiso 1 1 calc R . . C13 C 0.27217(15) 0.14862(13) 0.36023(8) 0.0248(3) Uani 1 1 d . . . C14 C 0.26329(18) 0.06930(15) 0.38369(9) 0.0342(4) Uani 1 1 d . . . H14 H 0.2760 0.0218 0.3603 0.041 Uiso 1 1 calc R . . C15 C 0.2356(2) 0.05978(19) 0.44156(11) 0.0461(6) Uani 1 1 d . . . H15 H 0.2295 0.0057 0.4576 0.055 Uiso 1 1 calc R . . C16 C 0.2171(2) 0.1283(2) 0.47551(10) 0.0484(7) Uani 1 1 d . . . H16 H 0.1980 0.1213 0.5149 0.058 Uiso 1 1 calc R . . C17 C 0.2262(2) 0.2071(2) 0.45271(10) 0.0435(6) Uani 1 1 d . . . H17 H 0.2139 0.2542 0.4764 0.052 Uiso 1 1 calc R . . C18 C 0.25328(18) 0.21756(15) 0.39512(9) 0.0330(4) Uani 1 1 d . . . H18 H 0.2590 0.2719 0.3794 0.040 Uiso 1 1 calc R . . C19 C 0.32651(14) 0.20851(12) 0.12131(7) 0.0211(3) Uani 1 1 d . . . C20 C 0.41166(16) 0.14970(13) 0.13187(9) 0.0278(4) Uani 1 1 d . . . H20 H 0.3933 0.0952 0.1440 0.033 Uiso 1 1 calc R . . C21 C 0.52328(18) 0.17104(16) 0.12464(11) 0.0370(5) Uani 1 1 d . . . H21 H 0.5811 0.1311 0.1322 0.044 Uiso 1 1 calc R . . C22 C 0.55059(18) 0.24996(17) 0.10657(11) 0.0397(5) Uani 1 1 d . . . H22 H 0.6272 0.2644 0.1023 0.048 Uiso 1 1 calc R . . C23 C 0.46682(19) 0.30788(15) 0.09469(11) 0.0370(5) Uani 1 1 d . . . H23 H 0.4857 0.3618 0.0815 0.044 Uiso 1 1 calc R . . C24 C 0.35468(16) 0.28753(13) 0.10201(9) 0.0281(4) Uani 1 1 d . . . H24 H 0.2972 0.3276 0.0938 0.034 Uiso 1 1 calc R . . C25 C 0.15630(15) 0.08444(11) 0.09774(8) 0.0222(3) Uani 1 1 d . . . C26 C 0.08403(17) 0.02543(12) 0.11977(9) 0.0273(4) Uani 1 1 d . . . H26 H 0.0488 0.0361 0.1551 0.033 Uiso 1 1 calc R . . C27 C 0.0634(2) -0.04886(14) 0.09024(11) 0.0390(5) Uani 1 1 d . . . H27 H 0.0143 -0.0888 0.1055 0.047 Uiso 1 1 calc R . . C28 C 0.1140(2) -0.06481(15) 0.03881(11) 0.0407(5) Uani 1 1 d . . . H28 H 0.0992 -0.1155 0.0186 0.049 Uiso 1 1 calc R . . C29 C 0.1860(2) -0.00719(15) 0.01664(10) 0.0398(5) Uani 1 1 d . . . H29 H 0.2208 -0.0184 -0.0188 0.048 Uiso 1 1 calc R . . C30 C 0.20773(19) 0.06701(14) 0.04579(9) 0.0326(4) Uani 1 1 d . . . H30 H 0.2578 0.1063 0.0304 0.039 Uiso 1 1 calc R . . C31 C 0.10298(14) 0.26311(12) 0.09373(8) 0.0229(3) Uani 1 1 d . . . C32 C 0.07359(17) 0.33477(13) 0.12330(10) 0.0301(4) Uani 1 1 d . . . H32 H 0.0928 0.3399 0.1640 0.036 Uiso 1 1 calc R . . C33 C 0.0162(2) 0.39899(15) 0.09370(13) 0.0433(6) Uani 1 1 d . . . H33 H -0.0030 0.4479 0.1140 0.052 Uiso 1 1 calc R . . C34 C -0.0123(2) 0.39136(18) 0.03500(13) 0.0485(7) Uani 1 1 d . . . H34 H -0.0518 0.4350 0.0148 0.058 Uiso 1 1 calc R . . C35 C 0.0159(2) 0.32094(19) 0.00533(11) 0.0471(7) Uani 1 1 d . . . H35 H -0.0049 0.3162 -0.0352 0.056 Uiso 1 1 calc R . . C36 C 0.07496(18) 0.25623(16) 0.03394(9) 0.0337(4) Uani 1 1 d . . . H36 H 0.0957 0.2082 0.0130 0.040 Uiso 1 1 calc R . . C37 C 0.5553(10) 0.8582(6) 0.0897(8) 0.0528(10) Uani 0.643(8) 1 d P A 1 H37 H 0.5348 0.8253 0.1245 0.063 Uiso 0.643(8) 1 calc PR A 1 Cl5 Cl 0.6607(4) 0.9255(3) 0.1130(2) 0.0718(10) Uani 0.643(8) 1 d P A 1 Cl6 Cl 0.5975(4) 0.78863(17) 0.03852(18) 0.0787(9) Uani 0.643(8) 1 d P A 1 Cl7 Cl 0.4375(2) 0.91223(16) 0.06549(12) 0.0754(6) Uani 0.643(8) 1 d P A 1 C37A C 0.5724(17) 0.8594(11) 0.0925(14) 0.0528(10) Uani 0.357(8) 1 d PD A 2 H37A H 0.5326 0.8341 0.1254 0.063 Uiso 0.357(8) 1 calc PR A 2 Cl5A Cl 0.6747(5) 0.9332(3) 0.1199(3) 0.0458(9) Uani 0.357(8) 1 d PD A 2 Cl6A Cl 0.6428(6) 0.7811(3) 0.0532(3) 0.0787(9) Uani 0.357(8) 1 d PD A 2 Cl7A Cl 0.4741(7) 0.9113(4) 0.0430(5) 0.138(3) Uani 0.357(8) 1 d PD A 2 C38 C 0.3227(3) 0.4441(2) 0.88639(19) 0.0352(5) Uani 0.888(4) 1 d P B 1 H38 H 0.3404 0.4079 0.8527 0.042 Uiso 0.888(4) 1 calc PR B 1 Cl8 Cl 0.20630(8) 0.40200(7) 0.92167(8) 0.0658(4) Uani 0.888(4) 1 d P B 1 Cl9 Cl 0.28648(11) 0.54452(7) 0.86080(6) 0.0461(2) Uani 0.888(4) 1 d P B 1 Cl10 Cl 0.44035(11) 0.44869(9) 0.93675(7) 0.0529(3) Uani 0.888(4) 1 d P B 1 C38A C 0.3296(16) 0.4428(12) 0.8903(13) 0.0352(5) Uani 0.112(4) 1 d PD B 2 H38A H 0.3698 0.4140 0.8590 0.042 Uiso 0.112(4) 1 calc PR B 2 Cl11 Cl 0.2149(7) 0.3861(6) 0.8928(6) 0.0658(4) Uani 0.112(4) 1 d PD B 2 Cl12 Cl 0.3127(9) 0.5366(7) 0.8625(6) 0.0461(2) Uani 0.112(4) 1 d PD B 2 Cl13 Cl 0.4217(10) 0.4343(8) 0.9466(6) 0.0529(3) Uani 0.112(4) 1 d PD B 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 0.01283(6) 0.02130(7) 0.01485(6) 0.00068(4) 0.00138(4) 0.00135(4) Sn1 0.01275(6) 0.02329(6) 0.02045(6) -0.00090(4) 0.00158(4) 0.00076(4) Cl1 0.02080(19) 0.0410(2) 0.01811(18) 0.00056(16) 0.00487(14) 0.00068(16) Cl2 0.0461(3) 0.0372(3) 0.0500(3) 0.0091(2) -0.0020(3) -0.0205(2) Cl3 0.0309(2) 0.0336(3) 0.0562(3) -0.0105(2) -0.0010(2) 0.0129(2) Cl4 0.0239(2) 0.0768(4) 0.0232(2) -0.0069(2) -0.00196(17) -0.0011(2) P1 0.01520(18) 0.02210(19) 0.01795(19) 0.00128(15) 0.00001(14) 0.00131(15) P2 0.01569(18) 0.0228(2) 0.01631(18) 0.00034(15) 0.00268(14) -0.00028(14) C1 0.0196(7) 0.0248(8) 0.0252(8) -0.0039(7) 0.0035(6) -0.0004(6) C2 0.0362(11) 0.0262(9) 0.0308(10) -0.0018(7) 0.0091(8) -0.0007(7) C3 0.0537(14) 0.0291(10) 0.0476(13) -0.0038(9) 0.0232(11) -0.0099(10) C4 0.0356(12) 0.0396(12) 0.0676(17) -0.0217(12) 0.0226(12) -0.0152(10) C5 0.0258(10) 0.0456(13) 0.0571(15) -0.0226(12) 0.0033(10) -0.0067(9) C6 0.0237(9) 0.0333(10) 0.0361(10) -0.0070(8) -0.0017(8) -0.0015(7) C7 0.0203(7) 0.0229(8) 0.0209(7) 0.0013(6) 0.0006(6) 0.0025(6) C8 0.0223(8) 0.0272(9) 0.0313(9) 0.0009(7) 0.0009(7) -0.0032(7) C9 0.0371(11) 0.0251(9) 0.0368(11) -0.0012(8) 0.0049(8) -0.0059(8) C10 0.0426(11) 0.0236(9) 0.0364(11) 0.0002(8) 0.0093(9) 0.0050(8) C11 0.0262(9) 0.0329(10) 0.0418(11) -0.0008(9) 0.0043(8) 0.0086(8) C12 0.0208(8) 0.0285(9) 0.0353(10) -0.0029(8) -0.0010(7) 0.0030(7) C13 0.0178(7) 0.0380(10) 0.0184(7) 0.0031(7) -0.0008(6) 0.0018(7) C14 0.0318(10) 0.0442(12) 0.0266(9) 0.0101(9) 0.0020(8) 0.0009(9) C15 0.0435(13) 0.0633(17) 0.0316(11) 0.0189(11) 0.0040(9) -0.0017(12) C16 0.0365(12) 0.087(2) 0.0215(10) 0.0111(11) 0.0026(8) 0.0025(12) C17 0.0360(11) 0.0714(17) 0.0229(10) -0.0069(10) 0.0011(8) 0.0057(11) C18 0.0320(10) 0.0443(12) 0.0224(9) -0.0018(8) 0.0001(7) 0.0053(9) C19 0.0175(7) 0.0276(8) 0.0186(7) 0.0000(6) 0.0045(6) -0.0012(6) C20 0.0218(8) 0.0334(10) 0.0285(9) 0.0061(7) 0.0054(7) 0.0025(7) C21 0.0204(9) 0.0500(13) 0.0410(12) 0.0079(10) 0.0053(8) 0.0041(8) C22 0.0195(9) 0.0541(14) 0.0461(13) 0.0056(11) 0.0058(8) -0.0067(9) C23 0.0273(10) 0.0399(12) 0.0442(12) 0.0077(9) 0.0061(9) -0.0106(8) C24 0.0227(8) 0.0297(9) 0.0321(9) 0.0034(8) 0.0042(7) -0.0031(7) C25 0.0212(8) 0.0248(8) 0.0209(8) -0.0019(6) 0.0041(6) -0.0015(6) C26 0.0305(9) 0.0267(9) 0.0253(8) -0.0020(7) 0.0079(7) -0.0049(7) C27 0.0488(13) 0.0293(10) 0.0402(12) -0.0051(9) 0.0149(10) -0.0125(9) C28 0.0535(14) 0.0319(11) 0.0376(12) -0.0128(9) 0.0101(10) -0.0082(10) C29 0.0489(13) 0.0402(12) 0.0318(11) -0.0130(9) 0.0162(10) -0.0073(10) C30 0.0373(11) 0.0348(10) 0.0271(9) -0.0064(8) 0.0133(8) -0.0082(8) C31 0.0166(7) 0.0304(9) 0.0218(8) 0.0060(7) 0.0011(6) -0.0020(6) C32 0.0271(9) 0.0289(9) 0.0341(10) 0.0045(8) -0.0005(8) 0.0020(7) C33 0.0321(11) 0.0312(11) 0.0662(17) 0.0116(11) -0.0008(11) 0.0045(9) C34 0.0327(11) 0.0479(14) 0.0635(17) 0.0285(13) -0.0103(11) -0.0007(10) C35 0.0372(12) 0.0685(18) 0.0339(12) 0.0258(12) -0.0111(10) -0.0106(11) C36 0.0295(9) 0.0474(12) 0.0238(9) 0.0076(8) -0.0020(7) -0.0063(9) C37 0.067(4) 0.0452(15) 0.048(2) 0.0060(12) 0.017(2) -0.001(2) Cl5 0.0566(13) 0.103(2) 0.0566(13) -0.0129(11) 0.0056(11) -0.0180(11) Cl6 0.109(2) 0.0516(7) 0.0802(17) -0.0090(9) 0.0458(16) -0.0030(12) Cl7 0.0594(11) 0.0786(11) 0.0869(13) -0.0007(9) -0.0071(9) -0.0004(8) C37A 0.067(4) 0.0452(15) 0.048(2) 0.0060(12) 0.017(2) -0.001(2) Cl5A 0.0463(17) 0.0412(14) 0.0489(18) 0.0010(12) -0.0050(12) -0.0017(12) Cl6A 0.109(2) 0.0516(7) 0.0802(17) -0.0090(9) 0.0458(16) -0.0030(12) Cl7A 0.089(4) 0.148(5) 0.172(7) 0.024(5) -0.049(4) -0.003(3) C38 0.0335(11) 0.0350(11) 0.0366(12) -0.0067(9) -0.0017(9) 0.0005(9) Cl8 0.0480(4) 0.0628(5) 0.0887(10) -0.0033(6) 0.0213(5) -0.0160(4) Cl9 0.0561(6) 0.0377(4) 0.0435(3) -0.0026(3) -0.0058(5) 0.0123(4) Cl10 0.0426(6) 0.0536(6) 0.0601(7) -0.0011(4) -0.0172(5) 0.0017(4) C38A 0.0335(11) 0.0350(11) 0.0366(12) -0.0067(9) -0.0017(9) 0.0005(9) Cl11 0.0480(4) 0.0628(5) 0.0887(10) -0.0033(6) 0.0213(5) -0.0160(4) Cl12 0.0561(6) 0.0377(4) 0.0435(3) -0.0026(3) -0.0058(5) 0.0123(4) Cl13 0.0426(6) 0.0536(6) 0.0601(7) -0.0011(4) -0.0172(5) 0.0017(4) _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 P2 2.2858(4) . ? Pd1 Cl1 2.3502(4) . ? Pd1 P1 2.3738(4) . ? Pd1 Sn1 2.57389(17) . ? Sn1 Cl3 2.3354(5) . ? Sn1 Cl2 2.3578(5) . ? Sn1 Cl4 2.3738(5) . ? P1 C1 1.8101(19) . ? P1 C7 1.8169(18) . ? P1 C13 1.8230(19) . ? P2 C25 1.8158(19) . ? P2 C19 1.8200(17) . ? P2 C31 1.8222(19) . ? C1 C2 1.391(3) . ? C1 C6 1.404(3) . ? C2 C3 1.399(3) . ? C2 H2 0.9500 . ? C3 C4 1.376(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(3) . ? C7 C12 1.397(2) . ? C8 C9 1.386(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.392(3) . ? C13 C18 1.394(3) . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(4) . ? C15 H15 0.9500 . ? C16 C17 1.378(4) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.394(3) . ? C19 C20 1.396(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C22 H22 0.9500 . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.395(2) . ? C25 C30 1.399(2) . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.380(3) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.393(3) . ? C31 C36 1.395(3) . ? C32 C33 1.392(3) . ? C32 H32 0.9500 . ? C33 C34 1.373(4) . ? C33 H33 0.9500 . ? C34 C35 1.374(4) . ? C34 H34 0.9500 . ? C35 C36 1.397(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 Cl7 1.712(6) . ? C37 Cl6 1.717(11) . ? C37 Cl5 1.718(10) . ? C37 H37 1.0000 . ? C37A Cl7A 1.787(15) . ? C37A Cl6A 1.787(15) . ? C37A Cl5A 1.787(15) . ? C37A H37A 1.0000 . ? C38 Cl10 1.761(3) . ? C38 Cl9 1.765(3) . ? C38 Cl8 1.777(4) . ? C38 H38 1.0000 . ? C38A Cl12 1.646(10) . ? C38A Cl11 1.646(11) . ? C38A Cl13 1.646(10) . ? C38A H38A 1.0000 . ? 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 P2 Pd1 Cl1 167.221(17) . . ? P2 Pd1 P1 100.914(16) . . ? Cl1 Pd1 P1 91.851(16) . . ? P2 Pd1 Sn1 92.866(12) . . ? Cl1 Pd1 Sn1 74.546(12) . . ? P1 Pd1 Sn1 164.521(12) . . ? Cl3 Sn1 Cl2 99.91(2) . . ? Cl3 Sn1 Cl4 97.61(2) . . ? Cl2 Sn1 Cl4 94.83(2) . . ? Cl3 Sn1 Pd1 117.129(15) . . ? Cl2 Sn1 Pd1 115.249(17) . . ? Cl4 Sn1 Pd1 126.915(14) . . ? C1 P1 C7 107.26(8) . . ? C1 P1 C13 103.08(9) . . ? C7 P1 C13 104.21(9) . . ? C1 P1 Pd1 120.65(6) . . ? C7 P1 Pd1 109.47(6) . . ? C13 P1 Pd1 110.83(6) . . ? C25 P2 C19 104.32(8) . . ? C25 P2 C31 108.14(9) . . ? C19 P2 C31 102.16(8) . . ? C25 P2 Pd1 112.86(6) . . ? C19 P2 Pd1 120.56(6) . . ? C31 P2 Pd1 107.81(6) . . ? C2 C1 C6 119.30(19) . . ? C2 C1 P1 120.61(15) . . ? C6 C1 P1 120.08(15) . . ? C1 C2 C3 119.8(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.2(2) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C8 C7 C12 119.04(17) . . ? C8 C7 P1 117.58(14) . . ? C12 C7 P1 123.39(14) . . ? C9 C8 C7 120.54(18) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 119.89(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.09(19) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.35(19) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.05(19) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.38(19) . . ? C14 C13 P1 121.54(16) . . ? C18 C13 P1 118.85(16) . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.3(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.2(2) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 119.24(17) . . ? C24 C19 P2 120.62(14) . . ? C20 C19 P2 120.11(14) . . ? C21 C20 C19 119.92(19) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.08(19) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.17(19) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C30 118.76(17) . . ? C26 C25 P2 120.75(14) . . ? C30 C25 P2 120.48(14) . . ? C27 C26 C25 120.30(18) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.1(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 120.33(19) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C32 C31 C36 119.43(19) . . ? C32 C31 P2 118.04(14) . . ? C36 C31 P2 122.50(16) . . ? C33 C32 C31 120.5(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.3(2) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 120.9(2) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C31 C36 C35 119.0(2) . . ? C31 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? Cl7 C37 Cl6 112.2(6) . . ? Cl7 C37 Cl5 110.3(5) . . ? Cl6 C37 Cl5 112.8(9) . . ? Cl7 C37 H37 107.1 . . ? Cl6 C37 H37 107.1 . . ? Cl5 C37 H37 107.1 . . ? Cl7A C37A Cl6A 108.5(13) . . ? Cl7A C37A Cl5A 108.5(13) . . ? Cl6A C37A Cl5A 108.4(13) . . ? Cl7A C37A H37A 110.5 . . ? Cl6A C37A H37A 110.5 . . ? Cl5A C37A H37A 110.5 . . ? Cl10 C38 Cl9 110.33(17) . . ? Cl10 C38 Cl8 109.1(2) . . ? Cl9 C38 Cl8 108.6(2) . . ? Cl10 C38 H38 109.6 . . ? Cl9 C38 H38 109.6 . . ? Cl8 C38 H38 109.6 . . ? Cl12 C38A Cl11 116.1(9) . . ? Cl12 C38A Cl13 116.1(9) . . ? Cl11 C38A Cl13 116.1(9) . . ? Cl12 C38A H38A 101.5 . . ? Cl11 C38A H38A 101.5 . . ? Cl13 C38A H38A 101.5 . . ? 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 P2 Pd1 Sn1 Cl3 -118.88(2) . . . . ? Cl1 Pd1 Sn1 Cl3 58.89(2) . . . . ? P1 Pd1 Sn1 Cl3 88.11(5) . . . . ? P2 Pd1 Sn1 Cl2 124.03(2) . . . . ? Cl1 Pd1 Sn1 Cl2 -58.20(2) . . . . ? P1 Pd1 Sn1 Cl2 -28.98(5) . . . . ? P2 Pd1 Sn1 Cl4 5.95(3) . . . . ? Cl1 Pd1 Sn1 Cl4 -176.28(3) . . . . ? P1 Pd1 Sn1 Cl4 -147.07(5) . . . . ? P2 Pd1 P1 C1 67.00(7) . . . . ? Cl1 Pd1 P1 C1 -112.41(7) . . . . ? Sn1 Pd1 P1 C1 -140.49(7) . . . . ? P2 Pd1 P1 C7 -58.13(6) . . . . ? Cl1 Pd1 P1 C7 122.46(6) . . . . ? Sn1 Pd1 P1 C7 94.38(8) . . . . ? P2 Pd1 P1 C13 -172.53(7) . . . . ? Cl1 Pd1 P1 C13 8.06(7) . . . . ? Sn1 Pd1 P1 C13 -20.02(10) . . . . ? Cl1 Pd1 P2 C25 -81.25(10) . . . . ? P1 Pd1 P2 C25 101.42(7) . . . . ? Sn1 Pd1 P2 C25 -71.49(7) . . . . ? Cl1 Pd1 P2 C19 154.64(10) . . . . ? P1 Pd1 P2 C19 -22.69(7) . . . . ? Sn1 Pd1 P2 C19 164.40(7) . . . . ? Cl1 Pd1 P2 C31 38.11(11) . . . . ? P1 Pd1 P2 C31 -139.22(6) . . . . ? Sn1 Pd1 P2 C31 47.87(6) . . . . ? C7 P1 C1 C2 114.57(16) . . . . ? C13 P1 C1 C2 -135.79(16) . . . . ? Pd1 P1 C1 C2 -11.58(18) . . . . ? C7 P1 C1 C6 -64.13(17) . . . . ? C13 P1 C1 C6 45.51(17) . . . . ? Pd1 P1 C1 C6 169.72(13) . . . . ? C6 C1 C2 C3 1.4(3) . . . . ? P1 C1 C2 C3 -177.28(16) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C1 1.8(3) . . . . ? C2 C1 C6 C5 -2.5(3) . . . . ? P1 C1 C6 C5 176.17(17) . . . . ? C1 P1 C7 C8 -160.24(15) . . . . ? C13 P1 C7 C8 90.90(16) . . . . ? Pd1 P1 C7 C8 -27.70(16) . . . . ? C1 P1 C7 C12 19.53(19) . . . . ? C13 P1 C7 C12 -89.33(18) . . . . ? Pd1 P1 C7 C12 152.07(15) . . . . ? C12 C7 C8 C9 0.5(3) . . . . ? P1 C7 C8 C9 -179.70(16) . . . . ? C7 C8 C9 C10 1.2(3) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 C7 1.2(3) . . . . ? C8 C7 C12 C11 -1.7(3) . . . . ? P1 C7 C12 C11 178.50(16) . . . . ? C1 P1 C13 C14 -135.89(16) . . . . ? C7 P1 C13 C14 -23.98(18) . . . . ? Pd1 P1 C13 C14 93.68(16) . . . . ? C1 P1 C13 C18 49.64(17) . . . . ? C7 P1 C13 C18 161.55(15) . . . . ? Pd1 P1 C13 C18 -80.79(16) . . . . ? C18 C13 C14 C15 0.1(3) . . . . ? P1 C13 C14 C15 -174.38(17) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C13 -0.4(3) . . . . ? C14 C13 C18 C17 0.2(3) . . . . ? P1 C13 C18 C17 174.76(17) . . . . ? C25 P2 C19 C24 131.93(16) . . . . ? C31 P2 C19 C24 19.37(17) . . . . ? Pd1 P2 C19 C24 -100.01(15) . . . . ? C25 P2 C19 C20 -50.04(17) . . . . ? C31 P2 C19 C20 -162.60(16) . . . . ? Pd1 P2 C19 C20 78.02(16) . . . . ? C24 C19 C20 C21 1.8(3) . . . . ? P2 C19 C20 C21 -176.28(17) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 -1.0(4) . . . . ? C21 C22 C23 C24 1.3(4) . . . . ? C22 C23 C24 C19 -0.1(4) . . . . ? C20 C19 C24 C23 -1.5(3) . . . . ? P2 C19 C24 C23 176.59(17) . . . . ? C19 P2 C25 C26 147.28(16) . . . . ? C31 P2 C25 C26 -104.51(17) . . . . ? Pd1 P2 C25 C26 14.66(18) . . . . ? C19 P2 C25 C30 -33.88(19) . . . . ? C31 P2 C25 C30 74.33(18) . . . . ? Pd1 P2 C25 C30 -166.51(15) . . . . ? C30 C25 C26 C27 -0.4(3) . . . . ? P2 C25 C26 C27 178.46(18) . . . . ? C25 C26 C27 C28 -0.2(4) . . . . ? C26 C27 C28 C29 0.5(4) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? C28 C29 C30 C25 -0.4(4) . . . . ? C26 C25 C30 C29 0.7(3) . . . . ? P2 C25 C30 C29 -178.16(19) . . . . ? C25 P2 C31 C32 156.01(15) . . . . ? C19 P2 C31 C32 -94.30(16) . . . . ? Pd1 P2 C31 C32 33.69(16) . . . . ? C25 P2 C31 C36 -25.98(18) . . . . ? C19 P2 C31 C36 83.71(17) . . . . ? Pd1 P2 C31 C36 -148.30(15) . . . . ? C36 C31 C32 C33 0.3(3) . . . . ? P2 C31 C32 C33 178.39(17) . . . . ? C31 C32 C33 C34 0.5(3) . . . . ? C32 C33 C34 C35 -0.4(4) . . . . ? C33 C34 C35 C36 -0.6(4) . . . . ? C32 C31 C36 C35 -1.3(3) . . . . ? P2 C31 C36 C35 -179.23(16) . . . . ? C34 C35 C36 C31 1.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.536 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 963366' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rg12701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H31 N4 P Pd S4 Sn, C4 H8 O' _chemical_formula_sum 'C42 H39 N4 O P Pd S4 Sn' _chemical_formula_weight 1000.07 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' S S 0.1246 0.1234 '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' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9822(3) _cell_length_b 10.3340(4) _cell_length_c 23.1347(8) _cell_angle_alpha 100.226(3) _cell_angle_beta 98.001(3) _cell_angle_gamma 96.521(3) _cell_volume 2071.55(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55062 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.37 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8462 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details XShape _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 'Stoe IPDS-2T' _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 64042 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12068 _reflns_number_gt 10720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; This crystal structure exhibits two kinds of disorders: 1) One of the dangling pyridine-2-thiolato ligands is slightly disordered with site occupancies of 0.75(1) and 0.25(1) (basically same orientation within the molecule, but the Sn-S-C angles are slightly different, i.e., the alternative part of the pyridine moiety is located slightly closer to the Sn-Pd bond). 2) The solvent of crystallization (THF) is disordered with site occupancies of 0.75(1) and 0.25(1) (two almost identical envelope conformations but with opposite direction of the O atom). The alternative positions of the disordered sites were refined with individual free variables (21, -21 for the pyridine moiety, 31, -31 for THF), which yield the same disorder ratio, which confirms that the solvent disorder provokes slight disorder of the main molecule. For the refinement of the solvent disorder only two alternative sites for the oxygen atom were considered. The O-bound C atoms of the alternative parts were refined in the same positions and with the same displacement parameters. exyz c42 c42a exyz c39 c39a eadp c42 c42a eadp c39 c39a eadp o1 o1a The two alternative sites of the disordered dangling pyridinethiolato ligand were refined with same bond lengths of corresponding bonds and same displacement parameters of corresponding atoms. Furthermore, the corresponding 1,4 atomic separations of the alternative pyridine moieties were constrained to the same distances. sadi 0.001 n3 c15 n3a c15a sadi 0.001 c14 c15 c14a c15a sadi 0.001 c13 c14 c13a c14a sadi 0.001 c12 c13 c12a c13a sadi 0.001 c11 c12 c11a c12a sadi 0.001 n3 c11 n3a c11a sadi 0.001 n3 c13 n3a c13a sadi 0.001 c11 c14 c11a C14a sadi 0.001 c12 c15 c12a c15a sadi 0.001 c11 s3 c11a s3a eadp s3 s3a eadp c15 c15a eadp c14 c14a eadp c13 c13a eadp c12 c12a eadp c11 c11a eadp n3 n3a 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^)+(0.0000P)^2^+2.0215P] 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 12068 _refine_ls_number_parameters 513 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.002 _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 Sn1 Sn 0.889226(14) 0.086235(12) 0.358530(5) 0.01737(3) Uani 1 1 d . . . Pd1 Pd 0.804620(15) 0.053915(13) 0.247195(6) 0.01601(3) Uani 1 1 d . A . S1 S 0.72620(6) -0.16873(5) 0.24330(2) 0.02319(9) Uani 1 1 d . . . S2 S 0.90683(6) 0.26994(5) 0.24884(2) 0.02521(10) Uani 1 1 d . . . S4 S 1.12518(6) 0.08283(5) 0.42716(2) 0.02433(10) Uani 1 1 d . A . P1 P 0.68031(5) 0.02797(5) 0.14850(2) 0.01609(8) Uani 1 1 d . . . N1 N 0.81173(18) -0.13455(16) 0.36322(7) 0.0204(3) Uani 1 1 d . A . N2 N 0.97402(18) 0.31793(16) 0.36954(7) 0.0207(3) Uani 1 1 d . A . N4 N 1.1316(2) -0.08129(19) 0.32547(8) 0.0263(4) Uani 1 1 d . A . C1 C 0.7529(2) -0.21899(19) 0.31169(8) 0.0191(3) Uani 1 1 d . A . C2 C 0.7071(2) -0.3547(2) 0.31200(10) 0.0255(4) Uani 1 1 d . . . H2 H 0.6689 -0.4156 0.2757 0.031 Uiso 1 1 calc R A . C3 C 0.7183(3) -0.3981(2) 0.36523(11) 0.0293(4) Uani 1 1 d . A . H3 H 0.6874 -0.4888 0.3659 0.035 Uiso 1 1 calc R . . C4 C 0.7753(2) -0.3076(2) 0.41807(10) 0.0280(4) Uani 1 1 d . . . H4 H 0.7810 -0.3348 0.4554 0.034 Uiso 1 1 calc R A . C5 C 0.8228(2) -0.1787(2) 0.41506(9) 0.0247(4) Uani 1 1 d . A . H5 H 0.8654 -0.1177 0.4509 0.030 Uiso 1 1 calc R . . C6 C 0.9788(2) 0.36484(19) 0.31950(9) 0.0215(4) Uani 1 1 d . A . C7 C 1.0430(2) 0.4983(2) 0.32254(10) 0.0281(4) Uani 1 1 d . . . H7 H 1.0455 0.5323 0.2871 0.034 Uiso 1 1 calc R A . C8 C 1.1015(2) 0.5786(2) 0.37694(11) 0.0295(4) Uani 1 1 d . A . H8 H 1.1453 0.6679 0.3793 0.035 Uiso 1 1 calc R . . C9 C 1.0955(2) 0.5273(2) 0.42868(10) 0.0277(4) Uani 1 1 d . . . H9 H 1.1349 0.5807 0.4668 0.033 Uiso 1 1 calc R A . C10 C 1.0314(2) 0.3975(2) 0.42302(9) 0.0245(4) Uani 1 1 d . A . H10 H 1.0270 0.3621 0.4580 0.029 Uiso 1 1 calc R . . S3 S 0.7723(4) 0.1439(4) 0.45056(18) 0.0268(3) Uani 0.753(10) 1 d PD A 1 N3 N 0.6106(5) 0.2130(5) 0.3591(2) 0.0297(8) Uani 0.753(10) 1 d PD A 1 C11 C 0.6296(5) 0.2256(6) 0.4184(2) 0.0244(7) Uani 0.753(10) 1 d PD A 1 C12 C 0.5411(5) 0.2971(4) 0.4540(2) 0.0356(9) Uani 0.753(10) 1 d PD A 1 H12 H 0.5584 0.3050 0.4960 0.043 Uiso 0.753(10) 1 calc PR A 1 C13 C 0.4280(4) 0.3557(4) 0.4265(3) 0.0469(12) Uani 0.753(10) 1 d PD A 1 H13 H 0.3664 0.4054 0.4494 0.056 Uiso 0.753(10) 1 calc PR A 1 C14 C 0.4050(4) 0.3418(5) 0.3651(3) 0.0480(14) Uani 0.753(10) 1 d PD A 1 H14 H 0.3264 0.3800 0.3453 0.058 Uiso 0.753(10) 1 calc PR A 1 C15 C 0.4991(5) 0.2709(5) 0.3334(2) 0.0403(10) Uani 0.753(10) 1 d PD A 1 H15 H 0.4843 0.2627 0.2914 0.048 Uiso 0.753(10) 1 calc PR A 1 S3A S 0.7596(14) 0.1552(14) 0.4443(6) 0.0268(3) Uani 0.247(10) 1 d PD A 2 N3A N 0.6267(17) 0.2182(19) 0.3454(6) 0.0297(8) Uani 0.247(10) 1 d PD A 2 C11A C 0.6193(18) 0.224(2) 0.4032(6) 0.0244(7) Uani 0.247(10) 1 d PD A 2 C12A C 0.5119(15) 0.2868(15) 0.4319(6) 0.0356(9) Uani 0.247(10) 1 d PD A 2 H12A H 0.5131 0.2932 0.4734 0.043 Uiso 0.247(10) 1 calc PR A 2 C13A C 0.4041(16) 0.3389(18) 0.3979(8) 0.0469(12) Uani 0.247(10) 1 d PD A 2 H13A H 0.3296 0.3822 0.4160 0.056 Uiso 0.247(10) 1 calc PR A 2 C14A C 0.4046(14) 0.3279(16) 0.3374(7) 0.0480(14) Uani 0.247(10) 1 d PD A 2 H14A H 0.3280 0.3589 0.3130 0.058 Uiso 0.247(10) 1 calc PR A 2 C15A C 0.5199(17) 0.2705(18) 0.3137(6) 0.0403(10) Uani 0.247(10) 1 d PD A 2 H15A H 0.5241 0.2677 0.2727 0.048 Uiso 0.247(10) 1 calc PR A 2 C16 C 1.2090(2) -0.03052(19) 0.38011(9) 0.0216(4) Uani 1 1 d . . . C17 C 1.3511(2) -0.0639(2) 0.40075(11) 0.0296(4) Uani 1 1 d . A . H17 H 1.4025 -0.0268 0.4399 0.036 Uiso 1 1 calc R . . C18 C 1.4142(3) -0.1524(3) 0.36253(13) 0.0394(6) Uani 1 1 d . . . H18 H 1.5104 -0.1769 0.3752 0.047 Uiso 1 1 calc R A . C19 C 1.3362(3) -0.2051(3) 0.30569(12) 0.0401(6) Uani 1 1 d . A . H19 H 1.3783 -0.2653 0.2786 0.048 Uiso 1 1 calc R . . C20 C 1.1953(3) -0.1681(2) 0.28921(10) 0.0334(5) Uani 1 1 d . . . H20 H 1.1409 -0.2056 0.2505 0.040 Uiso 1 1 calc R A . C21 C 0.4798(2) 0.04736(18) 0.14661(8) 0.0183(3) Uani 1 1 d . A . C22 C 0.4109(2) 0.0327(2) 0.19609(9) 0.0247(4) Uani 1 1 d . . . H22 H 0.4664 0.0076 0.2294 0.030 Uiso 1 1 calc R A . C23 C 0.2601(2) 0.0548(2) 0.19658(10) 0.0296(4) Uani 1 1 d . A . H23 H 0.2138 0.0453 0.2304 0.036 Uiso 1 1 calc R . . C24 C 0.1783(2) 0.0907(2) 0.14797(10) 0.0284(4) Uani 1 1 d . . . H24 H 0.0766 0.1072 0.1488 0.034 Uiso 1 1 calc R A . C25 C 0.2450(2) 0.1024(2) 0.09798(10) 0.0279(4) Uani 1 1 d . A . H25 H 0.1880 0.1246 0.0643 0.033 Uiso 1 1 calc R . . C26 C 0.3951(2) 0.0817(2) 0.09741(9) 0.0232(4) Uani 1 1 d . . . H26 H 0.4406 0.0909 0.0634 0.028 Uiso 1 1 calc R A . C27 C 0.7445(2) 0.14647(19) 0.10375(8) 0.0190(3) Uani 1 1 d . A . C28 C 0.7258(2) 0.2803(2) 0.12060(9) 0.0238(4) Uani 1 1 d . . . H28 H 0.6762 0.3070 0.1535 0.029 Uiso 1 1 calc R A . C29 C 0.7797(3) 0.3736(2) 0.08918(11) 0.0298(4) Uani 1 1 d . A . H29 H 0.7670 0.4641 0.1009 0.036 Uiso 1 1 calc R . . C30 C 0.8520(3) 0.3355(2) 0.04068(11) 0.0323(5) Uani 1 1 d . . . H30 H 0.8900 0.3998 0.0197 0.039 Uiso 1 1 calc R A . C31 C 0.8684(2) 0.2028(2) 0.02312(10) 0.0288(4) Uani 1 1 d . A . H31 H 0.9156 0.1762 -0.0105 0.035 Uiso 1 1 calc R . . C32 C 0.8159(2) 0.1086(2) 0.05467(9) 0.0231(4) Uani 1 1 d . . . H32 H 0.8286 0.0182 0.0427 0.028 Uiso 1 1 calc R A . C33 C 0.6885(2) -0.13020(18) 0.10013(8) 0.0179(3) Uani 1 1 d . A . C34 C 0.5736(2) -0.1897(2) 0.05286(9) 0.0233(4) Uani 1 1 d . . . H34 H 0.4805 -0.1544 0.0480 0.028 Uiso 1 1 calc R A . C35 C 0.5952(3) -0.3011(2) 0.01273(10) 0.0308(5) Uani 1 1 d . A . H35 H 0.5160 -0.3423 -0.0191 0.037 Uiso 1 1 calc R . . C36 C 0.7317(3) -0.3519(2) 0.01904(10) 0.0299(4) Uani 1 1 d . . . H36 H 0.7473 -0.4254 -0.0094 0.036 Uiso 1 1 calc R A . C37 C 0.8456(2) -0.2956(2) 0.06682(10) 0.0253(4) Uani 1 1 d . A . H37 H 0.9376 -0.3324 0.0719 0.030 Uiso 1 1 calc R . . C38 C 0.8242(2) -0.18465(19) 0.10735(9) 0.0207(3) Uani 1 1 d . . . H38 H 0.9021 -0.1459 0.1400 0.025 Uiso 1 1 calc R A . O1 O 0.1651(3) 0.5565(3) 0.11134(19) 0.0500(8) Uani 0.748(6) 1 d P B 1 C39 C 0.3052(4) 0.6433(3) 0.12731(16) 0.0592(8) Uani 0.748(6) 1 d P B 1 H39A H 0.3009 0.7147 0.1615 0.071 Uiso 0.748(6) 1 calc PR B 1 H39B H 0.3282 0.6845 0.0935 0.071 Uiso 0.748(6) 1 calc PR B 1 C42 C 0.1776(4) 0.4607(4) 0.15154(18) 0.0622(9) Uani 0.748(6) 1 d P B 1 H42A H 0.1345 0.3701 0.1295 0.075 Uiso 0.748(6) 1 calc PR B 1 H42B H 0.1202 0.4842 0.1845 0.075 Uiso 0.748(6) 1 calc PR B 1 O1A O 0.1694(10) 0.5866(10) 0.1476(6) 0.0500(8) Uani 0.252(6) 1 d P B 2 C39A C 0.3052(4) 0.6433(3) 0.12731(16) 0.0592(8) Uani 0.252(6) 1 d P B 2 H39C H 0.3371 0.7372 0.1476 0.071 Uiso 0.252(6) 1 calc PR B 2 H39D H 0.2861 0.6389 0.0838 0.071 Uiso 0.252(6) 1 calc PR B 2 C42A C 0.1776(4) 0.4607(4) 0.15154(18) 0.0622(9) Uani 0.252(6) 1 d P B 2 H42C H 0.1490 0.4011 0.1120 0.075 Uiso 0.252(6) 1 calc PR B 2 H42D H 0.1114 0.4311 0.1789 0.075 Uiso 0.252(6) 1 calc PR B 2 C40 C 0.4234(4) 0.5592(4) 0.14356(16) 0.0642(10) Uani 1 1 d . . . H40A H 0.5136 0.6138 0.1698 0.077 Uiso 1 1 calc R B 1 H40B H 0.4555 0.5104 0.1076 0.077 Uiso 1 1 calc R B 1 C41 C 0.3427(4) 0.4648(3) 0.1759(2) 0.0746(12) Uani 1 1 d . B . H41A H 0.3742 0.3756 0.1673 0.090 Uiso 1 1 calc R C 1 H41B H 0.3634 0.4987 0.2195 0.090 Uiso 1 1 calc R C 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 Sn1 0.01866(6) 0.01881(6) 0.01273(6) 0.00079(4) -0.00055(4) 0.00214(4) Pd1 0.01705(6) 0.01654(6) 0.01291(6) 0.00224(5) -0.00072(4) 0.00090(5) S1 0.0319(2) 0.0189(2) 0.0155(2) 0.00323(16) -0.00307(17) -0.00177(18) S2 0.0333(3) 0.0210(2) 0.0183(2) 0.00359(17) 0.00069(18) -0.00433(19) S4 0.0224(2) 0.0277(2) 0.0196(2) -0.00101(18) -0.00337(17) 0.00738(19) P1 0.01741(19) 0.0169(2) 0.0135(2) 0.00335(16) 0.00086(15) 0.00195(16) N1 0.0226(7) 0.0218(8) 0.0162(7) 0.0038(6) 0.0015(6) 0.0019(6) N2 0.0194(7) 0.0196(7) 0.0199(8) -0.0007(6) -0.0012(6) 0.0025(6) N4 0.0291(9) 0.0305(9) 0.0201(8) 0.0058(7) 0.0041(7) 0.0066(7) C1 0.0172(8) 0.0215(9) 0.0190(8) 0.0052(7) 0.0020(6) 0.0033(7) C2 0.0273(9) 0.0207(9) 0.0267(10) 0.0054(8) -0.0013(8) 0.0013(8) C3 0.0311(10) 0.0241(10) 0.0349(12) 0.0132(9) 0.0036(9) 0.0033(8) C4 0.0280(10) 0.0355(11) 0.0242(10) 0.0150(9) 0.0034(8) 0.0065(9) C5 0.0272(9) 0.0301(10) 0.0169(9) 0.0068(8) 0.0012(7) 0.0041(8) C6 0.0177(8) 0.0208(9) 0.0241(9) 0.0014(7) 0.0020(7) 0.0013(7) C7 0.0293(10) 0.0221(9) 0.0310(11) 0.0017(8) 0.0072(8) -0.0015(8) C8 0.0267(10) 0.0199(9) 0.0381(12) -0.0029(8) 0.0073(9) -0.0022(8) C9 0.0222(9) 0.0244(10) 0.0299(11) -0.0081(8) 0.0004(8) 0.0020(8) C10 0.0230(9) 0.0250(9) 0.0212(9) -0.0037(7) -0.0012(7) 0.0042(8) S3 0.0313(7) 0.0270(8) 0.0256(9) 0.0050(5) 0.0121(6) 0.0101(4) N3 0.0276(14) 0.0260(11) 0.032(2) -0.0011(16) 0.0028(12) 0.0020(11) C11 0.0205(11) 0.0206(10) 0.030(2) -0.001(2) 0.0064(16) -0.0001(9) C12 0.0265(17) 0.0380(16) 0.041(3) -0.0023(19) 0.0122(17) 0.0056(14) C13 0.0244(16) 0.049(2) 0.066(4) 0.000(2) 0.012(2) 0.0120(15) C14 0.0245(13) 0.046(2) 0.067(5) 0.004(3) -0.007(2) 0.0090(13) C15 0.0371(18) 0.0361(14) 0.040(3) 0.002(2) -0.0087(17) 0.0026(14) S3A 0.0313(7) 0.0270(8) 0.0256(9) 0.0050(5) 0.0121(6) 0.0101(4) N3A 0.0276(14) 0.0260(11) 0.032(2) -0.0011(16) 0.0028(12) 0.0020(11) C11A 0.0205(11) 0.0206(10) 0.030(2) -0.001(2) 0.0064(16) -0.0001(9) C12A 0.0265(17) 0.0380(16) 0.041(3) -0.0023(19) 0.0122(17) 0.0056(14) C13A 0.0244(16) 0.049(2) 0.066(4) 0.000(2) 0.012(2) 0.0120(15) C14A 0.0245(13) 0.046(2) 0.067(5) 0.004(3) -0.007(2) 0.0090(13) C15A 0.0371(18) 0.0361(14) 0.040(3) 0.002(2) -0.0087(17) 0.0026(14) C16 0.0209(8) 0.0204(9) 0.0242(9) 0.0068(7) 0.0047(7) 0.0015(7) C17 0.0185(9) 0.0321(11) 0.0368(12) 0.0057(9) 0.0020(8) 0.0023(8) C18 0.0221(10) 0.0430(14) 0.0573(16) 0.0112(12) 0.0132(10) 0.0118(10) C19 0.0417(13) 0.0397(13) 0.0442(14) 0.0044(11) 0.0229(11) 0.0141(11) C20 0.0437(13) 0.0349(12) 0.0234(10) 0.0035(9) 0.0115(9) 0.0089(10) C21 0.0177(8) 0.0186(8) 0.0173(8) 0.0027(6) 0.0004(6) 0.0016(6) C22 0.0232(9) 0.0304(10) 0.0224(9) 0.0089(8) 0.0051(7) 0.0040(8) C23 0.0248(10) 0.0354(11) 0.0311(11) 0.0098(9) 0.0097(8) 0.0034(9) C24 0.0195(9) 0.0291(10) 0.0351(11) 0.0034(9) 0.0033(8) 0.0037(8) C25 0.0234(9) 0.0328(11) 0.0258(10) 0.0043(8) -0.0028(8) 0.0074(8) C26 0.0227(9) 0.0284(10) 0.0183(9) 0.0042(7) 0.0005(7) 0.0072(8) C27 0.0173(8) 0.0216(9) 0.0187(8) 0.0080(7) 0.0007(6) 0.0022(7) C28 0.0253(9) 0.0222(9) 0.0243(9) 0.0069(8) 0.0026(7) 0.0032(7) C29 0.0333(11) 0.0224(10) 0.0353(12) 0.0123(9) 0.0029(9) 0.0028(8) C30 0.0310(11) 0.0316(11) 0.0382(12) 0.0187(10) 0.0074(9) 0.0007(9) C31 0.0269(10) 0.0343(11) 0.0287(11) 0.0137(9) 0.0086(8) 0.0022(9) C32 0.0237(9) 0.0240(9) 0.0224(9) 0.0076(7) 0.0036(7) 0.0023(7) C33 0.0211(8) 0.0176(8) 0.0152(8) 0.0046(6) 0.0027(6) 0.0016(7) C34 0.0259(9) 0.0208(9) 0.0207(9) 0.0027(7) -0.0029(7) 0.0033(7) C35 0.0403(12) 0.0243(10) 0.0224(10) -0.0011(8) -0.0059(9) 0.0040(9) C36 0.0457(13) 0.0221(10) 0.0223(10) 0.0026(8) 0.0054(9) 0.0097(9) C37 0.0308(10) 0.0215(9) 0.0272(10) 0.0074(8) 0.0097(8) 0.0082(8) C38 0.0211(8) 0.0200(9) 0.0212(9) 0.0054(7) 0.0026(7) 0.0023(7) O1 0.0406(12) 0.0473(16) 0.065(2) 0.0199(17) 0.0066(16) 0.0077(11) C39 0.069(2) 0.0506(18) 0.0478(18) 0.0000(14) 0.0096(15) -0.0175(16) C42 0.0555(19) 0.063(2) 0.071(2) 0.0270(18) 0.0105(17) -0.0031(16) O1A 0.0406(12) 0.0473(16) 0.065(2) 0.0199(17) 0.0066(16) 0.0077(11) C39A 0.069(2) 0.0506(18) 0.0478(18) 0.0000(14) 0.0096(15) -0.0175(16) C42A 0.0555(19) 0.063(2) 0.071(2) 0.0270(18) 0.0105(17) -0.0031(16) C40 0.0401(15) 0.077(2) 0.054(2) -0.0228(17) -0.0070(14) -0.0055(16) C41 0.078(2) 0.0362(16) 0.089(3) 0.0006(17) -0.033(2) -0.0003(16) _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 Sn1 N1 2.3345(16) . ? Sn1 N2 2.3860(17) . ? Sn1 S4 2.4726(5) . ? Sn1 S3A 2.475(14) . ? Sn1 S3 2.511(4) . ? Sn1 Pd1 2.5328(2) . ? Pd1 S2 2.3071(5) . ? Pd1 S1 2.3105(5) . ? Pd1 P1 2.3531(5) . ? S1 C1 1.7451(19) . ? S2 C6 1.745(2) . ? S4 C16 1.760(2) . ? P1 C33 1.8249(19) . ? P1 C21 1.8300(18) . ? P1 C27 1.8330(18) . ? N1 C1 1.346(2) . ? N1 C5 1.352(2) . ? N2 C6 1.336(3) . ? N2 C10 1.356(3) . ? N4 C16 1.339(3) . ? N4 C20 1.348(3) . ? C1 C2 1.418(3) . ? C2 C3 1.378(3) . ? C2 H2 0.9500 . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.368(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.419(3) . ? C7 C8 1.376(3) . ? C7 H7 0.9500 . ? C8 C9 1.398(3) . ? C8 H8 0.9500 . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? S3 C11 1.765(3) . ? N3 C11 1.339(4) . ? N3 C15 1.346(3) . ? C11 C12 1.398(3) . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.382(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? S3A C11A 1.765(3) . ? N3A C11A 1.339(4) . ? N3A C15A 1.346(4) . ? C11A C12A 1.398(3) . ? C12A C13A 1.379(5) . ? C12A H12A 0.9500 . ? C13A C14A 1.385(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.382(6) . ? C14A H14A 0.9500 . ? C15A H15A 0.9500 . ? C16 C17 1.402(3) . ? C17 C18 1.382(3) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.398(3) . ? C21 C26 1.402(3) . ? C22 C23 1.400(3) . ? C22 H22 0.9500 . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.392(3) . ? C24 H24 0.9500 . ? C25 C26 1.390(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.398(3) . ? C27 C28 1.404(3) . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.393(3) . ? C29 H29 0.9500 . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 C32 1.396(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 C38 1.401(3) . ? C34 C35 1.394(3) . ? C34 H34 0.9500 . ? C35 C36 1.387(3) . ? C35 H35 0.9500 . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.396(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? O1 C39 1.421(4) . ? O1 C42 1.477(5) . ? C39 C40 1.497(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C42 C41 1.504(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C40 C41 1.513(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 Sn1 N2 171.46(6) . . ? N1 Sn1 S4 89.11(4) . . ? N2 Sn1 S4 85.68(4) . . ? N1 Sn1 S3A 88.5(3) . . ? N2 Sn1 S3A 84.8(3) . . ? S4 Sn1 S3A 90.3(2) . . ? N1 Sn1 S3 85.58(11) . . ? N2 Sn1 S3 87.31(11) . . ? S4 Sn1 S3 85.98(7) . . ? S3A Sn1 S3 5.2(2) . . ? N1 Sn1 Pd1 94.72(4) . . ? N2 Sn1 Pd1 93.69(4) . . ? S4 Sn1 Pd1 137.333(13) . . ? S3A Sn1 Pd1 132.2(2) . . ? S3 Sn1 Pd1 136.66(7) . . ? S2 Pd1 S1 174.01(2) . . ? S2 Pd1 P1 92.059(18) . . ? S1 Pd1 P1 88.723(17) . . ? S2 Pd1 Sn1 90.415(14) . . ? S1 Pd1 Sn1 89.914(13) . . ? P1 Pd1 Sn1 169.171(13) . . ? C1 S1 Pd1 114.95(7) . . ? C6 S2 Pd1 115.17(7) . . ? C16 S4 Sn1 98.87(7) . . ? C33 P1 C21 107.43(9) . . ? C33 P1 C27 101.39(8) . . ? C21 P1 C27 102.41(8) . . ? C33 P1 Pd1 115.36(6) . . ? C21 P1 Pd1 110.78(6) . . ? C27 P1 Pd1 118.13(6) . . ? C1 N1 C5 119.90(17) . . ? C1 N1 Sn1 117.47(12) . . ? C5 N1 Sn1 122.62(14) . . ? C6 N2 C10 120.00(17) . . ? C6 N2 Sn1 116.78(13) . . ? C10 N2 Sn1 122.81(14) . . ? C16 N4 C20 117.65(19) . . ? N1 C1 C2 119.65(17) . . ? N1 C1 S1 122.89(14) . . ? C2 C1 S1 117.45(15) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.31(19) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.55(19) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N2 C6 C7 119.84(19) . . ? N2 C6 S2 123.13(15) . . ? C7 C6 S2 117.03(16) . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.2(2) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 118.3(2) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 122.7(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C11 S3 Sn1 96.27(17) . . ? C11 N3 C15 117.5(3) . . ? N3 C11 C12 123.0(3) . . ? N3 C11 S3 116.5(3) . . ? C12 C11 S3 120.5(3) . . ? C13 C12 C11 118.3(4) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 C14 119.5(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 118.4(3) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N3 C15 C14 123.3(4) . . ? N3 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C11A S3A Sn1 94.6(6) . . ? C11A N3A C15A 117.1(9) . . ? N3A C11A C12A 123.3(9) . . ? N3A C11A S3A 116.6(9) . . ? C12A C11A S3A 120.0(10) . . ? C13A C12A C11A 117.9(9) . . ? C13A C12A H12A 121.1 . . ? C11A C12A H12A 121.1 . . ? C12A C13A C14A 119.9(9) . . ? C12A C13A H13A 120.1 . . ? C14A C13A H13A 120.1 . . ? C15A C14A C13A 118.0(9) . . ? C15A C14A H14A 121.0 . . ? C13A C14A H14A 121.0 . . ? N3A C15A C14A 123.6(10) . . ? N3A C15A H15A 118.2 . . ? C14A C15A H15A 118.2 . . ? N4 C16 C17 123.0(2) . . ? N4 C16 S4 117.36(15) . . ? C17 C16 S4 119.64(17) . . ? C18 C17 C16 118.2(2) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C19 119.6(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 118.5(2) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 123.1(2) . . ? N4 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? C22 C21 C26 119.12(17) . . ? C22 C21 P1 119.47(14) . . ? C26 C21 P1 121.36(14) . . ? C21 C22 C23 120.03(19) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.26(19) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.02(19) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.01(19) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.53(18) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C27 C28 119.13(17) . . ? C32 C27 P1 122.06(15) . . ? C28 C27 P1 118.78(14) . . ? C29 C28 C27 120.13(19) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 119.68(19) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 120.31(19) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 119.34(18) . . ? C34 C33 P1 122.79(14) . . ? C38 C33 P1 117.46(14) . . ? C33 C34 C35 120.05(19) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 120.2(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 119.70(19) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 120.37(19) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C39 O1 C42 104.5(3) . . ? O1 C39 C40 106.0(3) . . ? O1 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? O1 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? O1 C42 C41 108.5(3) . . ? O1 C42 H42A 110.0 . . ? C41 C42 H42A 110.0 . . ? O1 C42 H42B 110.0 . . ? C41 C42 H42B 110.0 . . ? H42A C42 H42B 108.4 . . ? C39 C40 C41 103.1(3) . . ? C39 C40 H40A 111.1 . . ? C41 C40 H40A 111.1 . . ? C39 C40 H40B 111.1 . . ? C41 C40 H40B 111.1 . . ? H40A C40 H40B 109.1 . . ? C42 C41 C40 103.5(3) . . ? C42 C41 H41A 111.1 . . ? C40 C41 H41A 111.1 . . ? C42 C41 H41B 111.1 . . ? C40 C41 H41B 111.1 . . ? H41A C41 H41B 109.0 . . ? 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 Sn1 Pd1 S2 -175.18(4) . . . . ? N2 Sn1 Pd1 S2 6.28(4) . . . . ? S4 Sn1 Pd1 S2 -81.35(2) . . . . ? S3A Sn1 Pd1 S2 92.6(5) . . . . ? S3 Sn1 Pd1 S2 96.26(14) . . . . ? N1 Sn1 Pd1 S1 -1.16(4) . . . . ? N2 Sn1 Pd1 S1 -179.70(4) . . . . ? S4 Sn1 Pd1 S1 92.67(2) . . . . ? S3A Sn1 Pd1 S1 -93.4(5) . . . . ? S3 Sn1 Pd1 S1 -89.72(14) . . . . ? N1 Sn1 Pd1 P1 81.58(8) . . . . ? N2 Sn1 Pd1 P1 -96.97(8) . . . . ? S4 Sn1 Pd1 P1 175.40(7) . . . . ? S3A Sn1 Pd1 P1 -10.7(5) . . . . ? S3 Sn1 Pd1 P1 -6.99(16) . . . . ? P1 Pd1 S1 C1 -168.82(7) . . . . ? Sn1 Pd1 S1 C1 0.44(7) . . . . ? P1 Pd1 S2 C6 164.35(7) . . . . ? Sn1 Pd1 S2 C6 -5.11(7) . . . . ? N1 Sn1 S4 C16 66.97(8) . . . . ? N2 Sn1 S4 C16 -119.80(8) . . . . ? S3A Sn1 S4 C16 155.5(3) . . . . ? S3 Sn1 S4 C16 152.61(12) . . . . ? Pd1 Sn1 S4 C16 -29.04(7) . . . . ? S2 Pd1 P1 C33 137.66(7) . . . . ? S1 Pd1 P1 C33 -36.40(7) . . . . ? Sn1 Pd1 P1 C33 -119.25(9) . . . . ? S2 Pd1 P1 C21 -100.03(7) . . . . ? S1 Pd1 P1 C21 85.91(7) . . . . ? Sn1 Pd1 P1 C21 3.06(11) . . . . ? S2 Pd1 P1 C27 17.58(7) . . . . ? S1 Pd1 P1 C27 -156.48(7) . . . . ? Sn1 Pd1 P1 C27 120.67(9) . . . . ? S4 Sn1 N1 C1 -135.07(13) . . . . ? S3A Sn1 N1 C1 134.6(3) . . . . ? S3 Sn1 N1 C1 138.89(15) . . . . ? Pd1 Sn1 N1 C1 2.37(13) . . . . ? S4 Sn1 N1 C5 45.49(15) . . . . ? S3A Sn1 N1 C5 -44.9(3) . . . . ? S3 Sn1 N1 C5 -40.55(16) . . . . ? Pd1 Sn1 N1 C5 -177.07(15) . . . . ? S4 Sn1 N2 C6 127.83(13) . . . . ? S3A Sn1 N2 C6 -141.4(3) . . . . ? S3 Sn1 N2 C6 -146.00(15) . . . . ? Pd1 Sn1 N2 C6 -9.40(13) . . . . ? S4 Sn1 N2 C10 -44.85(14) . . . . ? S3A Sn1 N2 C10 45.9(3) . . . . ? S3 Sn1 N2 C10 41.32(16) . . . . ? Pd1 Sn1 N2 C10 177.92(14) . . . . ? C5 N1 C1 C2 -1.9(3) . . . . ? Sn1 N1 C1 C2 178.66(14) . . . . ? C5 N1 C1 S1 176.89(15) . . . . ? Sn1 N1 C1 S1 -2.6(2) . . . . ? Pd1 S1 C1 N1 1.33(18) . . . . ? Pd1 S1 C1 C2 -179.87(13) . . . . ? N1 C1 C2 C3 2.3(3) . . . . ? S1 C1 C2 C3 -176.56(16) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -2.0(3) . . . . ? C1 N1 C5 C4 -0.5(3) . . . . ? Sn1 N1 C5 C4 178.93(16) . . . . ? C3 C4 C5 N1 2.5(3) . . . . ? C10 N2 C6 C7 -0.5(3) . . . . ? Sn1 N2 C6 C7 -173.39(14) . . . . ? C10 N2 C6 S2 -179.61(15) . . . . ? Sn1 N2 C6 S2 7.5(2) . . . . ? Pd1 S2 C6 N2 -0.94(19) . . . . ? Pd1 S2 C6 C7 179.92(13) . . . . ? N2 C6 C7 C8 0.7(3) . . . . ? S2 C6 C7 C8 179.86(17) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C6 N2 C10 C9 0.1(3) . . . . ? Sn1 N2 C10 C9 172.60(15) . . . . ? C8 C9 C10 N2 0.0(3) . . . . ? N1 Sn1 S3 C11 -115.9(3) . . . . ? N2 Sn1 S3 C11 68.8(3) . . . . ? S4 Sn1 S3 C11 154.6(3) . . . . ? S3A Sn1 S3 C11 8(5) . . . . ? Pd1 Sn1 S3 C11 -23.7(3) . . . . ? C15 N3 C11 C12 -1.0(10) . . . . ? C15 N3 C11 S3 177.9(5) . . . . ? Sn1 S3 C11 N3 10.6(6) . . . . ? Sn1 S3 C11 C12 -170.4(5) . . . . ? N3 C11 C12 C13 0.8(9) . . . . ? S3 C11 C12 C13 -178.1(4) . . . . ? C11 C12 C13 C14 0.4(7) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C11 N3 C15 C14 0.1(9) . . . . ? C13 C14 C15 N3 1.1(8) . . . . ? N1 Sn1 S3A C11A -113.0(10) . . . . ? N2 Sn1 S3A C11A 72.2(10) . . . . ? S4 Sn1 S3A C11A 157.9(10) . . . . ? S3 Sn1 S3A C11A -169(6) . . . . ? Pd1 Sn1 S3A C11A -18.0(12) . . . . ? C15A N3A C11A C12A -3(4) . . . . ? C15A N3A C11A S3A 179.9(17) . . . . ? Sn1 S3A C11A N3A 0(2) . . . . ? Sn1 S3A C11A C12A -177.3(17) . . . . ? N3A C11A C12A C13A 3(3) . . . . ? S3A C11A C12A C13A -179.7(16) . . . . ? C11A C12A C13A C14A 0(3) . . . . ? C12A C13A C14A C15A -3(3) . . . . ? C11A N3A C15A C14A -1(3) . . . . ? C13A C14A C15A N3A 4(3) . . . . ? C20 N4 C16 C17 -0.2(3) . . . . ? C20 N4 C16 S4 179.93(16) . . . . ? Sn1 S4 C16 N4 -0.55(16) . . . . ? Sn1 S4 C16 C17 179.58(15) . . . . ? N4 C16 C17 C18 0.6(3) . . . . ? S4 C16 C17 C18 -179.49(18) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? C16 N4 C20 C19 -0.8(3) . . . . ? C18 C19 C20 N4 1.2(4) . . . . ? C33 P1 C21 C22 107.08(17) . . . . ? C27 P1 C21 C22 -146.60(16) . . . . ? Pd1 P1 C21 C22 -19.74(18) . . . . ? C33 P1 C21 C26 -75.41(18) . . . . ? C27 P1 C21 C26 30.90(18) . . . . ? Pd1 P1 C21 C26 157.76(15) . . . . ? C26 C21 C22 C23 -1.3(3) . . . . ? P1 C21 C22 C23 176.28(17) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 1.1(3) . . . . ? C23 C24 C25 C26 -1.7(3) . . . . ? C24 C25 C26 C21 0.8(3) . . . . ? C22 C21 C26 C25 0.7(3) . . . . ? P1 C21 C26 C25 -176.80(16) . . . . ? C33 P1 C27 C32 -14.55(18) . . . . ? C21 P1 C27 C32 -125.48(16) . . . . ? Pd1 P1 C27 C32 112.55(16) . . . . ? C33 P1 C27 C28 167.58(15) . . . . ? C21 P1 C27 C28 56.65(17) . . . . ? Pd1 P1 C27 C28 -65.33(16) . . . . ? C32 C27 C28 C29 -0.9(3) . . . . ? P1 C27 C28 C29 177.03(16) . . . . ? C27 C28 C29 C30 0.3(3) . . . . ? C28 C29 C30 C31 0.9(4) . . . . ? C29 C30 C31 C32 -1.5(3) . . . . ? C30 C31 C32 C27 0.8(3) . . . . ? C28 C27 C32 C31 0.4(3) . . . . ? P1 C27 C32 C31 -177.50(16) . . . . ? C21 P1 C33 C34 25.34(18) . . . . ? C27 P1 C33 C34 -81.69(17) . . . . ? Pd1 P1 C33 C34 149.42(14) . . . . ? C21 P1 C33 C38 -162.05(14) . . . . ? C27 P1 C33 C38 90.91(15) . . . . ? Pd1 P1 C33 C38 -37.97(16) . . . . ? C38 C33 C34 C35 -1.1(3) . . . . ? P1 C33 C34 C35 171.41(16) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C34 C35 C36 C37 2.7(3) . . . . ? C35 C36 C37 C38 -2.3(3) . . . . ? C36 C37 C38 C33 0.2(3) . . . . ? C34 C33 C38 C37 1.5(3) . . . . ? P1 C33 C38 C37 -171.37(14) . . . . ? C42 O1 C39 C40 35.3(4) . . . . ? C39 O1 C42 C41 -18.9(4) . . . . ? O1 C39 C40 C41 -38.2(4) . . . . ? O1 C42 C41 C40 -4.5(4) . . . . ? C39 C40 C41 C42 24.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.539 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 963367' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ew12401 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H33 N2 P Pd S2 Sn' _chemical_formula_sum 'C40 H33 N2 P Pd S2 Sn' _chemical_formula_weight 861.86 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' S S 0.1246 0.1234 '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' Sn Sn -0.6537 1.4246 '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 16.3741(5) _cell_length_b 9.4293(2) _cell_length_c 23.7358(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.305(2) _cell_angle_gamma 90.00 _cell_volume 3551.09(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54887 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 32.32 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7565 _exptl_absorpt_correction_T_max 0.8507 _exptl_absorpt_process_details xshape _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 'STOE IPDS 2' _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 47294 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 32.00 _reflns_number_total 12310 _reflns_number_gt 10715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _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^)+(0.0294P)^2^+3.3569P] 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 12310 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _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 0.257015(8) 0.907037(13) 0.374357(6) 0.01300(3) Uani 1 1 d . . . Sn1 Sn 0.259986(7) 0.798600(12) 0.472662(5) 0.01363(3) Uani 1 1 d . . . S1 S 0.38677(3) 0.81037(6) 0.37742(2) 0.02256(9) Uani 1 1 d . . . S2 S 0.12871(3) 1.00979(5) 0.37408(2) 0.01872(8) Uani 1 1 d . . . P1 P 0.24554(3) 1.00923(5) 0.28110(2) 0.01441(8) Uani 1 1 d . . . N1 N 0.40501(10) 0.75204(18) 0.49155(7) 0.0190(3) Uani 1 1 d . . . N2 N 0.11032(10) 0.81758(17) 0.45402(7) 0.0188(3) Uani 1 1 d . . . C1 C 0.44024(11) 0.7514(2) 0.44622(9) 0.0177(3) Uani 1 1 d . . . C2 C 0.52358(12) 0.7022(2) 0.45342(10) 0.0250(4) Uani 1 1 d . . . H2 H 0.5489 0.7020 0.4215 0.030 Uiso 1 1 calc R . . C3 C 0.56818(13) 0.6543(3) 0.50730(11) 0.0279(4) Uani 1 1 d . . . H3 H 0.6243 0.6206 0.5126 0.033 Uiso 1 1 calc R . . C4 C 0.53046(13) 0.6559(3) 0.55332(10) 0.0273(4) Uani 1 1 d . . . H4 H 0.5601 0.6237 0.5907 0.033 Uiso 1 1 calc R . . C5 C 0.44919(13) 0.7050(2) 0.54392(9) 0.0243(4) Uani 1 1 d . . . H5 H 0.4231 0.7058 0.5755 0.029 Uiso 1 1 calc R . . C6 C 0.07288(11) 0.91674(18) 0.41584(8) 0.0161(3) Uani 1 1 d . . . C7 C -0.01354(13) 0.9454(2) 0.40810(10) 0.0256(4) Uani 1 1 d . . . H7 H -0.0397 1.0183 0.3822 0.031 Uiso 1 1 calc R . . C8 C -0.06007(13) 0.8680(3) 0.43806(11) 0.0301(5) Uani 1 1 d . . . H8 H -0.1184 0.8871 0.4330 0.036 Uiso 1 1 calc R . . C9 C -0.02105(13) 0.7612(3) 0.47593(11) 0.0286(4) Uani 1 1 d . . . H9 H -0.0522 0.7046 0.4964 0.034 Uiso 1 1 calc R . . C10 C 0.06376(13) 0.7406(2) 0.48259(10) 0.0245(4) Uani 1 1 d . . . H10 H 0.0910 0.6687 0.5085 0.029 Uiso 1 1 calc R . . C11 C 0.33312(12) 0.9902(2) 0.24633(8) 0.0175(3) Uani 1 1 d . . . C12 C 0.35177(14) 0.8535(2) 0.23143(10) 0.0252(4) Uani 1 1 d . . . H12 H 0.3195 0.7759 0.2397 0.030 Uiso 1 1 calc R . . C13 C 0.41692(16) 0.8289(3) 0.20467(11) 0.0315(5) Uani 1 1 d . . . H13 H 0.4282 0.7351 0.1940 0.038 Uiso 1 1 calc R . . C14 C 0.46536(15) 0.9405(3) 0.19356(11) 0.0328(5) Uani 1 1 d . . . H14 H 0.5106 0.9235 0.1759 0.039 Uiso 1 1 calc R . . C15 C 0.44777(16) 1.0766(3) 0.20826(11) 0.0341(5) Uani 1 1 d . . . H15 H 0.4810 1.1535 0.2007 0.041 Uiso 1 1 calc R . . C16 C 0.38157(14) 1.1020(2) 0.23418(10) 0.0266(4) Uani 1 1 d . . . H16 H 0.3694 1.1963 0.2436 0.032 Uiso 1 1 calc R . . C17 C 0.15792(12) 0.9414(2) 0.22443(8) 0.0176(3) Uani 1 1 d . . . C18 C 0.14488(15) 0.9890(2) 0.16694(9) 0.0273(4) Uani 1 1 d . . . H18 H 0.1820 1.0568 0.1571 0.033 Uiso 1 1 calc R . . C19 C 0.07735(17) 0.9365(3) 0.12431(10) 0.0349(5) Uani 1 1 d . . . H19 H 0.0675 0.9706 0.0856 0.042 Uiso 1 1 calc R . . C20 C 0.02472(15) 0.8351(3) 0.13808(11) 0.0352(5) Uani 1 1 d . . . H20 H -0.0208 0.7988 0.1087 0.042 Uiso 1 1 calc R . . C21 C 0.03800(14) 0.7861(3) 0.19453(11) 0.0310(5) Uani 1 1 d . . . H21 H 0.0020 0.7154 0.2037 0.037 Uiso 1 1 calc R . . C22 C 0.10386(13) 0.8401(2) 0.23796(9) 0.0220(4) Uani 1 1 d . . . H22 H 0.1120 0.8079 0.2769 0.026 Uiso 1 1 calc R . . C23 C 0.22810(12) 1.19961(19) 0.28298(8) 0.0170(3) Uani 1 1 d . . . C24 C 0.15512(13) 1.2671(2) 0.25122(9) 0.0231(4) Uani 1 1 d . . . H24 H 0.1120 1.2136 0.2260 0.028 Uiso 1 1 calc R . . C25 C 0.14578(15) 1.4127(2) 0.25655(10) 0.0284(4) Uani 1 1 d . . . H25 H 0.0955 1.4577 0.2356 0.034 Uiso 1 1 calc R . . C26 C 0.20869(16) 1.4925(2) 0.29191(10) 0.0283(4) Uani 1 1 d . . . H26 H 0.2025 1.5923 0.2942 0.034 Uiso 1 1 calc R . . C27 C 0.28070(16) 1.4267(2) 0.32397(11) 0.0291(4) Uani 1 1 d . . . H27 H 0.3240 1.4814 0.3484 0.035 Uiso 1 1 calc R . . C28 C 0.28975(14) 1.2805(2) 0.32045(10) 0.0243(4) Uani 1 1 d . . . H28 H 0.3383 1.2353 0.3438 0.029 Uiso 1 1 calc R . . C29 C 0.24181(11) 0.57842(19) 0.49056(8) 0.0164(3) Uani 1 1 d . . . C30 C 0.20762(12) 0.4886(2) 0.44428(10) 0.0243(4) Uani 1 1 d . . . H30 H 0.1886 0.5271 0.4063 0.029 Uiso 1 1 calc R . . C31 C 0.20078(14) 0.3435(2) 0.45255(13) 0.0347(6) Uani 1 1 d . . . H31 H 0.1787 0.2835 0.4202 0.042 Uiso 1 1 calc R . . C32 C 0.22594(15) 0.2869(2) 0.50740(15) 0.0374(6) Uani 1 1 d . . . H32 H 0.2214 0.1876 0.5129 0.045 Uiso 1 1 calc R . . C33 C 0.25807(16) 0.3744(2) 0.55501(12) 0.0338(5) Uani 1 1 d . . . H33 H 0.2746 0.3354 0.5930 0.041 Uiso 1 1 calc R . . C34 C 0.26580(13) 0.5194(2) 0.54648(9) 0.0229(4) Uani 1 1 d . . . H34 H 0.2876 0.5792 0.5789 0.027 Uiso 1 1 calc R . . C35 C 0.28143(13) 0.90247(19) 0.55638(8) 0.0195(3) Uani 1 1 d . . . C36 C 0.22901(15) 0.8764(2) 0.59312(9) 0.0270(4) Uani 1 1 d . . . H36 H 0.1812 0.8170 0.5800 0.032 Uiso 1 1 calc R . . C37 C 0.24455(18) 0.9351(3) 0.64888(10) 0.0359(6) Uani 1 1 d . . . H37 H 0.2074 0.9170 0.6731 0.043 Uiso 1 1 calc R . . C38 C 0.3151(2) 1.0204(3) 0.66823(11) 0.0435(7) Uani 1 1 d . . . H38 H 0.3265 1.0608 0.7060 0.052 Uiso 1 1 calc R . . C39 C 0.3687(2) 1.0464(3) 0.63269(12) 0.0438(7) Uani 1 1 d . . . H39 H 0.4170 1.1043 0.6463 0.053 Uiso 1 1 calc R . . C40 C 0.35227(17) 0.9882(2) 0.57708(10) 0.0312(5) Uani 1 1 d . . . H40 H 0.3895 1.0070 0.5530 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01362(6) 0.01495(6) 0.01075(6) 0.00228(4) 0.00362(4) 0.00043(4) Sn1 0.01392(5) 0.01657(5) 0.01100(5) 0.00270(4) 0.00423(4) 0.00214(4) S1 0.0182(2) 0.0341(2) 0.0171(2) 0.00635(18) 0.00784(17) 0.00663(18) S2 0.01889(19) 0.01931(19) 0.0193(2) 0.00615(16) 0.00719(16) 0.00571(15) P1 0.01565(19) 0.01646(18) 0.01128(19) 0.00164(15) 0.00360(15) -0.00116(15) N1 0.0140(7) 0.0258(7) 0.0168(7) 0.0027(6) 0.0030(6) 0.0011(6) N2 0.0144(7) 0.0228(7) 0.0199(8) 0.0064(6) 0.0057(6) 0.0028(5) C1 0.0128(7) 0.0208(8) 0.0201(9) 0.0036(7) 0.0052(6) 0.0003(6) C2 0.0159(8) 0.0323(10) 0.0287(10) 0.0089(8) 0.0094(8) 0.0051(7) C3 0.0133(8) 0.0372(11) 0.0328(11) 0.0091(9) 0.0049(8) 0.0040(7) C4 0.0150(8) 0.0389(11) 0.0252(10) 0.0086(9) -0.0002(7) 0.0019(8) C5 0.0173(8) 0.0357(10) 0.0193(9) 0.0058(8) 0.0034(7) 0.0023(7) C6 0.0147(7) 0.0181(7) 0.0155(8) 0.0008(6) 0.0037(6) 0.0029(6) C7 0.0167(8) 0.0312(10) 0.0291(11) 0.0090(8) 0.0060(8) 0.0083(7) C8 0.0152(8) 0.0396(11) 0.0372(12) 0.0101(10) 0.0096(8) 0.0052(8) C9 0.0177(9) 0.0366(11) 0.0341(12) 0.0112(9) 0.0115(8) 0.0025(8) C10 0.0185(8) 0.0296(9) 0.0277(10) 0.0116(8) 0.0099(8) 0.0034(7) C11 0.0182(8) 0.0219(8) 0.0131(7) 0.0005(6) 0.0049(6) -0.0007(6) C12 0.0300(10) 0.0253(9) 0.0232(10) -0.0020(8) 0.0119(8) -0.0002(8) C13 0.0345(12) 0.0371(11) 0.0266(11) -0.0061(9) 0.0144(9) 0.0070(9) C14 0.0239(10) 0.0523(14) 0.0254(11) -0.0058(10) 0.0122(9) 0.0006(9) C15 0.0289(11) 0.0461(13) 0.0328(12) -0.0006(10) 0.0179(10) -0.0089(10) C16 0.0278(10) 0.0269(9) 0.0289(11) 0.0000(8) 0.0142(9) -0.0050(8) C17 0.0169(8) 0.0214(8) 0.0139(8) -0.0016(6) 0.0024(6) -0.0013(6) C18 0.0350(11) 0.0316(10) 0.0139(8) -0.0007(7) 0.0031(8) -0.0025(9) C19 0.0394(13) 0.0435(13) 0.0160(9) -0.0043(9) -0.0042(9) 0.0037(10) C20 0.0259(11) 0.0435(13) 0.0297(12) -0.0151(10) -0.0052(9) -0.0001(9) C21 0.0223(10) 0.0347(11) 0.0350(12) -0.0121(9) 0.0053(9) -0.0069(8) C22 0.0198(8) 0.0235(8) 0.0233(9) -0.0036(7) 0.0064(7) -0.0028(7) C23 0.0206(8) 0.0182(7) 0.0131(7) 0.0033(6) 0.0058(6) 0.0007(6) C24 0.0223(9) 0.0254(9) 0.0211(9) 0.0039(7) 0.0045(7) 0.0031(7) C25 0.0327(11) 0.0263(9) 0.0266(10) 0.0085(8) 0.0081(9) 0.0120(8) C26 0.0398(12) 0.0215(9) 0.0267(10) 0.0032(8) 0.0140(9) 0.0060(8) C27 0.0371(12) 0.0198(9) 0.0288(11) -0.0026(8) 0.0054(9) 0.0000(8) C28 0.0269(10) 0.0204(8) 0.0229(10) -0.0011(7) 0.0007(8) 0.0019(7) C29 0.0127(7) 0.0181(7) 0.0197(8) 0.0036(6) 0.0063(6) 0.0027(6) C30 0.0180(8) 0.0259(9) 0.0282(10) -0.0048(8) 0.0042(7) 0.0014(7) C31 0.0208(10) 0.0250(10) 0.0598(17) -0.0131(10) 0.0126(10) -0.0028(8) C32 0.0277(11) 0.0182(9) 0.075(2) 0.0069(10) 0.0299(12) 0.0015(8) C33 0.0335(11) 0.0299(10) 0.0466(14) 0.0196(10) 0.0262(11) 0.0129(9) C34 0.0232(9) 0.0247(9) 0.0225(9) 0.0062(7) 0.0090(7) 0.0050(7) C35 0.0269(9) 0.0177(7) 0.0144(8) 0.0012(6) 0.0060(7) 0.0040(7) C36 0.0294(10) 0.0341(10) 0.0187(9) -0.0008(8) 0.0083(8) 0.0098(8) C37 0.0491(15) 0.0407(12) 0.0198(10) -0.0013(9) 0.0122(10) 0.0172(11) C38 0.080(2) 0.0278(11) 0.0216(11) -0.0047(9) 0.0104(13) 0.0071(12) C39 0.074(2) 0.0260(11) 0.0267(12) -0.0040(9) 0.0045(13) -0.0153(12) C40 0.0469(13) 0.0239(9) 0.0221(10) -0.0015(8) 0.0073(9) -0.0101(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 S1 2.2965(5) . ? Pd1 S2 2.3121(5) . ? Pd1 P1 2.3786(5) . ? Pd1 Sn1 2.53697(18) . ? Sn1 C29 2.1545(18) . ? Sn1 C35 2.1647(19) . ? Sn1 N1 2.3466(16) . ? Sn1 N2 2.3869(16) . ? S1 C1 1.742(2) . ? S2 C6 1.7423(19) . ? P1 C23 1.8200(18) . ? P1 C17 1.8230(19) . ? P1 C11 1.8316(19) . ? N1 C1 1.341(2) . ? N1 C5 1.349(3) . ? N2 C6 1.340(2) . ? N2 C10 1.350(2) . ? C1 C2 1.411(3) . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.407(3) . ? C7 C8 1.374(3) . ? C7 H7 0.9500 . ? C8 C9 1.395(3) . ? C8 H8 0.9500 . ? C9 C10 1.372(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.391(3) . ? C11 C16 1.391(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.379(4) . ? C14 H14 0.9500 . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(3) . ? C17 C18 1.402(3) . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 H19 0.9500 . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.396(3) . ? C23 C24 1.399(3) . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 C26 1.380(3) . ? C25 H25 0.9500 . ? C26 C27 1.382(3) . ? C26 H26 0.9500 . ? C27 C28 1.391(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.390(3) . ? C29 C34 1.403(3) . ? C30 C31 1.391(3) . ? C30 H30 0.9500 . ? C31 C32 1.373(4) . ? C31 H31 0.9500 . ? C32 C33 1.393(4) . ? C32 H32 0.9500 . ? C33 C34 1.393(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.388(3) . ? C35 C40 1.400(3) . ? C36 C37 1.399(3) . ? C36 H36 0.9500 . ? C37 C38 1.389(4) . ? C37 H37 0.9500 . ? C38 C39 1.381(4) . ? C38 H38 0.9500 . ? C39 C40 1.393(3) . ? C39 H39 0.9500 . ? C40 H40 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 S1 Pd1 S2 177.89(2) . . ? S1 Pd1 P1 92.866(17) . . ? S2 Pd1 P1 87.984(17) . . ? S1 Pd1 Sn1 90.204(13) . . ? S2 Pd1 Sn1 88.991(13) . . ? P1 Pd1 Sn1 176.669(12) . . ? C29 Sn1 C35 104.71(7) . . ? C29 Sn1 N1 87.97(6) . . ? C35 Sn1 N1 88.98(7) . . ? C29 Sn1 N2 85.60(6) . . ? C35 Sn1 N2 93.58(7) . . ? N1 Sn1 N2 173.50(6) . . ? C29 Sn1 Pd1 126.69(5) . . ? C35 Sn1 Pd1 128.59(5) . . ? N1 Sn1 Pd1 92.27(4) . . ? N2 Sn1 Pd1 90.79(4) . . ? C1 S1 Pd1 113.78(7) . . ? C6 S2 Pd1 113.05(6) . . ? C23 P1 C17 105.34(9) . . ? C23 P1 C11 104.63(9) . . ? C17 P1 C11 101.20(9) . . ? C23 P1 Pd1 110.71(6) . . ? C17 P1 Pd1 114.29(6) . . ? C11 P1 Pd1 119.28(6) . . ? C1 N1 C5 119.92(17) . . ? C1 N1 Sn1 117.60(12) . . ? C5 N1 Sn1 121.63(13) . . ? C6 N2 C10 119.60(17) . . ? C6 N2 Sn1 117.05(12) . . ? C10 N2 Sn1 123.21(13) . . ? N1 C1 C2 119.96(18) . . ? N1 C1 S1 122.30(14) . . ? C2 C1 S1 117.74(15) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 119.39(19) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 118.7(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.5(2) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 119.97(17) . . ? N2 C6 S2 121.28(14) . . ? C7 C6 S2 118.74(14) . . ? C8 C7 C6 119.91(19) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.53(19) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 117.8(2) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? N2 C10 C9 123.15(19) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C12 C11 C16 118.49(18) . . ? C12 C11 P1 116.80(14) . . ? C16 C11 P1 124.71(15) . . ? C13 C12 C11 120.9(2) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.5(2) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C22 C17 C18 119.44(19) . . ? C22 C17 P1 119.97(15) . . ? C18 C17 P1 120.59(15) . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.3(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C17 120.0(2) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C28 C23 C24 118.79(18) . . ? C28 C23 P1 117.48(14) . . ? C24 C23 P1 123.66(15) . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.7(2) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 120.0(2) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 120.6(2) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C30 C29 C34 118.05(18) . . ? C30 C29 Sn1 118.63(15) . . ? C34 C29 Sn1 123.27(15) . . ? C29 C30 C31 121.2(2) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 120.1(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.2(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 119.6(2) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C29 120.8(2) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.6 . . ? C36 C35 C40 118.0(2) . . ? C36 C35 Sn1 120.75(16) . . ? C40 C35 Sn1 121.08(16) . . ? C35 C36 C37 121.9(2) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C38 C37 C36 119.0(2) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.4(3) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 120.6(2) . . ? C39 C40 H40 119.7 . . ? C35 C40 H40 119.7 . . ? 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 S1 Pd1 Sn1 C29 -74.15(6) . . . . ? S2 Pd1 Sn1 C29 107.81(6) . . . . ? S1 Pd1 Sn1 C35 105.53(7) . . . . ? S2 Pd1 Sn1 C35 -72.51(7) . . . . ? S1 Pd1 Sn1 N1 15.02(5) . . . . ? S2 Pd1 Sn1 N1 -163.03(4) . . . . ? S1 Pd1 Sn1 N2 -159.25(4) . . . . ? S2 Pd1 Sn1 N2 22.71(4) . . . . ? P1 Pd1 S1 C1 166.08(7) . . . . ? Sn1 Pd1 S1 C1 -15.22(7) . . . . ? P1 Pd1 S2 C6 152.44(7) . . . . ? Sn1 Pd1 S2 C6 -26.16(7) . . . . ? S1 Pd1 P1 C23 -124.01(7) . . . . ? S2 Pd1 P1 C23 54.05(7) . . . . ? S1 Pd1 P1 C17 117.24(7) . . . . ? S2 Pd1 P1 C17 -64.69(7) . . . . ? S1 Pd1 P1 C11 -2.58(7) . . . . ? S2 Pd1 P1 C11 175.49(7) . . . . ? C29 Sn1 N1 C1 108.29(15) . . . . ? C35 Sn1 N1 C1 -146.95(15) . . . . ? Pd1 Sn1 N1 C1 -18.36(14) . . . . ? C29 Sn1 N1 C5 -61.11(17) . . . . ? C35 Sn1 N1 C5 43.66(17) . . . . ? Pd1 Sn1 N1 C5 172.24(16) . . . . ? C29 Sn1 N2 C6 -151.17(15) . . . . ? C35 Sn1 N2 C6 104.32(15) . . . . ? Pd1 Sn1 N2 C6 -24.43(14) . . . . ? C29 Sn1 N2 C10 33.23(18) . . . . ? C35 Sn1 N2 C10 -71.27(18) . . . . ? Pd1 Sn1 N2 C10 159.98(17) . . . . ? C5 N1 C1 C2 -0.3(3) . . . . ? Sn1 N1 C1 C2 -169.93(15) . . . . ? C5 N1 C1 S1 179.91(16) . . . . ? Sn1 N1 C1 S1 10.3(2) . . . . ? Pd1 S1 C1 N1 5.38(19) . . . . ? Pd1 S1 C1 C2 -174.37(14) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? S1 C1 C2 C3 -179.92(17) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C1 N1 C5 C4 0.3(3) . . . . ? Sn1 N1 C5 C4 169.45(17) . . . . ? C3 C4 C5 N1 -0.2(4) . . . . ? C10 N2 C6 C7 3.5(3) . . . . ? Sn1 N2 C6 C7 -172.27(15) . . . . ? C10 N2 C6 S2 -175.28(16) . . . . ? Sn1 N2 C6 S2 9.0(2) . . . . ? Pd1 S2 C6 N2 14.61(18) . . . . ? Pd1 S2 C6 C7 -164.18(15) . . . . ? N2 C6 C7 C8 -2.5(3) . . . . ? S2 C6 C7 C8 176.33(19) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 1.6(4) . . . . ? C6 N2 C10 C9 -2.0(3) . . . . ? Sn1 N2 C10 C9 173.48(19) . . . . ? C8 C9 C10 N2 -0.6(4) . . . . ? C23 P1 C11 C12 -170.75(16) . . . . ? C17 P1 C11 C12 -61.46(17) . . . . ? Pd1 P1 C11 C12 64.82(17) . . . . ? C23 P1 C11 C16 9.4(2) . . . . ? C17 P1 C11 C16 118.70(19) . . . . ? Pd1 P1 C11 C16 -115.02(17) . . . . ? C16 C11 C12 C13 -0.4(3) . . . . ? P1 C11 C12 C13 179.73(18) . . . . ? C11 C12 C13 C14 1.3(4) . . . . ? C12 C13 C14 C15 -1.1(4) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C12 C11 C16 C15 -0.7(3) . . . . ? P1 C11 C16 C15 179.14(19) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C23 P1 C17 C22 -120.66(16) . . . . ? C11 P1 C17 C22 130.60(16) . . . . ? Pd1 P1 C17 C22 1.08(18) . . . . ? C23 P1 C17 C18 60.12(19) . . . . ? C11 P1 C17 C18 -48.62(18) . . . . ? Pd1 P1 C17 C18 -178.14(15) . . . . ? C22 C17 C18 C19 1.1(3) . . . . ? P1 C17 C18 C19 -179.66(18) . . . . ? C17 C18 C19 C20 -1.8(4) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? C19 C20 C21 C22 0.8(4) . . . . ? C20 C21 C22 C17 -1.5(3) . . . . ? C18 C17 C22 C21 0.5(3) . . . . ? P1 C17 C22 C21 -178.69(16) . . . . ? C17 P1 C23 C28 -175.83(16) . . . . ? C11 P1 C23 C28 -69.58(17) . . . . ? Pd1 P1 C23 C28 60.14(17) . . . . ? C17 P1 C23 C24 7.28(19) . . . . ? C11 P1 C23 C24 113.53(17) . . . . ? Pd1 P1 C23 C24 -116.75(16) . . . . ? C28 C23 C24 C25 1.2(3) . . . . ? P1 C23 C24 C25 178.02(17) . . . . ? C23 C24 C25 C26 1.5(3) . . . . ? C24 C25 C26 C27 -2.2(4) . . . . ? C25 C26 C27 C28 0.2(4) . . . . ? C26 C27 C28 C23 2.5(4) . . . . ? C24 C23 C28 C27 -3.2(3) . . . . ? P1 C23 C28 C27 179.77(18) . . . . ? C35 Sn1 C29 C30 165.37(14) . . . . ? N1 Sn1 C29 C30 -106.21(15) . . . . ? N2 Sn1 C29 C30 72.82(15) . . . . ? Pd1 Sn1 C29 C30 -14.89(17) . . . . ? C35 Sn1 C29 C34 -17.20(17) . . . . ? N1 Sn1 C29 C34 71.22(16) . . . . ? N2 Sn1 C29 C34 -109.76(16) . . . . ? Pd1 Sn1 C29 C34 162.54(13) . . . . ? C34 C29 C30 C31 -2.9(3) . . . . ? Sn1 C29 C30 C31 174.69(16) . . . . ? C29 C30 C31 C32 1.7(3) . . . . ? C30 C31 C32 C33 0.3(3) . . . . ? C31 C32 C33 C34 -1.1(3) . . . . ? C32 C33 C34 C29 -0.1(3) . . . . ? C30 C29 C34 C33 2.1(3) . . . . ? Sn1 C29 C34 C33 -175.38(15) . . . . ? C29 Sn1 C35 C36 -47.54(17) . . . . ? N1 Sn1 C35 C36 -135.18(16) . . . . ? N2 Sn1 C35 C36 38.84(16) . . . . ? Pd1 Sn1 C35 C36 132.72(14) . . . . ? C29 Sn1 C35 C40 127.07(17) . . . . ? N1 Sn1 C35 C40 39.43(17) . . . . ? N2 Sn1 C35 C40 -146.55(17) . . . . ? Pd1 Sn1 C35 C40 -52.67(19) . . . . ? C40 C35 C36 C37 1.1(3) . . . . ? Sn1 C35 C36 C37 175.90(17) . . . . ? C35 C36 C37 C38 -0.9(4) . . . . ? C36 C37 C38 C39 0.1(4) . . . . ? C37 C38 C39 C40 0.4(4) . . . . ? C38 C39 C40 C35 -0.1(4) . . . . ? C36 C35 C40 C39 -0.6(3) . . . . ? Sn1 C35 C40 C39 -175.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.909 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 963368' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rg131c02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H46 N4 P2 Pd2 S4 Sn, 2(C4 H8 O)' _chemical_formula_sum 'C64 H62 N4 O2 P2 Pd2 S4 Sn' _chemical_formula_weight 1440.85 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' S S 0.1246 0.1234 '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' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8400(6) _cell_length_b 14.3813(6) _cell_length_c 17.0641(7) _cell_angle_alpha 71.399(3) _cell_angle_beta 75.459(3) _cell_angle_gamma 72.174(3) _cell_volume 3019.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 38505 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.32 _exptl_crystal_description piece _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 1.238 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7510 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details XShape _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Stoe IPDS-2T' _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 44439 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17590 _reflns_number_gt 14717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _refine_special_details ; This crystal structure contains two molecules of crystallization (THF) in the asymmetric unit. One of them is heavily disordered and was therefore refined and three alternative positions. Only one set of translational thermal motion variables was refined for each of the three alternatives (i.e., the five atoms within one molecule were refined anisotropically but with the same displacement parameters). All C-O bonds were restrained to the same length, and the same was done with all C-C bonds. eadp o2 c61 c62 c63 c64 eadp o2a c61a c62a c63a c64a eadp o2b c61b c62b c63b c64b sadi 0.001 o2 c61 o2 c64 o2a c61a o2a c64a o2b c61b o2b c64b sadi 0.001 c61 c62 c62 c63 c63 c64 c61a c62a c62a c63a c63a c64a c61b c62b C62B C63B C63B C64B Initially, three individual free variables were used for the refinement of the site occupancies (in combination with a SUMP instruction to yield full occupancy of this solvent site). In the final refinement cycles, for the sake of stabilizing the refinement the site occupancies were fixed to 0.60, 0.19 and 0.21. 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^)+(0.0312P)^2^+2.2015P] 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 17590 _refine_ls_number_parameters 730 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _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 Sn1 Sn 0.336557(10) 0.455699(9) 0.317905(7) 0.02007(3) Uani 1 1 d . . . Pd1 Pd 0.397128(11) 0.615685(10) 0.223395(8) 0.02099(3) Uani 1 1 d . . . Pd2 Pd 0.285330(11) 0.287839(10) 0.402883(9) 0.02227(3) Uani 1 1 d . . . S1 S 0.56037(4) 0.51988(4) 0.18669(3) 0.02914(10) Uani 1 1 d . . . S2 S 0.23483(5) 0.71212(4) 0.25831(4) 0.03612(12) Uani 1 1 d . . . S3 S 0.28942(5) 0.31730(4) 0.52660(3) 0.03085(11) Uani 1 1 d . . . S4 S 0.29252(6) 0.24854(4) 0.28059(3) 0.04001(14) Uani 1 1 d . . . P1 P 0.44407(4) 0.76615(4) 0.12836(3) 0.02316(9) Uani 1 1 d . . . P2 P 0.20979(4) 0.14605(4) 0.46986(3) 0.02494(10) Uani 1 1 d . . . N1 N 0.51810(14) 0.35937(12) 0.31188(11) 0.0274(3) Uani 1 1 d . . . N2 N 0.16199(14) 0.54552(13) 0.33658(11) 0.0288(3) Uani 1 1 d . . . N3 N 0.34864(13) 0.49078(12) 0.44288(10) 0.0252(3) Uani 1 1 d . . . N4 N 0.29897(15) 0.43824(13) 0.19072(11) 0.0293(3) Uani 1 1 d . . . C1 C 0.58825(15) 0.39561(14) 0.24909(12) 0.0251(4) Uani 1 1 d . . . C2 C 0.68869(17) 0.33413(17) 0.23298(15) 0.0332(4) Uani 1 1 d . . . H2 H 0.7378 0.3589 0.1872 0.040 Uiso 1 1 calc R . . C3 C 0.71434(19) 0.23764(18) 0.28463(17) 0.0400(5) Uani 1 1 d . . . H3 H 0.7814 0.1954 0.2743 0.048 Uiso 1 1 calc R . . C4 C 0.6422(2) 0.20213(17) 0.35179(17) 0.0398(5) Uani 1 1 d . . . H4 H 0.6594 0.1367 0.3890 0.048 Uiso 1 1 calc R . . C5 C 0.54506(19) 0.26485(16) 0.36260(15) 0.0342(4) Uani 1 1 d . . . H5 H 0.4947 0.2409 0.4076 0.041 Uiso 1 1 calc R . . C6 C 0.13992(16) 0.64609(15) 0.30367(13) 0.0282(4) Uani 1 1 d . . . C7 C 0.03632(19) 0.70249(18) 0.30612(16) 0.0385(5) Uani 1 1 d . . . H7 H 0.0207 0.7734 0.2809 0.046 Uiso 1 1 calc R . . C8 C -0.04139(18) 0.6550(2) 0.34477(17) 0.0420(5) Uani 1 1 d . . . H8 H -0.1112 0.6925 0.3466 0.050 Uiso 1 1 calc R . . C9 C -0.01736(19) 0.5511(2) 0.38140(18) 0.0456(6) Uani 1 1 d . . . H9 H -0.0701 0.5169 0.4105 0.055 Uiso 1 1 calc R . . C10 C 0.08454(18) 0.49909(18) 0.37452(17) 0.0391(5) Uani 1 1 d . . . H10 H 0.1012 0.4278 0.3973 0.047 Uiso 1 1 calc R . . C11 C 0.32364(15) 0.42796(14) 0.51743(12) 0.0246(4) Uani 1 1 d . . . C12 C 0.3258(2) 0.44932(17) 0.59223(13) 0.0342(5) Uani 1 1 d . . . H12 H 0.3054 0.4061 0.6451 0.041 Uiso 1 1 calc R . . C13 C 0.3574(2) 0.53254(18) 0.58833(14) 0.0378(5) Uani 1 1 d . . . H13 H 0.3599 0.5467 0.6384 0.045 Uiso 1 1 calc R . . C14 C 0.3856(2) 0.59589(16) 0.51074(15) 0.0359(5) Uani 1 1 d . . . H14 H 0.4087 0.6533 0.5065 0.043 Uiso 1 1 calc R . . C15 C 0.37889(18) 0.57296(16) 0.43991(14) 0.0316(4) Uani 1 1 d . . . H15 H 0.3964 0.6170 0.3866 0.038 Uiso 1 1 calc R . . C16 C 0.29145(17) 0.34776(16) 0.19035(13) 0.0292(4) Uani 1 1 d . . . C17 C 0.2849(2) 0.33012(19) 0.11492(14) 0.0370(5) Uani 1 1 d . . . H17 H 0.2795 0.2658 0.1150 0.044 Uiso 1 1 calc R . . C18 C 0.2865(2) 0.4059(2) 0.04210(15) 0.0424(5) Uani 1 1 d . . . H18 H 0.2835 0.3942 -0.0089 0.051 Uiso 1 1 calc R . . C19 C 0.2926(2) 0.4995(2) 0.04324(15) 0.0446(6) Uani 1 1 d . . . H19 H 0.2927 0.5534 -0.0065 0.053 Uiso 1 1 calc R . . C20 C 0.2985(2) 0.51299(18) 0.11834(14) 0.0387(5) Uani 1 1 d . . . H20 H 0.3023 0.5775 0.1193 0.046 Uiso 1 1 calc R . . C21 C 0.56957(16) 0.78035(14) 0.13155(12) 0.0263(4) Uani 1 1 d . . . C22 C 0.63486(19) 0.82239(18) 0.06118(14) 0.0362(5) Uani 1 1 d . . . H22 H 0.6172 0.8406 0.0070 0.043 Uiso 1 1 calc R . . C23 C 0.7254(2) 0.8378(2) 0.06985(17) 0.0479(6) Uani 1 1 d . . . H23 H 0.7703 0.8646 0.0215 0.058 Uiso 1 1 calc R . . C24 C 0.7508(2) 0.8142(2) 0.14830(18) 0.0469(6) Uani 1 1 d . . . H24 H 0.8118 0.8269 0.1539 0.056 Uiso 1 1 calc R . . C25 C 0.6874(2) 0.7723(2) 0.21868(16) 0.0432(6) Uani 1 1 d . . . H25 H 0.7048 0.7563 0.2727 0.052 Uiso 1 1 calc R . . C26 C 0.59847(19) 0.75361(17) 0.21032(14) 0.0348(5) Uani 1 1 d . . . H26 H 0.5566 0.7223 0.2587 0.042 Uiso 1 1 calc R . . C27 C 0.35773(17) 0.88725(14) 0.14247(12) 0.0274(4) Uani 1 1 d . . . C28 C 0.26064(19) 0.91630(17) 0.11990(15) 0.0368(5) Uani 1 1 d . . . H28 H 0.2428 0.8759 0.0939 0.044 Uiso 1 1 calc R . . C29 C 0.1896(2) 1.00350(18) 0.13484(17) 0.0434(6) Uani 1 1 d . . . H29 H 0.1237 1.0226 0.1191 0.052 Uiso 1 1 calc R . . C30 C 0.2154(2) 1.06268(18) 0.17289(17) 0.0477(7) Uani 1 1 d . . . H30 H 0.1670 1.1223 0.1835 0.057 Uiso 1 1 calc R . . C31 C 0.3108(3) 1.0350(2) 0.19516(18) 0.0510(7) Uani 1 1 d . . . H31 H 0.3283 1.0758 0.2210 0.061 Uiso 1 1 calc R . . C32 C 0.3823(2) 0.94755(17) 0.18025(15) 0.0385(5) Uani 1 1 d . . . H32 H 0.4482 0.9291 0.1960 0.046 Uiso 1 1 calc R . . C33 C 0.44499(16) 0.77705(16) 0.01840(12) 0.0276(4) Uani 1 1 d . . . C34 C 0.4367(2) 0.86946(18) -0.04229(14) 0.0377(5) Uani 1 1 d . . . H34 H 0.4302 0.9293 -0.0270 0.045 Uiso 1 1 calc R . . C35 C 0.4379(2) 0.8744(2) -0.12526(15) 0.0459(6) Uani 1 1 d . . . H35 H 0.4331 0.9375 -0.1665 0.055 Uiso 1 1 calc R . . C36 C 0.4460(2) 0.7877(2) -0.14800(15) 0.0452(6) Uani 1 1 d . . . H36 H 0.4461 0.7915 -0.2046 0.054 Uiso 1 1 calc R . . C37 C 0.4541(2) 0.6957(2) -0.08831(15) 0.0426(6) Uani 1 1 d . . . H37 H 0.4599 0.6363 -0.1040 0.051 Uiso 1 1 calc R . . C38 C 0.45360(18) 0.68989(17) -0.00526(14) 0.0326(4) Uani 1 1 d . . . H38 H 0.4591 0.6264 0.0356 0.039 Uiso 1 1 calc R . . C39 C 0.08251(16) 0.18636(15) 0.44060(13) 0.0286(4) Uani 1 1 d . . . C40 C 0.00642(19) 0.25476(18) 0.47997(16) 0.0366(5) Uani 1 1 d . . . H40 H 0.0211 0.2743 0.5230 0.044 Uiso 1 1 calc R . . C41 C -0.0901(2) 0.2943(2) 0.45687(19) 0.0451(6) Uani 1 1 d . . . H41 H -0.1413 0.3402 0.4843 0.054 Uiso 1 1 calc R . . C42 C -0.1117(2) 0.2668(2) 0.3938(2) 0.0560(7) Uani 1 1 d . . . H42 H -0.1780 0.2933 0.3781 0.067 Uiso 1 1 calc R . . C43 C -0.0367(2) 0.2007(3) 0.3538(2) 0.0609(8) Uani 1 1 d . . . H43 H -0.0516 0.1823 0.3102 0.073 Uiso 1 1 calc R . . C44 C 0.0607(2) 0.1605(2) 0.37647(16) 0.0424(5) Uani 1 1 d . . . H44 H 0.1119 0.1155 0.3481 0.051 Uiso 1 1 calc R . . C45 C 0.27814(18) 0.03003(15) 0.43696(13) 0.0307(4) Uani 1 1 d . . . C46 C 0.3831(2) 0.01510(19) 0.40671(17) 0.0430(5) Uani 1 1 d . . . H46 H 0.4170 0.0660 0.4007 0.052 Uiso 1 1 calc R . . C47 C 0.4390(2) -0.0748(2) 0.3852(2) 0.0560(8) Uani 1 1 d . . . H47 H 0.5110 -0.0853 0.3654 0.067 Uiso 1 1 calc R . . C48 C 0.3910(3) -0.14736(19) 0.39233(19) 0.0587(9) Uani 1 1 d . . . H48 H 0.4296 -0.2077 0.3766 0.070 Uiso 1 1 calc R . . C49 C 0.2873(3) -0.13415(19) 0.42209(19) 0.0569(8) Uani 1 1 d . . . H49 H 0.2542 -0.1849 0.4265 0.068 Uiso 1 1 calc R . . C50 C 0.2309(2) -0.04634(17) 0.44578(17) 0.0424(6) Uani 1 1 d . . . H50 H 0.1596 -0.0383 0.4681 0.051 Uiso 1 1 calc R . . C51 C 0.1838(2) 0.09438(15) 0.58425(13) 0.0340(5) Uani 1 1 d . . . C52 C 0.2599(3) 0.08226(19) 0.62861(19) 0.0566(8) Uani 1 1 d . . . H52 H 0.3213 0.1029 0.6002 0.068 Uiso 1 1 calc R . . C53 C 0.2462(4) 0.0396(2) 0.7152(2) 0.0868(16) Uani 1 1 d . . . H53 H 0.2989 0.0312 0.7452 0.104 Uiso 1 1 calc R . . C54 C 0.1586(5) 0.0099(2) 0.7573(2) 0.0908(17) Uani 1 1 d . . . H54 H 0.1499 -0.0183 0.8163 0.109 Uiso 1 1 calc R . . C55 C 0.0836(4) 0.0211(2) 0.7141(2) 0.0754(13) Uani 1 1 d . . . H55 H 0.0225 0.0003 0.7434 0.090 Uiso 1 1 calc R . . C56 C 0.0953(2) 0.06277(19) 0.62708(16) 0.0482(7) Uani 1 1 d . . . H56 H 0.0428 0.0693 0.5975 0.058 Uiso 1 1 calc R . . O1 O 0.8991(2) 0.4372(3) 0.1231(3) 0.1139(13) Uani 1 1 d . . . C57 C 0.8557(3) 0.5296(4) 0.1440(3) 0.0868(13) Uani 1 1 d . . . H57A H 0.7810 0.5378 0.1653 0.104 Uiso 1 1 calc R . . H57B H 0.8656 0.5867 0.0941 0.104 Uiso 1 1 calc R . . C58 C 0.9072(4) 0.5275(4) 0.2073(3) 0.0968(15) Uani 1 1 d . . . H58A H 0.8725 0.4970 0.2638 0.116 Uiso 1 1 calc R . . H58B H 0.9092 0.5966 0.2048 0.116 Uiso 1 1 calc R . . C59 C 1.0149(3) 0.4629(4) 0.1874(3) 0.0876(13) Uani 1 1 d . . . H59A H 1.0645 0.5055 0.1597 0.105 Uiso 1 1 calc R . . H59B H 1.0382 0.4144 0.2391 0.105 Uiso 1 1 calc R . . C60 C 1.0043(4) 0.4097(4) 0.1306(4) 0.1005(16) Uani 1 1 d . . . H60A H 1.0470 0.4293 0.0750 0.121 Uiso 1 1 calc R . . H60B H 1.0273 0.3356 0.1537 0.121 Uiso 1 1 calc R . . O2 O 0.9700(9) 0.1146(6) 1.0486(6) 0.135(2) Uani 0.60 1 d PD A 1 C61 C 0.9343(12) 0.1315(5) 0.9757(7) 0.135(2) Uani 0.60 1 d PD A 1 H61A H 0.8746 0.1020 0.9876 0.162 Uiso 0.60 1 calc PR A 1 H61B H 0.9890 0.0999 0.9354 0.162 Uiso 0.60 1 calc PR A 1 C62 C 0.9052(11) 0.2363(5) 0.9421(7) 0.135(2) Uani 0.60 1 d PD A 1 H62A H 0.9380 0.2548 0.8826 0.162 Uiso 0.60 1 calc PR A 1 H62B H 0.8295 0.2593 0.9452 0.162 Uiso 0.60 1 calc PR A 1 C63 C 0.9369(12) 0.2823(6) 0.9889(6) 0.135(2) Uani 0.60 1 d PD A 1 H63A H 0.8820 0.3412 1.0015 0.162 Uiso 0.60 1 calc PR A 1 H63B H 0.9997 0.3054 0.9580 0.162 Uiso 0.60 1 calc PR A 1 C64 C 0.9567(13) 0.2071(6) 1.0627(7) 0.135(2) Uani 0.60 1 d PD A 1 H64A H 1.0196 0.2096 1.0788 0.162 Uiso 0.60 1 calc PR A 1 H64B H 0.8983 0.2178 1.1090 0.162 Uiso 0.60 1 calc PR A 1 O2A O 0.9585(13) 0.1124(16) 1.0658(12) 0.071(3) Uani 0.19 1 d PD B 2 C61A C 0.9644(15) 0.2022(14) 1.0748(15) 0.071(3) Uani 0.19 1 d PD B 2 H61C H 1.0299 0.2199 1.0440 0.086 Uiso 0.19 1 calc PR B 2 H61D H 0.9560 0.2006 1.1345 0.086 Uiso 0.19 1 calc PR B 2 C62A C 0.8802(14) 0.2678(14) 1.0382(15) 0.071(3) Uani 0.19 1 d PD B 2 H62C H 0.9030 0.3105 0.9823 0.086 Uiso 0.19 1 calc PR B 2 H62D H 0.8361 0.3121 1.0743 0.086 Uiso 0.19 1 calc PR B 2 C63A C 0.8281(15) 0.2019(13) 1.0317(14) 0.071(3) Uani 0.19 1 d PD B 2 H63C H 0.7819 0.1822 1.0854 0.086 Uiso 0.19 1 calc PR B 2 H63D H 0.7851 0.2370 0.9873 0.086 Uiso 0.19 1 calc PR B 2 C64A C 0.8972(15) 0.1150(14) 1.0125(13) 0.071(3) Uani 0.19 1 d PD B 2 H64C H 0.8672 0.0557 1.0301 0.086 Uiso 0.19 1 calc PR B 2 H64D H 0.9311 0.1262 0.9529 0.086 Uiso 0.19 1 calc PR B 2 O2B O 1.0206(11) 0.1492(15) 0.9801(12) 0.102(4) Uani 0.21 1 d PD C 3 C61B C 0.9833(14) 0.2340(19) 1.010(2) 0.102(4) Uani 0.21 1 d PD C 3 H61E H 0.9787 0.2967 0.9634 0.123 Uiso 0.21 1 calc PR C 3 H61F H 1.0271 0.2346 1.0474 0.123 Uiso 0.21 1 calc PR C 3 C62B C 0.8855(16) 0.224(3) 1.0540(15) 0.102(4) Uani 0.21 1 d PD C 3 H62E H 0.8438 0.2842 1.0740 0.123 Uiso 0.21 1 calc PR C 3 H62F H 0.8872 0.1617 1.1006 0.123 Uiso 0.21 1 calc PR C 3 C63B C 0.8567(16) 0.218(2) 0.9832(17) 0.102(4) Uani 0.21 1 d PD C 3 H63E H 0.8011 0.1821 1.0005 0.123 Uiso 0.21 1 calc PR C 3 H63F H 0.8304 0.2872 0.9483 0.123 Uiso 0.21 1 calc PR C 3 C64B C 0.9425(13) 0.166(2) 0.9368(15) 0.102(4) Uani 0.21 1 d PD C 3 H64E H 0.9322 0.1018 0.9353 0.123 Uiso 0.21 1 calc PR C 3 H64F H 0.9572 0.2081 0.8786 0.123 Uiso 0.21 1 calc PR C 3 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 Sn1 0.02420(6) 0.01664(5) 0.02034(6) -0.00548(4) -0.00192(4) -0.00726(4) Pd1 0.02620(7) 0.01712(6) 0.02065(6) -0.00564(5) -0.00222(5) -0.00746(5) Pd2 0.02771(7) 0.01795(6) 0.02306(7) -0.00565(5) -0.00322(5) -0.00894(5) S1 0.0282(2) 0.0261(2) 0.0297(2) -0.00669(18) 0.00035(18) -0.00672(18) S2 0.0333(3) 0.0198(2) 0.0481(3) -0.0077(2) 0.0029(2) -0.00551(19) S3 0.0447(3) 0.0292(2) 0.0230(2) -0.00524(18) -0.0034(2) -0.0188(2) S4 0.0721(4) 0.0291(3) 0.0265(2) -0.0100(2) -0.0020(2) -0.0257(3) P1 0.0320(3) 0.0189(2) 0.0206(2) -0.00524(16) -0.00428(18) -0.00928(18) P2 0.0299(2) 0.0200(2) 0.0269(2) -0.00419(17) -0.00711(19) -0.00924(18) N1 0.0311(9) 0.0221(7) 0.0298(8) -0.0079(6) -0.0071(7) -0.0049(6) N2 0.0269(8) 0.0249(8) 0.0320(9) -0.0063(7) -0.0034(7) -0.0052(6) N3 0.0316(8) 0.0220(7) 0.0253(8) -0.0079(6) -0.0056(6) -0.0087(6) N4 0.0376(10) 0.0289(8) 0.0253(8) -0.0068(7) -0.0062(7) -0.0136(7) C1 0.0264(9) 0.0239(8) 0.0301(9) -0.0134(7) -0.0084(7) -0.0040(7) C2 0.0277(10) 0.0352(11) 0.0406(11) -0.0185(9) -0.0054(8) -0.0045(8) C3 0.0310(11) 0.0360(11) 0.0567(15) -0.0226(11) -0.0157(10) 0.0039(9) C4 0.0420(13) 0.0279(10) 0.0480(13) -0.0068(9) -0.0206(11) 0.0005(9) C5 0.0387(12) 0.0264(10) 0.0360(11) -0.0042(8) -0.0113(9) -0.0060(8) C6 0.0284(10) 0.0258(9) 0.0282(9) -0.0089(7) -0.0012(7) -0.0045(7) C7 0.0347(12) 0.0287(10) 0.0439(12) -0.0095(9) -0.0028(9) 0.0004(9) C8 0.0254(10) 0.0461(13) 0.0497(14) -0.0174(11) -0.0031(9) 0.0005(9) C9 0.0284(11) 0.0470(14) 0.0574(16) -0.0114(12) 0.0005(10) -0.0125(10) C10 0.0288(11) 0.0314(11) 0.0515(14) -0.0037(10) -0.0032(10) -0.0102(8) C11 0.0283(9) 0.0235(8) 0.0236(8) -0.0080(7) -0.0043(7) -0.0070(7) C12 0.0485(13) 0.0336(10) 0.0240(9) -0.0075(8) -0.0074(9) -0.0142(9) C13 0.0544(14) 0.0374(11) 0.0309(10) -0.0157(9) -0.0150(10) -0.0110(10) C14 0.0507(14) 0.0269(10) 0.0397(11) -0.0122(9) -0.0165(10) -0.0124(9) C15 0.0441(12) 0.0248(9) 0.0307(10) -0.0067(8) -0.0105(9) -0.0124(8) C16 0.0338(10) 0.0323(10) 0.0263(9) -0.0113(8) -0.0026(8) -0.0131(8) C17 0.0469(13) 0.0422(12) 0.0312(10) -0.0168(9) -0.0046(9) -0.0182(10) C18 0.0523(15) 0.0548(15) 0.0285(10) -0.0132(10) -0.0101(10) -0.0200(12) C19 0.0628(17) 0.0464(14) 0.0284(11) -0.0013(10) -0.0153(11) -0.0218(12) C20 0.0562(15) 0.0327(11) 0.0323(11) -0.0027(9) -0.0143(10) -0.0188(10) C21 0.0329(10) 0.0227(8) 0.0255(9) -0.0061(7) -0.0047(7) -0.0104(7) C22 0.0413(12) 0.0421(12) 0.0262(10) -0.0038(9) -0.0034(9) -0.0189(10) C23 0.0448(14) 0.0587(16) 0.0420(13) -0.0039(12) -0.0004(11) -0.0304(13) C24 0.0413(14) 0.0492(14) 0.0569(16) -0.0083(12) -0.0154(12) -0.0209(11) C25 0.0534(15) 0.0439(13) 0.0398(12) -0.0031(10) -0.0199(11) -0.0209(11) C26 0.0439(12) 0.0365(11) 0.0276(10) -0.0026(8) -0.0095(9) -0.0181(9) C27 0.0374(11) 0.0191(8) 0.0238(9) -0.0044(7) -0.0015(7) -0.0086(7) C28 0.0420(12) 0.0265(10) 0.0413(12) -0.0070(9) -0.0071(10) -0.0095(9) C29 0.0392(13) 0.0333(11) 0.0457(13) -0.0037(10) -0.0019(10) -0.0031(10) C30 0.0585(17) 0.0275(11) 0.0440(13) -0.0114(10) 0.0026(12) 0.0007(10) C31 0.074(2) 0.0335(12) 0.0506(15) -0.0240(11) -0.0130(14) -0.0045(12) C32 0.0542(15) 0.0282(10) 0.0379(11) -0.0131(9) -0.0122(10) -0.0089(10) C33 0.0318(10) 0.0308(9) 0.0235(9) -0.0078(7) -0.0061(7) -0.0107(8) C34 0.0548(15) 0.0346(11) 0.0280(10) -0.0031(8) -0.0131(10) -0.0178(10) C35 0.0562(16) 0.0536(15) 0.0283(11) 0.0041(10) -0.0174(11) -0.0215(12) C36 0.0488(14) 0.0688(17) 0.0262(10) -0.0138(11) -0.0119(10) -0.0202(13) C37 0.0482(14) 0.0560(15) 0.0348(12) -0.0240(11) -0.0078(10) -0.0154(12) C38 0.0375(11) 0.0349(11) 0.0299(10) -0.0132(8) -0.0057(8) -0.0104(9) C39 0.0294(10) 0.0281(9) 0.0302(10) -0.0057(8) -0.0046(8) -0.0122(8) C40 0.0367(12) 0.0342(11) 0.0422(12) -0.0142(9) -0.0069(9) -0.0090(9) C41 0.0323(12) 0.0422(13) 0.0616(16) -0.0182(12) -0.0068(11) -0.0063(10) C42 0.0364(14) 0.0636(18) 0.074(2) -0.0216(16) -0.0235(14) -0.0065(12) C43 0.0490(17) 0.081(2) 0.070(2) -0.0379(18) -0.0280(15) -0.0080(15) C44 0.0386(13) 0.0540(15) 0.0443(13) -0.0238(11) -0.0120(10) -0.0096(11) C45 0.0390(11) 0.0203(8) 0.0311(10) -0.0053(7) -0.0067(8) -0.0060(8) C46 0.0393(13) 0.0343(11) 0.0507(14) -0.0105(10) -0.0059(11) -0.0049(10) C47 0.0489(16) 0.0425(14) 0.0582(17) -0.0110(13) 0.0000(13) 0.0050(12) C48 0.080(2) 0.0262(11) 0.0490(15) -0.0090(11) 0.0078(14) 0.0005(12) C49 0.085(2) 0.0273(11) 0.0564(16) -0.0154(11) 0.0052(15) -0.0204(13) C50 0.0527(15) 0.0279(10) 0.0464(13) -0.0103(10) 0.0008(11) -0.0164(10) C51 0.0555(14) 0.0206(9) 0.0273(10) -0.0037(7) -0.0111(9) -0.0108(9) C52 0.097(3) 0.0307(12) 0.0512(16) 0.0034(11) -0.0432(16) -0.0189(14) C53 0.180(5) 0.0389(15) 0.058(2) 0.0044(15) -0.074(3) -0.026(2) C54 0.202(5) 0.0329(14) 0.0310(14) -0.0021(11) -0.024(2) -0.022(2) C55 0.125(3) 0.0337(14) 0.0411(16) -0.0050(12) 0.0215(19) -0.0162(17) C56 0.0640(18) 0.0321(11) 0.0352(12) -0.0032(9) 0.0053(11) -0.0099(11) O1 0.0665(19) 0.147(3) 0.176(4) -0.111(3) 0.002(2) -0.040(2) C57 0.062(2) 0.100(3) 0.117(4) -0.050(3) -0.024(2) -0.017(2) C58 0.073(3) 0.112(4) 0.113(4) -0.057(3) -0.037(3) 0.012(3) C59 0.064(2) 0.098(3) 0.110(3) -0.048(3) -0.031(2) 0.000(2) C60 0.073(3) 0.121(4) 0.122(4) -0.069(3) -0.005(3) -0.013(3) O2 0.230(6) 0.061(2) 0.136(4) -0.015(3) -0.124(4) -0.006(3) C61 0.230(6) 0.061(2) 0.136(4) -0.015(3) -0.124(4) -0.006(3) C62 0.230(6) 0.061(2) 0.136(4) -0.015(3) -0.124(4) -0.006(3) C63 0.230(6) 0.061(2) 0.136(4) -0.015(3) -0.124(4) -0.006(3) C64 0.230(6) 0.061(2) 0.136(4) -0.015(3) -0.124(4) -0.006(3) O2A 0.075(6) 0.075(6) 0.066(5) -0.011(5) -0.008(5) -0.031(5) C61A 0.075(6) 0.075(6) 0.066(5) -0.011(5) -0.008(5) -0.031(5) C62A 0.075(6) 0.075(6) 0.066(5) -0.011(5) -0.008(5) -0.031(5) C63A 0.075(6) 0.075(6) 0.066(5) -0.011(5) -0.008(5) -0.031(5) C64A 0.075(6) 0.075(6) 0.066(5) -0.011(5) -0.008(5) -0.031(5) O2B 0.068(6) 0.141(11) 0.114(9) -0.062(8) -0.001(5) -0.030(6) C61B 0.068(6) 0.141(11) 0.114(9) -0.062(8) -0.001(5) -0.030(6) C62B 0.068(6) 0.141(11) 0.114(9) -0.062(8) -0.001(5) -0.030(6) C63B 0.068(6) 0.141(11) 0.114(9) -0.062(8) -0.001(5) -0.030(6) C64B 0.068(6) 0.141(11) 0.114(9) -0.062(8) -0.001(5) -0.030(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N2 2.3607(18) . ? Sn1 N3 2.3973(16) . ? Sn1 N4 2.4573(17) . ? Sn1 N1 2.4643(18) . ? Sn1 Pd2 2.5945(2) . ? Sn1 Pd1 2.5946(2) . ? Pd1 S2 2.2960(6) . ? Pd1 S1 2.3085(5) . ? Pd1 P1 2.4139(5) . ? Pd2 S3 2.2989(5) . ? Pd2 S4 2.3017(6) . ? Pd2 P2 2.4033(5) . ? S1 C1 1.745(2) . ? S2 C6 1.735(2) . ? S3 C11 1.746(2) . ? S4 C16 1.733(2) . ? P1 C21 1.826(2) . ? P1 C33 1.829(2) . ? P1 C27 1.835(2) . ? P2 C39 1.822(2) . ? P2 C45 1.833(2) . ? P2 C51 1.838(2) . ? N1 C1 1.339(3) . ? N1 C5 1.355(3) . ? N2 C6 1.341(3) . ? N2 C10 1.352(3) . ? N3 C11 1.339(2) . ? N3 C15 1.352(3) . ? N4 C16 1.339(3) . ? N4 C20 1.354(3) . ? C1 C2 1.414(3) . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.412(3) . ? C7 C8 1.366(4) . ? C7 H7 0.9500 . ? C8 C9 1.392(4) . ? C8 H8 0.9500 . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.414(3) . ? C12 C13 1.372(3) . ? C12 H12 0.9500 . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.418(3) . ? C17 C18 1.367(3) . ? C17 H17 0.9500 . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.381(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.397(3) . ? C21 C26 1.400(3) . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(4) . ? C23 H23 0.9500 . ? C24 C25 1.381(4) . ? C24 H24 0.9500 . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.389(3) . ? C27 C28 1.394(3) . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 C31 1.372(4) . ? C30 H30 0.9500 . ? C31 C32 1.393(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.393(3) . ? C33 C38 1.398(3) . ? C34 C35 1.391(3) . ? C34 H34 0.9500 . ? C35 C36 1.385(4) . ? C35 H35 0.9500 . ? C36 C37 1.380(4) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.387(3) . ? C39 C40 1.400(3) . ? C40 C41 1.385(3) . ? C40 H40 0.9500 . ? C41 C42 1.382(4) . ? C41 H41 0.9500 . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 C44 1.394(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 C50 1.393(3) . ? C46 C47 1.397(4) . ? C46 H46 0.9500 . ? C47 C48 1.359(5) . ? C47 H47 0.9500 . ? C48 C49 1.372(5) . ? C48 H48 0.9500 . ? C49 C50 1.390(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.384(4) . ? C51 C56 1.385(4) . ? C52 C53 1.395(5) . ? C52 H52 0.9500 . ? C53 C54 1.361(7) . ? C53 H53 0.9500 . ? C54 C55 1.361(7) . ? C54 H54 0.9500 . ? C55 C56 1.401(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? O1 C57 1.400(5) . ? O1 C60 1.415(6) . ? C57 C58 1.424(6) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.516(6) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.470(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? O2 C61 1.376(5) . ? O2 C64 1.376(5) . ? C61 C62 1.399(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.398(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.398(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? O2A C64A 1.376(5) . ? O2A C61A 1.376(5) . ? C61A C62A 1.398(5) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C62A C63A 1.398(5) . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? C63A C64A 1.398(5) . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C64A H64C 0.9900 . ? C64A H64D 0.9900 . ? O2B C64B 1.376(5) . ? O2B C61B 1.376(5) . ? C61B C62B 1.399(5) . ? C61B H61E 0.9900 . ? C61B H61F 0.9900 . ? C62B C63B 1.399(5) . ? C62B H62E 0.9900 . ? C62B H62F 0.9900 . ? C63B C64B 1.399(5) . ? C63B H63E 0.9900 . ? C63B H63F 0.9900 . ? C64B H64E 0.9900 . ? C64B H64F 0.9900 . ? 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 N2 Sn1 N3 87.27(6) . . ? N2 Sn1 N4 84.30(6) . . ? N3 Sn1 N4 171.40(6) . . ? N2 Sn1 N1 174.90(6) . . ? N3 Sn1 N1 88.05(6) . . ? N4 Sn1 N1 100.44(6) . . ? N2 Sn1 Pd2 90.21(4) . . ? N3 Sn1 Pd2 91.89(4) . . ? N4 Sn1 Pd2 89.83(4) . . ? N1 Sn1 Pd2 87.95(4) . . ? N2 Sn1 Pd1 93.02(4) . . ? N3 Sn1 Pd1 91.88(4) . . ? N4 Sn1 Pd1 86.89(4) . . ? N1 Sn1 Pd1 89.13(4) . . ? Pd2 Sn1 Pd1 175.149(6) . . ? S2 Pd1 S1 179.33(2) . . ? S2 Pd1 P1 89.288(19) . . ? S1 Pd1 P1 90.175(19) . . ? S2 Pd1 Sn1 88.841(15) . . ? S1 Pd1 Sn1 91.666(14) . . ? P1 Pd1 Sn1 175.464(14) . . ? S3 Pd2 S4 175.60(2) . . ? S3 Pd2 P2 94.545(18) . . ? S4 Pd2 P2 84.714(19) . . ? S3 Pd2 Sn1 90.766(14) . . ? S4 Pd2 Sn1 90.671(15) . . ? P2 Pd2 Sn1 169.401(14) . . ? C1 S1 Pd1 114.97(7) . . ? C6 S2 Pd1 115.57(7) . . ? C11 S3 Pd2 116.00(7) . . ? C16 S4 Pd2 115.99(7) . . ? C21 P1 C33 105.66(9) . . ? C21 P1 C27 102.42(9) . . ? C33 P1 C27 102.23(9) . . ? C21 P1 Pd1 115.64(7) . . ? C33 P1 Pd1 113.25(7) . . ? C27 P1 Pd1 116.08(7) . . ? C39 P2 C45 107.32(10) . . ? C39 P2 C51 103.35(11) . . ? C45 P2 C51 100.60(10) . . ? C39 P2 Pd2 105.42(7) . . ? C45 P2 Pd2 115.42(7) . . ? C51 P2 Pd2 123.36(7) . . ? C1 N1 C5 119.69(18) . . ? C1 N1 Sn1 118.44(13) . . ? C5 N1 Sn1 121.12(15) . . ? C6 N2 C10 119.56(19) . . ? C6 N2 Sn1 117.64(14) . . ? C10 N2 Sn1 122.69(14) . . ? C11 N3 C15 119.29(17) . . ? C11 N3 Sn1 119.05(12) . . ? C15 N3 Sn1 121.66(13) . . ? C16 N4 C20 119.00(18) . . ? C16 N4 Sn1 118.48(14) . . ? C20 N4 Sn1 122.01(14) . . ? N1 C1 C2 120.38(19) . . ? N1 C1 S1 121.57(15) . . ? C2 C1 S1 118.03(17) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 117.8(2) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N2 C6 C7 120.1(2) . . ? N2 C6 S2 122.40(16) . . ? C7 C6 S2 117.50(17) . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.4(2) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 118.4(2) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? N2 C10 C9 122.6(2) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N3 C11 C12 120.16(18) . . ? N3 C11 S3 122.18(14) . . ? C12 C11 S3 117.66(15) . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.5(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.0(2) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N3 C15 C14 123.1(2) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N4 C16 C17 120.4(2) . . ? N4 C16 S4 121.39(15) . . ? C17 C16 S4 118.21(17) . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.5(2) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 118.5(2) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N4 C20 C19 122.8(2) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C22 C21 C26 118.3(2) . . ? C22 C21 P1 124.02(16) . . ? C26 C21 P1 117.55(16) . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.9(2) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C32 C27 C28 118.6(2) . . ? C32 C27 P1 122.64(18) . . ? C28 C27 P1 118.59(16) . . ? C29 C28 C27 120.9(2) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 119.7(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 119.9(2) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.5(2) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C27 C32 C31 120.3(3) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C38 119.04(19) . . ? C34 C33 P1 122.08(16) . . ? C38 C33 P1 118.88(16) . . ? C35 C34 C33 120.2(2) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 119.9(2) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.2(2) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.3(2) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C44 C39 C40 118.9(2) . . ? C44 C39 P2 123.34(18) . . ? C40 C39 P2 117.43(17) . . ? C41 C40 C39 120.8(2) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C42 C41 C40 119.9(2) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 119.7(3) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.9(3) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C39 C44 C43 119.8(2) . . ? C39 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C50 118.7(2) . . ? C46 C45 P2 118.24(18) . . ? C50 C45 P2 122.98(18) . . ? C45 C46 C47 119.9(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.5(3) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 120.5(2) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C48 C49 C50 119.9(3) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C45 120.5(3) . . ? C49 C50 H50 119.8 . . ? C45 C50 H50 119.8 . . ? C52 C51 C56 118.9(2) . . ? C52 C51 P2 117.3(2) . . ? C56 C51 P2 123.7(2) . . ? C51 C52 C53 119.9(4) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 121.0(4) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C55 C54 C53 119.5(3) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 120.9(4) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C51 C56 C55 119.7(3) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C57 O1 C60 106.7(3) . . ? O1 C57 C58 106.5(4) . . ? O1 C57 H57A 110.4 . . ? C58 C57 H57A 110.4 . . ? O1 C57 H57B 110.4 . . ? C58 C57 H57B 110.4 . . ? H57A C57 H57B 108.6 . . ? C57 C58 C59 104.4(4) . . ? C57 C58 H58A 110.9 . . ? C59 C58 H58A 110.9 . . ? C57 C58 H58B 110.9 . . ? C59 C58 H58B 110.9 . . ? H58A C58 H58B 108.9 . . ? C60 C59 C58 103.8(4) . . ? C60 C59 H59A 111.0 . . ? C58 C59 H59A 111.0 . . ? C60 C59 H59B 111.0 . . ? C58 C59 H59B 111.0 . . ? H59A C59 H59B 109.0 . . ? O1 C60 C59 107.5(4) . . ? O1 C60 H60A 110.2 . . ? C59 C60 H60A 110.2 . . ? O1 C60 H60B 110.2 . . ? C59 C60 H60B 110.2 . . ? H60A C60 H60B 108.5 . . ? C61 O2 C64 107.9(7) . . ? O2 C61 C62 107.4(7) . . ? O2 C61 H61A 110.2 . . ? C62 C61 H61A 110.2 . . ? O2 C61 H61B 110.2 . . ? C62 C61 H61B 110.2 . . ? H61A C61 H61B 108.5 . . ? C63 C62 C61 108.0(7) . . ? C63 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? C63 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? C62 C63 C64 105.0(8) . . ? C62 C63 H63A 110.7 . . ? C64 C63 H63A 110.7 . . ? C62 C63 H63B 110.7 . . ? C64 C63 H63B 110.7 . . ? H63A C63 H63B 108.8 . . ? O2 C64 C63 108.2(7) . . ? O2 C64 H64A 110.0 . . ? C63 C64 H64A 110.0 . . ? O2 C64 H64B 110.0 . . ? C63 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? C64A O2A C61A 119.1(18) . . ? O2A C61A C62A 99.6(16) . . ? O2A C61A H61C 111.9 . . ? C62A C61A H61C 111.9 . . ? O2A C61A H61D 111.9 . . ? C62A C61A H61D 111.9 . . ? H61C C61A H61D 109.6 . . ? C61A C62A C63A 103.2(17) . . ? C61A C62A H62C 111.1 . . ? C63A C62A H62C 111.1 . . ? C61A C62A H62D 111.1 . . ? C63A C62A H62D 111.1 . . ? H62C C62A H62D 109.1 . . ? C64A C63A C62A 111.2(18) . . ? C64A C63A H63C 109.4 . . ? C62A C63A H63C 109.4 . . ? C64A C63A H63D 109.4 . . ? C62A C63A H63D 109.4 . . ? H63C C63A H63D 108.0 . . ? O2A C64A C63A 90.4(16) . . ? O2A C64A H64C 113.6 . . ? C63A C64A H64C 113.6 . . ? O2A C64A H64D 113.6 . . ? C63A C64A H64D 113.6 . . ? H64C C64A H64D 110.8 . . ? C64B O2B C61B 97.6(19) . . ? O2B C61B C62B 102.7(18) . . ? O2B C61B H61E 111.2 . . ? C62B C61B H61E 111.2 . . ? O2B C61B H61F 111.2 . . ? C62B C61B H61F 111.2 . . ? H61E C61B H61F 109.1 . . ? C61B C62B C63B 92(2) . . ? C61B C62B H62E 113.3 . . ? C63B C62B H62E 113.3 . . ? C61B C62B H62F 113.3 . . ? C63B C62B H62F 113.3 . . ? H62E C62B H62F 110.6 . . ? C64B C63B C62B 108.9(19) . . ? C64B C63B H63E 109.9 . . ? C62B C63B H63E 109.9 . . ? C64B C63B H63F 109.9 . . ? C62B C63B H63F 109.9 . . ? H63E C63B H63F 108.3 . . ? O2B C64B C63B 103.2(16) . . ? O2B C64B H64E 111.1 . . ? C63B C64B H64E 111.1 . . ? O2B C64B H64F 111.1 . . ? C63B C64B H64F 111.1 . . ? H64E C64B H64F 109.1 . . ? 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 N2 Sn1 Pd1 S2 9.71(5) . . . . ? N3 Sn1 Pd1 S2 -77.65(4) . . . . ? N4 Sn1 Pd1 S2 93.83(5) . . . . ? N1 Sn1 Pd1 S2 -165.67(4) . . . . ? N2 Sn1 Pd1 S1 -169.85(5) . . . . ? N3 Sn1 Pd1 S1 102.79(4) . . . . ? N4 Sn1 Pd1 S1 -85.73(5) . . . . ? N1 Sn1 Pd1 S1 14.77(4) . . . . ? N2 Sn1 Pd2 S3 -85.46(5) . . . . ? N3 Sn1 Pd2 S3 1.81(4) . . . . ? N4 Sn1 Pd2 S3 -169.76(5) . . . . ? N1 Sn1 Pd2 S3 89.79(4) . . . . ? N2 Sn1 Pd2 S4 98.70(5) . . . . ? N3 Sn1 Pd2 S4 -174.03(5) . . . . ? N4 Sn1 Pd2 S4 14.40(5) . . . . ? N1 Sn1 Pd2 S4 -86.06(4) . . . . ? N2 Sn1 Pd2 P2 34.69(9) . . . . ? N3 Sn1 Pd2 P2 121.96(8) . . . . ? N4 Sn1 Pd2 P2 -49.61(9) . . . . ? N1 Sn1 Pd2 P2 -150.06(8) . . . . ? P1 Pd1 S1 C1 169.99(7) . . . . ? Sn1 Pd1 S1 C1 -14.15(7) . . . . ? P1 Pd1 S2 C6 160.36(8) . . . . ? Sn1 Pd1 S2 C6 -15.51(8) . . . . ? P2 Pd2 S3 C11 -171.72(8) . . . . ? Sn1 Pd2 S3 C11 -0.90(8) . . . . ? P2 Pd2 S4 C16 153.90(9) . . . . ? Sn1 Pd2 S4 C16 -16.55(9) . . . . ? S2 Pd1 P1 C21 136.02(7) . . . . ? S1 Pd1 P1 C21 -44.38(7) . . . . ? S2 Pd1 P1 C33 -101.85(8) . . . . ? S1 Pd1 P1 C33 77.75(8) . . . . ? S2 Pd1 P1 C27 15.99(8) . . . . ? S1 Pd1 P1 C27 -164.41(8) . . . . ? S3 Pd2 P2 C39 114.30(7) . . . . ? S4 Pd2 P2 C39 -70.06(7) . . . . ? Sn1 Pd2 P2 C39 -5.56(11) . . . . ? S3 Pd2 P2 C45 -127.47(8) . . . . ? S4 Pd2 P2 C45 48.18(8) . . . . ? Sn1 Pd2 P2 C45 112.68(10) . . . . ? S3 Pd2 P2 C51 -3.64(10) . . . . ? S4 Pd2 P2 C51 172.01(10) . . . . ? Sn1 Pd2 P2 C51 -123.49(11) . . . . ? N3 Sn1 N1 C1 -112.47(14) . . . . ? N4 Sn1 N1 C1 66.12(15) . . . . ? Pd2 Sn1 N1 C1 155.57(14) . . . . ? Pd1 Sn1 N1 C1 -20.56(14) . . . . ? N3 Sn1 N1 C5 77.45(16) . . . . ? N4 Sn1 N1 C5 -103.95(16) . . . . ? Pd2 Sn1 N1 C5 -14.51(16) . . . . ? Pd1 Sn1 N1 C5 169.37(16) . . . . ? N3 Sn1 N2 C6 87.11(16) . . . . ? N4 Sn1 N2 C6 -91.20(16) . . . . ? Pd2 Sn1 N2 C6 178.99(15) . . . . ? Pd1 Sn1 N2 C6 -4.63(15) . . . . ? N3 Sn1 N2 C10 -96.64(19) . . . . ? N4 Sn1 N2 C10 85.04(19) . . . . ? Pd2 Sn1 N2 C10 -4.76(19) . . . . ? Pd1 Sn1 N2 C10 171.62(18) . . . . ? N2 Sn1 N3 C11 86.56(15) . . . . ? N1 Sn1 N3 C11 -91.44(15) . . . . ? Pd2 Sn1 N3 C11 -3.56(15) . . . . ? Pd1 Sn1 N3 C11 179.50(14) . . . . ? N2 Sn1 N3 C15 -92.66(17) . . . . ? N1 Sn1 N3 C15 89.34(17) . . . . ? Pd2 Sn1 N3 C15 177.22(16) . . . . ? Pd1 Sn1 N3 C15 0.27(16) . . . . ? N2 Sn1 N4 C16 -106.80(16) . . . . ? N1 Sn1 N4 C16 71.31(17) . . . . ? Pd2 Sn1 N4 C16 -16.57(16) . . . . ? Pd1 Sn1 N4 C16 159.85(16) . . . . ? N2 Sn1 N4 C20 81.57(19) . . . . ? N1 Sn1 N4 C20 -100.32(19) . . . . ? Pd2 Sn1 N4 C20 171.80(18) . . . . ? Pd1 Sn1 N4 C20 -11.78(18) . . . . ? C5 N1 C1 C2 3.1(3) . . . . ? Sn1 N1 C1 C2 -167.17(14) . . . . ? C5 N1 C1 S1 -175.30(16) . . . . ? Sn1 N1 C1 S1 14.5(2) . . . . ? Pd1 S1 C1 N1 1.64(18) . . . . ? Pd1 S1 C1 C2 -176.75(13) . . . . ? N1 C1 C2 C3 -2.2(3) . . . . ? S1 C1 C2 C3 176.19(17) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 2.1(4) . . . . ? C1 N1 C5 C4 -1.3(3) . . . . ? Sn1 N1 C5 C4 168.66(18) . . . . ? C3 C4 C5 N1 -1.3(4) . . . . ? C10 N2 C6 C7 -2.2(3) . . . . ? Sn1 N2 C6 C7 174.16(17) . . . . ? C10 N2 C6 S2 176.93(18) . . . . ? Sn1 N2 C6 S2 -6.7(2) . . . . ? Pd1 S2 C6 N2 17.0(2) . . . . ? Pd1 S2 C6 C7 -163.83(16) . . . . ? N2 C6 C7 C8 2.4(4) . . . . ? S2 C6 C7 C8 -176.8(2) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 -2.4(4) . . . . ? C6 N2 C10 C9 -0.3(4) . . . . ? Sn1 N2 C10 C9 -176.5(2) . . . . ? C8 C9 C10 N2 2.7(4) . . . . ? C15 N3 C11 C12 2.0(3) . . . . ? Sn1 N3 C11 C12 -177.25(16) . . . . ? C15 N3 C11 S3 -177.07(16) . . . . ? Sn1 N3 C11 S3 3.7(2) . . . . ? Pd2 S3 C11 N3 -1.7(2) . . . . ? Pd2 S3 C11 C12 179.25(15) . . . . ? N3 C11 C12 C13 -2.5(3) . . . . ? S3 C11 C12 C13 176.61(19) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C12 C13 C14 C15 1.1(4) . . . . ? C11 N3 C15 C14 0.0(3) . . . . ? Sn1 N3 C15 C14 179.27(18) . . . . ? C13 C14 C15 N3 -1.6(4) . . . . ? C20 N4 C16 C17 1.1(3) . . . . ? Sn1 N4 C16 C17 -170.75(17) . . . . ? C20 N4 C16 S4 179.55(19) . . . . ? Sn1 N4 C16 S4 7.7(2) . . . . ? Pd2 S4 C16 N4 8.0(2) . . . . ? Pd2 S4 C16 C17 -173.55(16) . . . . ? N4 C16 C17 C18 0.1(4) . . . . ? S4 C16 C17 C18 -178.3(2) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C17 C18 C19 C20 1.0(4) . . . . ? C16 N4 C20 C19 -1.4(4) . . . . ? Sn1 N4 C20 C19 170.2(2) . . . . ? C18 C19 C20 N4 0.3(4) . . . . ? C33 P1 C21 C22 18.0(2) . . . . ? C27 P1 C21 C22 -88.7(2) . . . . ? Pd1 P1 C21 C22 144.07(17) . . . . ? C33 P1 C21 C26 -166.51(17) . . . . ? C27 P1 C21 C26 86.82(18) . . . . ? Pd1 P1 C21 C26 -40.41(18) . . . . ? C26 C21 C22 C23 -0.5(4) . . . . ? P1 C21 C22 C23 174.9(2) . . . . ? C21 C22 C23 C24 -1.8(4) . . . . ? C22 C23 C24 C25 1.9(5) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C24 C25 C26 C21 -2.5(4) . . . . ? C22 C21 C26 C25 2.7(3) . . . . ? P1 C21 C26 C25 -173.10(19) . . . . ? C21 P1 C27 C32 -22.9(2) . . . . ? C33 P1 C27 C32 -132.16(19) . . . . ? Pd1 P1 C27 C32 104.08(18) . . . . ? C21 P1 C27 C28 161.90(17) . . . . ? C33 P1 C27 C28 52.60(19) . . . . ? Pd1 P1 C27 C28 -71.16(18) . . . . ? C32 C27 C28 C29 -0.1(3) . . . . ? P1 C27 C28 C29 175.34(18) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? C28 C29 C30 C31 0.3(4) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C28 C27 C32 C31 0.1(4) . . . . ? P1 C27 C32 C31 -175.1(2) . . . . ? C30 C31 C32 C27 0.1(4) . . . . ? C21 P1 C33 C34 -73.7(2) . . . . ? C27 P1 C33 C34 33.1(2) . . . . ? Pd1 P1 C33 C34 158.75(18) . . . . ? C21 P1 C33 C38 106.74(18) . . . . ? C27 P1 C33 C38 -146.45(18) . . . . ? Pd1 P1 C33 C38 -20.8(2) . . . . ? C38 C33 C34 C35 -0.6(4) . . . . ? P1 C33 C34 C35 179.9(2) . . . . ? C33 C34 C35 C36 0.8(4) . . . . ? C34 C35 C36 C37 -0.7(4) . . . . ? C35 C36 C37 C38 0.3(4) . . . . ? C36 C37 C38 C33 0.0(4) . . . . ? C34 C33 C38 C37 0.1(3) . . . . ? P1 C33 C38 C37 179.72(19) . . . . ? C45 P2 C39 C44 -24.5(2) . . . . ? C51 P2 C39 C44 -130.3(2) . . . . ? Pd2 P2 C39 C44 99.0(2) . . . . ? C45 P2 C39 C40 161.84(17) . . . . ? C51 P2 C39 C40 56.06(19) . . . . ? Pd2 P2 C39 C40 -74.62(17) . . . . ? C44 C39 C40 C41 1.6(4) . . . . ? P2 C39 C40 C41 175.5(2) . . . . ? C39 C40 C41 C42 -0.5(4) . . . . ? C40 C41 C42 C43 -0.5(5) . . . . ? C41 C42 C43 C44 0.5(5) . . . . ? C40 C39 C44 C43 -1.6(4) . . . . ? P2 C39 C44 C43 -175.1(2) . . . . ? C42 C43 C44 C39 0.6(5) . . . . ? C39 P2 C45 C46 143.57(19) . . . . ? C51 P2 C45 C46 -108.7(2) . . . . ? Pd2 P2 C45 C46 26.4(2) . . . . ? C39 P2 C45 C50 -40.5(2) . . . . ? C51 P2 C45 C50 67.2(2) . . . . ? Pd2 P2 C45 C50 -157.69(18) . . . . ? C50 C45 C46 C47 0.5(4) . . . . ? P2 C45 C46 C47 176.6(2) . . . . ? C45 C46 C47 C48 1.0(5) . . . . ? C46 C47 C48 C49 -1.0(5) . . . . ? C47 C48 C49 C50 -0.5(5) . . . . ? C48 C49 C50 C45 2.1(5) . . . . ? C46 C45 C50 C49 -2.1(4) . . . . ? P2 C45 C50 C49 -178.0(2) . . . . ? C39 P2 C51 C52 -162.98(19) . . . . ? C45 P2 C51 C52 86.2(2) . . . . ? Pd2 P2 C51 C52 -44.1(2) . . . . ? C39 P2 C51 C56 20.3(2) . . . . ? C45 P2 C51 C56 -90.5(2) . . . . ? Pd2 P2 C51 C56 139.23(17) . . . . ? C56 C51 C52 C53 -0.6(4) . . . . ? P2 C51 C52 C53 -177.4(2) . . . . ? C51 C52 C53 C54 -0.3(5) . . . . ? C52 C53 C54 C55 0.7(5) . . . . ? C53 C54 C55 C56 -0.1(5) . . . . ? C52 C51 C56 C55 1.2(4) . . . . ? P2 C51 C56 C55 177.8(2) . . . . ? C54 C55 C56 C51 -0.8(4) . . . . ? C60 O1 C57 C58 -34.0(6) . . . . ? O1 C57 C58 C59 31.1(6) . . . . ? C57 C58 C59 C60 -16.8(6) . . . . ? C57 O1 C60 C59 22.5(6) . . . . ? C58 C59 C60 O1 -3.1(6) . . . . ? C64 O2 C61 C62 3.9(19) . . . . ? O2 C61 C62 C63 8.2(19) . . . . ? C61 C62 C63 C64 -16.7(19) . . . . ? C61 O2 C64 C63 -15(2) . . . . ? C62 C63 C64 O2 19.2(19) . . . . ? C64A O2A C61A C62A 14(3) . . . . ? O2A C61A C62A C63A 13(2) . . . . ? C61A C62A C63A C64A -36(3) . . . . ? C61A O2A C64A C63A -33(2) . . . . ? C62A C63A C64A O2A 40(2) . . . . ? C64B O2B C61B C62B 57(3) . . . . ? C64B O2B C61B C63B 21(2) . . . . ? O2B C61B C62B C63B -56(3) . . . . ? C61B C62B C63B C64B 35(4) . . . . ? O2B C61B C63B C64B -21(2) . . . . ? C62B C61B C63B C64B -145(4) . . . . ? O2B C61B C63B C62B 124(3) . . . . ? C61B O2B C64B C63B -31(3) . . . . ? C62B C63B C64B O2B -4(4) . . . . ? C61B C63B C64B O2B 21(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.731 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 963369'