# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/205 data_alpha-ET2[Pd(dto)2] _publ_section_title ; Formation of 2:1 Insulating Complexes of D+ED+EA2- Alternatin Stack and 4:1 Semimetallic Complex Using M(dto)2 Dianions@iM=Ni, Pd, Pt and dto = dithiooxalate) ; _publ_contact_author_name 'Gunzi Saito' _publ_contact_author_address 'saito@kuchem.kyoto-u.ac.jp' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_abstract ; We present the crystal and molecular structure of alpha-ET2[Pd(dto)2]. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using Crystan (MacScience, Japan). ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Block' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _chemical_formula_moiety 'C24 H16 O4 S20 Pd1 ' _chemical_formula_weight 1116.13 _cell_length_a 9.808(1) _cell_length_b 12.617(2) _cell_length_c 8.3870(9) _cell_angle_alpha 107.391(7) _cell_angle_beta 112.572(8) _cell_angle_gamma 78.912(6) _cell_volume 911.0(2) _cell_measurement_reflns_used '???' _cell_measurement_theta_min '1' _cell_measurement_theta_max '27.5' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_meas 2.0357 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.6413 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 3491 _reflns_number_total 3387 _reflns_number_observed 2895 _reflns_observed_criterion 'refl_observed_if_I_>_2.00_sigma(I)' _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.53 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.044 _refine_ls_wR_factor_obs 0.045 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 2895 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 1.478 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.3155 _refine_ls_shift/esd_mean 0.0472 _refine_diff_density_min -0.94 _refine_diff_density_max 1.67 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.06248 _diffrn_orient_matrix_UB_12 -0.10837 _diffrn_orient_matrix_UB_13 0.01487 _diffrn_orient_matrix_UB_21 -0.10689 _diffrn_orient_matrix_UB_22 -0.01968 _diffrn_orient_matrix_UB_23 -0.00259 _diffrn_orient_matrix_UB_31 0.04804 _diffrn_orient_matrix_UB_32 -0.00883 _diffrn_orient_matrix_UB_33 -0.08160 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.5990(7) 0.0085(5) -0.2533(9) 0.045(3) 1.000 Uij C10 0.6807(8) -0.0032(5) -0.0702(9) 0.052(3) 1.000 Uij C11 0.4718(6) 0.2056(4) -0.1077(8) 0.034(3) 1.000 Uij C12 0.5947(6) 0.2201(4) 0.0393(7) 0.032(2) 1.000 Uij C13 0.4326(6) 0.4063(5) 0.0693(7) 0.034(3) 1.000 Uij C14 0.3663(6) 0.5095(4) 0.1261(8) 0.033(3) 1.000 Uij C15 0.1725(6) 0.6761(5) 0.1483(8) 0.036(3) 1.000 Uij C16 0.2895(6) 0.7007(4) 0.3019(8) 0.032(2) 1.000 Uij C17 0.0466(8) 0.8841(7) 0.2308(11) 0.067(4) 1.000 Uij C18 0.1266(7) 0.8926(5) 0.4247(8) 0.040(3) 1.000 Uij C21 0.2237(6) 0.3091(5) 0.3493(8) 0.040(3) 1.000 Uij C22 0.1157(6) 0.2428(5) 0.3691(8) 0.036(3) 1.000 Uij O23 0.3276(5) 0.2577(4) 0.3076(8) 0.063(3) 1.000 Uij O24 0.1325(5) 0.1416(3) 0.3293(8) 0.061(3) 1.000 Uij S1 0.42230(18) 0.08730(13) -0.28380(22) 0.0449(8) 1.000 Uij S2 0.74840(19) 0.12390(13) 0.09730(21) 0.0452(8) 1.000 Uij S3 0.34340(15) 0.32020(12) -0.13440(20) 0.0367(7) 1.000 Uij S4 0.60370(15) 0.35170(11) 0.18950(19) 0.0331(6) 1.000 Uij S5 0.19370(16) 0.55410(12) -0.00610(20) 0.0381(7) 1.000 Uij S6 0.44410(14) 0.60320(11) 0.32590(19) 0.0314(6) 1.000 Uij S7 -0.00020(18) 0.75130(16) 0.08930(25) 0.0551(9) 1.000 Uij S8 0.30720(16) 0.81610(12) 0.48390(20) 0.0358(6) 1.000 Uij S19 0.18950(16) 0.45240(12) 0.38780(23) 0.0433(7) 1.000 Uij S20 -0.02630(18) 0.31510(12) 0.44280(26) 0.0496(8) 1.000 Uij Pd1 0.00000 0.50000 0.50000 0.0278(3) 0.500 Uij H9A 0.58350 -0.06750 -0.33560 0.05 1.000 Uiso H9B 0.66040 0.04630 -0.28570 0.05 1.000 Uiso H10A 0.76850 -0.05930 -0.07120 0.05 1.000 Uiso H10B 0.61290 -0.03190 -0.03280 0.05 1.000 Uiso H17A 0.09980 0.91000 0.18800 0.05 1.000 Uiso H17B -0.06040 0.93550 0.21530 0.05 1.000 Uiso H18A 0.04960 0.86420 0.46760 0.05 1.000 Uiso H18B 0.12530 0.97300 0.48760 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.038(3) 0.035(3) 0.043(4) 0.004(3) 0.011(3) -0.001(3) C10 0.058(4) 0.034(3) 0.048(4) 0.012(3) 0.021(3) 0.007(3) C11 0.030(3) 0.028(3) 0.034(3) 0.001(2) 0.011(2) 0.007(2) C12 0.033(3) 0.024(3) 0.030(3) 0.004(2) 0.010(2) 0.005(2) C13 0.026(3) 0.035(3) 0.031(3) -0.004(2) 0.010(2) 0.005(2) C14 0.026(3) 0.030(3) 0.035(3) 0.003(2) 0.010(2) 0.009(2) C15 0.028(3) 0.035(3) 0.034(3) 0.004(2) 0.011(2) 0.003(2) C16 0.032(3) 0.023(3) 0.035(3) 0.003(2) 0.016(2) 0.010(2) C17 0.048(4) 0.055(4) 0.071(5) 0.020(3) 0.011(4) 0.012(4) C18 0.035(3) 0.029(3) 0.042(3) 0.006(2) 0.012(3) 0.004(2) C21 0.035(3) 0.031(3) 0.042(4) -0.001(2) 0.010(3) 0.005(2) C22 0.027(3) 0.028(3) 0.040(3) -0.002(2) 0.002(2) 0.008(2) O23 0.041(3) 0.040(3) 0.090(4) 0.007(2) 0.036(3) 0.004(2) O24 0.049(3) 0.026(2) 0.090(4) 0.004(2) 0.029(3) 0.010(2) S1 0.0396(8) 0.0360(8) 0.0397(9) -.0051(7) 0.0064(7) -.0073(7) S2 0.0466(9) 0.0324(8) 0.0349(8) 0.0132(7) 0.0023(7) 0.0019(6) S3 0.0266(7) 0.0329(7) 0.0355(8) 0.0000(6) 0.0036(6) 0.0010(6) S4 0.0312(7) 0.0248(6) 0.0291(7) 0.0031(5) 0.0037(6) 0.0010(5) S5 0.0288(7) 0.0358(8) 0.0329(8) 0.0067(6) 0.0028(6) 0.0016(6) S6 0.0248(6) 0.0270(7) 0.0313(7) 0.0021(5) 0.0053(5) 0.0057(5) S7 0.0335(8) 0.0545(10) 0.0492(10) 0.0154(7) -.0004(7) -.0013(8) S8 0.0303(7) 0.0301(7) 0.0334(8) 0.0036(5) 0.0071(6) 0.0027(6) S19 0.0346(8) 0.0289(7) 0.0573(10) -.0014(6) 0.0256(7) 0.0071(7) S20 0.0415(9) 0.0244(7) 0.0717(12) -.0049(6) 0.0295(8) 0.0060(7) Pd1 0.0230(3) 0.0206(3) 0.0313(3) -.0025(2) 0.0087(2) 0.0034(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 C10 C9 S1 C11 49.8(5) . . . . yes S1 C9 C10 S2 -68.5(5) . . . . yes C9 C10 S2 C12 43.0(5) . . . . yes C12 C11 S1 C9 -17.7(6) . . . . yes S1 C11 C12 S2 2.0(4) . . . . yes S1 C11 C12 S4 -179.1(8) . . . . yes C12 C11 S3 C13 -5.4(5) . . . . yes S3 C11 C12 S2 -175.9(8) . . . . yes S3 C11 C12 S4 3.0(3) . . . . yes S3 C11 S1 C9 160.3(4) . . . . yes S1 C11 S3 C13 176.3(4) . . . . yes C11 C12 S2 C10 -9.8(6) . . . . yes C11 C12 S4 C13 1.1(5) . . . . yes S4 C12 S2 C10 171.2(4) . . . . yes S2 C12 S4 C13 -179.9(4) . . . . yes C14 C13 S3 C11 -173.3(5) . . . . yes S3 C13 C14 S5 -0.3(3) . . . . yes S3 C13 C14 S6 -179.7(7) . . . . yes C14 C13 S4 C12 174.5(6) . . . . yes S4 C13 C14 S5 -179.4(7) . . . . yes S4 C13 C14 S6 1.1(4) . . . . yes S4 C13 S3 C11 6.0(4) . . . . yes S3 C13 S4 C12 -4.7(4) . . . . yes C13 C14 S5 C15 174.5(5) . . . . yes C13 C14 S6 C16 -175.4(6) . . . . yes S6 C14 S5 C15 -6.0(4) . . . . yes S5 C14 S6 C16 5.2(4) . . . . yes C16 C15 S5 C14 4.8(5) . . . . yes S5 C15 C16 S6 -2.0(3) . . . . yes S5 C15 C16 S8 179.4(8) . . . . yes C16 C15 S7 C17 22.6(6) . . . . yes S7 C15 C16 S6 176.1(8) . . . . yes S7 C15 C16 S8 -2.5(4) . . . . yes S7 C15 S5 C14 -173.6(4) . . . . yes S5 C15 S7 C17 -159.3(5) . . . . yes C15 C16 S6 C14 -1.9(5) . . . . yes C15 C16 S8 C18 3.2(6) . . . . yes S8 C16 S6 C14 176.9(4) . . . . yes S6 C16 S8 C18 -175.4(4) . . . . yes C18 C17 S7 C15 -52.5(6) . . . . yes S7 C17 C18 S8 62.0(5) . . . . yes C17 C18 S8 C16 -31.7(5) . . . . yes O23 C21 C22 O24 -5.5(6) . . . . yes O23 C21 C22 S20 175.8(8) . . . . yes S19 C21 C22 O24 174.5(8) . . . . yes S19 C21 C22 S20 -4.3(4) . . . . yes C22 C21 S19 Pd1 8.1(4) . . . . yes O23 C21 S19 Pd1 -171.9(6) . . . . yes C21 C22 S20 Pd1 -2.0(4) . . . . yes O24 C22 S20 Pd1 179.2(6) . . . . yes C21 S19 Pd1 S20 -7.2(3) . . . . yes Pd1 S19 C21 C22 8.1(4) . . . . yes Pd1 S19 C21 O23 -171.9(6) . . . . yes C21 S19 Pd1 S20 -7.2(3) . . . . yes C22 S20 Pd1 S19 5.3(3) . . . . yes Pd1 S20 C22 C21 -2.0(4) . . . . yes Pd1 S20 C22 O24 179.2(6) . . . . yes C22 S20 Pd1 S19 5.3(3) . . . . yes S20 Pd1 S19 C21 172.8(3) . . . . yes S19 Pd1 S20 C22 -174.7(3) . . . . yes S1 C9 C10 H10A 170.0(8) . . . . yes S1 C9 C10 H10B 52.1(6) . . . . yes H9A C9 C10 S2 170.1(8) . . . . yes H9A C9 C10 H10A 48.6(6) . . . . yes H9A C9 C10 H10B -69.3(7) . . . . yes H9B C9 C10 S2 51.9(6) . . . . yes H9B C9 C10 H10A -69.6(7) . . . . yes H9B C9 C10 H10B 172.5(8) . . . . yes H9A C9 S1 C11 171.4(6) . . . . yes H9B C9 S1 C11 -70.6(5) . . . . yes H10A C10 S2 C12 164.8(6) . . . . yes H10B C10 S2 C12 -77.5(5) . . . . yes S7 C17 C18 H18A -61.5(6) . . . . yes S7 C17 C18 H18B -168.2(8) . . . . yes H17A C17 C18 S8 -60.2(7) . . . . yes H17A C17 C18 H18A 176.3(9) . . . . yes H17A C17 C18 H18B 69.6(8) . . . . yes H17B C17 C18 S8 -179.3(8) . . . . yes H17B C17 C18 H18A 57.2(6) . . . . yes H17B C17 C18 H18B -49.5(7) . . . . yes H17A C17 S7 C15 71.3(7) . . . . yes H17B C17 S7 C15 -172.7(6) . . . . yes H18A C18 S8 C16 87.9(5) . . . . yes H18B C18 S8 C16 -158.1(6) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.472(10) . . yes C9 S1 1.791(7) . . yes C10 S2 1.826(7) . . yes C11 C12 1.347(8) . . yes C11 S1 1.748(6) . . yes C11 S3 1.733(6) . . yes C12 S2 1.752(6) . . yes C12 S4 1.753(6) . . yes C13 C14 1.374(8) . . yes C13 S3 1.724(6) . . yes C13 S4 1.726(6) . . yes C14 S5 1.726(6) . . yes C14 S6 1.723(6) . . yes C15 C16 1.355(8) . . yes C15 S5 1.727(7) . . yes C15 S7 1.742(6) . . yes C16 S6 1.746(6) . . yes C16 S8 1.745(6) . . yes C17 C18 1.490(11) . . yes C17 S7 1.765(9) . . yes C18 S8 1.808(7) . . yes C21 C22 1.552(7) . . yes C21 O23 1.210(8) . . yes C21 S19 1.728(6) . . yes C22 O24 1.215(7) . . yes C22 S20 1.729(6) . . yes S19 Pd1 2.297(2) . . yes S19 Pd1 2.297(2) . 2_556 yes S20 Pd1 2.282(2) . . yes S20 Pd1 2.282(2) . 2_556 yes C9 H9A 0.999(7) . . yes C9 H9B 0.989(6) . . yes C10 H10A 1.005(8) . . yes C10 H10B 0.996(7) . . yes C17 H17A 0.887(7) . . yes C17 H17B 1.106(8) . . yes C18 H18A 1.104(6) . . yes C18 H18B 0.994(6) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 S1 114.5(5) . . . yes C9 C10 S2 116.1(5) . . . yes C12 C11 S1 129.5(5) . . . yes C12 C11 S3 117.0(5) . . . yes S1 C11 S3 113.5(4) . . . yes C11 C12 S2 127.9(5) . . . yes C11 C12 S4 116.3(4) . . . yes S2 C12 S4 115.8(4) . . . yes C14 C13 S3 120.2(5) . . . yes C14 C13 S4 124.7(5) . . . yes S3 C13 S4 115.1(4) . . . yes C13 C14 S5 120.3(5) . . . yes C13 C14 S6 124.6(5) . . . yes S5 C14 S6 115.1(3) . . . yes C16 C15 S5 116.8(5) . . . yes C16 C15 S7 127.7(5) . . . yes S5 C15 S7 115.5(4) . . . yes C15 C16 S6 116.4(5) . . . yes C15 C16 S8 129.0(5) . . . yes S6 C16 S8 114.5(4) . . . yes C18 C17 S7 118.0(6) . . . yes C17 C18 S8 116.0(5) . . . yes C22 C21 O23 118.3(5) . . . yes C22 C21 S19 118.4(4) . . . yes O23 C21 S19 123.4(5) . . . yes C21 C22 O24 118.7(5) . . . yes C21 C22 S20 119.0(4) . . . yes O24 C22 S20 122.2(5) . . . yes C9 S1 C11 100.4(3) . . . yes C10 S2 C12 101.0(3) . . . yes C11 S3 C13 95.8(3) . . . yes C12 S4 C13 95.5(3) . . . yes C14 S5 C15 95.9(3) . . . yes C14 S6 C16 95.4(3) . . . yes C15 S7 C17 100.0(4) . . . yes C16 S8 C18 103.2(3) . . . yes C21 S19 Pd1 106.3(2) . . . yes C21 S19 Pd1 106.3(2) . . 2_556 yes C22 S20 Pd1 106.5(2) . . . yes C22 S20 Pd1 106.5(2) . . 2_556 yes S19 Pd1 S19 180.0 . . 2_556 yes S19 Pd1 S20 89.2(1) . . . yes S19 Pd1 S20 90.8(1) . . 2_556 yes S19 Pd1 S20 90.8(1) 2_556 . . yes S19 Pd1 S20 89.2(1) 2_556 . 2_556 yes S20 Pd1 S20 180.0 . . 2_556 yes C10 C9 H9A 108.7(6) . . . yes C10 C9 H9B 108.1(6) . . . yes S1 C9 H9A 108.4(5) . . . yes S1 C9 H9B 108.0(5) . . . yes H9A C9 H9B 109.0(6) . . . yes C9 C10 H10A 108.4(6) . . . yes C9 C10 H10B 107.5(6) . . . yes S2 C10 H10A 107.8(6) . . . yes S2 C10 H10B 107.7(6) . . . yes H10A C10 H10B 109.2(6) . . . yes C18 C17 H17A 109.6(7) . . . yes C18 C17 H17B 107.9(7) . . . yes S7 C17 H17A 106.6(7) . . . yes S7 C17 H17B 105.0(6) . . . yes H17A C17 H17B 109.4(8) . . . yes C17 C18 H18A 104.4(6) . . . yes C17 C18 H18B 107.6(6) . . . yes S8 C18 H18A 111.7(5) . . . yes S8 C18 H18B 114.5(5) . . . yes H18A C18 H18B 101.0(5) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 C9 3.795(9) 1_555 2_654 ? C9 C17 3.887(9) 1_555 2_665 ? C9 C22 3.957(9) 1_555 2_655 ? C9 O23 3.227(7) 1_555 2_655 ? C9 O24 3.095(8) 1_555 2_655 ? C9 S1 3.640(7) 1_555 2_654 ? C9 S8 3.684(6) 1_555 1_544 ? C9 S8 3.767(6) 1_555 2_665 ? C9 H17A 3.110(6) 1_555 2_665 ? C10 C17 3.81(1) 1_555 1_645 ? C10 O23 3.230(8) 1_555 2_655 ? C10 O24 3.269(9) 1_555 2_655 ? C10 H17B 2.909(7) 1_555 1_645 ? C11 C16 3.831(7) 1_555 2_665 ? C11 S6 3.796(5) 1_555 2_665 ? C11 H10B 3.143(5) 1_555 2_655 ? C12 C15 3.814(7) 1_555 2_665 ? C12 C16 3.888(7) 1_555 2_665 ? C12 S8 3.885(5) 1_555 2_666 ? C13 C13 3.566(7) 1_555 2_665 ? C13 C14 3.469(7) 1_555 2_665 ? C14 C14 3.889(7) 1_555 2_665 ? C14 S3 3.852(5) 1_555 2_665 ? C14 S4 3.705(5) 1_555 2_665 ? C17 O24 3.296(8) 1_555 1_565 ? C17 S2 3.882(8) 1_555 1_465 ? C17 H9B 2.992(7) 1_555 2_665 ? C17 H10A 3.065(8) 1_555 1_465 ? C18 C18 3.589(9) 1_555 2_576 ? C18 S1 3.759(6) 1_555 1_566 ? C18 S2 3.774(6) 1_555 2_666 ? C18 S20 3.556(5) 1_555 2_566 ? C18 H9B 3.057(5) 1_555 2_665 ? C18 H18B 2.926(6) 1_555 2_576 ? C21 S6 3.469(6) 1_555 2_666 ? C21 S7 3.420(6) 1_555 2_565 ? C21 Pd1 3.239(6) 1_555 2_566 ? C22 S2 3.762(6) 1_555 1_455 ? C22 S3 3.814(6) 1_555 1_556 ? C22 S7 3.587(6) 1_555 2_565 ? C22 Pd1 3.230(6) 1_555 2_566 ? C22 H18A 3.159(5) 1_555 2_566 ? O23 S6 3.247(5) 1_555 2_666 ? O23 H9A 2.439(4) 1_555 2_655 ? O24 H10A 2.567(5) 1_555 2_655 ? S1 S8 3.548(2) 1_555 1_544 ? S1 H10B 3.093(2) 1_555 2_655 ? S2 S8 3.596(2) 1_555 2_666 ? S2 S20 3.472(2) 1_555 1_655 ? S2 H17B 2.901(2) 1_555 1_645 ? S3 S6 3.483(2) 1_555 2_665 ? S3 Pd1 4.380(1) 1_555 1_554 ? S3 Pd1 4.380(1) 1_555 2_565 ? S4 S5 3.475(2) 1_555 2_665 ? S4 S8 3.697(2) 1_555 2_666 ? S4 S19 3.736(2) 1_555 2_666 ? S4 S20 3.452(2) 1_555 1_655 ? S4 Pd1 4.184(1) 1_555 1_655 ? S4 Pd1 4.184(1) 1_555 2_666 ? S5 Pd1 3.742(2) 1_555 1_554 ? S5 Pd1 3.742(2) 1_555 2_565 ? S6 S19 3.548(2) 1_555 2_666 ? S8 S20 3.791(2) 1_555 2_566 ? S8 H9A 2.974(1) 1_555 1_566 ? S8 H9B 2.867(1) 1_555 2_665 ? S19 S20 3.261(2) 1_555 2_566 ? S20 H18A 2.661(1) 1_555 2_566 ? H9B H17A 2.2927 1_555 2_665 ? H10A H17B 2.3560 1_555 1_645 ? C9 C9 3.795(9) 1_555 2_654 ? C9 C17 3.887(9) 1_555 2_665 ? C9 C22 3.957(9) 1_555 2_655 ? C9 O23 3.227(7) 1_555 2_655 ? C9 O24 3.095(8) 1_555 2_655 ? C9 S1 3.640(7) 1_555 2_654 ? C9 S8 3.684(6) 1_555 1_544 ? C9 S8 3.767(6) 1_555 2_665 ? C9 H17A 3.110(6) 1_555 2_665 ? C10 C17 3.81(1) 1_555 1_645 ? C10 O23 3.230(8) 1_555 2_655 ? C10 O24 3.269(9) 1_555 2_655 ? C10 H17B 2.909(7) 1_555 1_645 ? C11 C16 3.831(7) 1_555 2_665 ? C11 S6 3.796(5) 1_555 2_665 ? C11 H10B 3.143(5) 1_555 2_655 ? C12 C15 3.814(7) 1_555 2_665 ? C12 C16 3.888(7) 1_555 2_665 ? C12 S8 3.885(5) 1_555 2_666 ? C13 C13 3.566(7) 1_555 2_665 ? C13 C14 3.469(7) 1_555 2_665 ? C14 C14 3.889(7) 1_555 2_665 ? C14 S3 3.852(5) 1_555 2_665 ? C14 S4 3.705(5) 1_555 2_665 ? C17 O24 3.296(8) 1_555 1_565 ? C17 S2 3.882(8) 1_555 1_465 ? C17 H9B 2.992(7) 1_555 2_665 ? C17 H10A 3.065(8) 1_555 1_465 ? C18 C18 3.589(9) 1_555 2_576 ? C18 S1 3.759(6) 1_555 1_566 ? C18 S2 3.774(6) 1_555 2_666 ? C18 S20 3.556(5) 1_555 2_566 ? C18 H9B 3.057(5) 1_555 2_665 ? C18 H18B 2.926(6) 1_555 2_576 ? C21 S6 3.469(6) 1_555 2_666 ? C21 S7 3.420(6) 1_555 2_565 ? C21 Pd1 3.239(6) 1_555 2_566 ? C22 S2 3.762(6) 1_555 1_455 ? C22 S3 3.814(6) 1_555 1_556 ? C22 S7 3.587(6) 1_555 2_565 ? C22 Pd1 3.230(6) 1_555 2_566 ? C22 H18A 3.159(5) 1_555 2_566 ? O23 S6 3.247(5) 1_555 2_666 ? O23 H9A 2.439(4) 1_555 2_655 ? O24 H10A 2.567(5) 1_555 2_655 ? S1 S8 3.548(2) 1_555 1_544 ? S1 H10B 3.093(2) 1_555 2_655 ? S2 S8 3.596(2) 1_555 2_666 ? S2 S20 3.472(2) 1_555 1_655 ? S2 H17B 2.901(2) 1_555 1_645 ? S3 S6 3.483(2) 1_555 2_665 ? S3 Pd1 4.380(1) 1_555 1_554 ? S3 Pd1 4.380(1) 1_555 2_565 ? S4 S5 3.475(2) 1_555 2_665 ? S4 S8 3.697(2) 1_555 2_666 ? S4 S19 3.736(2) 1_555 2_666 ? S4 S20 3.452(2) 1_555 1_655 ? S4 Pd1 4.184(1) 1_555 1_655 ? S4 Pd1 4.184(1) 1_555 2_666 ? S5 Pd1 3.742(2) 1_555 1_554 ? S5 Pd1 3.742(2) 1_555 2_565 ? S6 S19 3.548(2) 1_555 2_666 ? S8 S20 3.791(2) 1_555 2_566 ? S8 H9A 2.974(1) 1_555 1_566 ? S8 H9B 2.867(1) 1_555 2_665 ? S19 S20 3.261(2) 1_555 2_566 ? S20 H18A 2.661(1) 1_555 2_566 ? H9B H17A 2.2927 1_555 2_665 ? H10A H17B 2.3560 1_555 1_645 ? #===END data_beta-ET2[Pd(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.01 _chemical_formula_moiety 'C24 H16 O4 S20 Pd1 ' _chemical_formula_weight 1116.13 _cell_length_a 14.000(3) _cell_length_b 9.843(2) _cell_length_c 13.640(3) _cell_angle_alpha 90.000000(0) _cell_angle_beta 100.10(3) _cell_angle_gamma 90.000000(0) _cell_volume 1850.6(7) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '35' _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_meas 2.030 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 1.616 _diffrn_ambient_temperature 298 _cell_measurement_temperature 298 _exptl_cryst_F_000 1115.95 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 4616 _reflns_number_total 4369 _reflns_number_observed 1808 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents ??? _diffrn_reflns_theta_max 21.91 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.067 _refine_ls_wR_factor_obs 0.100 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 1808 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 5.990 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.3224 _refine_ls_shift/esd_mean 0.0158 _refine_diff_density_min -0.98 _refine_diff_density_max 1.18 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _atom_sites_solution_primary 'direct' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X,+Y+0.5,-Z+0.5 +X,-Y+0.5,+Z+0.5 _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting 'Monoclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.022(2) 0.091(3) 0.658(3) 0.10(2) 1.000 Uij C10 0.022(3) -0.033(4) 0.660(4) 0.14(3) 1.000 Uij C11 0.2050(14) 0.0846(21) 0.7673(16) 0.04(1) 1.000 Uij C12 0.2007(15) -0.0505(22) 0.7567(17) 0.04(1) 1.000 Uij C13 0.3798(13) 0.0177(18) 0.8266(12) 0.03(1) 1.000 Uij C14 0.4775(12) 0.0193(18) 0.8618(13) 0.03(1) 1.000 Uij C15 0.6539(14) 0.0915(19) 0.9261(15) 0.03(1) 1.000 Uij C16 0.6571(13) -0.0477(19) 0.9192(14) 0.029(9) 1.000 Uij C17 0.8506(17) 0.0956(28) 0.9922(18) 0.06(1) 1.000 Uij C18 0.8515(14) -0.0270(25) 0.9261(18) 0.06(1) 1.000 Uij C21 0.7324(13) -0.0250(17) 0.5288(14) 0.03(1) 1.000 Uij C22 0.7157(15) 0.0313(21) 0.6323(15) 0.04(1) 1.000 Uij O23 0.8176(10) -0.0349(16) 0.5176(12) 0.057(9) 1.000 Uij O24 0.7836(10) 0.0602(20) 0.6941(11) 0.07(1) 1.000 Uij S1 0.1013(5) 0.1909(7) 0.7442(6) 0.067(4) 1.000 Uij S2 0.1054(4) -0.1558(6) 0.7163(5) 0.056(3) 1.000 Uij S3 0.3131(4) 0.1650(5) 0.8094(5) 0.042(3) 1.000 Uij S4 0.3162(4) -0.1312(5) 0.7907(4) 0.037(3) 1.000 Uij S5 0.5414(4) 0.1665(5) 0.8948(4) 0.036(3) 1.000 Uij S6 0.5461(3) -0.1303(5) 0.8787(4) 0.034(3) 1.000 Uij S7 0.7483(4) 0.2030(5) 0.9642(5) 0.047(3) 1.000 Uij S8 0.7588(4) -0.1533(5) 0.9434(5) 0.045(3) 1.000 Uij S19 0.6364(3) -0.0474(6) 0.4346(4) 0.041(3) 1.000 Uij S20 0.5959(3) 0.0377(6) 0.6522(3) 0.039(3) 1.000 Uij Pd1 0.50000 0.00000 0.50000 0.026(1) 0.500 Uij H10A 0.02280 -0.05160 0.58820 0.05 1.000 Uiso H10B -0.04180 -0.06150 0.67630 0.05 1.000 Uiso H9A -0.04490 0.11460 0.66970 0.05 1.000 Uiso H9B 0.02940 0.12440 0.59050 0.05 1.000 Uiso H17A 0.90980 0.15080 0.98870 0.05 1.000 Uiso H17B 0.85400 0.06170 1.06190 0.05 1.000 Uiso H18A 0.91670 -0.07120 0.94100 0.05 1.000 Uiso H18B 0.83930 0.00440 0.85530 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.07(2) 0.08(2) 0.14(3) 0.06(2) -0.03(2) -0.02(2) C10 0.10(3) 0.07(2) 0.22(5) -0.02(2) -0.12(3) 0.06(3) C11 0.02(1) 0.05(1) 0.05(1) 0.00(1) 0.00(1) 0.00(1) C12 0.03(1) 0.04(1) 0.06(1) 0.01(1) 0.01(1) -0.01(1) C13 0.04(1) 0.02(1) 0.03(1) 0.01(1) 0.00(1) 0.00(1) C14 0.027(9) 0.022(9) 0.039(10) -0.004(8) 0.011(8) -0.002(9) C15 0.03(1) 0.03(1) 0.04(1) -0.01(1) 0.00(1) 0.00(1) C16 0.02(1) 0.04(1) 0.03(1) 0.00(1) 0.00(1) -0.01(1) C17 0.05(1) 0.08(2) 0.05(1) 0.00(1) 0.00(1) 0.01(1) C18 0.02(1) 0.07(2) 0.08(2) -0.02(1) 0.00(1) -0.01(1) C21 0.03(1) 0.02(1) 0.04(1) 0.01(1) 0.00(1) 0.00(1) C22 0.05(1) 0.04(1) 0.04(1) 0.02(1) 0.01(1) 0.00(1) O23 0.026(8) 0.068(11) 0.074(10) 0.011(7) 0.005(7) -0.019(9) O24 0.031(8) 0.123(16) 0.046(9) -0.012(9) -0.018(7) -0.024(10) S1 0.038(4) 0.062(4) 0.097(6) 0.021(3) 0.006(4) -0.014(4) S2 0.028(3) 0.051(4) 0.084(5) -0.005(3) 0.003(3) 0.006(3) S3 0.036(3) 0.030(3) 0.060(4) 0.007(2) 0.008(3) 0.005(3) S4 0.028(3) 0.034(3) 0.048(3) 0.002(2) 0.002(2) -0.002(2) S5 0.034(3) 0.028(3) 0.045(3) 0.000(2) 0.004(2) -0.002(2) S6 0.028(3) 0.028(3) 0.045(3) 0.002(2) 0.001(2) -0.006(2) S7 0.039(3) 0.037(3) 0.061(4) -0.010(2) 0.000(3) -0.004(3) S8 0.034(3) 0.035(3) 0.063(4) 0.004(2) 0.004(3) -0.003(3) S19 0.032(3) 0.054(3) 0.037(3) 0.000(2) 0.011(2) -0.009(2) S20 0.031(3) 0.051(3) 0.032(3) -0.005(2) 0.002(2) -0.005(2) Pd1 0.024(1) 0.026(1) 0.028(1) -0.001(1) 0.003(1) -0.003(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 C10 C9 S1 C11 32.3(33) . . . . yes S1 C9 C10 S2 -17.1(28) . . . . yes C9 C10 S2 C12 -8.6(44) . . . . yes C12 C11 S1 C9 -25.8(21) . . . . yes S1 C11 C12 S2 3.1(14) . . . . yes S1 C11 C12 S4 -177.3(25) . . . . yes C12 C11 S3 C13 -2.0(19) . . . . yes S3 C11 C12 S2 -179.4(32) . . . . yes S3 C11 C12 S4 0.1(12) . . . . yes S3 C11 S1 C9 156.6(17) . . . . yes S1 C11 S3 C13 175.6(14) . . . . yes C11 C12 S2 C10 15.8(25) . . . . yes C11 C12 S4 C13 1.8(17) . . . . yes S4 C12 S2 C10 -163.8(19) . . . . yes S2 C12 S4 C13 -178.5(14) . . . . yes C14 C13 S3 C11 -179.8(17) . . . . yes S3 C13 C14 S5 1.7(11) . . . . yes S3 C13 C14 S6 -179.5(23) . . . . yes C14 C13 S4 C12 179.8(18) . . . . yes S4 C13 C14 S5 178.5(23) . . . . yes S4 C13 C14 S6 -2.8(10) . . . . yes S4 C13 S3 C11 3.2(12) . . . . yes S3 C13 S4 C12 -3.2(12) . . . . yes C13 C14 S5 C15 -178.2(18) . . . . yes C13 C14 S6 C16 178.4(17) . . . . yes S6 C14 S5 C15 3.0(11) . . . . yes S5 C14 S6 C16 -2.8(11) . . . . yes C16 C15 S5 C14 -2.0(16) . . . . yes S5 C15 C16 S6 0.4(11) . . . . yes S5 C15 C16 S8 178.9(25) . . . . yes C16 C15 S7 C17 0.1(19) . . . . yes S7 C15 C16 S6 179.3(25) . . . . yes S7 C15 C16 S8 -2.2(12) . . . . yes S7 C15 S5 C14 178.9(13) . . . . yes S5 C15 S7 C17 179.0(15) . . . . yes C15 C16 S6 C14 1.5(16) . . . . yes C15 C16 S8 C18 -22.6(19) . . . . yes S8 C16 S6 C14 -177.3(12) . . . . yes S6 C16 S8 C18 155.9(13) . . . . yes C18 C17 S7 C15 36.1(18) . . . . yes S7 C17 C18 S8 -68.8(17) . . . . yes C17 C18 S8 C16 56.1(17) . . . . yes O23 C21 C22 O24 -0.6(19) . . . . yes O23 C21 C22 S20 -176.7(23) . . . . yes S19 C21 C22 O24 -172.1(26) . . . . yes S19 C21 C22 S20 11.8(11) . . . . yes C22 C21 S19 Pd1 -5.0(13) . . . . yes O23 C21 S19 Pd1 -175.8(18) . . . . yes C21 C22 S20 Pd1 -11.8(13) . . . . yes O24 C22 S20 Pd1 172.2(21) . . . . yes C21 S19 Pd1 S20 -1.8(7) . . . . yes Pd1 S19 C21 C22 -5.0(13) . . . . yes Pd1 S19 C21 O23 -175.8(18) . . . . yes C21 S19 Pd1 S20 -1.8(7) . . . . yes C22 S20 Pd1 S19 7.1(8) . . . . yes Pd1 S20 C22 C21 -11.8(13) . . . . yes Pd1 S20 C22 O24 172.2(21) . . . . yes C22 S20 Pd1 S19 7.1(8) . . . . yes S20 Pd1 S19 C21 178.2(7) . . . . yes S19 Pd1 S20 C22 -172.9(8) . . . . yes S1 C9 C10 H10A -131.8(43) . . . . yes S1 C9 C10 H10B 114.9(44) . . . . yes H9A C9 C10 S2 -135.2(54) . . . . yes H9A C9 C10 H10A 110.1(37) . . . . yes H9A C9 C10 H10B -3.1(32) . . . . yes H9B C9 C10 S2 108.5(52) . . . . yes H9B C9 C10 H10A -6.2(31) . . . . yes H9B C9 C10 H10B -119.4(44) . . . . yes H9A C9 S1 C11 149.3(26) . . . . yes H9B C9 S1 C11 -95.2(25) . . . . yes H10A C10 S2 C12 105.7(28) . . . . yes H10B C10 S2 C12 -141.2(30) . . . . yes S7 C17 C18 H18A 170.5(28) . . . . yes S7 C17 C18 H18B 51.9(19) . . . . yes H17A C17 C18 S8 169.4(27) . . . . yes H17A C17 C18 H18A 48.6(23) . . . . yes H17A C17 C18 H18B -70.0(24) . . . . yes H17B C17 C18 S8 51.9(19) . . . . yes H17B C17 C18 H18A -68.8(24) . . . . yes H17B C17 C18 H18B 172.6(29) . . . . yes H17A C17 S7 C15 157.9(21) . . . . yes H17B C17 S7 C15 -84.3(19) . . . . yes H18A C18 S8 C16 177.2(19) . . . . yes H18B C18 S8 C16 -64.1(18) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.22(5) . . yes C9 S1 1.77(4) . . yes C10 S2 1.76(4) . . yes C11 C12 1.34(3) . . yes C11 S1 1.77(3) . . yes C11 S3 1.72(3) . . yes C12 S2 1.70(3) . . yes C12 S4 1.79(3) . . yes C13 C14 1.37(3) . . yes C13 S3 1.718(19) . . yes C13 S4 1.740(19) . . yes C14 S5 1.721(19) . . yes C14 S6 1.751(19) . . yes C15 C16 1.37(3) . . yes C15 S5 1.72(3) . . yes C15 S7 1.73(2) . . yes C16 S6 1.755(19) . . yes C16 S8 1.747(19) . . yes C17 C18 1.51(4) . . yes C17 S7 1.77(3) . . yes C18 S8 1.84(3) . . yes C21 C22 1.57(3) . . yes C21 O23 1.23(3) . . yes C21 S19 1.703(19) . . yes C22 O24 1.19(3) . . yes C22 S20 1.75(3) . . yes S19 Pd1 2.293(5) . . yes S19 Pd1 2.293(5) . 2_656 yes S20 Pd1 2.296(5) . . yes S20 Pd1 2.296(5) . 2_656 yes C9 H9A 1.00(4) . . yes C9 H9B 1.00(4) . . yes C10 H10A 1.00(5) . . yes C10 H10B 1.00(4) . . yes C17 H17A 1.00(3) . . yes C17 H17B 1.00(3) . . yes C18 H18A 1.00(3) . . yes C18 H18B 1.00(3) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 S1 122.6(32) . . . yes C9 C10 S2 134.3(33) . . . yes C12 C11 S1 123.2(16) . . . yes C12 C11 S3 121.0(16) . . . yes S1 C11 S3 115.7(12) . . . yes C11 C12 S2 131.1(17) . . . yes C11 C12 S4 113.1(16) . . . yes S2 C12 S4 115.8(13) . . . yes C14 C13 S3 121.6(15) . . . yes C14 C13 S4 122.6(15) . . . yes S3 C13 S4 115.7(10) . . . yes C13 C14 S5 122.9(14) . . . yes C13 C14 S6 121.9(14) . . . yes S5 C14 S6 115.2(10) . . . yes C16 C15 S5 116.7(15) . . . yes C16 C15 S7 128.5(16) . . . yes S5 C15 S7 114.8(11) . . . yes C15 C16 S6 116.5(14) . . . yes C15 C16 S8 128.0(15) . . . yes S6 C16 S8 115.5(11) . . . yes C18 C17 S7 116.2(17) . . . yes C17 C18 S8 112.6(16) . . . yes C22 C21 O23 116.0(17) . . . yes C22 C21 S19 120.1(14) . . . yes O23 C21 S19 123.3(15) . . . yes C21 C22 O24 119.6(18) . . . yes C21 C22 S20 116.8(14) . . . yes O24 C22 S20 123.5(17) . . . yes C9 S1 C11 101.1(13) . . . yes C10 S2 C12 98.2(15) . . . yes C11 S3 C13 94.8(10) . . . yes C12 S4 C13 95.4(10) . . . yes C14 S5 C15 96.6(9) . . . yes C14 S6 C16 95.0(9) . . . yes C15 S7 C17 103.5(11) . . . yes C16 S8 C18 98.2(10) . . . yes C21 S19 Pd1 106.3(7) . . . yes C21 S19 Pd1 106.3(7) . . 2_656 yes C22 S20 Pd1 106.2(7) . . . yes C22 S20 Pd1 106.2(7) . . 2_656 yes S19 Pd1 S19 180.0 . . 2_656 yes S19 Pd1 S20 89.4(2) . . . yes S19 Pd1 S20 90.6(2) . . 2_656 yes S19 Pd1 S20 90.6(2) 2_656 . . yes S19 Pd1 S20 89.4(2) 2_656 . 2_656 yes S20 Pd1 S20 180.0 . . 2_656 yes C10 C9 H9A 103.1(31) . . . yes C10 C9 H9B 110.3(37) . . . yes S1 C9 H9A 105.3(25) . . . yes S1 C9 H9B 105.9(24) . . . yes H9A C9 H9B 109.0(31) . . . yes C9 C10 H10A 99.4(38) . . . yes C9 C10 H10B 106.6(34) . . . yes S2 C10 H10A 100.4(26) . . . yes S2 C10 H10B 105.0(29) . . . yes H10A C10 H10B 109.1(39) . . . yes C18 C17 H17A 108.2(21) . . . yes C18 C17 H17B 107.3(24) . . . yes S7 C17 H17A 108.2(21) . . . yes S7 C17 H17B 107.8(18) . . . yes H17A C17 H17B 109.0(22) . . . yes C17 C18 H18A 109.3(21) . . . yes C17 C18 H18B 108.2(22) . . . yes S8 C18 H18A 108.6(19) . . . yes S8 C18 H18B 109.1(17) . . . yes H18A C18 H18B 109.0(20) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 O23 3.38(3) 1_555 1_455 ? C9 S2 3.66(3) 1_555 3_556 ? C10 O23 3.17(4) 1_555 1_455 ? C10 S1 3.59(4) 1_555 3_546 ? C11 C17 3.93(3) 1_555 2_657 ? C11 S19 3.85(2) 1_555 2_656 ? C11 H17B 2.98(2) 1_555 2_657 ? C12 C17 3.65(3) 1_555 2_657 ? C12 S19 3.88(2) 1_555 2_656 ? C12 H17B 2.72(2) 1_555 2_657 ? C13 C15 3.65(3) 1_555 2_657 ? C13 C16 3.61(2) 1_555 2_657 ? C13 S19 3.54(2) 1_555 2_656 ? C14 C14 3.73(2) 1_555 2_657 ? C14 C15 3.85(3) 1_555 2_657 ? C14 C16 3.81(2) 1_555 2_657 ? C14 S5 3.84(2) 1_555 2_657 ? C14 S6 3.77(2) 1_555 2_657 ? C15 S4 3.83(2) 1_555 2_657 ? C16 S3 3.83(2) 1_555 2_657 ? C17 S2 3.88(3) 1_555 3_656 ? C18 S1 3.75(3) 1_555 3_646 ? C21 S3 3.88(2) 1_555 3_646 ? C21 S7 3.31(2) 1_555 4_565 ? C21 S8 3.42(2) 1_555 4_555 ? C21 Pd1 3.22(2) 1_555 2_656 ? C22 S3 3.73(2) 1_555 3_646 ? C22 S4 3.54(2) 1_555 3_656 ? C22 S7 3.56(2) 1_555 4_565 ? C22 Pd1 3.25(2) 1_555 2_656 ? O23 S8 3.29(2) 1_555 4_555 ? O24 H9A 2.54(1) 1_555 1_655 ? S1 S2 3.389(9) 1_555 3_556 ? S1 H10B 2.851(7) 1_555 3_556 ? S2 S7 3.736(9) 1_555 3_646 ? S2 H9A 2.950(7) 1_555 3_546 ? S3 S8 3.686(9) 1_555 2_657 ? S3 S19 3.707(8) 1_555 2_656 ? S4 S7 3.681(8) 1_555 2_657 ? S4 S19 3.700(8) 1_555 2_656 ? S4 S20 3.522(7) 1_555 3_646 ? S5 S6 3.535(8) 1_555 2_657 ? S5 Pd1 3.669(5) 1_555 3_656 ? S5 Pd1 3.669(5) 1_555 4_566 ? S6 S19 3.450(7) 1_555 4_556 ? S6 Pd1 4.095(5) 1_555 3_646 ? S6 Pd1 4.095(5) 1_555 4_556 ? S7 S19 3.727(8) 1_555 4_566 ? S8 S19 3.400(8) 1_555 4_556 ? S19 S20 3.261(7) 1_555 2_656 ? C9 O23 3.38(3) 1_555 1_455 ? C9 S2 3.66(3) 1_555 3_556 ? C10 O23 3.17(4) 1_555 1_455 ? C10 S1 3.59(4) 1_555 3_546 ? C11 C17 3.93(3) 1_555 2_657 ? C11 S19 3.85(2) 1_555 2_656 ? C11 H17B 2.98(2) 1_555 2_657 ? C12 C17 3.65(3) 1_555 2_657 ? C12 S19 3.88(2) 1_555 2_656 ? C12 H17B 2.72(2) 1_555 2_657 ? C13 C15 3.65(3) 1_555 2_657 ? C13 C16 3.61(2) 1_555 2_657 ? C13 S19 3.54(2) 1_555 2_656 ? C14 C14 3.73(2) 1_555 2_657 ? C14 C15 3.85(3) 1_555 2_657 ? C14 C16 3.81(2) 1_555 2_657 ? C14 S5 3.84(2) 1_555 2_657 ? C14 S6 3.77(2) 1_555 2_657 ? C15 S4 3.83(2) 1_555 2_657 ? C16 S3 3.83(2) 1_555 2_657 ? C17 S2 3.88(3) 1_555 3_656 ? C18 S1 3.75(3) 1_555 3_646 ? C21 S3 3.88(2) 1_555 3_646 ? C21 S7 3.31(2) 1_555 4_565 ? C21 S8 3.42(2) 1_555 4_555 ? C21 Pd1 3.22(2) 1_555 2_656 ? C22 S3 3.73(2) 1_555 3_646 ? C22 S4 3.54(2) 1_555 3_656 ? C22 S7 3.56(2) 1_555 4_565 ? C22 Pd1 3.25(2) 1_555 2_656 ? O23 S8 3.29(2) 1_555 4_555 ? O24 H9A 2.54(1) 1_555 1_655 ? S1 S2 3.389(9) 1_555 3_556 ? S1 H10B 2.851(7) 1_555 3_556 ? S2 S7 3.736(9) 1_555 3_646 ? S2 H9A 2.950(7) 1_555 3_546 ? S3 S8 3.686(9) 1_555 2_657 ? S3 S19 3.707(8) 1_555 2_656 ? S4 S7 3.681(8) 1_555 2_657 ? S4 S19 3.700(8) 1_555 2_656 ? S4 S20 3.522(7) 1_555 3_646 ? S5 S6 3.535(8) 1_555 2_657 ? S5 Pd1 3.669(5) 1_555 3_656 ? S5 Pd1 3.669(5) 1_555 4_566 ? S6 S19 3.450(7) 1_555 4_556 ? S6 Pd1 4.095(5) 1_555 3_646 ? S6 Pd1 4.095(5) 1_555 4_556 ? S7 S19 3.727(8) 1_555 4_566 ? S8 S19 3.400(8) 1_555 4_556 ? S19 S20 3.261(7) 1_555 2_656 ? #===END data_gamma-ET2[Pd(dto)2] _chemical_compound_source 'Local Laboratory' _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _chemical_formula_moiety 'C24 H16 O4 S20 Pd1 ' _chemical_formula_weight 1116.129 _cell_length_a 9.1000(7) _cell_length_b 13.148(1) _cell_length_c 8.9930(7) _cell_angle_alpha 67.257(4) _cell_angle_beta 91.603(5) _cell_angle_gamma 69.220(4) _cell_volume 910.6(1) _cell_measurement_reflns_used '28' _cell_measurement_theta_min '??' _cell_measurement_theta_max '25' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_meas 2.033 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_cryst_F000 557.98 _exptl_absorpt_coefficient_mu 1.642 _cell_measurement_temperature '298' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 3486 _reflns_number_total 3465 _reflns_number_observed 2703 _reflns_observed_criterion 'refl_observed_if_I_>_2.00_sigma(I)' _diffrn_reflns_av_R_equivalents ??? _diffrn_reflns_theta_max 24.23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.037 _refine_ls_wR_factor_obs 0.042 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 2703 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 1.335 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.2489 _refine_ls_shift/esd_mean 0.0229 _refine_diff_density_min -0.77 _refine_diff_density_max 0.50 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 -0.04669 _diffrn_orient_matrix_UB_12 -0.02245 _diffrn_orient_matrix_UB_13 0.05719 _diffrn_orient_matrix_UB_21 0.09698 _diffrn_orient_matrix_UB_22 -0.04220 _diffrn_orient_matrix_UB_23 0.03346 _diffrn_orient_matrix_UB_31 0.04608 _diffrn_orient_matrix_UB_32 0.10722 _diffrn_orient_matrix_UB_33 0.06033 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.3899(8) 0.0862(5) 0.2010(9) 0.061(4) 1.000 Uij C10 0.4498(8) 0.1313(6) 0.0490(10) 0.070(4) 1.000 Uij C11 0.1994(6) 0.3091(5) 0.1547(7) 0.041(3) 1.000 Uij C12 0.3063(7) 0.3469(5) 0.0765(7) 0.041(3) 1.000 Uij C13 0.1527(6) 0.5056(5) 0.1760(6) 0.037(3) 1.000 Uij C14 0.0982(6) 0.6057(4) 0.2083(6) 0.036(3) 1.000 Uij C15 -0.0572(6) 0.7718(4) 0.2987(6) 0.036(3) 1.000 Uij C16 0.0620(6) 0.8007(5) 0.2318(7) 0.039(3) 1.000 Uij C17 -0.1348(8) 0.9573(5) 0.3898(8) 0.055(3) 1.000 Uij C18 -0.0815(8) 1.0192(5) 0.2353(8) 0.053(3) 1.000 Uij C21 0.5734(7) 0.2549(5) 0.4535(7) 0.045(3) 1.000 Uij C22 0.6923(7) 0.3056(5) 0.3632(7) 0.048(3) 1.000 Uij O23 0.5697(6) 0.1639(4) 0.4511(6) 0.068(3) 1.000 Uij O24 0.7839(7) 0.2486(4) 0.3010(7) 0.082(3) 1.000 Uij S1 0.10790(18) 0.92350(13) 0.21260(20) 0.0521(8) 1.000 Uij S2 -0.20650(18) 0.84790(12) 0.37960(19) 0.0477(8) 1.000 Uij S3 0.18890(17) 0.70560(13) 0.15850(19) 0.0473(8) 1.000 Uij S4 -0.06230(17) 0.63830(12) 0.30580(18) 0.0435(7) 1.000 Uij S5 0.30900(18) 0.47940(13) 0.07280(19) 0.0499(8) 1.000 Uij S6 0.07480(17) 0.39780(12) 0.23900(19) 0.0445(7) 1.000 Uij S7 0.4455(2) 0.2809(2) -0.0222(2) 0.063(1) 1.000 Uij S8 0.18230(19) 0.17430(14) 0.18700(23) 0.0602(9) 1.000 Uij S19 0.45560(19) 0.32720(13) 0.55960(20) 0.0527(8) 1.000 Uij S20 0.69100(18) 0.43890(13) 0.35580(19) 0.0507(8) 1.000 Uij Pd1 0.50000 0.50000 0.50000 0.0361(3) 0.500 Uij H9A 0.46160 0.08760 0.29060 0.05 1.000 Uiso H9B 0.40610 0.00150 0.22960 0.05 1.000 Uiso H10A 0.38600 0.13020 -0.03940 0.05 1.000 Uiso H10B 0.56610 0.07500 0.06450 0.05 1.000 Uiso H17A -0.15270 1.02800 0.41430 0.05 1.000 Uiso H17B -0.00570 0.91570 0.48270 0.05 1.000 Uiso H18A -0.03350 1.09280 0.23470 0.05 1.000 Uiso H18B -0.12900 1.04340 0.13960 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.053(4) 0.035(3) 0.074(5) -0.018(3) 0.017(3) -0.022(3) C10 0.056(4) 0.047(4) 0.084(5) -0.012(3) 0.027(4) -0.039(4) C11 0.033(3) 0.034(3) 0.043(3) -0.015(2) 0.009(2) -0.022(2) C12 0.039(3) 0.035(3) 0.040(3) -0.017(2) 0.012(3) -0.022(3) C13 0.030(3) 0.032(3) 0.035(3) -0.012(2) 0.005(2) -0.015(2) C14 0.029(3) 0.031(3) 0.035(3) -0.012(2) 0.006(2) -0.015(2) C15 0.037(3) 0.030(3) 0.030(3) -0.015(2) 0.005(2) -0.014(2) C16 0.034(3) 0.035(3) 0.038(3) -0.015(2) 0.010(2) -0.021(2) C17 0.058(4) 0.041(3) 0.059(4) -0.027(3) 0.022(3) -0.035(3) C18 0.053(4) 0.038(3) 0.054(4) -0.022(3) 0.018(3) -0.027(3) C21 0.048(3) 0.036(3) 0.037(3) -0.010(3) 0.000(3) -0.021(3) C22 0.048(3) 0.037(3) 0.044(3) -0.010(3) 0.012(3) -0.024(3) O23 0.075(3) 0.046(3) 0.068(3) -0.026(2) 0.015(3) -0.040(2) O24 0.090(4) 0.051(3) 0.081(3) -0.018(3) 0.045(3) -0.045(3) S1 0.0453(8) 0.0432(8) 0.0590(9) -.0289(7) 0.0201(7) -.0318(8) S2 0.0430(8) 0.0351(7) 0.0541(9) -.0197(6) 0.0223(7) -.0259(7) S3 0.0390(8) 0.0401(8) 0.0531(9) -.0219(6) 0.0201(7) -.0285(7) S4 0.0380(7) 0.0323(7) 0.0504(8) -.0187(6) 0.0178(7) -.0238(6) S5 0.0467(8) 0.0406(8) 0.0540(9) -.0273(7) 0.0259(7) -.0298(7) S6 0.0365(7) 0.0346(7) 0.0513(8) -.0178(6) 0.0195(7) -.0236(7) S7 0.062(1) 0.048(1) 0.068(1) -0.029(1) 0.042(1) -0.038(1) S8 0.0483(9) 0.0427(8) 0.0798(11) -.0298(7) 0.0286(9) -.0380(8) S19 0.0502(9) 0.0426(8) 0.0571(9) -.0289(7) 0.0246(8) -.0327(8) S20 0.0421(8) 0.0445(8) 0.0539(9) -.0207(7) 0.0254(7) -.0307(7) Pd1 0.0304(3) 0.0316(3) 0.0386(3) -.0154(2) 0.0127(3) -.0230(3) 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 C10 C9 S8 C11 -63.0(6) . . . . yes S8 C9 C10 S7 61.2(5) . . . . yes C9 C10 S7 C12 -19.9(6) . . . . yes C12 C11 S6 C13 0.4(5) . . . . yes S6 C11 C12 S5 1.2(3) . . . . yes S6 C11 C12 S7 -179.3(8) . . . . yes C12 C11 S8 C9 31.2(6) . . . . yes S8 C11 C12 S5 -175.5(7) . . . . yes S8 C11 C12 S7 4.0(4) . . . . yes S6 C11 S8 C9 -145.5(4) . . . . yes S8 C11 S6 C13 177.4(4) . . . . yes C11 C12 S5 C13 -2.1(5) . . . . yes C11 C12 S7 C10 -14.3(6) . . . . yes S5 C12 S7 C10 165.3(5) . . . . yes S7 C12 S5 C13 178.3(4) . . . . yes C14 C13 S5 C12 -179.3(5) . . . . yes S5 C13 C14 S3 -3.7(3) . . . . yes S5 C13 C14 S4 177.9(7) . . . . yes C14 C13 S6 C11 179.8(5) . . . . yes S6 C13 C14 S3 174.6(7) . . . . yes S6 C13 C14 S4 -3.8(3) . . . . yes S5 C13 S6 C11 -1.8(4) . . . . yes S6 C13 S5 C12 2.3(4) . . . . yes C13 C14 S3 C16 -180.0(5) . . . . yes C13 C14 S4 C15 -179.4(5) . . . . yes S3 C14 S4 C15 2.1(4) . . . . yes S4 C14 S3 C16 -1.5(4) . . . . yes C16 C15 S2 C17 -11.5(6) . . . . yes S2 C15 C16 S1 2.6(4) . . . . yes S2 C15 C16 S3 -178.7(8) . . . . yes C16 C15 S4 C14 -2.2(5) . . . . yes S4 C15 C16 S1 -177.2(7) . . . . yes S4 C15 C16 S3 1.5(3) . . . . yes S2 C15 S4 C14 178.0(4) . . . . yes S4 C15 S2 C17 168.3(4) . . . . yes C15 C16 S1 C18 -19.4(6) . . . . yes C15 C16 S3 C14 0.0(5) . . . . yes S1 C16 S3 C14 178.8(4) . . . . yes S3 C16 S1 C18 161.8(4) . . . . yes C18 C17 S2 C15 46.1(5) . . . . yes S2 C17 C18 S1 -73.7(5) . . . . yes C17 C18 S1 C16 53.9(5) . . . . yes O23 C21 C22 O24 -4.1(6) . . . . yes O23 C21 C22 S20 176.4(8) . . . . yes S19 C21 C22 O24 173.8(8) . . . . yes S19 C21 C22 S20 -5.7(4) . . . . yes C22 C21 S19 Pd1 6.8(4) . . . . yes O23 C21 S19 Pd1 -175.4(6) . . . . yes C21 C22 S20 Pd1 1.3(4) . . . . yes O24 C22 S20 Pd1 -178.2(6) . . . . yes C21 S19 Pd1 S20 -4.6(3) . . . . yes Pd1 S19 C21 C22 6.8(4) . . . . yes Pd1 S19 C21 O23 -175.4(6) . . . . yes C21 S19 Pd1 S20 -4.6(3) . . . . yes C22 S20 Pd1 S19 2.2(3) . . . . yes Pd1 S20 C22 C21 1.3(4) . . . . yes Pd1 S20 C22 O24 -178.2(6) . . . . yes C22 S20 Pd1 S19 2.2(3) . . . . yes S20 Pd1 S19 C21 175.4(3) . . . . yes S19 Pd1 S20 C22 -177.8(3) . . . . yes S8 C9 C10 H10A -59.8(6) . . . . yes S8 C9 C10 H10B -177.5(8) . . . . yes H9A C9 C10 S7 -59.9(6) . . . . yes H9A C9 C10 H10A 179.0(9) . . . . yes H9A C9 C10 H10B 61.4(7) . . . . yes H9B C9 C10 S7 -176.2(9) . . . . yes H9B C9 C10 H10A 62.8(7) . . . . yes H9B C9 C10 H10B -54.9(7) . . . . yes H9A C9 S8 C11 55.3(5) . . . . yes H9B C9 S8 C11 175.1(6) . . . . yes H10A C10 S7 C12 101.8(6) . . . . yes H10B C10 S7 C12 -142.4(6) . . . . yes S2 C17 C18 H18A 179.7(7) . . . . yes S2 C17 C18 H18B 41.7(7) . . . . yes H17A C17 C18 S1 130.0(6) . . . . yes H17A C17 C18 H18A 23.4(6) . . . . yes H17A C17 C18 H18B -114.6(9) . . . . yes H17B C17 C18 S1 47.4(4) . . . . yes H17B C17 C18 H18A -59.1(6) . . . . yes H17B C17 C18 H18B 162.9(9) . . . . yes H17A C17 S2 C15 175.8(11) . . . . yes H17B C17 S2 C15 -63.4(5) . . . . yes H18A C18 S1 C16 174.4(4) . . . . yes H18B C18 S1 C16 -78.3(5) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.470(12) . . yes C9 S8 1.802(7) . . yes C10 S7 1.803(7) . . yes C11 C12 1.341(9) . . yes C11 S6 1.736(6) . . yes C11 S8 1.746(6) . . yes C12 S5 1.738(6) . . yes C12 S7 1.739(7) . . yes C13 C14 1.379(8) . . yes C13 S5 1.725(6) . . yes C13 S6 1.717(6) . . yes C14 S3 1.715(6) . . yes C14 S4 1.733(6) . . yes C15 C16 1.355(8) . . yes C15 S2 1.741(6) . . yes C15 S4 1.749(6) . . yes C16 S1 1.754(6) . . yes C16 S3 1.728(6) . . yes C17 C18 1.507(10) . . yes C17 S2 1.808(7) . . yes C18 S1 1.810(7) . . yes C21 C22 1.555(9) . . yes C21 O23 1.217(7) . . yes C21 S19 1.732(7) . . yes C22 O24 1.215(9) . . yes C22 S20 1.724(6) . . yes S19 Pd1 2.310(2) . . yes S19 Pd1 2.310(2) . 2_656 yes S20 Pd1 2.300(2) . . yes S20 Pd1 2.300(2) . 2_656 yes C9 H9A 1.032(7) . . yes C9 H9B 0.994(6) . . yes C10 H10A 0.979(8) . . yes C10 H10B 1.022(8) . . yes C17 H17A 0.996(6) . . yes C17 H17B 1.230(6) . . yes C18 H18A 1.193(6) . . yes C18 H18B 0.836(6) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 S8 113.5(5) . . . yes C9 C10 S7 117.3(5) . . . yes C12 C11 S6 117.3(5) . . . yes C12 C11 S8 125.2(5) . . . yes S6 C11 S8 117.5(4) . . . yes C11 C12 S5 116.5(5) . . . yes C11 C12 S7 128.9(5) . . . yes S5 C12 S7 114.6(4) . . . yes C14 C13 S5 121.4(4) . . . yes C14 C13 S6 123.0(5) . . . yes S5 C13 S6 115.7(3) . . . yes C13 C14 S3 121.9(5) . . . yes C13 C14 S4 123.1(4) . . . yes S3 C14 S4 115.0(3) . . . yes C16 C15 S2 129.5(5) . . . yes C16 C15 S4 115.6(4) . . . yes S2 C15 S4 114.9(4) . . . yes C15 C16 S1 127.9(5) . . . yes C15 C16 S3 117.5(5) . . . yes S1 C16 S3 114.6(4) . . . yes C18 C17 S2 113.3(5) . . . yes C17 C18 S1 112.8(5) . . . yes C22 C21 O23 118.9(6) . . . yes C22 C21 S19 118.8(5) . . . yes O23 C21 S19 122.3(5) . . . yes C21 C22 O24 118.2(6) . . . yes C21 C22 S20 119.4(5) . . . yes O24 C22 S20 122.4(6) . . . yes C16 S1 C18 99.2(3) . . . yes C15 S2 C17 100.8(3) . . . yes C14 S3 C16 96.0(3) . . . yes C14 S4 C15 95.8(3) . . . yes C12 S5 C13 95.3(3) . . . yes C11 S6 C13 95.2(3) . . . yes C10 S7 C12 103.5(4) . . . yes C9 S8 C11 98.0(3) . . . yes C21 S19 Pd1 106.0(3) . . . yes C21 S19 Pd1 106.0(3) . . 2_656 yes C22 S20 Pd1 106.3(3) . . . yes C22 S20 Pd1 106.3(3) . . 2_656 yes S19 Pd1 S19 180.0 . . 2_656 yes S19 Pd1 S20 89.2(1) . . . yes S19 Pd1 S20 90.8(1) . . 2_656 yes S19 Pd1 S20 90.8(1) 2_656 . . yes S19 Pd1 S20 89.2(1) 2_656 . 2_656 yes S20 Pd1 S20 180.0 . . 2_656 yes C10 C9 H9A 105.5(6) . . . yes C10 C9 H9B 108.6(6) . . . yes S8 C9 H9A 110.5(5) . . . yes S8 C9 H9B 109.9(6) . . . yes H9A C9 H9B 108.6(7) . . . yes C9 C10 H10A 108.3(7) . . . yes C9 C10 H10B 109.0(7) . . . yes S7 C10 H10A 106.9(6) . . . yes S7 C10 H10B 106.7(6) . . . yes H10A C10 H10B 108.4(7) . . . yes C18 C17 H17A 88.3(5) . . . yes C18 C17 H17B 96.2(5) . . . yes S2 C17 H17A 148.5(6) . . . yes S2 C17 H17B 115.5(5) . . . yes H17A C17 H17B 82.8(5) . . . yes C17 C18 H18A 116.2(6) . . . yes C17 C18 H18B 125.3(7) . . . yes S1 C18 H18A 93.7(4) . . . yes S1 C18 H18B 95.7(5) . . . yes H18A C18 H18B 106.8(6) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 S1 3.861(7) 1_555 1_545 ? C9 S2 3.674(6) 1_555 1_645 ? C10 C10 3.700(9) 1_555 2_655 ? C10 S2 3.892(7) 1_555 1_645 ? C11 C13 3.657(7) 1_555 2_565 ? C11 C14 3.711(7) 1_555 2_565 ? C11 S2 3.874(6) 1_555 2_566 ? C12 S6 3.895(5) 1_555 2_565 ? C12 S20 3.826(6) 1_555 2_665 ? C13 S6 3.724(5) 1_555 2_565 ? C13 Pd1 4.200(5) 1_555 2_666 ? C14 S8 3.718(5) 1_555 2_565 ? C14 Pd1 3.901(5) 1_555 2_666 ? C15 C22 3.994(7) 1_555 2_666 ? C15 S20 3.827(5) 1_555 2_666 ? C16 C18 3.992(8) 1_555 2_575 ? C16 C21 3.963(7) 1_555 2_666 ? C16 C22 3.689(7) 1_555 2_666 ? C16 S20 3.769(5) 1_555 2_666 ? C16 Pd1 4.271(5) 1_555 2_666 ? C17 C17 3.823(8) 1_555 2_576 ? C17 O23 3.312(8) 1_555 1_465 ? C17 O24 3.383(7) 1_555 1_465 ? C17 S8 3.633(7) 1_555 2_566 ? C17 H17B 2.941(6) 1_555 2_576 ? C18 O24 3.121(8) 1_555 1_465 ? C18 S1 3.784(7) 1_555 2_575 ? C18 S3 3.739(6) 1_555 2_575 ? C18 S8 3.600(6) 1_555 1_565 ? C18 H17B 3.137(6) 1_555 2_576 ? C21 S1 3.488(6) 1_555 2_666 ? C21 Pd1 3.246(6) 1_555 2_666 ? C22 S1 3.711(6) 1_555 2_666 ? C22 S5 3.843(6) 1_555 2_665 ? C22 Pd1 3.238(6) 1_555 2_666 ? C22 H17B 3.048(6) 1_555 2_666 ? O24 H17A 2.506(5) 1_555 1_645 ? O24 H17B 2.442(5) 1_555 2_666 ? O24 H18A 2.428(5) 1_555 1_645 ? S1 S1 3.654(2) 1_555 2_575 ? S1 S8 3.520(2) 1_555 1_565 ? S1 H18B 3.047(2) 1_555 2_575 ? S2 S6 3.477(2) 1_555 2_566 ? S2 S8 3.788(2) 1_555 2_566 ? S2 S19 3.679(2) 1_555 2_566 ? S3 S7 3.617(2) 1_555 2_665 ? S3 Pd1 3.524(1) 1_555 2_666 ? S4 S4 3.707(2) 1_555 2_566 ? S4 S19 3.741(2) 1_555 2_566 ? S5 S20 3.579(2) 1_555 2_665 ? S5 Pd1 4.315(1) 1_555 2_666 ? S6 S20 3.591(2) 1_555 1_455 ? S7 S19 3.579(3) 1_555 1_554 ? S7 S20 3.481(2) 1_555 2_665 ? S7 Pd1 4.309(2) 1_555 1_554 ? S7 Pd1 4.309(2) 1_555 2_665 ? S8 H18A 2.525(2) 1_555 1_545 ? S19 S20 3.282(2) 1_555 2_666 ? H17A H17B 2.1671 1_555 2_576 ? H17B H17B 2.3909 1_555 2_576 ? C9 S1 3.861(7) 1_555 1_545 ? C9 S2 3.674(6) 1_555 1_645 ? C10 C10 3.700(9) 1_555 2_655 ? C10 S2 3.892(7) 1_555 1_645 ? C11 C13 3.657(7) 1_555 2_565 ? C11 C14 3.711(7) 1_555 2_565 ? C11 S2 3.874(6) 1_555 2_566 ? C12 S6 3.895(5) 1_555 2_565 ? C12 S20 3.826(6) 1_555 2_665 ? C13 S6 3.724(5) 1_555 2_565 ? C13 Pd1 4.200(5) 1_555 2_666 ? C14 S8 3.718(5) 1_555 2_565 ? C14 Pd1 3.901(5) 1_555 2_666 ? C15 C22 3.994(7) 1_555 2_666 ? C15 S20 3.827(5) 1_555 2_666 ? C16 C18 3.992(8) 1_555 2_575 ? C16 C21 3.963(7) 1_555 2_666 ? C16 C22 3.689(7) 1_555 2_666 ? C16 S20 3.769(5) 1_555 2_666 ? C16 Pd1 4.271(5) 1_555 2_666 ? C17 C17 3.823(8) 1_555 2_576 ? C17 O23 3.312(8) 1_555 1_465 ? C17 O24 3.383(7) 1_555 1_465 ? C17 S8 3.633(7) 1_555 2_566 ? C17 H17B 2.941(6) 1_555 2_576 ? C18 O24 3.121(8) 1_555 1_465 ? C18 S1 3.784(7) 1_555 2_575 ? C18 S3 3.739(6) 1_555 2_575 ? C18 S8 3.600(6) 1_555 1_565 ? C18 H17B 3.137(6) 1_555 2_576 ? C21 S1 3.488(6) 1_555 2_666 ? C21 Pd1 3.246(6) 1_555 2_666 ? C22 S1 3.711(6) 1_555 2_666 ? C22 S5 3.843(6) 1_555 2_665 ? C22 Pd1 3.238(6) 1_555 2_666 ? C22 H17B 3.048(6) 1_555 2_666 ? O24 H17A 2.506(5) 1_555 1_645 ? O24 H17B 2.442(5) 1_555 2_666 ? O24 H18A 2.428(5) 1_555 1_645 ? S1 S1 3.654(2) 1_555 2_575 ? S1 S8 3.520(2) 1_555 1_565 ? S1 H18B 3.047(2) 1_555 2_575 ? S2 S6 3.477(2) 1_555 2_566 ? S2 S8 3.788(2) 1_555 2_566 ? S2 S19 3.679(2) 1_555 2_566 ? S3 S7 3.617(2) 1_555 2_665 ? S3 Pd1 3.524(1) 1_555 2_666 ? S4 S4 3.707(2) 1_555 2_566 ? S4 S19 3.741(2) 1_555 2_566 ? S5 S20 3.579(2) 1_555 2_665 ? S5 Pd1 4.315(1) 1_555 2_666 ? S6 S20 3.591(2) 1_555 1_455 ? S7 S19 3.579(3) 1_555 1_554 ? S7 S20 3.481(2) 1_555 2_665 ? S7 Pd1 4.309(2) 1_555 1_554 ? S7 Pd1 4.309(2) 1_555 2_665 ? S8 H18A 2.525(2) 1_555 1_545 ? S19 S20 3.282(2) 1_555 2_666 ? H17A H17B 2.1671 1_555 2_576 ? H17B H17B 2.3909 1_555 2_576 ? #===END data_ET2[Ni(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.1 _chemical_formula_moiety 'C24 H16 Ni1 O4 S20 ' _chemical_formula_weight 1068.41 _cell_length_a 9.715(2) _cell_length_b 12.679(3) _cell_length_c 8.320(2) _cell_angle_alpha 108.12(2) _cell_angle_beta 111.95(2) _cell_angle_gamma 79.22(2) _cell_volume 900.5(4) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '35' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_meas 1.977 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 16.926 _diffrn_ambient_temperature 298 _cell_measurement_temperature 298 _exptl_cryst_F_000 539.96 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 7914 _reflns_number_total 7216 _reflns_number_observed 6010 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents ??? _diffrn_reflns_theta_max 32.86 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.061 _refine_ls_wR_factor_obs 0.067 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 6010 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 1.456 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.4408 _refine_ls_shift/esd_mean 0.0273 _refine_diff_density_min -1.52 _refine_diff_density_max 2.23 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ni1 0.00000 0.50000 0.50000 0.0242(3) 0.500 Uij S1 0.42802(14) 0.07855(10) -0.28410(17) 0.0387(5) 1.000 Uij S2 0.75249(15) 0.12405(10) 0.10042(17) 0.0395(5) 1.000 Uij S3 0.34559(12) 0.31223(9) -0.13947(15) 0.0314(4) 1.000 Uij S4 0.60341(12) 0.35027(8) 0.18841(14) 0.0287(4) 1.000 Uij S5 0.19237(12) 0.54765(9) -0.01204(15) 0.0330(4) 1.000 Uij S6 0.44178(11) 0.60043(8) 0.32226(14) 0.0264(4) 1.000 Uij S7 -0.00067(14) 0.74728(13) 0.08155(20) 0.0490(6) 1.000 Uij S8 0.30638(12) 0.81525(9) 0.47908(15) 0.0306(4) 1.000 Uij S19 0.18608(13) 0.45586(9) 0.39929(18) 0.0385(5) 1.000 Uij S20 -0.03067(14) 0.32683(9) 0.45108(21) 0.0441(5) 1.000 Uij O23 0.3269(4) 0.2619(3) 0.3162(7) 0.057(2) 1.000 Uij O24 0.1307(5) 0.1475(3) 0.3495(7) 0.056(2) 1.000 Uij C9 0.6043(6) 0.0024(4) -0.2546(7) 0.044(2) 1.000 Uij C10 0.6887(8) -0.0044(4) -0.0678(8) 0.052(3) 1.000 Uij C11 0.4747(5) 0.2000(3) -0.1099(6) 0.028(2) 1.000 Uij C12 0.5974(5) 0.2169(3) 0.0405(5) 0.028(2) 1.000 Uij C13 0.4326(4) 0.4012(3) 0.0644(5) 0.026(1) 1.000 Uij C14 0.3636(4) 0.5056(3) 0.1201(5) 0.027(2) 1.000 Uij C15 0.1707(5) 0.6726(3) 0.1419(6) 0.030(2) 1.000 Uij C16 0.2887(4) 0.6982(3) 0.2971(5) 0.025(1) 1.000 Uij C17 0.0436(7) 0.8805(5) 0.2289(9) 0.056(3) 1.000 Uij C18 0.1230(5) 0.8885(4) 0.4231(6) 0.035(2) 1.000 Uij C21 0.2227(5) 0.3139(3) 0.3604(6) 0.034(2) 1.000 Uij C22 0.1120(5) 0.2479(3) 0.3809(7) 0.035(2) 1.000 Uij H17A -0.06464 0.92899 0.21705 0.05 1.000 Uiso H17B 0.09546 0.91069 0.18675 0.05 1.000 Uiso H18A 0.12065 0.96888 0.48920 0.05 1.000 Uiso H18B 0.04825 0.85758 0.46580 0.05 1.000 Uiso H9A 0.66464 0.03922 -0.29133 0.05 1.000 Uiso H9B 0.58954 -0.07478 -0.33503 0.05 1.000 Uiso H10A 0.62279 -0.03467 -0.02838 0.05 1.000 Uiso H10B 0.77879 -0.05807 -0.06958 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0190(3) 0.0185(3) 0.0288(3) -.0014(2) 0.0096(3) 0.0047(3) S1 0.0369(6) 0.0305(5) 0.0336(6) -.0055(4) 0.0089(5) -.0062(4) S2 0.0413(6) 0.0293(5) 0.0314(5) 0.0111(4) 0.0061(5) 0.0033(4) S3 0.0240(4) 0.0286(5) 0.0296(5) -.0008(3) 0.0048(4) 0.0013(4) S4 0.0278(4) 0.0225(4) 0.0250(4) 0.0022(3) 0.0057(3) 0.0017(3) S5 0.0260(5) 0.0311(5) 0.0282(5) 0.0038(4) 0.0046(4) 0.0001(4) S6 0.0214(4) 0.0232(4) 0.0263(4) 0.0018(3) 0.0072(3) 0.0047(3) S7 0.0293(6) 0.0500(8) 0.0426(7) 0.0142(5) 0.0007(5) -.0032(6) S8 0.0270(5) 0.0257(4) 0.0285(5) 0.0011(3) 0.0085(4) 0.0007(4) S19 0.0312(5) 0.0250(4) 0.0522(7) -.0012(4) 0.0251(5) 0.0065(4) S20 0.0338(5) 0.0214(4) 0.0685(9) -.0013(4) 0.0292(6) 0.0089(5) O23 0.038(2) 0.036(2) 0.083(3) 0.004(1) 0.038(2) 0.002(2) O24 0.048(2) 0.023(1) 0.085(3) 0.005(1) 0.033(2) 0.013(2) C9 0.044(3) 0.035(2) 0.039(3) 0.000(2) 0.016(2) -0.003(2) C10 0.068(4) 0.031(2) 0.040(3) 0.008(2) 0.021(3) 0.005(2) C11 0.027(2) 0.023(2) 0.027(2) -0.002(1) 0.012(1) 0.002(1) C12 0.030(2) 0.020(1) 0.025(2) 0.001(1) 0.010(1) 0.003(1) C13 0.023(2) 0.022(2) 0.026(2) 0.001(1) 0.009(1) 0.003(1) C14 0.025(2) 0.024(2) 0.025(2) 0.001(1) 0.010(1) 0.004(1) C15 0.023(2) 0.028(2) 0.029(2) 0.003(1) 0.007(1) 0.003(1) C16 0.022(2) 0.022(1) 0.026(2) 0.001(1) 0.010(1) 0.005(1) C17 0.047(3) 0.045(3) 0.058(4) 0.010(2) 0.015(3) 0.013(3) C18 0.032(2) 0.029(2) 0.036(2) 0.005(2) 0.015(2) 0.007(2) C21 0.025(2) 0.027(2) 0.038(2) -0.001(1) 0.010(2) 0.003(2) C22 0.026(2) 0.024(2) 0.044(2) 0.001(1) 0.012(2) 0.008(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 S20 Ni1 S19 C21 -6.6(2) . . . . yes S19 Ni1 S20 C22 5.2(2) . . . . yes S20 Ni1 S19 C21 173.4(2) . . . . yes S19 Ni1 S20 C22 -174.8(2) . . . . yes C9 S1 C11 S3 159.6(3) . . . . yes C11 S1 C9 C10 49.1(4) . . . . yes C9 S1 C11 C12 -19.5(5) . . . . yes C10 S2 C12 S4 172.5(4) . . . . yes C12 S2 C10 C9 41.5(5) . . . . yes C10 S2 C12 C11 -10.1(5) . . . . yes C13 S3 C11 S1 175.9(3) . . . . yes C11 S3 C13 S4 5.7(3) . . . . yes C13 S3 C11 C12 -4.8(4) . . . . yes C11 S3 C13 C14 -173.2(4) . . . . yes C13 S4 C12 S2 179.2(3) . . . . yes C12 S4 C13 S3 -4.8(3) . . . . yes C13 S4 C12 C11 1.5(4) . . . . yes C12 S4 C13 C14 174.1(4) . . . . yes C15 S5 C14 S6 -4.9(3) . . . . yes C14 S5 C15 S7 -174.2(3) . . . . yes C15 S5 C14 C13 175.3(4) . . . . yes C14 S5 C15 C16 4.1(4) . . . . yes C16 S6 C14 S5 4.0(3) . . . . yes C14 S6 C16 S8 177.3(3) . . . . yes C16 S6 C14 C13 -176.2(4) . . . . yes C14 S6 C16 C15 -1.2(4) . . . . yes C17 S7 C15 S5 -162.0(4) . . . . yes C17 S7 C15 C16 20.0(5) . . . . yes C15 S7 C17 C18 -50.4(5) . . . . yes C18 S8 C16 S6 -172.6(3) . . . . yes C18 S8 C16 C15 5.6(4) . . . . yes C16 S8 C18 C17 -34.5(4) . . . . yes Ni1 S19 C21 O23 -174.2(5) . . . . yes Ni1 S19 C21 C22 6.7(3) . . . . yes C21 S19 Ni1 S20 -6.6(2) . . . . yes Ni1 S19 C21 O23 -174.2(5) . . . . yes Ni1 S19 C21 C22 6.7(3) . . . . yes Ni1 S20 C22 O24 176.8(5) . . . . yes Ni1 S20 C22 C21 -2.5(3) . . . . yes C22 S20 Ni1 S19 5.2(2) . . . . yes Ni1 S20 C22 O24 176.8(5) . . . . yes Ni1 S20 C22 C21 -2.5(3) . . . . yes S1 C9 C10 S2 -66.6(4) . . . . yes S1 C11 C12 S2 4.0(3) . . . . yes S1 C11 C12 S4 -178.6(6) . . . . yes S3 C11 C12 S2 -175.1(6) . . . . yes S3 C11 C12 S4 2.3(3) . . . . yes S3 C13 C14 S5 -0.3(3) . . . . yes S3 C13 C14 S6 179.9(5) . . . . yes S4 C13 C14 S5 -179.1(6) . . . . yes S4 C13 C14 S6 1.1(3) . . . . yes S5 C15 C16 S6 -2.0(3) . . . . yes S5 C15 C16 S8 179.8(6) . . . . yes S7 C15 C16 S6 176.0(6) . . . . yes S7 C15 C16 S8 -2.2(3) . . . . yes S7 C17 C18 S8 62.4(4) . . . . yes S19 C21 C22 S20 -2.9(3) . . . . yes S19 C21 C22 O24 177.8(6) . . . . yes O23 C21 C22 S20 178.0(6) . . . . yes O23 C21 C22 O24 -1.3(5) . . . . yes C11 S1 C9 H9A -71.2(4) . . . . yes C11 S1 C9 H9B 170.9(5) . . . . yes C12 S2 C10 H10A -79.3(5) . . . . yes C12 S2 C10 H10B 163.3(5) . . . . yes C15 S7 C17 H17A -169.4(5) . . . . yes C15 S7 C17 H17B 75.0(6) . . . . yes C16 S8 C18 H18A -160.1(4) . . . . yes C16 S8 C18 H18B 85.6(4) . . . . yes S1 C9 C10 H10A 54.4(5) . . . . yes S1 C9 C10 H10B 171.8(7) . . . . yes H9A C9 C10 S2 53.6(5) . . . . yes H9A C9 C10 H10A 174.6(7) . . . . yes H9A C9 C10 H10B -68.0(6) . . . . yes H9B C9 C10 S2 171.8(7) . . . . yes H9B C9 C10 H10A -67.3(6) . . . . yes H9B C9 C10 H10B 50.2(6) . . . . yes S7 C17 C18 H18A -168.6(7) . . . . yes S7 C17 C18 H18B -61.0(5) . . . . yes H17A C17 C18 S8 -179.8(7) . . . . yes H17A C17 C18 H18A -50.8(5) . . . . yes H17A C17 C18 H18B 56.8(5) . . . . yes H17B C17 C18 S8 -61.8(6) . . . . yes H17B C17 C18 H18A 67.1(6) . . . . yes H17B C17 C18 H18B 174.8(7) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S19 2.178(2) . . yes Ni1 S19 2.178(2) . 2_556 yes Ni1 S20 2.162(2) . . yes Ni1 S20 2.162(2) . 2_556 yes S1 C9 1.772(6) . . yes S1 C11 1.750(5) . . yes S2 C10 1.818(6) . . yes S2 C12 1.745(5) . . yes S3 C11 1.725(5) . . yes S3 C13 1.720(5) . . yes S4 C12 1.751(5) . . yes S4 C13 1.723(5) . . yes S5 C14 1.710(5) . . yes S5 C15 1.734(5) . . yes S6 C14 1.727(5) . . yes S6 C16 1.741(4) . . yes S7 C15 1.733(5) . . yes S7 C17 1.769(7) . . yes S8 C16 1.740(4) . . yes S8 C18 1.812(5) . . yes S19 C21 1.719(5) . . yes S20 C22 1.728(5) . . yes O23 C21 1.214(6) . . yes O24 C22 1.210(6) . . yes C9 C10 1.483(8) . . yes C11 C12 1.359(6) . . yes C13 C14 1.391(6) . . yes C15 C16 1.363(6) . . yes C17 C18 1.487(9) . . yes C21 C22 1.565(6) . . yes C9 H9A 0.989(5) . . yes C9 H9B 1.000(6) . . yes C10 H10A 0.996(6) . . yes C10 H10B 1.005(7) . . yes C17 H17A 1.101(7) . . yes C17 H17B 0.901(6) . . yes C18 H18A 0.997(5) . . yes C18 H18B 1.092(4) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S19 Ni1 S19 180.0 . . 2_556 yes S19 Ni1 S20 91.7(1) . . . yes S19 Ni1 S20 88.3(1) . . 2_556 yes S19 Ni1 S20 88.3(1) 2_556 . . yes S19 Ni1 S20 91.7(1) 2_556 . 2_556 yes S20 Ni1 S20 180.0 . . 2_556 yes C9 S1 C11 101.1(3) . . . yes C10 S2 C12 101.0(3) . . . yes C11 S3 C13 95.7(2) . . . yes C12 S4 C13 95.5(2) . . . yes C14 S5 C15 96.0(2) . . . yes C14 S6 C16 95.2(2) . . . yes C15 S7 C17 100.6(3) . . . yes C16 S8 C18 103.2(2) . . . yes Ni1 S19 C21 106.8(2) . . . yes Ni1 S19 C21 106.8(2) 2_556 . . yes Ni1 S20 C22 107.6(2) . . . yes Ni1 S20 C22 107.6(2) 2_556 . . yes S1 C9 C10 114.6(5) . . . yes S2 C10 C9 117.5(4) . . . yes S1 C11 S3 113.9(3) . . . yes S1 C11 C12 128.9(4) . . . yes S3 C11 C12 117.2(3) . . . yes S2 C12 S4 116.0(3) . . . yes S2 C12 C11 128.1(4) . . . yes S4 C12 C11 115.8(3) . . . yes S3 C13 S4 115.4(3) . . . yes S3 C13 C14 120.0(3) . . . yes S4 C13 C14 124.5(4) . . . yes S5 C14 S6 115.7(3) . . . yes S5 C14 C13 120.9(4) . . . yes S6 C14 C13 123.4(4) . . . yes S5 C15 S7 115.7(3) . . . yes S5 C15 C16 116.1(3) . . . yes S7 C15 C16 128.1(4) . . . yes S6 C16 S8 114.6(3) . . . yes S6 C16 C15 116.7(3) . . . yes S8 C16 C15 128.7(3) . . . yes S7 C17 C18 118.0(5) . . . yes S8 C18 C17 115.8(4) . . . yes S19 C21 O23 124.5(4) . . . yes S19 C21 C22 117.3(3) . . . yes O23 C21 C22 118.2(4) . . . yes S20 C22 O24 124.3(4) . . . yes S20 C22 C21 116.1(3) . . . yes O24 C22 C21 119.6(4) . . . yes S1 C9 H9A 107.8(4) . . . yes S1 C9 H9B 108.5(4) . . . yes C10 C9 H9A 108.0(5) . . . yes C10 C9 H9B 108.8(5) . . . yes H9A C9 H9B 109.0(6) . . . yes S2 C10 H10A 107.4(5) . . . yes S2 C10 H10B 107.5(5) . . . yes C9 C10 H10A 107.1(6) . . . yes C9 C10 H10B 107.9(5) . . . yes H10A C10 H10B 109.1(5) . . . yes S7 C17 H17A 104.8(5) . . . yes S7 C17 H17B 107.8(6) . . . yes C18 C17 H17A 107.1(6) . . . yes C18 C17 H17B 110.0(6) . . . yes H17A C17 H17B 108.7(6) . . . yes S8 C18 H18A 114.1(4) . . . yes S8 C18 H18B 111.3(4) . . . yes C17 C18 H18A 107.5(5) . . . yes C17 C18 H18B 105.2(4) . . . yes H18A C18 H18B 101.6(4) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni1 S3 4.457(1) 1_555 1_556 ? Ni1 S3 4.457(1) 1_555 2_565 ? Ni1 S4 4.169(1) 1_555 1_455 ? Ni1 S4 4.169(1) 1_555 2_666 ? Ni1 S5 3.683(1) 1_555 1_556 ? Ni1 S5 3.683(1) 1_555 2_565 ? Ni1 C21 3.140(4) 1_555 2_566 ? Ni1 C22 3.150(4) 1_555 2_566 ? S1 S8 3.474(2) 1_555 1_544 ? S1 C9 3.557(5) 1_555 2_654 ? S1 C18 3.761(4) 1_555 1_544 ? S1 H9B 3.095(1) 1_555 2_654 ? S1 H10A 3.045(1) 1_555 2_655 ? S2 S8 3.580(2) 1_555 2_666 ? S2 S20 3.511(2) 1_555 1_655 ? S2 C17 3.899(7) 1_555 1_645 ? S2 C18 3.733(5) 1_555 2_666 ? S2 C22 3.713(4) 1_555 1_655 ? S2 H17A 2.962(1) 1_555 1_645 ? S3 S6 3.472(1) 1_555 2_665 ? S3 S7 3.796(2) 1_555 2_565 ? S3 C21 3.883(5) 1_555 1_554 ? S3 C22 3.693(5) 1_555 1_554 ? S4 S5 3.476(1) 1_555 2_665 ? S4 S8 3.733(1) 1_555 2_666 ? S4 S19 3.658(2) 1_555 2_666 ? S4 S20 3.421(2) 1_555 1_655 ? S4 C14 3.713(4) 1_555 2_665 ? S6 S19 3.571(2) 1_555 2_666 ? S6 O23 3.208(4) 1_555 2_666 ? S6 C11 3.847(4) 1_555 2_665 ? S6 C13 3.837(4) 1_555 2_665 ? S6 C21 3.447(4) 1_555 2_666 ? S7 C21 3.420(5) 1_555 2_565 ? S7 C22 3.604(5) 1_555 2_565 ? S8 S20 3.792(1) 1_555 2_566 ? S8 C9 3.664(5) 1_555 1_566 ? S8 C9 3.772(5) 1_555 2_665 ? S8 C12 3.885(4) 1_555 2_666 ? S8 H9A 2.8705 1_555 2_665 ? S8 H9B 2.969(1) 1_555 1_566 ? S19 S20 3.023(2) 1_555 2_566 ? S20 C18 3.570(4) 1_555 2_566 ? S20 H18B 2.687(1) 1_555 2_566 ? O23 C9 3.207(6) 1_555 2_655 ? O23 C10 3.272(7) 1_555 2_655 ? O23 H9B 2.393(4) 1_555 2_655 ? O24 C9 3.101(7) 1_555 2_655 ? O24 C10 3.332(8) 1_555 2_655 ? O24 C17 3.392(7) 1_555 1_545 ? C9 C9 3.806(8) 1_555 2_654 ? C9 C17 3.886(8) 1_555 2_665 ? C9 C22 3.948(7) 1_555 2_655 ? C9 H17B 3.102(5) 1_555 2_665 ? C10 C17 3.756(9) 1_555 1_645 ? C10 H17A 2.884(6) 1_555 1_645 ? C10 H17B 3.163(6) 1_555 2_665 ? C11 C16 3.796(5) 1_555 2_665 ? C11 H10A 3.110(3) 1_555 2_655 ? C12 C15 3.795(5) 1_555 2_665 ? C12 C16 3.863(5) 1_555 2_665 ? C13 C13 3.617(5) 1_555 2_665 ? C13 C14 3.457(5) 1_555 2_665 ? C14 C14 3.832(5) 1_555 2_665 ? C17 H9A 2.999(6) 1_555 2_665 ? C17 H10B 3.011(7) 1_555 1_465 ? C18 C18 3.585(7) 1_555 2_576 ? C18 H18A 2.876(5) 1_555 2_576 ? C18 H9A 3.054(4) 1_555 2_665 ? C22 H18B 3.027(4) 1_555 2_566 ? H17A H10B 2.3379 1_555 1_465 ? H17B H9A 2.2992 1_555 2_665 ? H18A H18A 2.3844 1_555 2_576 ? Ni1 S3 4.457(1) 1_555 1_556 ? Ni1 S3 4.457(1) 1_555 2_565 ? Ni1 S4 4.169(1) 1_555 1_455 ? Ni1 S4 4.169(1) 1_555 2_666 ? Ni1 S5 3.683(1) 1_555 1_556 ? Ni1 S5 3.683(1) 1_555 2_565 ? Ni1 C21 3.140(4) 1_555 2_566 ? Ni1 C22 3.150(4) 1_555 2_566 ? S1 S8 3.474(2) 1_555 1_544 ? S1 C9 3.557(5) 1_555 2_654 ? S1 C18 3.761(4) 1_555 1_544 ? S1 H9B 3.095(1) 1_555 2_654 ? S1 H10A 3.045(1) 1_555 2_655 ? S2 S8 3.580(2) 1_555 2_666 ? S2 S20 3.511(2) 1_555 1_655 ? S2 C17 3.899(7) 1_555 1_645 ? S2 C18 3.733(5) 1_555 2_666 ? S2 C22 3.713(4) 1_555 1_655 ? S2 H17A 2.962(1) 1_555 1_645 ? S3 S6 3.472(1) 1_555 2_665 ? S3 S7 3.796(2) 1_555 2_565 ? S3 C21 3.883(5) 1_555 1_554 ? S3 C22 3.693(5) 1_555 1_554 ? S4 S5 3.476(1) 1_555 2_665 ? S4 S8 3.733(1) 1_555 2_666 ? S4 S19 3.658(2) 1_555 2_666 ? S4 S20 3.421(2) 1_555 1_655 ? S4 C14 3.713(4) 1_555 2_665 ? S6 S19 3.571(2) 1_555 2_666 ? S6 O23 3.208(4) 1_555 2_666 ? S6 C11 3.847(4) 1_555 2_665 ? S6 C13 3.837(4) 1_555 2_665 ? S6 C21 3.447(4) 1_555 2_666 ? S7 C21 3.420(5) 1_555 2_565 ? S7 C22 3.604(5) 1_555 2_565 ? S8 S20 3.792(1) 1_555 2_566 ? S8 C9 3.664(5) 1_555 1_566 ? S8 C9 3.772(5) 1_555 2_665 ? S8 C12 3.885(4) 1_555 2_666 ? S8 H9A 2.8705 1_555 2_665 ? S8 H9B 2.969(1) 1_555 1_566 ? S19 S20 3.023(2) 1_555 2_566 ? S20 C18 3.570(4) 1_555 2_566 ? S20 H18B 2.687(1) 1_555 2_566 ? O23 C9 3.207(6) 1_555 2_655 ? O23 C10 3.272(7) 1_555 2_655 ? O23 H9B 2.393(4) 1_555 2_655 ? O24 C9 3.101(7) 1_555 2_655 ? O24 C10 3.332(8) 1_555 2_655 ? O24 C17 3.392(7) 1_555 1_545 ? C9 C9 3.806(8) 1_555 2_654 ? C9 C17 3.886(8) 1_555 2_665 ? C9 C22 3.948(7) 1_555 2_655 ? C9 H17B 3.102(5) 1_555 2_665 ? C10 C17 3.756(9) 1_555 1_645 ? C10 H17A 2.884(6) 1_555 1_645 ? C10 H17B 3.163(6) 1_555 2_665 ? C11 C16 3.796(5) 1_555 2_665 ? C11 H10A 3.110(3) 1_555 2_655 ? C12 C15 3.795(5) 1_555 2_665 ? C12 C16 3.863(5) 1_555 2_665 ? C13 C13 3.617(5) 1_555 2_665 ? C13 C14 3.457(5) 1_555 2_665 ? C14 C14 3.832(5) 1_555 2_665 ? C17 H9A 2.999(6) 1_555 2_665 ? C17 H10B 3.011(7) 1_555 1_465 ? C18 C18 3.585(7) 1_555 2_576 ? C18 H18A 2.876(5) 1_555 2_576 ? C18 H9A 3.054(4) 1_555 2_665 ? C22 H18B 3.027(4) 1_555 2_566 ? H17A H10B 2.3379 1_555 1_465 ? H17B H9A 2.2992 1_555 2_665 ? H18A H18A 2.3844 1_555 2_576 ? #===END data_ET2[Pt(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.03 _chemical_formula_moiety 'C24 H16 O4 S20 Pt1 ' _chemical_formula_weight 1204.79 _cell_length_a 9.097(1) _cell_length_b 13.124(2) _cell_length_c 8.949(2) _cell_angle_alpha 67.37(1) _cell_angle_beta 91.71(1) _cell_angle_gamma 69.56(1) _cell_volume 907.3(3) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '35' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_meas 2.206 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 5.0501 _cell_measurement_temperature '298' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _diffrn_radiation_monochromator 'graphite' _exptl_cryst_F_000 589.93 _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 7979 _reflns_number_total 7381 _reflns_number_observed 3962 _reflns_observed_criterion 'refl_observed_if_I_>_2.50_sigma(I)' _diffrn_reflns_av_R_equivalents ??? _diffrn_reflns_theta_max 32.82 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.068 _refine_ls_wR_factor_obs 0.089 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 3962 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 3.980 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.4158 _refine_ls_shift/esd_mean 0.0852 _refine_diff_density_min -6.59 _refine_diff_density_max 4.97 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.05501 _diffrn_orient_matrix_UB_12 -0.08276 _diffrn_orient_matrix_UB_13 0.08970 _diffrn_orient_matrix_UB_21 -0.10605 _diffrn_orient_matrix_UB_22 -0.00284 _diffrn_orient_matrix_UB_23 0.02156 _diffrn_orient_matrix_UB_31 -0.00181 _diffrn_orient_matrix_UB_32 -0.03444 _diffrn_orient_matrix_UB_33 -0.08183 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.605(2) 0.916(1) 0.794(2) 0.047(8) 1.000 Uij C10 0.548(2) 0.866(2) 0.952(3) 0.06(1) 1.000 Uij C11 0.7998(15) 0.6908(11) 0.8457(17) 0.032(6) 1.000 Uij C12 0.6918(16) 0.6518(12) 0.9241(17) 0.032(6) 1.000 Uij C13 0.8466(14) 0.4933(11) 0.8253(16) 0.028(6) 1.000 Uij C14 0.9026(14) 0.3935(12) 0.7910(17) 0.029(6) 1.000 Uij C15 1.0556(14) 0.2286(11) 0.7015(16) 0.027(5) 1.000 Uij C16 0.9390(16) 0.1977(12) 0.7699(17) 0.033(6) 1.000 Uij C17 1.1342(18) 0.0423(13) 0.6098(20) 0.043(7) 1.000 Uij C18 1.0849(18) -0.0220(12) 0.7691(20) 0.041(7) 1.000 Uij C21 0.4254(17) 0.7447(13) 0.5460(19) 0.039(7) 1.000 Uij C22 0.3077(18) 0.6934(13) 0.6377(19) 0.040(7) 1.000 Uij H9A 0.6296 1.0007 0.7650 0.05 1.000 Uiso H9B 0.5765 0.9136 0.7031 0.05 1.000 Uiso H10A 0.4733 0.9217 0.9382 0.05 1.000 Uiso H10B 0.6538 0.8677 1.0402 0.05 1.000 Uiso H17A 1.0465 0.0844 0.5186 0.05 1.000 Uiso H17B 1.2248 -0.0181 0.5849 0.05 1.000 Uiso H18A 1.1751 -0.0448 0.8646 0.05 1.000 Uiso H18B 1.0811 -0.0963 0.7702 0.05 1.000 Uiso O23 0.4276(15) 0.8375(11) 0.5479(17) 0.063(7) 1.000 Uij O24 0.2147(17) 0.7513(12) 0.6989(18) 0.074(8) 1.000 Uij S1 0.8931(4) 0.0753(3) 0.7874(5) 0.041(2) 1.000 Uij S2 1.2071(4) 0.1522(3) 0.6200(5) 0.038(2) 1.000 Uij S3 0.8127(4) 0.2925(3) 0.8424(5) 0.038(2) 1.000 Uij S4 1.0631(4) 0.3614(3) 0.6942(5) 0.035(2) 1.000 Uij S5 0.6892(4) 0.5200(3) 0.9259(5) 0.041(2) 1.000 Uij S6 0.9248(4) 0.6020(3) 0.7615(5) 0.035(2) 1.000 Uij S7 0.5525(5) 0.7184(4) 1.0214(6) 0.055(2) 1.000 Uij S8 0.8169(5) 0.8256(4) 0.8140(6) 0.051(2) 1.000 Uij S19 0.5431(5) 0.6732(3) 0.4397(5) 0.043(2) 1.000 Uij S20 0.3073(4) 0.5616(3) 0.6418(5) 0.041(2) 1.000 Uij Pt1 0.50000 0.50000 0.50000 0.0255(4) 0.500 Uij loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.051(9) 0.019(6) 0.054(10)-0.009(6) 0.009(8) -0.012(7) C10 0.045(9) 0.038(9) 0.086(14)-0.009(7) 0.037(10)-0.033(10) C11 0.028(6) 0.024(6) 0.035(7) -0.013(5) 0.015(5) -0.016(5) C12 0.030(6) 0.026(6) 0.033(7) -0.013(5) 0.016(5) -0.015(5) C13 0.023(6) 0.019(5) 0.033(7) -0.006(5) 0.011(5) -0.012(5) C14 0.020(5) 0.025(6) 0.034(7) -0.007(5) 0.007(5) -0.016(6) C15 0.021(5) 0.021(5) 0.033(7) -0.011(4) 0.012(5) -0.014(5) C16 0.031(6) 0.028(6) 0.033(7) -0.016(5) 0.012(5) -0.018(6) C17 0.041(8) 0.033(7) 0.047(9) -0.017(6) 0.025(7) -0.025(7) C18 0.043(8) 0.024(6) 0.045(8) -0.018(6) 0.016(7) -0.016(6) C21 0.034(7) 0.030(7) 0.041(8) -0.008(6) 0.004(6) -0.024(6) C22 0.035(7) 0.032(7) 0.037(8) -0.005(6) 0.012(6) -0.018(6) O23 0.055(7) 0.048(7) 0.077(9) -0.025(6) 0.021(6) -0.047(7) O24 0.075(9) 0.051(8) 0.079(9) -0.016(7) 0.049(8) -0.048(7) S1 0.033(2) 0.036(2) 0.048(2) -0.023(2) 0.018(2) -0.027(2) S2 0.033(2) 0.030(2) 0.044(2) -0.015(1) 0.023(2) -0.023(2) S3 0.029(2) 0.034(2) 0.043(2) -0.018(1) 0.020(1) -0.025(2) S4 0.028(2) 0.028(2) 0.041(2) -0.015(1) 0.017(1) -0.021(2) S5 0.037(2) 0.035(2) 0.044(2) -0.022(2) 0.024(2) -0.025(2) S6 0.028(2) 0.031(2) 0.039(2) -0.015(1) 0.019(1) -0.020(2) S7 0.052(2) 0.045(2) 0.060(3) -0.027(2) 0.043(2) -0.035(2) S8 0.039(2) 0.040(2) 0.067(3) -0.026(2) 0.028(2) -0.035(2) S19 0.040(2) 0.036(2) 0.048(2) -0.025(2) 0.025(2) -0.028(2) S20 0.031(2) 0.039(2) 0.044(2) -0.016(2) 0.023(2) -0.026(2) Pt1 0.0178(3) 0.0262(4) 0.0280(4) -.0110(3) 0.0112(3) -.0190(3) 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 C10 C9 S8 C11 63.4(13) . . . . yes S8 C9 C10 S7 -62.6(13) . . . . yes C9 C10 S7 C12 21.8(14) . . . . yes C12 C11 S6 C13 -0.6(12) . . . . yes S6 C11 C12 S5 -1.5(8) . . . . yes S6 C11 C12 S7 179.5(18) . . . . yes C12 C11 S8 C9 -32.5(13) . . . . yes S8 C11 C12 S5 175.2(18) . . . . yes S8 C11 C12 S7 -3.8(9) . . . . yes S6 C11 S8 C9 144.2(10) . . . . yes S8 C11 S6 C13 -177.6(10) . . . . yes C11 C12 S5 C13 2.8(12) . . . . yes C11 C12 S7 C10 14.1(14) . . . . yes S5 C12 S7 C10 -164.9(11) . . . . yes S7 C12 S5 C13 -178.1(9) . . . . yes C14 C13 S5 C12 179.6(13) . . . . yes S5 C13 C14 S3 2.0(8) . . . . yes S5 C13 C14 S4 -178.5(18) . . . . yes C14 C13 S6 C11 179.8(13) . . . . yes S6 C13 C14 S3 -175.1(17) . . . . yes S6 C13 C14 S4 4.4(8) . . . . yes S5 C13 S6 C11 2.6(8) . . . . yes S6 C13 S5 C12 -3.2(8) . . . . yes C13 C14 S3 C16 -179.3(13) . . . . yes C13 C14 S4 C15 179.2(13) . . . . yes S3 C14 S4 C15 -1.3(8) . . . . yes S4 C14 S3 C16 1.2(8) . . . . yes C16 C15 S2 C17 12.8(13) . . . . yes S2 C15 C16 S1 -4.6(8) . . . . yes S2 C15 C16 S3 178.4(18) . . . . yes C16 C15 S4 C14 0.9(11) . . . . yes S4 C15 C16 S1 176.7(18) . . . . yes S4 C15 C16 S3 -0.3(8) . . . . yes S2 C15 S4 C14 -177.9(9) . . . . yes S4 C15 S2 C17 -168.5(9) . . . . yes C15 C16 S1 C18 22.0(14) . . . . yes C15 C16 S3 C14 -0.5(12) . . . . yes S1 C16 S3 C14 -177.9(9) . . . . yes S3 C16 S1 C18 -160.9(10) . . . . yes C18 C17 S2 C15 -48.0(11) . . . . yes S2 C17 C18 S1 75.7(11) . . . . yes C17 C18 S1 C16 -55.9(11) . . . . yes O23 C21 C22 O24 4.7(16) . . . . yes O23 C21 C22 S20 -178.0(20) . . . . yes S19 C21 C22 O24 -173.1(20) . . . . yes S19 C21 C22 S20 4.2(9) . . . . yes C22 C21 S19 Pt1 -6.6(11) . . . . yes O23 C21 S19 Pt1 175.7(15) . . . . yes C21 C22 S20 Pt1 0.7(10) . . . . yes O24 C22 S20 Pt1 177.8(16) . . . . yes C21 S19 Pt1 S20 5.3(6) . . . . yes Pt1 S19 C21 C22 -6.6(11) . . . . yes Pt1 S19 C21 O23 175.7(15) . . . . yes C21 S19 Pt1 S20 5.3(6) . . . . yes C22 S20 Pt1 S19 -3.5(6) . . . . yes Pt1 S20 C22 C21 0.7(10) . . . . yes Pt1 S20 C22 O24 177.8(16) . . . . yes C22 S20 Pt1 S19 -3.5(6) . . . . yes S20 Pt1 S19 C21 -174.7(6) . . . . yes S19 Pt1 S20 C22 176.5(6) . . . . yes H9A C9 C10 H10A 57.2(21) . . . . yes H9A C9 C10 H10B -49.9(17) . . . . yes H9A C9 C10 S7 -166.2(23) . . . . yes H9B C9 C10 H10A -88.4(28) . . . . yes H9B C9 C10 H10B 164.5(27) . . . . yes H9B C9 C10 S7 48.3(22) . . . . yes S8 C9 C10 H10A 160.8(21) . . . . yes S8 C9 C10 H10B 53.6(12) . . . . yes H9A C9 S8 C11 -176.3(13) . . . . yes H9B C9 S8 C11 -66.6(16) . . . . yes H10A C10 S7 C12 147.0(24) . . . . yes H10B C10 S7 C12 -86.1(14) . . . . yes H17A C17 C18 H18A -164.8(20) . . . . yes H17A C17 C18 H18B 78.7(17) . . . . yes H17A C17 C18 S1 -44.1(13) . . . . yes H17B C17 C18 H18A 74.2(16) . . . . yes H17B C17 C18 H18B -42.4(15) . . . . yes H17B C17 C18 S1 -165.1(17) . . . . yes S2 C17 C18 H18A -45.0(12) . . . . yes S2 C17 C18 H18B -161.5(17) . . . . yes H17A C17 S2 C15 74.6(13) . . . . yes H17B C17 S2 C15 -169.1(13) . . . . yes H18A C18 S1 C16 61.8(12) . . . . yes H18B C18 S1 C16 -176.9(14) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.51(3) . . yes C9 S8 1.834(18) . . yes C10 S7 1.782(19) . . yes C11 C12 1.35(2) . . yes C11 S6 1.738(15) . . yes C11 S8 1.744(14) . . yes C12 S5 1.732(14) . . yes C12 S7 1.734(16) . . yes C13 C14 1.386(19) . . yes C13 S5 1.718(15) . . yes C13 S6 1.724(13) . . yes C14 S3 1.717(14) . . yes C14 S4 1.728(15) . . yes C15 C16 1.346(19) . . yes C15 S2 1.759(14) . . yes C15 S4 1.744(13) . . yes C16 S1 1.749(14) . . yes C16 S3 1.719(15) . . yes C17 C18 1.52(3) . . yes C17 S2 1.815(16) . . yes C18 S1 1.823(17) . . yes C21 C22 1.55(3) . . yes C21 O23 1.23(2) . . yes C21 S19 1.726(17) . . yes C22 O24 1.22(3) . . yes C22 S20 1.717(16) . . yes S19 Pt1 2.303(4) . . yes S19 Pt1 2.303(4) . 2_656 yes S20 Pt1 2.296(5) . . yes S20 Pt1 2.296(5) . 2_656 yes C9 H9A 1.15(2) . . yes C9 H9B 0.86(3) . . yes C10 H10A 0.766(19) . . yes C10 H10B 1.235(19) . . yes C17 H17A 0.956(15) . . yes C17 H17B 1.024(17) . . yes C18 H18A 1.041(16) . . yes C18 H18B 0.984(15) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 S8 110.4(13) . . . yes C9 C10 S7 117.9(13) . . . yes C12 C11 S6 116.9(11) . . . yes C12 C11 S8 125.4(11) . . . yes S6 C11 S8 117.6(8) . . . yes C11 C12 S5 116.5(11) . . . yes C11 C12 S7 128.2(11) . . . yes S5 C12 S7 115.3(8) . . . yes C14 C13 S5 122.2(10) . . . yes C14 C13 S6 122.0(10) . . . yes S5 C13 S6 115.7(8) . . . yes C13 C14 S3 121.0(10) . . . yes C13 C14 S4 123.8(10) . . . yes S3 C14 S4 115.2(8) . . . yes C16 C15 S2 129.2(11) . . . yes C16 C15 S4 116.8(10) . . . yes S2 C15 S4 114.1(7) . . . yes C15 C16 S1 128.1(11) . . . yes C15 C16 S3 116.9(11) . . . yes S1 C16 S3 114.9(8) . . . yes C18 C17 S2 112.8(11) . . . yes C17 C18 S1 110.6(11) . . . yes C22 C21 O23 118.4(14) . . . yes C22 C21 S19 119.1(11) . . . yes O23 C21 S19 122.5(13) . . . yes C21 C22 O24 118.2(14) . . . yes C21 C22 S20 119.0(11) . . . yes O24 C22 S20 122.7(13) . . . yes C16 S1 C18 99.4(7) . . . yes C15 S2 C17 100.2(7) . . . yes C14 S3 C16 96.1(7) . . . yes C14 S4 C15 95.1(7) . . . yes C12 S5 C13 95.6(7) . . . yes C11 S6 C13 95.1(7) . . . yes C10 S7 C12 104.1(9) . . . yes C9 S8 C11 98.1(7) . . . yes C21 S19 Pt1 105.9(6) . . . yes C21 S19 Pt1 105.9(6) . . 2_656 yes C22 S20 Pt1 106.5(6) . . . yes C22 S20 Pt1 106.5(6) . . 2_656 yes S19 Pt1 S19 180.0 . . 2_656 yes S19 Pt1 S20 89.1(2) . . . yes S19 Pt1 S20 90.9(2) . . 2_656 yes S19 Pt1 S20 90.9(2) 2_656 . . yes S19 Pt1 S20 89.1(2) 2_656 . 2_656 yes S20 Pt1 S20 180.0 . . 2_656 yes C10 C9 H9A 117.4(16) . . . yes C10 C9 H9B 125.2(20) . . . yes H9A C9 H9B 109.5(20) . . . yes H9A C9 S8 92.0(13) . . . yes H9B C9 S8 94.1(16) . . . yes C9 C10 H10A 99.2(20) . . . yes C9 C10 H10B 95.3(14) . . . yes H10A C10 H10B 105.9(19) . . . yes H10A C10 S7 124.0(19) . . . yes H10B C10 S7 110.2(14) . . . yes C18 C17 H17A 111.4(15) . . . yes C18 C17 H17B 110.2(14) . . . yes H17A C17 H17B 108.9(16) . . . yes H17A C17 S2 106.6(12) . . . yes H17B C17 S2 106.7(12) . . . yes C17 C18 H18A 106.2(14) . . . yes C17 C18 H18B 108.6(14) . . . yes H18A C18 H18B 108.5(15) . . . yes H18A C18 S1 111.1(12) . . . yes H18B C18 S1 111.6(13) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 S1 3.87(2) 1_555 1_565 ? C9 S2 3.64(2) 1_555 1_465 ? C10 C10 3.75(3) 1_555 2_677 ? C10 H18A 3.14(2) 1_555 1_465 ? C11 C13 3.66(2) 1_555 2_767 ? C11 C14 3.71(2) 1_555 2_767 ? C11 S2 3.86(1) 1_555 2_766 ? C12 S20 3.81(1) 1_555 2_667 ? C13 S6 3.71(1) 1_555 2_767 ? C13 Pt1 4.18(1) 1_555 2_666 ? C14 S8 3.71(1) 1_555 2_767 ? C14 Pt1 3.90(1) 1_555 2_666 ? C15 C22 3.98(2) 1_555 2_666 ? C15 H10B 3.00(1) 1_555 2_767 ? C15 S20 3.80(1) 1_555 2_666 ? C16 C18 3.93(2) 1_555 2_757 ? C16 C21 3.95(2) 1_555 2_666 ? C16 C22 3.69(2) 1_555 2_666 ? C16 S20 3.77(1) 1_555 2_666 ? C16 Pt1 4.30(1) 1_555 2_666 ? C17 C17 3.79(2) 1_555 2_756 ? C17 H17A 3.17(2) 1_555 2_756 ? C17 O23 3.30(2) 1_555 1_645 ? C17 O24 3.38(2) 1_555 1_645 ? C17 S8 3.63(2) 1_555 2_766 ? C18 O24 3.11(2) 1_555 1_645 ? C18 S1 3.74(2) 1_555 2_757 ? C18 S3 3.68(2) 1_555 2_757 ? C18 S8 3.60(2) 1_555 1_545 ? C21 H17B 3.17(2) 1_555 1_465 ? C21 S1 3.49(1) 1_555 2_666 ? C21 Pt1 3.23(1) 1_555 2_666 ? C22 S1 3.72(1) 1_555 2_666 ? C22 S5 3.82(2) 1_555 2_667 ? C22 Pt1 3.23(2) 1_555 2_666 ? H9A S1 2.92(1) 1_555 1_565 ? H17B O23 2.28(1) 1_555 1_645 ? H18A S1 3.094(6) 1_555 2_757 ? H18B O24 2.28(1) 1_555 1_645 ? H18B S8 2.907(5) 1_555 1_545 ? S1 S1 3.641(5) 1_555 2_757 ? S1 S8 3.503(6) 1_555 1_545 ? S2 S6 3.475(5) 1_555 2_766 ? S2 S8 3.775(6) 1_555 2_766 ? S2 S19 3.670(5) 1_555 2_766 ? S3 S7 3.603(6) 1_555 2_667 ? S3 Pt1 3.542(3) 1_555 2_666 ? S4 S4 3.708(5) 1_555 2_766 ? S4 S19 3.744(5) 1_555 2_766 ? S5 S20 3.591(6) 1_555 2_667 ? S5 Pt1 4.272(4) 1_555 2_666 ? S6 S20 3.593(5) 1_555 1_655 ? S7 S19 3.566(6) 1_555 1_556 ? S7 S20 3.491(6) 1_555 2_667 ? S7 Pt1 4.292(5) 1_555 1_556 ? S7 Pt1 4.292(5) 1_555 2_667 ? S19 S20 3.277(6) 1_555 2_666 ? C9 S1 3.87(2) 1_555 1_565 ? C9 S2 3.64(2) 1_555 1_465 ? C10 C10 3.75(3) 1_555 2_677 ? C10 H18A 3.14(2) 1_555 1_465 ? C11 C13 3.66(2) 1_555 2_767 ? C11 C14 3.71(2) 1_555 2_767 ? C11 S2 3.86(1) 1_555 2_766 ? C12 S20 3.81(1) 1_555 2_667 ? C13 S6 3.71(1) 1_555 2_767 ? C13 Pt1 4.18(1) 1_555 2_666 ? C14 S8 3.71(1) 1_555 2_767 ? C14 Pt1 3.90(1) 1_555 2_666 ? C15 C22 3.98(2) 1_555 2_666 ? C15 H10B 3.00(1) 1_555 2_767 ? C15 S20 3.80(1) 1_555 2_666 ? C16 C18 3.93(2) 1_555 2_757 ? C16 C21 3.95(2) 1_555 2_666 ? C16 C22 3.69(2) 1_555 2_666 ? C16 S20 3.77(1) 1_555 2_666 ? C16 Pt1 4.30(1) 1_555 2_666 ? C17 C17 3.79(2) 1_555 2_756 ? C17 H17A 3.17(2) 1_555 2_756 ? C17 O23 3.30(2) 1_555 1_645 ? C17 O24 3.38(2) 1_555 1_645 ? C17 S8 3.63(2) 1_555 2_766 ? C18 O24 3.11(2) 1_555 1_645 ? C18 S1 3.74(2) 1_555 2_757 ? C18 S3 3.68(2) 1_555 2_757 ? C18 S8 3.60(2) 1_555 1_545 ? C21 H17B 3.17(2) 1_555 1_465 ? C21 S1 3.49(1) 1_555 2_666 ? C21 Pt1 3.23(1) 1_555 2_666 ? C22 S1 3.72(1) 1_555 2_666 ? C22 S5 3.82(2) 1_555 2_667 ? C22 Pt1 3.23(2) 1_555 2_666 ? H9A S1 2.92(1) 1_555 1_565 ? H17B O23 2.28(1) 1_555 1_645 ? H18A S1 3.094(6) 1_555 2_757 ? H18B O24 2.28(1) 1_555 1_645 ? H18B S8 2.907(5) 1_555 1_545 ? S1 S1 3.641(5) 1_555 2_757 ? S1 S8 3.503(6) 1_555 1_545 ? S2 S6 3.475(5) 1_555 2_766 ? S2 S8 3.775(6) 1_555 2_766 ? S2 S19 3.670(5) 1_555 2_766 ? S3 S7 3.603(6) 1_555 2_667 ? S3 Pt1 3.542(3) 1_555 2_666 ? S4 S4 3.708(5) 1_555 2_766 ? S4 S19 3.744(5) 1_555 2_766 ? S5 S20 3.591(6) 1_555 2_667 ? S5 Pt1 4.272(4) 1_555 2_666 ? S6 S20 3.593(5) 1_555 1_655 ? S7 S19 3.566(6) 1_555 1_556 ? S7 S20 3.491(6) 1_555 2_667 ? S7 Pt1 4.292(5) 1_555 1_556 ? S7 Pt1 4.292(5) 1_555 2_667 ? S19 S20 3.277(6) 1_555 2_666 ? #===END data_ET4[Pd(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _chemical_formula_moiety 'C48 H32 O4 S36 Pd1 ' _chemical_formula_weight 1933.58 _cell_length_a 12.818(4) _cell_length_b 17.867(2) _cell_length_c 7.627(1) _cell_angle_alpha 95.66(1) _cell_angle_beta 102.99(2) _cell_angle_gamma 104.63(3) _cell_volume 1624.3(6) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '28.5' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_meas ???? _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_cryst_F_000 973.96 _exptl_absorpt_coefficient_mu 1.4417 _cell_measurement_temperature '298' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _diffrn_radiation_monochromator 'graphite' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 8745 _reflns_number_total 8144 _reflns_number_observed 4969 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents 0.007 _diffrn_reflns_theta_max 24.23 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.035 _refine_ls_wR_factor_obs 0.041 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 4969 _refine_ls_number_parameters 385 _refine_ls_goodness_of_fit_obs 1.633 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.1490 _refine_ls_shift/esd_mean 0.0138 _refine_diff_density_min -0.86 _refine_diff_density_max 0.64 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.02473 _diffrn_orient_matrix_UB_12 -0.03240 _diffrn_orient_matrix_UB_13 0.09192 _diffrn_orient_matrix_UB_21 0.05386 _diffrn_orient_matrix_UB_22 0.04837 _diffrn_orient_matrix_UB_23 0.07984 _diffrn_orient_matrix_UB_31 -0.05880 _diffrn_orient_matrix_UB_32 0.00709 _diffrn_orient_matrix_UB_33 0.06154 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C10 0.6693(6) 0.7725(3) 0.2291(14) 0.098(5) 1.000 Uij C11 0.7571(6) 0.7685(4) 0.1648(15) 0.111(5) 1.000 Uij C12 0.6177(4) 0.6156(2) 0.2319(7) 0.035(2) 1.000 Uij C13 0.7208(4) 0.6162(2) 0.2208(7) 0.033(2) 1.000 Uij C14 0.6299(4) 0.4756(3) 0.2638(7) 0.035(2) 1.000 Uij C15 0.6066(4) 0.3980(3) 0.2792(7) 0.034(2) 1.000 Uij C16 0.5064(4) 0.2553(2) 0.2968(7) 0.033(2) 1.000 Uij C17 0.6071(4) 0.2536(2) 0.2778(7) 0.033(2) 1.000 Uij C18 0.4484(4) 0.0944(3) 0.2923(7) 0.037(2) 1.000 Uij C19 0.5249(4) 0.0970(3) 0.1663(7) 0.038(2) 1.000 Uij C20 0.9224(4) 0.8035(3) 0.7861(8) 0.045(3) 1.000 Uij C21 1.0035(4) 0.8031(3) 0.6683(8) 0.047(3) 1.000 Uij C22 0.8574(4) 0.6445(2) 0.7152(7) 0.033(2) 1.000 Uij C23 0.9611(4) 0.6460(3) 0.7069(7) 0.035(2) 1.000 Uij C24 0.8701(4) 0.5047(3) 0.7453(7) 0.037(2) 1.000 Uij C25 0.8452(4) 0.4271(3) 0.7586(7) 0.037(2) 1.000 Uij C26 0.7406(4) 0.2839(2) 0.7605(7) 0.034(2) 1.000 Uij C27 0.8429(4) 0.2823(3) 0.7497(7) 0.035(2) 1.000 Uij C28 0.6805(4) 0.1220(3) 0.7596(7) 0.041(3) 1.000 Uij C29 0.8023(4) 0.1410(3) 0.8567(7) 0.041(3) 1.000 Uij C33 0.2226(4) 0.0078(3) 0.7992(7) 0.039(2) 1.000 Uij C34 0.2649(4) 0.0242(3) 0.6277(7) 0.042(3) 1.000 Uij O35 0.2865(3) -0.0071(3) 0.9265(6) 0.065(3) 1.000 Uij O36 0.3643(3) 0.0354(3) 0.6424(6) 0.070(3) 1.000 Uij S10 0.55537(11) 0.69139(7) 0.21965(24) 0.0555(7) 1.000 Uij S11 0.82653(11) 0.69387(7) 0.19410(20) 0.0430(6) 1.000 Uij S12 0.53287(10) 0.52793(7) 0.26706(20) 0.0417(6) 1.000 Uij S13 0.75772(10) 0.52906(7) 0.23940(20) 0.0425(6) 1.000 Uij S14 0.47919(10) 0.34678(6) 0.30912(19) 0.0384(6) 1.000 Uij S15 0.69884(10) 0.34293(7) 0.26560(20) 0.0401(6) 1.000 Uij S16 0.39355(11) 0.17812(7) 0.30686(21) 0.0459(7) 1.000 Uij S17 0.65694(10) 0.17136(6) 0.25707(19) 0.0384(6) 1.000 Uij S20 0.79738(11) 0.72182(7) 0.70306(20) 0.0430(6) 1.000 Uij S21 1.06761(11) 0.72431(7) 0.68447(22) 0.0482(7) 1.000 Uij S22 0.77305(10) 0.55743(7) 0.75212(20) 0.0430(6) 1.000 Uij S23 0.99948(10) 0.55946(7) 0.72908(21) 0.0429(6) 1.000 Uij S24 0.71661(10) 0.37620(7) 0.78530(20) 0.0434(6) 1.000 Uij S25 0.94033(10) 0.37277(7) 0.76155(21) 0.0443(6) 1.000 Uij S26 0.62549(11) 0.20634(7) 0.75969(20) 0.0428(6) 1.000 Uij S27 0.89115(11) 0.19919(7) 0.73605(20) 0.0450(7) 1.000 Uij S31 0.09046(11) 0.01344(7) 0.80447(18) 0.0420(6) 1.000 Uij S32 0.17019(11) 0.02709(8) 0.43075(19) 0.0463(7) 1.000 Uij Pd1 0.0000(12) 0.0000(8) 0.5000(19) 0.0334(2) 0.500 Uij H18A 0.49130 0.09190 0.41717 0.05 1.000 Uiso H18B 0.38407 0.04578 0.24851 0.05 1.000 Uiso H19A 0.48612 0.10847 0.04685 0.05 1.000 Uiso H19B 0.53892 0.04465 0.14589 0.05 1.000 Uiso H10A 0.63393 0.81356 0.17603 0.05 1.000 Uiso H10B 0.70121 0.79125 0.36219 0.05 1.000 Uiso H11A 0.81187 0.82000 0.20549 0.05 1.000 Uiso H11B 0.72106 0.76139 0.03004 0.05 1.000 Uiso H21A 1.05978 0.85399 0.70366 0.05 1.000 Uiso H21B 0.95750 0.79839 0.53850 0.05 1.000 Uiso H20A 0.89729 0.85371 0.78763 0.05 1.000 Uiso H20B 0.95483 0.79960 0.91332 0.05 1.000 Uiso H28A 0.63656 0.08233 0.81903 0.05 1.000 Uiso H28B 0.67041 0.09865 0.63013 0.05 1.000 Uiso H29A 0.82293 0.09116 0.86980 0.05 1.000 Uiso H29B 0.81395 0.17114 0.98084 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C10 0.066(4) 0.031(3) 0.197(9) 0.022(3) 0.067(5) 0.046(4) C11 0.067(5) 0.032(3) 0.232(11) 0.022(3) 0.075(6) 0.056(5) C12 0.032(2) 0.019(2) 0.049(3) 0.006(2) 0.018(2) 0.007(2) C13 0.034(2) 0.017(2) 0.043(3) 0.006(2) 0.015(2) 0.005(2) C14 0.028(2) 0.020(2) 0.053(3) 0.005(2) 0.016(2) 0.009(2) C15 0.030(2) 0.021(2) 0.048(3) 0.007(2) 0.015(2) 0.008(2) C16 0.036(3) 0.020(2) 0.042(3) 0.008(2) 0.017(2) 0.008(2) C17 0.034(2) 0.019(2) 0.041(3) 0.008(2) 0.014(2) 0.010(2) C18 0.036(3) 0.020(2) 0.049(3) 0.006(2) 0.014(2) 0.009(2) C19 0.036(3) 0.024(2) 0.048(3) 0.008(2) 0.013(2) 0.002(2) C20 0.046(3) 0.027(2) 0.056(3) 0.013(2) 0.016(3) 0.006(2) C21 0.045(3) 0.026(2) 0.064(4) 0.008(2) 0.019(3) 0.014(2) C22 0.031(2) 0.021(2) 0.042(3) 0.008(2) 0.013(2) 0.007(2) C23 0.033(2) 0.019(2) 0.049(3) 0.006(2) 0.017(2) 0.004(2) C24 0.033(2) 0.022(2) 0.052(3) 0.007(2) 0.017(2) 0.008(2) C25 0.033(2) 0.022(2) 0.052(3) 0.007(2) 0.017(2) 0.008(2) C26 0.038(3) 0.019(2) 0.043(3) 0.008(2) 0.015(2) 0.008(2) C27 0.036(3) 0.022(2) 0.044(3) 0.008(2) 0.014(2) 0.008(2) C28 0.045(3) 0.021(2) 0.052(3) 0.008(2) 0.016(2) 0.008(2) C29 0.048(3) 0.028(2) 0.044(3) 0.012(2) 0.017(2) 0.014(2) C33 0.041(3) 0.025(2) 0.042(3) 0.004(2) 0.006(2) 0.008(2) C34 0.044(3) 0.030(2) 0.050(3) 0.014(2) 0.018(2) 0.013(2) O35 0.049(2) 0.083(3) 0.053(3) 0.018(2) 0.009(2) 0.027(2) O36 0.047(2) 0.088(3) 0.073(3) 0.030(2) 0.026(2) 0.041(3) S10 0.0397(7) 0.0263(6) 0.0992(12)0.0163(6) 0.0332(8) 0.0206(7) S11 0.0359(7) 0.0228(6) 0.0668(9) 0.0056(5) 0.0266(6) 0.0128(6) S12 0.0311(6) 0.0215(6) 0.0694(9) 0.0073(5) 0.0238(6) 0.0128(6) S13 0.0313(6) 0.0216(6) 0.0721(9) 0.0094(5) 0.0241(6) 0.0147(6) S14 0.0326(6) 0.0187(5) 0.0609(8) 0.0071(5) 0.0225(6) 0.0088(5) S15 0.0310(6) 0.0210(5) 0.0654(9) 0.0075(5) 0.0221(6) 0.0129(5) S16 0.0357(7) 0.0214(6) 0.0779(10)0.0077(5) 0.0296(7) 0.0139(6) S17 0.0307(6) 0.0220(5) 0.0588(8) 0.0099(5) 0.0160(6) 0.0099(5) S20 0.0355(7) 0.0284(6) 0.0625(9) 0.0138(5) 0.0195(6) 0.0164(6) S21 0.0365(7) 0.0230(6) 0.0803(10)0.0036(5) 0.0297(7) 0.0087(6) S22 0.0338(6) 0.0235(6) 0.0693(9) 0.0087(5) 0.0257(6) 0.0137(6) S23 0.0314(6) 0.0218(6) 0.0716(9) 0.0081(5) 0.0214(6) 0.0094(6) S24 0.0363(7) 0.0212(6) 0.0697(9) 0.0091(5) 0.0256(6) 0.0121(6) S25 0.0339(7) 0.0219(6) 0.0725(10)0.0076(5) 0.0219(6) 0.0085(6) S26 0.0356(7) 0.0226(6) 0.0662(9) 0.0077(5) 0.0207(6) 0.0142(6) S27 0.0440(7) 0.0260(6) 0.0636(9) 0.0155(5) 0.0270(7) 0.0141(6) S31 0.0433(7) 0.0364(7) 0.0406(7) 0.0094(6) 0.0153(6) 0.0082(5) S32 0.0445(7) 0.0477(8) 0.0429(7) 0.0160(6) 0.0180(6) 0.0168(6) Pd1 0.0368(3) 0.0221(2) 0.0372(3) 0.0095(2) 0.0122(2) 0.0079(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 C11 C10 S10 C12 30.5(8) . . . . yes S10 C10 C11 S11 -42.6(7) . . . . yes C10 C11 S11 C13 25.8(8) . . . . yes C13 C12 S10 C10 -9.8(6) . . . . yes S10 C12 C13 S11 1.2(3) . . . . yes S10 C12 C13 S13 179.8(7) . . . . yes C13 C12 S12 C14 -2.0(4) . . . . yes S12 C12 C13 S11 -177.7(7) . . . . yes S12 C12 C13 S13 0.9(3) . . . . yes S12 C12 S10 C10 169.1(4) . . . . yes S10 C12 S12 C14 178.9(4) . . . . yes C12 C13 S11 C11 -5.1(6) . . . . yes C12 C13 S13 C14 0.7(4) . . . . yes S13 C13 S11 C11 176.3(4) . . . . yes S11 C13 S13 C14 179.5(3) . . . . yes C15 C14 S12 C12 -177.5(5) . . . . yes S12 C14 C15 S14 -1.7(3) . . . . yes S12 C14 C15 S15 176.8(7) . . . . yes C15 C14 S13 C13 177.9(5) . . . . yes S13 C14 C15 S14 178.4(7) . . . . yes S13 C14 C15 S15 -3.1(3) . . . . yes S13 C14 S12 C12 2.4(3) . . . . yes S12 C14 S13 C13 -2.1(3) . . . . yes C14 C15 S14 C16 175.2(5) . . . . yes C14 C15 S15 C17 -175.4(5) . . . . yes S15 C15 S14 C16 -3.4(3) . . . . yes S14 C15 S15 C17 3.2(3) . . . . yes C17 C16 S14 C15 2.4(4) . . . . yes S14 C16 C17 S15 -0.5(3) . . . . yes S14 C16 C17 S17 -178.6(7) . . . . yes C17 C16 S16 C18 1.8(5) . . . . yes S16 C16 C17 S15 177.9(7) . . . . yes S16 C16 C17 S17 -0.1(3) . . . . yes S16 C16 S14 C15 -176.3(3) . . . . yes S14 C16 S16 C18 -179.7(4) . . . . yes C16 C17 S15 C15 -1.6(4) . . . . yes C16 C17 S17 C19 24.9(5) . . . . yes S17 C17 S15 C15 176.6(4) . . . . yes S15 C17 S17 C19 -153.2(4) . . . . yes C19 C18 S16 C16 -36.8(4) . . . . yes S16 C18 C19 S17 70.2(4) . . . . yes C18 C19 S17 C17 -58.8(4) . . . . yes C21 C20 S20 C22 58.7(4) . . . . yes S20 C20 C21 S21 -69.2(4) . . . . yes C20 C21 S21 C23 36.3(4) . . . . yes C23 C22 S20 C20 -26.0(5) . . . . yes S20 C22 C23 S21 0.9(3) . . . . yes S20 C22 C23 S23 178.3(7) . . . . yes C23 C22 S22 C24 -4.1(4) . . . . yes S22 C22 C23 S21 -176.1(7) . . . . yes S22 C22 C23 S23 1.3(3) . . . . yes S22 C22 S20 C20 151.0(4) . . . . yes S20 C22 S22 C24 178.5(4) . . . . yes C22 C23 S21 C21 -1.6(5) . . . . yes C22 C23 S23 C24 2.2(4) . . . . yes S23 C23 S21 C21 -179.2(4) . . . . yes S21 C23 S23 C24 -179.9(4) . . . . yes C25 C24 S22 C22 -176.7(5) . . . . yes S22 C24 C25 S24 -0.6(3) . . . . yes S22 C24 C25 S25 -177.4(7) . . . . yes C25 C24 S23 C23 177.3(5) . . . . yes S23 C24 C25 S24 176.9(7) . . . . yes S23 C24 C25 S25 0.1(3) . . . . yes S23 C24 S22 C22 5.6(3) . . . . yes S22 C24 S23 C23 -5.0(3) . . . . yes C24 C25 S24 C26 172.5(5) . . . . yes C24 C25 S25 C27 -172.6(5) . . . . yes S25 C25 S24 C26 -10.4(3) . . . . yes S24 C25 S25 C27 10.4(3) . . . . yes C27 C26 S24 C25 6.3(4) . . . . yes S24 C26 C27 S25 0.0(3) . . . . yes S24 C26 C27 S27 176.6(7) . . . . yes C27 C26 S26 C28 4.6(5) . . . . yes S26 C26 C27 S25 -178.1(7) . . . . yes S26 C26 C27 S27 -1.4(3) . . . . yes S26 C26 S24 C25 -175.4(4) . . . . yes S24 C26 S26 C28 -173.5(4) . . . . yes C26 C27 S25 C25 -6.2(4) . . . . yes C26 C27 S27 C29 -28.3(5) . . . . yes S27 C27 S25 C25 176.8(4) . . . . yes S25 C27 S27 C29 148.3(4) . . . . yes C29 C28 S26 C26 31.0(4) . . . . yes S26 C28 C29 S27 -68.7(4) . . . . yes C28 C29 S27 C27 62.9(4) . . . . yes O35 C33 C34 O36 -13.2(6) . . . . yes O35 C33 C34 S32 168.0(7) . . . . yes S31 C33 C34 O36 165.4(7) . . . . yes S31 C33 C34 S32 -13.5(3) . . . . yes C34 C33 S31 Pd1 20.4(5) . . . . yes O35 C33 S31 Pd1 -161.1(7) . . . . yes C33 C34 S32 Pd1 -1.6(5) . . . . yes O36 C34 S32 Pd1 179.6(7) . . . . yes C33 S31 Pd1 S32 -16.2(4) . . . . yes Pd1 S31 C33 C34 20.4(5) . . . . yes Pd1 S31 C33 O35 -161.1(7) . . . . yes C33 S31 Pd1 S32 -16.2(4) . . . . yes C34 S32 Pd1 S31 10.7(4) . . . . yes Pd1 S32 C34 C33 -1.6(5) . . . . yes Pd1 S32 C34 O36 179.6(7) . . . . yes C34 S32 Pd1 S31 10.7(4) . . . . yes S32 Pd1 S31 C33 163.8(5) . . . . yes S31 Pd1 S32 C34 -169.3(5) . . . . yes S10 C10 C11 H11A -171.2(12) . . . . yes S10 C10 C11 H11B 74.5(8) . . . . yes H10A C10 C11 S11 -169.2(12) . . . . yes H10A C10 C11 H11A 62.2(9) . . . . yes H10A C10 C11 H11B -52.0(8) . . . . yes H10B C10 C11 S11 75.1(9) . . . . yes H10B C10 C11 H11A -53.6(8) . . . . yes H10B C10 C11 H11B -167.8(10) . . . . yes H10A C10 S10 C12 159.7(7) . . . . yes H10B C10 S10 C12 -87.9(6) . . . . yes H11A C11 S11 C13 153.2(8) . . . . yes H11B C11 S11 C13 -88.0(7) . . . . yes S16 C18 C19 H19A -50.1(4) . . . . yes S16 C18 C19 H19B -168.6(6) . . . . yes H18A C18 C19 S17 -50.4(4) . . . . yes H18A C18 C19 H19A -170.7(6) . . . . yes H18A C18 C19 H19B 70.8(5) . . . . yes H18B C18 C19 S17 -168.5(6) . . . . yes H18B C18 C19 H19A 71.2(5) . . . . yes H18B C18 C19 H19B -47.3(5) . . . . yes H18A C18 S16 C16 83.8(4) . . . . yes H18B C18 S16 C16 -158.2(5) . . . . yes H19A C19 S17 C17 60.9(4) . . . . yes H19B C19 S17 C17 180.0(5) . . . . yes S20 C20 C21 H21A 167.6(6) . . . . yes S20 C20 C21 H21B 51.4(4) . . . . yes H20A C20 C21 S21 171.3(7) . . . . yes H20A C20 C21 H21A 48.1(5) . . . . yes H20A C20 C21 H21B -68.2(6) . . . . yes H20B C20 C21 S21 50.5(5) . . . . yes H20B C20 C21 H21A -72.7(6) . . . . yes H20B C20 C21 H21B 171.1(7) . . . . yes H20A C20 S20 C22 -179.0(5) . . . . yes H20B C20 S20 C22 -64.3(4) . . . . yes H21A C21 S21 C23 157.2(5) . . . . yes H21B C21 S21 C23 -81.6(5) . . . . yes S26 C28 C29 H29A 170.2(6) . . . . yes S26 C28 C29 H29B 51.6(4) . . . . yes H28A C28 C29 S27 170.0(6) . . . . yes H28A C28 C29 H29A 49.0(5) . . . . yes H28A C28 C29 H29B -69.6(5) . . . . yes H28B C28 C29 S27 51.8(4) . . . . yes H28B C28 C29 H29A -69.2(5) . . . . yes H28B C28 C29 H29B 172.2(7) . . . . yes H28A C28 S26 C26 152.5(5) . . . . yes H28B C28 S26 C26 -89.4(4) . . . . yes H29A C29 S27 C27 -176.0(5) . . . . yes H29B C29 S27 C27 -56.8(4) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 C11 1.340(12) . . yes C10 S10 1.761(7) . . yes C11 S11 1.785(7) . . yes C12 C13 1.340(7) . . yes C12 S10 1.738(5) . . yes C12 S12 1.750(5) . . yes C13 S11 1.741(5) . . yes C13 S13 1.748(5) . . yes C14 C15 1.365(7) . . yes C14 S12 1.738(5) . . yes C14 S13 1.735(5) . . yes C15 S14 1.735(5) . . yes C15 S15 1.731(5) . . yes C16 C17 1.338(7) . . yes C16 S14 1.754(5) . . yes C16 S16 1.750(5) . . yes C17 S15 1.752(5) . . yes C17 S17 1.750(5) . . yes C18 C19 1.516(8) . . yes C18 S16 1.810(5) . . yes C19 S17 1.807(5) . . yes C20 C21 1.520(8) . . yes C20 S20 1.810(6) . . yes C21 S21 1.802(6) . . yes C22 C23 1.339(7) . . yes C22 S20 1.743(5) . . yes C22 S22 1.744(5) . . yes C23 S21 1.743(5) . . yes C23 S23 1.749(5) . . yes C24 C25 1.361(7) . . yes C24 S22 1.747(5) . . yes C24 S23 1.738(5) . . yes C25 S24 1.737(5) . . yes C25 S25 1.737(5) . . yes C26 C27 1.340(7) . . yes C26 S24 1.753(5) . . yes C26 S26 1.748(5) . . yes C27 S25 1.755(5) . . yes C27 S27 1.749(5) . . yes C28 C29 1.504(8) . . yes C28 S26 1.819(5) . . yes C29 S27 1.812(6) . . yes C33 C34 1.550(8) . . yes C33 O35 1.219(7) . . yes C33 S31 1.731(6) . . yes C34 O36 1.215(7) . . yes C34 S32 1.721(6) . . yes S31 Pd1 2.309(14) . . yes S31 Pd1 2.309(14) . 2_556 yes S32 Pd1 2.304(15) . . yes S32 Pd1 2.304(15) . 2_556 yes C10 H10A 1.026(8) . . yes C10 H10B 0.993(10) . . yes C11 H11A 0.977(7) . . yes C11 H11B 1.008(11) . . yes C18 H18A 0.998(6) . . yes C18 H18B 1.001(5) . . yes C19 H19A 1.002(6) . . yes C19 H19B 1.000(5) . . yes C20 H20A 1.026(5) . . yes C20 H20B 0.983(6) . . yes C21 H21A 0.976(5) . . yes C21 H21B 1.015(6) . . yes C28 H28A 1.000(6) . . yes C28 H28B 1.000(6) . . yes C29 H29A 1.000(5) . . yes C29 H29B 1.002(5) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 C10 S10 124.4(6) . . . yes C10 C11 S11 124.6(7) . . . yes C13 C12 S10 128.8(4) . . . yes C13 C12 S12 117.1(4) . . . yes S10 C12 S12 114.2(3) . . . yes C12 C13 S11 128.6(4) . . . yes C12 C13 S13 117.1(4) . . . yes S11 C13 S13 114.3(3) . . . yes C15 C14 S12 122.1(4) . . . yes C15 C14 S13 122.8(4) . . . yes S12 C14 S13 115.2(3) . . . yes C14 C15 S14 121.6(4) . . . yes C14 C15 S15 123.3(4) . . . yes S14 C15 S15 115.1(3) . . . yes C17 C16 S14 117.0(4) . . . yes C17 C16 S16 129.4(4) . . . yes S14 C16 S16 113.6(3) . . . yes C16 C17 S15 116.8(4) . . . yes C16 C17 S17 127.3(4) . . . yes S15 C17 S17 115.8(3) . . . yes C19 C18 S16 114.2(4) . . . yes C18 C19 S17 112.4(4) . . . yes C21 C20 S20 111.5(4) . . . yes C20 C21 S21 114.5(4) . . . yes C23 C22 S20 127.3(4) . . . yes C23 C22 S22 117.4(4) . . . yes S20 C22 S22 115.2(3) . . . yes C22 C23 S21 128.8(4) . . . yes C22 C23 S23 117.1(4) . . . yes S21 C23 S23 114.1(3) . . . yes C25 C24 S22 121.3(4) . . . yes C25 C24 S23 123.7(4) . . . yes S22 C24 S23 115.0(3) . . . yes C24 C25 S24 121.8(4) . . . yes C24 C25 S25 123.2(4) . . . yes S24 C25 S25 115.0(3) . . . yes C27 C26 S24 116.9(4) . . . yes C27 C26 S26 129.3(4) . . . yes S24 C26 S26 113.8(3) . . . yes C26 C27 S25 117.0(4) . . . yes C26 C27 S27 126.3(4) . . . yes S25 C27 S27 116.6(3) . . . yes C29 C28 S26 114.0(4) . . . yes C28 C29 S27 112.2(4) . . . yes C34 C33 O35 117.3(5) . . . yes C34 C33 S31 119.5(4) . . . yes O35 C33 S31 123.2(5) . . . yes C33 C34 O36 117.3(5) . . . yes C33 C34 S32 118.7(4) . . . yes O36 C34 S32 124.0(5) . . . yes C10 S10 C12 101.8(3) . . . yes C11 S11 C13 101.7(3) . . . yes C12 S12 C14 95.3(3) . . . yes C13 S13 C14 95.4(3) . . . yes C15 S14 C16 95.4(3) . . . yes C15 S15 C17 95.6(3) . . . yes C16 S16 C18 102.5(3) . . . yes C17 S17 C19 98.8(3) . . . yes C20 S20 C22 99.5(3) . . . yes C21 S21 C23 103.3(3) . . . yes C22 S22 C24 95.0(3) . . . yes C23 S23 C24 95.2(3) . . . yes C25 S24 C26 95.1(3) . . . yes C25 S25 C27 94.9(3) . . . yes C26 S26 C28 103.3(3) . . . yes C27 S27 C29 98.1(3) . . . yes C33 S31 Pd1 103.4(4) . . . yes C33 S31 Pd1 103.4(4) . . 2_556 yes C34 S32 Pd1 105.3(4) . . . yes C34 S32 Pd1 105.3(4) . . 2_556 yes S31 Pd1 S31 180.0 . . 2_556 yes S31 Pd1 S32 89.5(5) . . . yes S31 Pd1 S32 90.5(5) . . 2_556 yes S31 Pd1 S32 90.5(5) 2_556 . . yes S31 Pd1 S32 89.5(5) 2_556 . 2_556 yes S32 Pd1 S32 180.0 . . 2_556 yes C11 C10 H10A 111.1(8) . . . yes C11 C10 H10B 104.7(8) . . . yes S10 C10 H10A 104.8(6) . . . yes S10 C10 H10B 103.1(6) . . . yes H10A C10 H10B 107.5(7) . . . yes C10 C11 H11A 106.3(8) . . . yes C10 C11 H11B 99.2(8) . . . yes S11 C11 H11A 109.4(7) . . . yes S11 C11 H11B 106.2(7) . . . yes H11A C11 H11B 110.1(8) . . . yes C19 C18 H18A 108.2(5) . . . yes C19 C18 H18B 108.7(5) . . . yes S16 C18 H18A 108.3(4) . . . yes S16 C18 H18B 108.4(4) . . . yes H18A C18 H18B 108.9(5) . . . yes C18 C19 H19A 108.0(5) . . . yes C18 C19 H19B 109.2(5) . . . yes S17 C19 H19A 109.0(4) . . . yes S17 C19 H19B 109.1(4) . . . yes H19A C19 H19B 109.1(5) . . . yes C21 C20 H20A 111.6(5) . . . yes C21 C20 H20B 112.3(5) . . . yes S20 C20 H20A 106.9(4) . . . yes S20 C20 H20B 106.7(4) . . . yes H20A C20 H20B 107.4(5) . . . yes C20 C21 H21A 106.7(5) . . . yes C20 C21 H21B 105.1(5) . . . yes S21 C21 H21A 110.9(5) . . . yes S21 C21 H21B 109.7(4) . . . yes H21A C21 H21B 109.5(5) . . . yes C29 C28 H28A 108.9(5) . . . yes C29 C28 H28B 108.2(5) . . . yes S26 C28 H28A 108.5(4) . . . yes S26 C28 H28B 108.3(4) . . . yes H28A C28 H28B 108.9(5) . . . yes C28 C29 H29A 109.2(5) . . . yes C28 C29 H29B 108.0(5) . . . yes S27 C29 H29A 109.1(4) . . . yes S27 C29 H29B 109.2(4) . . . yes H29A C29 H29B 109.2(5) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C10 C33 3.865(8) 1_555 2_666 ? C10 C34 3.516(8) 1_555 2_666 ? C10 S16 3.87(1) 1_555 2_666 ? C11 C20 3.96(1) 1_555 1_554 ? C11 C33 3.918(8) 1_555 2_666 ? C11 C34 3.985(8) 1_555 2_666 ? C11 S20 3.72(1) 1_555 1_554 ? C11 S31 3.850(6) 1_555 2_666 ? C13 S22 3.875(5) 1_555 1_554 ? C15 S10 3.862(5) 1_555 2_665 ? C18 C28 3.743(6) 1_555 2_656 ? C18 O35 3.143(6) 1_555 1_554 ? C18 H28A 3.032(4) 1_555 2_656 ? C19 C19 3.908(6) 1_555 2_655 ? C19 O35 3.176(6) 1_555 1_554 ? C19 O35 3.381(6) 1_555 2_656 ? C19 O36 3.344(7) 1_555 2_656 ? C19 H19B 3.103(5) 1_555 2_655 ? C20 C29 3.773(7) 1_555 2_767 ? C20 S27 3.895(6) 1_555 2_767 ? C20 S31 3.796(5) 1_555 1_665 ? C20 Pd1 4.34(2) 1_555 1_665 ? C20 Pd1 4.34(2) 1_555 2_666 ? C21 C29 3.781(8) 1_555 2_767 ? C21 C33 3.885(7) 1_555 1_665 ? C21 S27 3.635(6) 1_555 2_766 ? C21 S31 3.611(5) 1_555 1_665 ? C21 Pd1 3.87(1) 1_555 1_665 ? C21 Pd1 3.87(1) 1_555 2_666 ? C21 H29B 3.041(6) 1_555 2_767 ? C22 S11 3.803(5) 1_555 1_556 ? C27 S21 3.740(5) 1_555 2_766 ? C28 O35 3.328(7) 1_555 2_657 ? C28 H18B 2.891(4) 1_555 2_656 ? C29 C33 3.922(7) 1_555 2_657 ? C29 O35 3.164(7) 1_555 2_657 ? C29 S21 3.808(5) 1_555 2_767 ? C29 S32 3.680(5) 1_555 2_656 ? C29 H20B 3.066(5) 1_555 2_767 ? C33 Pd1 3.19(1) 1_555 2_556 ? C33 H21A 2.909(5) 1_555 1_445 ? C34 Pd1 3.22(1) 1_555 2_556 ? C34 H10A 2.950(5) 1_555 2_666 ? C34 H28B 3.189(5) 1_555 2_656 ? O35 H18B 2.460(4) 1_555 1_556 ? O36 H19B 2.577(5) 1_555 2_656 ? S10 S24 3.379(2) 1_555 2_666 ? S10 S26 3.314(2) 1_555 2_666 ? S11 S20 3.775(2) 1_555 1_554 ? S11 S22 3.778(2) 1_555 1_554 ? S11 S25 3.447(2) 1_555 2_766 ? S11 S27 3.531(2) 1_555 2_766 ? S12 S22 3.795(2) 1_555 2_666 ? S14 S20 3.422(2) 1_555 2_666 ? S15 S21 3.456(2) 1_555 2_766 ? S16 S20 3.368(2) 1_555 2_666 ? S16 H10B 3.096(1) 1_555 2_666 ? S16 H11B 3.095(1) 1_555 2_665 ? S17 S21 3.456(2) 1_555 2_766 ? S20 H11B 2.962(1) 1_555 1_556 ? S21 S25 3.631(2) 1_555 2_766 ? S21 S27 3.701(2) 1_555 2_766 ? S21 H29B 2.863(1) 1_555 2_767 ? S23 S25 3.796(2) 1_555 2_767 ? S27 Pd1 4.50(1) 1_555 1_655 ? S27 Pd1 4.50(1) 1_555 2_656 ? S27 H20B 2.940(1) 1_555 2_767 ? S31 S32 3.276(2) 1_555 2_556 ? S31 H11A 2.938(1) 1_555 2_666 ? S31 H21A 2.780(1) 1_555 1_445 ? S32 H20A 3.007(1) 1_555 2_666 ? S32 H29A 2.993(1) 1_555 2_656 ? Pd1 H11A 3.66(1) 1_555 1_445 ? Pd1 H11A 3.66(1) 1_555 2_666 ? Pd1 H21A 3.33(1) 1_555 1_445 ? Pd1 H21A 3.33(1) 1_555 2_666 ? Pd1 H21B 3.56(1) 1_555 1_445 ? Pd1 H21B 3.56(1) 1_555 2_666 ? Pd1 H20A 3.75(1) 1_555 1_445 ? Pd1 H20A 3.75(1) 1_555 2_666 ? H18B H28A 2.2305 1_555 2_656 ? C10 C33 3.865(8) 1_555 2_666 ? C10 C34 3.516(8) 1_555 2_666 ? C10 S16 3.87(1) 1_555 2_666 ? C11 C20 3.96(1) 1_555 1_554 ? C11 C33 3.918(8) 1_555 2_666 ? C11 C34 3.985(8) 1_555 2_666 ? C11 S20 3.72(1) 1_555 1_554 ? C11 S31 3.850(6) 1_555 2_666 ? C13 S22 3.875(5) 1_555 1_554 ? C15 S10 3.862(5) 1_555 2_665 ? C18 C28 3.743(6) 1_555 2_656 ? C18 O35 3.143(6) 1_555 1_554 ? C18 H28A 3.032(4) 1_555 2_656 ? C19 C19 3.908(6) 1_555 2_655 ? C19 O35 3.176(6) 1_555 1_554 ? C19 O35 3.381(6) 1_555 2_656 ? C19 O36 3.344(7) 1_555 2_656 ? C19 H19B 3.103(5) 1_555 2_655 ? C20 C29 3.773(7) 1_555 2_767 ? C20 S27 3.895(6) 1_555 2_767 ? C20 S31 3.796(5) 1_555 1_665 ? C20 Pd1 4.34(2) 1_555 1_665 ? C20 Pd1 4.34(2) 1_555 2_666 ? C21 C29 3.781(8) 1_555 2_767 ? C21 C33 3.885(7) 1_555 1_665 ? C21 S27 3.635(6) 1_555 2_766 ? C21 S31 3.611(5) 1_555 1_665 ? C21 Pd1 3.87(1) 1_555 1_665 ? C21 Pd1 3.87(1) 1_555 2_666 ? C21 H29B 3.041(6) 1_555 2_767 ? C22 S11 3.803(5) 1_555 1_556 ? C27 S21 3.740(5) 1_555 2_766 ? C28 O35 3.328(7) 1_555 2_657 ? C28 H18B 2.891(4) 1_555 2_656 ? C29 C33 3.922(7) 1_555 2_657 ? C29 O35 3.164(7) 1_555 2_657 ? C29 S21 3.808(5) 1_555 2_767 ? C29 S32 3.680(5) 1_555 2_656 ? C29 H20B 3.066(5) 1_555 2_767 ? C33 Pd1 3.19(1) 1_555 2_556 ? C33 H21A 2.909(5) 1_555 1_445 ? C34 Pd1 3.22(1) 1_555 2_556 ? C34 H10A 2.950(5) 1_555 2_666 ? C34 H28B 3.189(5) 1_555 2_656 ? O35 H18B 2.460(4) 1_555 1_556 ? O36 H19B 2.577(5) 1_555 2_656 ? S10 S24 3.379(2) 1_555 2_666 ? S10 S26 3.314(2) 1_555 2_666 ? S11 S20 3.775(2) 1_555 1_554 ? S11 S22 3.778(2) 1_555 1_554 ? S11 S25 3.447(2) 1_555 2_766 ? S11 S27 3.531(2) 1_555 2_766 ? S12 S22 3.795(2) 1_555 2_666 ? S14 S20 3.422(2) 1_555 2_666 ? S15 S21 3.456(2) 1_555 2_766 ? S16 S20 3.368(2) 1_555 2_666 ? S16 H10B 3.096(1) 1_555 2_666 ? S16 H11B 3.095(1) 1_555 2_665 ? S17 S21 3.456(2) 1_555 2_766 ? S20 H11B 2.962(1) 1_555 1_556 ? S21 S25 3.631(2) 1_555 2_766 ? S21 S27 3.701(2) 1_555 2_766 ? S21 H29B 2.863(1) 1_555 2_767 ? S23 S25 3.796(2) 1_555 2_767 ? S27 Pd1 4.50(1) 1_555 1_655 ? S27 Pd1 4.50(1) 1_555 2_656 ? S27 H20B 2.940(1) 1_555 2_767 ? S31 S32 3.276(2) 1_555 2_556 ? S31 H11A 2.938(1) 1_555 2_666 ? S31 H21A 2.780(1) 1_555 1_445 ? S32 H20A 3.007(1) 1_555 2_666 ? S32 H29A 2.993(1) 1_555 2_656 ? Pd1 H11A 3.66(1) 1_555 1_445 ? Pd1 H11A 3.66(1) 1_555 2_666 ? Pd1 H21A 3.33(1) 1_555 1_445 ? Pd1 H21A 3.33(1) 1_555 2_666 ? Pd1 H21B 3.56(1) 1_555 1_445 ? Pd1 H21B 3.56(1) 1_555 2_666 ? Pd1 H20A 3.75(1) 1_555 1_445 ? Pd1 H20A 3.75(1) 1_555 2_666 ? H18B H28A 2.2305 1_555 2_656 ? #===END data_BO2[Ni(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'plate' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _chemical_formula_moiety 'C24 H16 Ni1 O12 S12 ' _chemical_formula_weight 939.87 _cell_length_a 9.736(3) _cell_length_b 12.082(6) _cell_length_c 7.317(2) _cell_angle_alpha 98.36(3) _cell_angle_beta 111.26(2) _cell_angle_gamma 91.85(3) _cell_volume 790.2(5) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '35' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_meas 1.976 _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 1.4408 _diffrn_ambient_temperature 298 _cell_measurement_temperature 298 _exptl_cryst_F_000 475.96 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 6971 _reflns_number_total 7472 _reflns_number_observed 1666 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents ???? _diffrn_reflns_theta_max 21.91 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.057 _refine_ls_wR_factor_obs 0.082 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 1666 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 2.680 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0234 _refine_ls_shift/esd_mean 0.0035 _refine_diff_density_min -0.67 _refine_diff_density_max 0.78 _refine_ls_extinction_method 'None' _atom_sites_solution_primary 'direct' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.3429(14) 0.8966(10) 0.9628(22) 0.043(7) 1.000 Uij C10 0.4469(14) 0.8695(10) 1.1665(20) 0.037(7) 1.000 Uij C11 0.2189(13) 0.7232(10) 0.9277(18) 0.027(6) 1.000 Uij C12 0.3435(14) 0.6868(10) 1.0429(19) 0.036(7) 1.000 Uij C13 0.1610(13) 0.5139(10) 0.8884(17) 0.027(6) 1.000 Uij C14 0.0955(12) 0.4053(9) 0.8373(17) 0.026(6) 1.000 Uij C15 -0.0766(13) 0.2275(9) 0.6931(17) 0.026(6) 1.000 Uij C16 0.0477(12) 0.1945(9) 0.8033(18) 0.027(6) 1.000 Uij C17 -0.1746(15) 0.0421(11) 0.5643(20) 0.042(7) 1.000 Uij C18 -0.0682(14) 0.0169(10) 0.7616(19) 0.036(7) 1.000 Uij C21 0.2923(15) 0.2830(10) 0.4519(19) 0.037(7) 1.000 Uij C22 0.4186(14) 0.2375(10) 0.3801(19) 0.033(7) 1.000 Uij O1 0.1993(9) 0.8316(7) 0.8973(14) 0.039(5) 1.000 Uij O2 0.4713(8) 0.7525(7) 1.1522(13) 0.034(4) 1.000 Uij O7 -0.2073(9) 0.1595(7) 0.5833(13) 0.034(4) 1.000 Uij O8 0.0718(9) 0.0850(7) 0.8262(13) 0.037(5) 1.000 Uij O23 0.1970(11) 0.2168(8) 0.4503(16) 0.056(6) 1.000 Uij O24 0.4119(11) 0.1370(8) 0.3223(16) 0.056(6) 1.000 Uij S3 0.0683(3) 0.6245(3) 0.7978(5) 0.028(2) 1.000 Uij S4 0.3434(3) 0.5445(3) 1.0544(5) 0.030(2) 1.000 Uij S5 -0.0849(3) 0.3699(2) 0.6790(5) 0.027(1) 1.000 Uij S6 0.1968(3) 0.2946(3) 0.9258(5) 0.031(2) 1.000 Uij S19 0.3069(3) 0.4252(3) 0.5351(5) 0.031(2) 1.000 Uij S20 0.5502(3) 0.3365(3) 0.3803(5) 0.032(2) 1.000 Uij Ni1 0.50000 0.50000 0.50000 0.021(1) 0.500 Uij H18A -0.05050 -0.06440 0.74900 0.05 1.000 Uiso H18B -0.11410 0.03460 0.86340 0.05 1.000 Uiso H17A -0.26900 -0.00780 0.51910 0.05 1.000 Uiso H17B -0.12770 0.02700 0.46320 0.05 1.000 Uiso H9A 0.39130 0.87620 0.86200 0.05 1.000 Uiso H9B 0.33160 0.97860 0.97470 0.05 1.000 Uiso H10A 0.40200 0.88950 1.26630 0.05 1.000 Uiso H10B 0.54650 0.91540 1.21160 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.033(8) 0.026(7) 0.060(9) -0.010(6) 0.017(7) 0.000(7) C10 0.035(8) 0.026(7) 0.041(8) -0.010(6) 0.010(6) 0.000(6) C11 0.020(6) 0.021(7) 0.033(7) -0.004(5) 0.006(6) -0.001(5) C12 0.040(8) 0.025(7) 0.035(8) -0.004(6) 0.013(7) 0.002(6) C13 0.025(7) 0.030(7) 0.021(6) -0.007(5) 0.007(5) 0.004(5) C14 0.023(6) 0.024(7) 0.025(7) 0.000(5) 0.008(5) 0.000(5) C15 0.026(7) 0.019(6) 0.025(7) -0.005(5) 0.006(6) 0.002(5) C16 0.018(6) 0.020(6) 0.036(7) 0.003(5) 0.010(6) 0.004(5) C17 0.048(9) 0.023(7) 0.041(8) -0.001(6) 0.009(7) -0.007(6) C18 0.036(7) 0.025(7) 0.036(8) -0.002(6) 0.003(6) 0.005(6) C21 0.046(8) 0.024(7) 0.034(8) 0.000(6) 0.014(7) 0.000(6) C22 0.035(7) 0.026(8) 0.032(7) -0.007(6) 0.014(6) 0.003(6) O1 0.029(5) 0.026(5) 0.051(6) -0.002(4) 0.007(4) 0.010(4) O2 0.019(4) 0.029(5) 0.044(5) -0.010(4) 0.001(4) 0.005(4) O7 0.026(5) 0.027(5) 0.038(5) -0.001(4) 0.002(4) 0.009(4) O8 0.029(5) 0.027(5) 0.044(6) -0.002(4) 0.002(4) 0.005(4) O23 0.043(6) 0.034(6) 0.081(8) -0.022(5) 0.034(6) -0.002(5) O24 0.062(7) 0.026(6) 0.072(7) -0.007(5) 0.038(6) -0.010(5) S3 0.020(2) 0.026(2) 0.032(2) -0.001(1) 0.005(1) 0.005(1) S4 0.024(2) 0.025(2) 0.032(2) 0.001(1) 0.005(1) 0.006(1) S5 0.024(2) 0.021(2) 0.030(2) -0.001(1) 0.005(1) 0.006(1) S6 0.022(2) 0.026(2) 0.035(2) -0.001(1) 0.000(1) 0.005(1) S19 0.026(2) 0.021(2) 0.041(2) -0.002(1) 0.015(1) 0.002(1) S20 0.027(2) 0.021(2) 0.040(2) 0.001(1) 0.014(1) 0.000(1) Ni1 0.017(1) 0.016(1) 0.027(1) -0.001(1) 0.008(1) 0.001(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 C10 C9 O1 C11 -43.7(11) . . . . yes O1 C9 C10 O2 60.3(11) . . . . yes C9 C10 O2 C12 -42.6(11) . . . . yes C12 C11 O1 C9 15.7(13) . . . . yes O1 C11 C12 O2 1.2(11) . . . . yes O1 C11 C12 S4 -178.6(18) . . . . yes C12 C11 S3 C13 -0.1(11) . . . . yes S3 C11 C12 O2 179.3(18) . . . . yes S3 C11 C12 S4 -0.6(7) . . . . yes S3 C11 O1 C9 -162.3(13) . . . . yes O1 C11 S3 C13 178.1(10) . . . . yes C11 C12 O2 C10 13.7(13) . . . . yes C11 C12 S4 C13 0.9(11) . . . . yes S4 C12 O2 C10 -166.5(13) . . . . yes O2 C12 S4 C13 -178.9(11) . . . . yes C14 C13 S3 C11 179.6(11) . . . . yes S3 C13 C14 S5 -0.2(7) . . . . yes S3 C13 C14 S6 177.4(15) . . . . yes C14 C13 S4 C12 -179.8(11) . . . . yes S4 C13 C14 S5 178.5(15) . . . . yes S4 C13 C14 S6 -3.9(7) . . . . yes S4 C13 S3 C11 0.8(8) . . . . yes S3 C13 S4 C12 -1.0(8) . . . . yes C13 C14 S5 C15 179.4(11) . . . . yes C13 C14 S6 C16 -179.7(11) . . . . yes S6 C14 S5 C15 1.7(7) . . . . yes S5 C14 S6 C16 -2.0(8) . . . . yes C16 C15 O7 C17 -15.8(12) . . . . yes O7 C15 C16 O8 1.6(11) . . . . yes O7 C15 C16 S6 179.6(17) . . . . yes C16 C15 S5 C14 -0.5(11) . . . . yes S5 C15 C16 O8 -178.8(17) . . . . yes S5 C15 C16 S6 -0.8(7) . . . . yes O7 C15 S5 C14 179.1(10) . . . . yes S5 C15 O7 C17 164.6(12) . . . . yes C15 C16 O8 C18 -17.1(12) . . . . yes C15 C16 S6 C14 1.6(11) . . . . yes O8 C16 S6 C14 179.8(10) . . . . yes S6 C16 O8 C18 164.8(12) . . . . yes C18 C17 O7 C15 43.6(11) . . . . yes O7 C17 C18 O8 -61.5(11) . . . . yes C17 C18 O8 C16 45.2(11) . . . . yes O23 C21 C22 O24 1.4(13) . . . . yes O23 C21 C22 S20 178.6(17) . . . . yes S19 C21 C22 O24 179.3(16) . . . . yes S19 C21 C22 S20 -3.6(7) . . . . yes C22 C21 S19 Ni1 2.5(8) . . . . yes O23 C21 S19 Ni1 -179.8(14) . . . . yes C21 C22 S20 Ni1 2.7(8) . . . . yes O24 C22 S20 Ni1 179.7(13) . . . . yes C21 S19 Ni1 S20 -0.7(5) . . . . yes Ni1 S19 C21 C22 2.5(8) . . . . yes Ni1 S19 C21 O23 -179.8(14) . . . . yes C21 S19 Ni1 S20 -0.7(5) . . . . yes C22 S20 Ni1 S19 -1.0(5) . . . . yes Ni1 S20 C22 C21 2.7(8) . . . . yes Ni1 S20 C22 O24 179.7(13) . . . . yes C22 S20 Ni1 S19 -1.0(5) . . . . yes S20 Ni1 S19 C21 179.3(5) . . . . yes S19 Ni1 S20 C22 179.0(5) . . . . yes O1 C9 C10 H10A -60.5(12) . . . . yes O1 C9 C10 H10B -179.7(15) . . . . yes H9A C9 C10 O2 -59.7(12) . . . . yes H9A C9 C10 H10A 179.5(16) . . . . yes H9A C9 C10 H10B 60.2(13) . . . . yes H9B C9 C10 O2 -177.2(16) . . . . yes H9B C9 C10 H10A 62.0(13) . . . . yes H9B C9 C10 H10B -57.2(13) . . . . yes H9A C9 O1 C11 75.3(12) . . . . yes H9B C9 O1 C11 -165.4(15) . . . . yes H10A C10 O2 C12 78.1(13) . . . . yes H10B C10 O2 C12 -163.3(15) . . . . yes O7 C17 C18 H18A 177.1(16) . . . . yes O7 C17 C18 H18B 58.1(12) . . . . yes H17A C17 C18 O8 177.7(16) . . . . yes H17A C17 C18 H18A 56.3(13) . . . . yes H17A C17 C18 H18B -62.7(13) . . . . yes H17B C17 C18 O8 58.5(12) . . . . yes H17B C17 C18 H18A -62.9(13) . . . . yes H17B C17 C18 H18B 178.1(16) . . . . yes H17A C17 O7 C15 164.8(14) . . . . yes H17B C17 O7 C15 -76.0(12) . . . . yes H18A C18 O8 C16 167.0(14) . . . . yes H18B C18 O8 C16 -74.0(12) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.56(2) . . yes C9 O1 1.461(15) . . yes C10 O2 1.436(16) . . yes C11 C12 1.333(18) . . yes C11 O1 1.368(15) . . yes C11 S3 1.738(12) . . yes C12 O2 1.359(15) . . yes C12 S4 1.733(13) . . yes C13 C14 1.378(16) . . yes C13 S3 1.715(13) . . yes C13 S4 1.740(12) . . yes C14 S5 1.715(12) . . yes C14 S6 1.748(12) . . yes C15 C16 1.300(17) . . yes C15 O7 1.392(14) . . yes C15 S5 1.741(12) . . yes C16 O8 1.375(14) . . yes C16 S6 1.732(12) . . yes C17 C18 1.52(2) . . yes C17 O7 1.462(16) . . yes C18 O8 1.451(15) . . yes C21 C22 1.587(19) . . yes C21 O23 1.201(16) . . yes C21 S19 1.720(13) . . yes C22 O24 1.218(16) . . yes C22 S20 1.724(13) . . yes S19 Ni1 2.174(4) . . yes S19 Ni1 2.174(4) . 2_656 yes S20 Ni1 2.186(4) . . yes S20 Ni1 2.186(4) . 2_656 yes C9 H9A 1.017(15) . . yes C9 H9B 0.995(13) . . yes C10 H10A 0.985(14) . . yes C10 H10B 1.018(13) . . yes C17 H17A 1.002(14) . . yes C17 H17B 1.000(14) . . yes C18 H18A 1.000(13) . . yes C18 H18B 1.001(14) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 O1 110.1(11) . . . yes C9 C10 O2 111.2(11) . . . yes C12 C11 O1 125.8(11) . . . yes C12 C11 S3 117.7(10) . . . yes O1 C11 S3 116.4(9) . . . yes C11 C12 O2 125.1(11) . . . yes C11 C12 S4 117.7(10) . . . yes O2 C12 S4 117.2(9) . . . yes C14 C13 S3 122.5(9) . . . yes C14 C13 S4 120.5(9) . . . yes S3 C13 S4 117.0(7) . . . yes C13 C14 S5 122.8(9) . . . yes C13 C14 S6 120.8(9) . . . yes S5 C14 S6 116.4(7) . . . yes C16 C15 O7 126.2(11) . . . yes C16 C15 S5 118.3(10) . . . yes O7 C15 S5 115.4(8) . . . yes C15 C16 O8 125.0(11) . . . yes C15 C16 S6 118.1(9) . . . yes O8 C16 S6 116.9(9) . . . yes C18 C17 O7 110.8(11) . . . yes C17 C18 O8 110.9(11) . . . yes C22 C21 O23 118.6(12) . . . yes C22 C21 S19 116.5(10) . . . yes O23 C21 S19 124.8(11) . . . yes C21 C22 O24 118.0(12) . . . yes C21 C22 S20 116.7(9) . . . yes O24 C22 S20 125.3(11) . . . yes C9 O1 C11 109.9(9) . . . yes C10 O2 C12 111.2(10) . . . yes C15 O7 C17 109.2(9) . . . yes C16 O8 C18 110.2(9) . . . yes C11 S3 C13 93.9(6) . . . yes C12 S4 C13 93.6(6) . . . yes C14 S5 C15 93.7(6) . . . yes C14 S6 C16 93.5(6) . . . yes C21 S19 Ni1 107.7(5) . . . yes C21 S19 Ni1 107.7(5) . . 2_656 yes C22 S20 Ni1 107.2(5) . . . yes C22 S20 Ni1 107.2(5) . . 2_656 yes S19 Ni1 S19 180.0 . . 2_656 yes S19 Ni1 S20 91.8(2) . . . yes S19 Ni1 S20 88.2(2) . . 2_656 yes S19 Ni1 S20 88.2(2) 2_656 . . yes S19 Ni1 S20 91.8(2) 2_656 . 2_656 yes S20 Ni1 S20 180.0 . . 2_656 yes C10 C9 H9A 108.2(12) . . . yes C10 C9 H9B 109.7(13) . . . yes O1 C9 H9A 109.8(12) . . . yes O1 C9 H9B 111.0(11) . . . yes H9A C9 H9B 107.9(13) . . . yes C9 C10 H10A 109.2(12) . . . yes C9 C10 H10B 109.7(11) . . . yes O2 C10 H10A 109.4(11) . . . yes O2 C10 H10B 108.5(11) . . . yes H10A C10 H10B 108.8(13) . . . yes C18 C17 H17A 109.9(12) . . . yes C18 C17 H17B 108.6(12) . . . yes O7 C17 H17A 109.3(12) . . . yes O7 C17 H17B 109.3(11) . . . yes H17A C17 H17B 109.0(13) . . . yes C17 C18 H18A 110.2(12) . . . yes C17 C18 H18B 108.3(12) . . . yes O8 C18 H18A 109.5(11) . . . yes O8 C18 H18B 109.1(11) . . . yes H18A C18 H18B 108.9(12) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 C9 3.71(2) 1_555 2_677 ? C9 C10 3.86(2) 1_555 2_677 ? C9 C17 3.80(2) 1_555 2_566 ? C9 C18 3.97(2) 1_555 2_567 ? C9 H18B 3.02(1) 1_555 2_567 ? C9 H10B 3.10(1) 1_555 2_677 ? C10 C17 3.93(2) 1_555 2_567 ? C10 C21 3.78(2) 1_555 2_667 ? C10 C22 3.55(2) 1_555 2_667 ? C10 O24 3.34(2) 1_555 1_566 ? C10 H17A 3.15(1) 1_555 1_666 ? C11 C15 3.51(2) 1_555 2_567 ? C11 C16 3.86(2) 1_555 2_567 ? C11 S5 3.85(1) 1_555 2_567 ? C11 S20 3.74(1) 1_555 2_666 ? C12 C15 3.85(2) 1_555 2_567 ? C12 C22 3.96(2) 1_555 2_667 ? C12 S5 3.87(1) 1_555 2_567 ? C12 S20 3.58(1) 1_555 2_666 ? C12 Ni1 4.16(1) 1_555 1_556 ? C12 Ni1 4.16(1) 1_555 2_667 ? C13 C14 3.80(2) 1_555 2_567 ? C13 S5 3.61(1) 1_555 2_567 ? C13 Ni1 4.53(1) 1_555 1_556 ? C13 Ni1 4.53(1) 1_555 2_667 ? C14 S3 3.62(1) 1_555 2_567 ? C15 S3 3.86(1) 1_555 2_567 ? C17 C17 3.97(2) 1_555 2_556 ? C17 C18 3.94(2) 1_555 2_556 ? C17 O23 3.11(2) 1_555 2_556 ? C17 H17B 3.15(1) 1_555 2_556 ? C17 H10A 2.99(1) 1_555 2_567 ? C17 H10B 3.14(1) 1_555 1_444 ? C18 C18 3.35(2) 1_555 2_557 ? C18 C21 3.96(2) 1_555 2_556 ? C18 O23 3.01(2) 1_555 2_556 ? C18 H18B 2.85(1) 1_555 2_557 ? C18 H17B 2.95(1) 1_555 2_556 ? C21 O2 3.08(2) 1_555 2_667 ? C21 S3 3.62(1) 1_555 2_566 ? C21 S6 3.64(1) 1_555 1_554 ? C21 Ni1 3.16(1) 1_555 2_666 ? C22 O2 3.18(2) 1_555 2_667 ? C22 S6 3.43(1) 1_555 1_554 ? C22 Ni1 3.16(1) 1_555 2_666 ? C22 H10A 3.19(1) 1_555 2_667 ? O1 H18B 2.585(9) 1_555 2_567 ? O8 H17B 2.581(9) 1_555 2_556 ? O23 H18A 2.257(9) 1_555 2_556 ? S3 S5 3.561(4) 1_555 2_566 ? S3 S5 3.763(4) 1_555 2_567 ? S3 S19 3.552(4) 1_555 2_566 ? S4 S4 3.579(4) 1_555 2_667 ? S4 S5 3.788(4) 1_555 2_567 ? S4 S19 3.596(4) 1_555 2_667 ? S4 Ni1 3.194(3) 1_555 1_556 ? S4 Ni1 3.194(3) 1_555 2_667 ? S5 S19 3.503(4) 1_555 2_566 ? S5 S20 3.403(4) 1_555 1_455 ? S5 Ni1 4.206(3) 1_555 1_455 ? S5 Ni1 4.206(3) 1_555 2_566 ? S6 S20 3.775(4) 1_555 1_556 ? S6 Ni1 4.475(3) 1_555 1_556 ? S6 Ni1 4.475(3) 1_555 2_667 ? S19 S20 3.034(4) 1_555 2_666 ? S20 H9A 3.094(3) 1_555 2_666 ? H17A H10B 2.3461 1_555 1_444 ? C9 C9 3.71(2) 1_555 2_677 ? C9 C10 3.86(2) 1_555 2_677 ? C9 C17 3.80(2) 1_555 2_566 ? C9 C18 3.97(2) 1_555 2_567 ? C9 H18B 3.02(1) 1_555 2_567 ? C9 H10B 3.10(1) 1_555 2_677 ? C10 C17 3.93(2) 1_555 2_567 ? C10 C21 3.78(2) 1_555 2_667 ? C10 C22 3.55(2) 1_555 2_667 ? C10 O24 3.34(2) 1_555 1_566 ? C10 H17A 3.15(1) 1_555 1_666 ? C11 C15 3.51(2) 1_555 2_567 ? C11 C16 3.86(2) 1_555 2_567 ? C11 S5 3.85(1) 1_555 2_567 ? C11 S20 3.74(1) 1_555 2_666 ? C12 C15 3.85(2) 1_555 2_567 ? C12 C22 3.96(2) 1_555 2_667 ? C12 S5 3.87(1) 1_555 2_567 ? C12 S20 3.58(1) 1_555 2_666 ? C12 Ni1 4.16(1) 1_555 1_556 ? C12 Ni1 4.16(1) 1_555 2_667 ? C13 C14 3.80(2) 1_555 2_567 ? C13 S5 3.61(1) 1_555 2_567 ? C13 Ni1 4.53(1) 1_555 1_556 ? C13 Ni1 4.53(1) 1_555 2_667 ? C14 S3 3.62(1) 1_555 2_567 ? C15 S3 3.86(1) 1_555 2_567 ? C17 C17 3.97(2) 1_555 2_556 ? C17 C18 3.94(2) 1_555 2_556 ? C17 O23 3.11(2) 1_555 2_556 ? C17 H17B 3.15(1) 1_555 2_556 ? C17 H10A 2.99(1) 1_555 2_567 ? C17 H10B 3.14(1) 1_555 1_444 ? C18 C18 3.35(2) 1_555 2_557 ? C18 C21 3.96(2) 1_555 2_556 ? C18 O23 3.01(2) 1_555 2_556 ? C18 H18B 2.85(1) 1_555 2_557 ? C18 H17B 2.95(1) 1_555 2_556 ? C21 O2 3.08(2) 1_555 2_667 ? C21 S3 3.62(1) 1_555 2_566 ? C21 S6 3.64(1) 1_555 1_554 ? C21 Ni1 3.16(1) 1_555 2_666 ? C22 O2 3.18(2) 1_555 2_667 ? C22 S6 3.43(1) 1_555 1_554 ? C22 Ni1 3.16(1) 1_555 2_666 ? C22 H10A 3.19(1) 1_555 2_667 ? O1 H18B 2.585(9) 1_555 2_567 ? O8 H17B 2.581(9) 1_555 2_556 ? O23 H18A 2.257(9) 1_555 2_556 ? S3 S5 3.561(4) 1_555 2_566 ? S3 S5 3.763(4) 1_555 2_567 ? S3 S19 3.552(4) 1_555 2_566 ? S4 S4 3.579(4) 1_555 2_667 ? S4 S5 3.788(4) 1_555 2_567 ? S4 S19 3.596(4) 1_555 2_667 ? S4 Ni1 3.194(3) 1_555 1_556 ? S4 Ni1 3.194(3) 1_555 2_667 ? S5 S19 3.503(4) 1_555 2_566 ? S5 S20 3.403(4) 1_555 1_455 ? S5 Ni1 4.206(3) 1_555 1_455 ? S5 Ni1 4.206(3) 1_555 2_566 ? S6 S20 3.775(4) 1_555 1_556 ? S6 Ni1 4.475(3) 1_555 1_556 ? S6 Ni1 4.475(3) 1_555 2_667 ? S19 S20 3.034(4) 1_555 2_666 ? S20 H9A 3.094(3) 1_555 2_666 ? H17A H10B 2.3461 1_555 1_444 ? #===END data_BO2[Pd(dto)2] _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _chemical_formula_moiety 'C24 H16 O12 S12 Pd1 ' _chemical_formula_weight 987.60 _cell_length_a 9.757(2) _cell_length_b 12.1590(1) _cell_length_c 7.385(2) _cell_angle_alpha 98.38(2) _cell_angle_beta 111.200(2) _cell_angle_gamma 92.01(2) _cell_volume 804.5(3) _cell_measurement_reflns_used '??' _cell_measurement_theta_min '??' _cell_measurement_theta_max '32.5' _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_meas ??? _diffrn_radiation_type 'Mo K-alpha' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.3793 _cell_measurement_temperature '298' _diffrn_ambient_temperature 298 _exptl_cryst_F_000 493.97 _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method 'theta/2theta' _exptl_absorpt_correction_type 'none' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 6229 _reflns_number_total 5749 _reflns_number_observed 4447 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents 0.005 _diffrn_reflns_theta_max 28.63 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.028 _refine_ls_wR_factor_obs 0.039 _refine_ls_hydrogen_treatment 'nonref' _refine_ls_number_reflns 4447 _refine_ls_number_parameters 223 _refine_ls_goodness_of_fit_obs 0.962 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.0249 _refine_ls_shift/esd_mean 0.0055 _refine_diff_density_min -0.74 _refine_diff_density_max 0.67 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _atom_sites_solution_primary 'direct' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 -0.02395 _diffrn_orient_matrix_UB_12 -0.07842 _diffrn_orient_matrix_UB_13 -0.07348 _diffrn_orient_matrix_UB_21 0.05857 _diffrn_orient_matrix_UB_22 0.01778 _diffrn_orient_matrix_UB_23 -0.08040 _diffrn_orient_matrix_UB_31 0.09050 _diffrn_orient_matrix_UB_32 -0.02255 _diffrn_orient_matrix_UB_33 0.09929 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C9 0.3433(4) 0.8981(3) 0.9651(6) 0.041(2) 1.000 Uij C10 0.4418(4) 0.8731(3) 1.1620(6) 0.041(2) 1.000 Uij C11 0.2162(3) 0.7270(2) 0.9258(5) 0.031(1) 1.000 Uij C12 0.3411(3) 0.6907(2) 1.0403(5) 0.030(1) 1.000 Uij C13 0.1591(3) 0.5184(2) 0.8887(4) 0.027(1) 1.000 Uij C14 0.0945(3) 0.4090(2) 0.8372(4) 0.028(1) 1.000 Uij C15 -0.0797(3) 0.2313(2) 0.6919(5) 0.029(1) 1.000 Uij C16 0.0496(3) 0.1990(2) 0.8032(5) 0.031(1) 1.000 Uij C17 -0.1693(4) 0.0468(3) 0.5668(5) 0.039(1) 1.000 Uij C18 -0.0646(4) 0.0227(3) 0.7625(6) 0.040(2) 1.000 Uij C21 0.2920(4) 0.2768(3) 0.4542(5) 0.035(1) 1.000 Uij C22 0.4125(4) 0.2322(3) 0.3763(5) 0.035(1) 1.000 Uij O1 0.1993(3) 0.8345(2) 0.8987(4) 0.040(1) 1.000 Uij O2 0.4681(3) 0.7557(2) 1.1480(4) 0.037(1) 1.000 Uij O7 -0.2035(3) 0.1620(2) 0.5858(4) 0.037(1) 1.000 Uij O8 0.0752(3) 0.0922(2) 0.8277(4) 0.039(1) 1.000 Uij O23 0.1961(4) 0.2098(2) 0.4529(6) 0.069(2) 1.000 Uij O24 0.4047(4) 0.1326(2) 0.3193(5) 0.065(2) 1.000 Uij S3 0.06610(8) 0.62880(6) 0.79650(12) 0.0306(3) 1.000 Uij S4 0.34120(9) 0.54880(6) 1.04670(12) 0.0322(3) 1.000 Uij S5 -0.08760(8) 0.37290(6) 0.67950(12) 0.0297(3) 1.000 Uij S6 0.19550(9) 0.30110(7) 0.92450(13) 0.0346(3) 1.000 Uij S19 0.29960(8) 0.41720(6) 0.53900(13) 0.0333(3) 1.000 Uij S20 0.54660(9) 0.32730(6) 0.37240(13) 0.0339(3) 1.000 Uij Pd1 0.50000 0.50000 0.50000 0.0217(1) 0.500 Uij H17A -0.26280 -0.00380 0.52060 0.05 1.000 Uiso H17B -0.12150 0.03310 0.46760 0.05 1.000 Uiso H18A -0.04620 -0.05790 0.74920 0.05 1.000 Uiso H18B -0.11110 0.03920 0.86290 0.05 1.000 Uiso H9A 0.39300 0.87700 0.86680 0.05 1.000 Uiso H9B 0.33320 0.97970 0.97600 0.05 1.000 Uiso H10A 0.39510 0.89150 1.25890 0.05 1.000 Uiso H10B 0.54080 0.91990 1.20930 0.05 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C9 0.038(2) 0.024(1) 0.051(2) -0.006(1) 0.014(2) 0.008(1) C10 0.039(2) 0.025(1) 0.048(2) -0.008(1) 0.010(2) 0.000(1) C11 0.028(1) 0.022(1) 0.035(2) -0.002(1) 0.009(1) 0.004(1) C12 0.027(1) 0.023(1) 0.032(1) -0.005(1) 0.007(1) 0.003(1) C13 0.027(1) 0.023(1) 0.027(1) -0.002(1) 0.009(1) 0.003(1) C14 0.027(1) 0.023(1) 0.027(1) -0.002(1) 0.009(1) 0.003(1) C15 0.027(1) 0.019(1) 0.034(1) -0.002(1) 0.007(1) 0.005(1) C16 0.032(1) 0.020(1) 0.032(1) 0.000(1) 0.007(1) 0.004(1) C17 0.040(2) 0.022(1) 0.042(2) -0.002(1) 0.005(1) 0.000(1) C18 0.040(2) 0.022(1) 0.047(2) -0.005(1) 0.006(1) 0.007(1) C21 0.033(2) 0.023(1) 0.041(2) -0.006(1) 0.013(1) 0.002(1) C22 0.039(2) 0.021(1) 0.036(2) 0.000(1) 0.012(1) 0.001(1) O1 0.032(1) 0.022(1) 0.054(2) -0.001(1) 0.008(1) 0.010(1) O2 0.029(1) 0.027(1) 0.044(1) -0.007(1) 0.002(1) 0.004(1) O7 0.029(1) 0.021(1) 0.049(1) -0.004(1) 0.001(1) 0.004(1) O8 0.035(1) 0.021(1) 0.048(1) 0.001(1) 0.002(1) 0.008(1) O23 0.064(2) 0.033(1) 0.098(3) -0.024(1) 0.045(2) -0.009(2) O24 0.078(2) 0.019(1) 0.085(2) -0.006(1) 0.045(2) -0.008(1) S3 0.0249(3) 0.0248(3) 0.0341(4) -.0023(3) 0.0056(3) 0.0046(3) S4 0.0291(4) 0.0237(3) 0.0341(4) -.0013(3) 0.0029(3) 0.0047(3) S5 0.0273(3) 0.0203(3) 0.0341(4) -.0005(3) 0.0067(3) 0.0061(3) S6 0.0278(4) 0.0255(3) 0.0395(4) -.0022(3) 0.0015(3) 0.0063(3) S19 0.0279(3) 0.0216(3) 0.0445(4) -.0029(3) 0.0174(3) 0.0021(3) S20 0.0322(4) 0.0202(3) 0.0425(4) 0.0020(3) 0.0164(3) -.0002(3) Pd1 0.0200(1) 0.0145(1) 0.0254(1) -.0008(1) 0.0069(1) 0.0023(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 C10 C9 O1 C11 -45.2(3) . . . . yes O1 C9 C10 O2 62.0(3) . . . . yes C9 C10 O2 C12 -43.8(3) . . . . yes C12 C11 O1 C9 15.7(4) . . . . yes O1 C11 C12 O2 1.0(3) . . . . yes O1 C11 C12 S4 -177.5(5) . . . . yes C12 C11 S3 C13 0.5(3) . . . . yes S3 C11 C12 O2 179.0(5) . . . . yes S3 C11 C12 S4 0.5(2) . . . . yes S3 C11 O1 C9 -162.3(4) . . . . yes O1 C11 S3 C13 178.6(3) . . . . yes C11 C12 O2 C10 13.9(4) . . . . yes C11 C12 S4 C13 -1.2(3) . . . . yes S4 C12 O2 C10 -167.6(4) . . . . yes O2 C12 S4 C13 -179.8(3) . . . . yes C14 C13 S3 C11 -179.8(3) . . . . yes S3 C13 C14 S5 -1.6(2) . . . . yes S3 C13 C14 S6 176.8(4) . . . . yes C14 C13 S4 C12 -180.0(3) . . . . yes S4 C13 C14 S5 180.0(4) . . . . yes S4 C13 C14 S6 -1.6(2) . . . . yes S4 C13 S3 C11 -1.3(2) . . . . yes S3 C13 S4 C12 1.5(2) . . . . yes C13 C14 S5 C15 179.8(3) . . . . yes C13 C14 S6 C16 -179.7(3) . . . . yes S6 C14 S5 C15 1.3(2) . . . . yes S5 C14 S6 C16 -1.2(2) . . . . yes C16 C15 O7 C17 -14.6(4) . . . . yes O7 C15 C16 O8 -0.7(3) . . . . yes O7 C15 C16 S6 179.0(5) . . . . yes C16 C15 S5 C14 -1.0(3) . . . . yes S5 C15 C16 O8 -179.4(5) . . . . yes S5 C15 C16 S6 0.3(2) . . . . yes O7 C15 S5 C14 -179.8(3) . . . . yes S5 C15 O7 C17 164.1(4) . . . . yes C15 C16 O8 C18 -15.6(4) . . . . yes C15 C16 S6 C14 0.5(3) . . . . yes O8 C16 S6 C14 -179.7(3) . . . . yes S6 C16 O8 C18 164.7(4) . . . . yes C18 C17 O7 C15 44.1(3) . . . . yes O7 C17 C18 O8 -62.0(3) . . . . yes C17 C18 O8 C16 45.0(3) . . . . yes O23 C21 C22 O24 -0.4(4) . . . . yes O23 C21 C22 S20 178.5(5) . . . . yes S19 C21 C22 O24 179.3(5) . . . . yes S19 C21 C22 S20 -1.8(2) . . . . yes C22 C21 S19 Pd1 1.2(3) . . . . yes O23 C21 S19 Pd1 -179.1(4) . . . . yes C21 C22 S20 Pd1 1.3(3) . . . . yes O24 C22 S20 Pd1 -179.8(4) . . . . yes C21 S19 Pd1 S20 -0.3(2) . . . . yes Pd1 S19 C21 C22 1.2(3) . . . . yes Pd1 S19 C21 O23 -179.1(4) . . . . yes C21 S19 Pd1 S20 -0.3(2) . . . . yes C22 S20 Pd1 S19 -0.5(2) . . . . yes Pd1 S20 C22 C21 1.3(3) . . . . yes Pd1 S20 C22 O24 -179.8(4) . . . . yes C22 S20 Pd1 S19 -0.5(2) . . . . yes S20 Pd1 S19 C21 179.7(2) . . . . yes S19 Pd1 S20 C22 179.5(2) . . . . yes O1 C9 C10 H10A -58.4(4) . . . . yes O1 C9 C10 H10B -178.1(5) . . . . yes H9A C9 C10 O2 -58.5(4) . . . . yes H9A C9 C10 H10A -178.9(5) . . . . yes H9A C9 C10 H10B 61.5(4) . . . . yes H9B C9 C10 O2 -175.7(5) . . . . yes H9B C9 C10 H10A 63.9(4) . . . . yes H9B C9 C10 H10B -55.7(4) . . . . yes H9A C9 O1 C11 74.1(4) . . . . yes H9B C9 O1 C11 -166.6(4) . . . . yes H10A C10 O2 C12 77.0(4) . . . . yes H10B C10 O2 C12 -164.5(4) . . . . yes O7 C17 C18 H18A 177.0(5) . . . . yes O7 C17 C18 H18B 58.0(4) . . . . yes H17A C17 C18 O8 177.3(5) . . . . yes H17A C17 C18 H18A 56.3(4) . . . . yes H17A C17 C18 H18B -62.7(4) . . . . yes H17B C17 C18 O8 58.0(4) . . . . yes H17B C17 C18 H18A -63.1(4) . . . . yes H17B C17 C18 H18B 177.9(5) . . . . yes H17A C17 O7 C15 165.1(4) . . . . yes H17B C17 O7 C15 -75.7(4) . . . . yes H18A C18 O8 C16 166.1(4) . . . . yes H18B C18 O8 C16 -74.7(4) . . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 C10 1.506(6) . . yes C9 O1 1.459(5) . . yes C10 O2 1.455(5) . . yes C11 C12 1.340(5) . . yes C11 O1 1.358(4) . . yes C11 S3 1.737(3) . . yes C12 O2 1.352(4) . . yes C12 S4 1.733(3) . . yes C13 C14 1.390(4) . . yes C13 S3 1.730(3) . . yes C13 S4 1.727(3) . . yes C14 S5 1.734(3) . . yes C14 S6 1.728(4) . . yes C15 C16 1.342(5) . . yes C15 O7 1.354(4) . . yes C15 S5 1.740(3) . . yes C16 O8 1.356(4) . . yes C16 S6 1.732(3) . . yes C17 C18 1.515(6) . . yes C17 O7 1.450(4) . . yes C18 O8 1.460(5) . . yes C21 C22 1.565(5) . . yes C21 O23 1.215(5) . . yes C21 S19 1.720(4) . . yes C22 O24 1.213(4) . . yes C22 S20 1.726(4) . . yes S19 Pd1 2.296(1) . . yes S19 Pd1 2.296(1) . 2_656 yes S20 Pd1 2.303(1) . . yes S20 Pd1 2.303(1) . 2_656 yes C9 H9A 1.018(4) . . yes C9 H9B 0.995(4) . . yes C10 H10A 0.983(4) . . yes C10 H10B 1.019(4) . . yes C17 H17A 1.001(4) . . yes C17 H17B 0.999(4) . . yes C18 H18A 1.000(4) . . yes C18 H18B 1.001(4) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 C9 O1 110.4(3) . . . yes C9 C10 O2 110.9(3) . . . yes C12 C11 O1 124.9(3) . . . yes C12 C11 S3 117.7(3) . . . yes O1 C11 S3 117.4(3) . . . yes C11 C12 O2 125.2(3) . . . yes C11 C12 S4 117.5(3) . . . yes O2 C12 S4 117.4(3) . . . yes C14 C13 S3 122.9(3) . . . yes C14 C13 S4 120.2(3) . . . yes S3 C13 S4 116.9(2) . . . yes C13 C14 S5 122.5(3) . . . yes C13 C14 S6 120.8(3) . . . yes S5 C14 S6 116.7(2) . . . yes C16 C15 O7 125.1(3) . . . yes C16 C15 S5 117.3(3) . . . yes O7 C15 S5 117.6(3) . . . yes C15 C16 O8 125.0(3) . . . yes C15 C16 S6 117.7(3) . . . yes O8 C16 S6 117.3(3) . . . yes C18 C17 O7 110.5(3) . . . yes C17 C18 O8 110.6(3) . . . yes C22 C21 O23 118.1(3) . . . yes C22 C21 S19 119.5(3) . . . yes O23 C21 S19 122.4(3) . . . yes C21 C22 O24 117.8(4) . . . yes C21 C22 S20 118.4(3) . . . yes O24 C22 S20 123.8(3) . . . yes C9 O1 C11 110.1(3) . . . yes C10 O2 C12 110.5(3) . . . yes C15 O7 C17 110.7(3) . . . yes C16 O8 C18 110.0(3) . . . yes C11 S3 C13 93.8(2) . . . yes C12 S4 C13 94.1(2) . . . yes C14 S5 C15 94.0(2) . . . yes C14 S6 C16 94.3(2) . . . yes C21 S19 Pd1 106.3(2) . . . yes C21 S19 Pd1 106.3(2) . . 2_656 yes C22 S20 Pd1 106.5(2) . . . yes C22 S20 Pd1 106.5(2) . . 2_656 yes S19 Pd1 S19 180.0 . . 2_656 yes S19 Pd1 S20 89.3(1) . . . yes S19 Pd1 S20 90.7(1) . . 2_656 yes S19 Pd1 S20 90.7(1) 2_656 . . yes S19 Pd1 S20 89.3(1) 2_656 . 2_656 yes S20 Pd1 S20 180.0 . . 2_656 yes C10 C9 H9A 108.2(4) . . . yes C10 C9 H9B 109.4(4) . . . yes O1 C9 H9A 110.1(4) . . . yes O1 C9 H9B 110.9(3) . . . yes H9A C9 H9B 107.8(4) . . . yes C9 C10 H10A 109.6(4) . . . yes C9 C10 H10B 109.8(4) . . . yes O2 C10 H10A 109.0(3) . . . yes O2 C10 H10B 108.6(3) . . . yes H10A C10 H10B 108.9(4) . . . yes C18 C17 H17A 109.8(3) . . . yes C18 C17 H17B 109.0(4) . . . yes O7 C17 H17A 109.3(3) . . . yes O7 C17 H17B 109.2(3) . . . yes H17A C17 H17B 109.0(4) . . . yes C17 C18 H18A 109.7(4) . . . yes C17 C18 H18B 108.9(4) . . . yes O8 C18 H18A 109.7(4) . . . yes O8 C18 H18B 109.2(4) . . . yes H18A C18 H18B 108.8(4) . . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C9 C9 3.703(5) 1_555 2_677 ? C9 C10 3.846(5) 1_555 2_677 ? C9 C17 3.845(5) 1_555 2_566 ? C9 C18 3.993(5) 1_555 2_567 ? C9 S20 3.877(4) 1_555 2_666 ? C9 H18B 3.041(4) 1_555 2_567 ? C9 H10B 3.089(3) 1_555 2_677 ? C10 C17 3.936(5) 1_555 2_567 ? C10 C21 3.823(5) 1_555 2_667 ? C10 C22 3.630(5) 1_555 2_667 ? C10 O24 3.279(4) 1_555 1_566 ? C11 C15 3.514(4) 1_555 2_567 ? C11 C16 3.864(4) 1_555 2_567 ? C11 S5 3.888(3) 1_555 2_567 ? C11 S20 3.743(3) 1_555 2_666 ? C12 C15 3.819(4) 1_555 2_567 ? C12 S5 3.877(3) 1_555 2_567 ? C12 S20 3.574(3) 1_555 2_666 ? C12 Pd1 4.248(3) 1_555 1_556 ? C12 Pd1 4.248(3) 1_555 2_667 ? C13 C14 3.775(4) 1_555 2_567 ? C13 S5 3.584(3) 1_555 2_567 ? C13 Pd1 4.580(3) 1_555 1_556 ? C13 Pd1 4.580(3) 1_555 2_667 ? C14 S3 3.655(3) 1_555 2_567 ? C15 S3 3.864(3) 1_555 2_567 ? C15 S20 3.886(3) 1_555 1_455 ? C16 S3 3.895(3) 1_555 2_567 ? C17 C17 3.934(5) 1_555 2_556 ? C17 C18 3.923(5) 1_555 2_556 ? C17 O23 3.099(4) 1_555 2_556 ? C17 H17B 3.115(4) 1_555 2_556 ? C17 H10A 2.993(4) 1_555 2_567 ? C18 C18 3.408(5) 1_555 2_557 ? C18 C21 3.989(4) 1_555 2_556 ? C18 O23 3.021(4) 1_555 2_556 ? C18 H17B 2.937(4) 1_555 2_556 ? C18 H18B 2.903(4) 1_555 2_557 ? C21 O2 3.114(4) 1_555 2_667 ? C21 S3 3.630(3) 1_555 2_566 ? C21 S6 3.737(4) 1_555 1_554 ? C21 Pd1 3.232(3) 1_555 2_666 ? C22 O2 3.255(4) 1_555 2_667 ? C22 S6 3.485(3) 1_555 1_554 ? C22 Pd1 3.247(3) 1_555 2_666 ? O1 H18B 2.569(2) 1_555 2_567 ? O23 H18A 2.282(3) 1_555 2_556 ? S3 S5 3.594(1) 1_555 2_566 ? S3 S19 3.499(1) 1_555 2_566 ? S4 S4 3.613(1) 1_555 2_667 ? S4 S5 3.787(1) 1_555 2_567 ? S4 S19 3.686(1) 1_555 2_667 ? S4 Pd1 3.2941 1_555 1_556 ? S4 Pd1 3.2941 1_555 2_667 ? S5 S19 3.543(1) 1_555 2_566 ? S5 S20 3.439(1) 1_555 1_455 ? S5 Pd1 4.1847 1_555 1_455 ? S5 Pd1 4.1847 1_555 2_566 ? S6 S20 3.768(1) 1_555 1_556 ? S6 Pd1 4.4840 1_555 1_556 ? S6 Pd1 4.4840 1_555 2_667 ? S19 S20 3.271(1) 1_555 2_666 ? S20 H9A 3.0356 1_555 2_666 ? C9 C9 3.703(5) 1_555 2_677 ? C9 C10 3.846(5) 1_555 2_677 ? C9 C17 3.845(5) 1_555 2_566 ? C9 C18 3.993(5) 1_555 2_567 ? C9 S20 3.877(4) 1_555 2_666 ? C9 H18B 3.041(4) 1_555 2_567 ? C9 H10B 3.089(3) 1_555 2_677 ? C10 C17 3.936(5) 1_555 2_567 ? C10 C21 3.823(5) 1_555 2_667 ? C10 C22 3.630(5) 1_555 2_667 ? C10 O24 3.279(4) 1_555 1_566 ? C11 C15 3.514(4) 1_555 2_567 ? C11 C16 3.864(4) 1_555 2_567 ? C11 S5 3.888(3) 1_555 2_567 ? C11 S20 3.743(3) 1_555 2_666 ? C12 C15 3.819(4) 1_555 2_567 ? C12 S5 3.877(3) 1_555 2_567 ? C12 S20 3.574(3) 1_555 2_666 ? C12 Pd1 4.248(3) 1_555 1_556 ? C12 Pd1 4.248(3) 1_555 2_667 ? C13 C14 3.775(4) 1_555 2_567 ? C13 S5 3.584(3) 1_555 2_567 ? C13 Pd1 4.580(3) 1_555 1_556 ? C13 Pd1 4.580(3) 1_555 2_667 ? C14 S3 3.655(3) 1_555 2_567 ? C15 S3 3.864(3) 1_555 2_567 ? C15 S20 3.886(3) 1_555 1_455 ? C16 S3 3.895(3) 1_555 2_567 ? C17 C17 3.934(5) 1_555 2_556 ? C17 C18 3.923(5) 1_555 2_556 ? C17 O23 3.099(4) 1_555 2_556 ? C17 H17B 3.115(4) 1_555 2_556 ? C17 H10A 2.993(4) 1_555 2_567 ? C18 C18 3.408(5) 1_555 2_557 ? C18 C21 3.989(4) 1_555 2_556 ? C18 O23 3.021(4) 1_555 2_556 ? C18 H17B 2.937(4) 1_555 2_556 ? C18 H18B 2.903(4) 1_555 2_557 ? C21 O2 3.114(4) 1_555 2_667 ? C21 S3 3.630(3) 1_555 2_566 ? C21 S6 3.737(4) 1_555 1_554 ? C21 Pd1 3.232(3) 1_555 2_666 ? C22 O2 3.255(4) 1_555 2_667 ? C22 S6 3.485(3) 1_555 1_554 ? C22 Pd1 3.247(3) 1_555 2_666 ? O1 H18B 2.569(2) 1_555 2_567 ? O23 H18A 2.282(3) 1_555 2_556 ? S3 S5 3.594(1) 1_555 2_566 ? S3 S19 3.499(1) 1_555 2_566 ? S4 S4 3.613(1) 1_555 2_667 ? S4 S5 3.787(1) 1_555 2_567 ? S4 S19 3.686(1) 1_555 2_667 ? S4 Pd1 3.2941 1_555 1_556 ? S4 Pd1 3.2941 1_555 2_667 ? S5 S19 3.543(1) 1_555 2_566 ? S5 S20 3.439(1) 1_555 1_455 ? S5 Pd1 4.1847 1_555 1_455 ? S5 Pd1 4.1847 1_555 2_566 ? S6 S20 3.768(1) 1_555 1_556 ? S6 Pd1 4.4840 1_555 1_556 ? S6 Pd1 4.4840 1_555 2_667 ? S19 S20 3.271(1) 1_555 2_666 ? S20 H9A 3.0356 1_555 2_666 ? #===END