Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Inabe, Tamotsu' 'Kobayashi, H.' 'Kobayashi, A.' 'Naito, Toshio' _publ_contact_author_name 'Prof Toshio Naito' _publ_contact_author_address ; Prof Toshio Naito Division of Chemistry,Graduate School of Science Hokkaido University Sapporo 060-0810 JAPAN ; _publ_contact_author_email 'TNAITO@SCI.HOKUDAI.AC.JP' data_matrt _database_code_CSD 163763 # * next for test purposes _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic ; Quinuclidinium bis(1,3-dithiol-2-thione-4,5-dithiolato)palladium at 298K ; _chemical_name_common ? _chemical_formula_moiety '(C7 H14 N), 2(C6 Pd S10)' _chemical_formula_sum 'C19 H14 N Pd2 S20' _chemical_formula_weight 1110.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.603(3) _cell_length_b 6.3722(11) _cell_length_c 36.335(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.020(10) _cell_angle_gamma 90.00 _cell_volume 3381.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 15.37 _cell_measurement_theta_max 17.33 _exptl_crystal_description 'irregular plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 2.320 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_process_details ; North, Phillips and Mathews, 1968 ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC 18' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% none _diffrn_reflns_number 2876 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2673 _reflns_number_gt 2414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC System' _computing_cell_refinement 'MXC System' _computing_data_reduction 'MXC System (Mac Science, Japan)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In this refinement all non-H were refined isotropically and H placed in calculated positions and refined with a riding model. The disorder of the cation around a 2-fold crystallographic axis was modelled on the basis of a connected set of atoms with overall sof 0.5 but with C/N pairs of atoms with sof 0.25 in the C9 and C12 sites. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+434.6241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2673 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2506 _refine_ls_wR_factor_gt 0.2465 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.253 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.65700(9) 0.3170(2) -0.01824(4) 0.0267(4) Uani 1 d . . . S1 S 0.4598(4) 0.6155(11) 0.15561(15) 0.0507(15) Uani 1 d . . . S2 S 0.4968(3) 0.2995(9) 0.09775(14) 0.0372(12) Uani 1 d . . . S3 S 0.5608(4) 0.7252(8) 0.08728(14) 0.0387(12) Uani 1 d . . . S4 S 0.5747(3) 0.1498(8) 0.02673(15) 0.0362(11) Uani 1 d . . . S5 S 0.6493(3) 0.6253(7) 0.01515(14) 0.0332(11) Uani 1 d . . . C1 C 0.5044(11) 0.552(3) 0.1155(5) 0.034(4) Uani 1 d . . . C2 C 0.5567(11) 0.347(3) 0.0569(4) 0.026(4) Uani 1 d . . . C3 C 0.5882(12) 0.546(3) 0.0528(5) 0.031(4) Uani 1 d . . . S6 S 0.6539(3) 0.0095(7) -0.05128(13) 0.0318(11) Uani 1 d . . . S7 S 0.7314(3) 0.4826(8) -0.06625(14) 0.0336(11) Uani 1 d . . . S8 S 0.7142(4) -0.0904(8) -0.12798(14) 0.0383(12) Uani 1 d . . . S9 S 0.7842(4) 0.3256(9) -0.14162(14) 0.0406(12) Uani 1 d . . . S10 S 0.7991(5) -0.0012(12) -0.20010(17) 0.0620(18) Uani 1 d . . . C4 C 0.7038(12) 0.087(3) -0.0913(5) 0.033(4) Uani 1 d . . . C5 C 0.7367(12) 0.283(3) -0.0984(5) 0.031(4) Uani 1 d . . . C6 C 0.7675(13) 0.072(4) -0.1596(6) 0.040(5) Uani 1 d . . . C7 C 0.937(5) 0.644(13) 0.2200(19) 0.08(2) Uani 0.50 d P A -1 H7A H 0.9010 0.7692 0.2242 0.096 Uiso 0.50 calc PR A -1 H7B H 0.9294 0.6026 0.1945 0.096 Uiso 0.50 calc PR A -1 C8 C 0.905(4) 0.477(10) 0.2438(16) 0.067(16) Uani 0.50 d P A -1 H8A H 0.8880 0.3566 0.2289 0.081 Uiso 0.50 calc PR A -1 H8B H 0.8509 0.5238 0.2569 0.081 Uiso 0.50 calc PR A -1 C9 C 0.978(3) 0.411(7) 0.2716(13) 0.050(11) Uani 0.25 d P A -1 H9 H 0.9538 0.3046 0.2883 0.060 Uiso 0.50 calc PR A -1 N9 N 0.978(3) 0.411(7) 0.2716(13) 0.050(11) Uani 0.25 d P B -1 C10 C 1.060(4) 0.323(9) 0.2499(18) 0.070(17) Uani 0.50 d P A -1 H10A H 1.0411 0.2007 0.2358 0.084 Uiso 0.50 calc PR A -1 H10B H 1.1086 0.2824 0.2665 0.084 Uiso 0.50 calc PR A -1 C11 C 1.092(4) 0.501(7) 0.2238(14) 0.053(12) Uani 0.50 d P A -1 H11A H 1.1549 0.5359 0.2294 0.064 Uiso 0.50 calc PR A -1 H11B H 1.0892 0.4521 0.1986 0.064 Uiso 0.50 calc PR A -1 C12 C 1.036(3) 0.690(7) 0.2273(13) 0.048(10) Uani 0.25 d P A -1 H12 H 1.0580 0.7985 0.2103 0.057 Uiso 0.50 calc PR A -1 N12 N 1.036(3) 0.690(7) 0.2273(13) 0.048(10) Uani 0.25 d P C -1 C13 C 1.040(5) 0.766(9) 0.2654(19) 0.074(19) Uani 0.50 d P A -1 H13A H 1.0035 0.8925 0.2675 0.088 Uiso 0.50 calc PR A -1 H13B H 1.1031 0.8034 0.2711 0.088 Uiso 0.50 calc PR A -1 C14 C 1.007(4) 0.608(8) 0.2933(12) 0.048(13) Uani 0.50 d P A -1 H14A H 0.9554 0.6644 0.3069 0.058 Uiso 0.50 calc PR A -1 H14B H 1.0555 0.5745 0.3105 0.058 Uiso 0.50 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0281(7) 0.0247(7) 0.0273(7) -0.0020(6) 0.0018(5) -0.0021(6) S1 0.058(3) 0.068(4) 0.027(3) -0.010(3) 0.013(2) 0.009(3) S2 0.039(3) 0.041(3) 0.032(3) -0.001(2) 0.009(2) -0.006(2) S3 0.048(3) 0.032(3) 0.037(3) -0.008(2) 0.007(2) 0.002(2) S4 0.037(2) 0.026(2) 0.046(3) -0.004(2) 0.007(2) -0.008(2) S5 0.042(3) 0.024(2) 0.034(3) -0.005(2) 0.008(2) -0.002(2) C1 0.022(9) 0.049(12) 0.031(11) 0.000(9) -0.005(7) 0.003(8) C2 0.028(8) 0.036(10) 0.014(8) -0.004(8) -0.001(6) 0.005(8) C3 0.029(9) 0.033(10) 0.030(10) 0.000(8) -0.010(8) 0.006(8) S6 0.038(2) 0.027(2) 0.030(3) -0.004(2) 0.0048(19) -0.005(2) S7 0.042(3) 0.026(2) 0.032(3) 0.003(2) 0.006(2) -0.002(2) S8 0.049(3) 0.038(3) 0.028(3) -0.009(2) 0.007(2) 0.001(2) S9 0.044(3) 0.049(3) 0.029(3) -0.001(2) 0.010(2) -0.005(2) S10 0.069(4) 0.080(5) 0.037(3) -0.017(3) 0.019(3) -0.007(4) C4 0.033(9) 0.031(10) 0.035(11) -0.004(9) -0.004(8) 0.009(8) C5 0.029(9) 0.035(11) 0.031(10) -0.011(9) -0.005(7) 0.004(8) C6 0.029(9) 0.047(12) 0.044(13) 0.003(10) 0.003(9) 0.002(9) C7 0.10(5) 0.08(5) 0.06(4) 0.03(4) -0.03(4) -0.02(5) C8 0.05(3) 0.08(4) 0.07(4) -0.02(3) -0.02(3) 0.01(3) C9 0.06(3) 0.04(2) 0.06(3) 0.02(2) 0.02(2) -0.01(2) N9 0.06(3) 0.04(2) 0.06(3) 0.02(2) 0.02(2) -0.01(2) C10 0.05(3) 0.05(3) 0.11(5) 0.03(3) -0.03(3) -0.01(3) C11 0.07(3) 0.04(3) 0.05(3) 0.00(2) 0.02(3) 0.00(2) C12 0.06(3) 0.03(2) 0.05(3) 0.01(2) 0.00(2) -0.01(2) N12 0.06(3) 0.03(2) 0.05(3) 0.01(2) 0.00(2) -0.01(2) C13 0.07(4) 0.04(3) 0.11(6) 0.00(3) 0.03(4) 0.00(3) C14 0.06(3) 0.06(3) 0.02(3) 0.01(2) 0.02(2) 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S4 2.292(5) . ? Pd1 S6 2.298(5) . ? Pd1 S7 2.311(5) . ? Pd1 S5 2.312(5) . ? Pd1 Pd1 3.140(3) 7_655 ? S1 C1 1.648(19) . ? S2 C1 1.74(2) . ? S2 C2 1.751(17) . ? S3 C1 1.72(2) . ? S3 C3 1.744(19) . ? S4 C2 1.689(18) . ? S5 C3 1.71(2) . ? C2 C3 1.35(3) . ? S6 C4 1.70(2) . ? S7 C5 1.730(18) . ? S8 C6 1.73(2) . ? S8 C4 1.75(2) . ? S9 C5 1.739(19) . ? S9 C6 1.76(2) . ? S10 C6 1.61(2) . ? C4 C5 1.36(3) . ? C7 C8 1.45(8) . ? C7 C12 1.50(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.53(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.53(7) . ? C9 C14 1.54(7) . ? C9 H9 0.9800 . ? C10 C11 1.55(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.46(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.47(7) . ? C12 H12 0.9800 . ? C13 C14 1.51(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Pd1 S6 88.04(18) . . ? S4 Pd1 S7 176.05(19) . . ? S6 Pd1 S7 90.25(18) . . ? S4 Pd1 S5 89.73(18) . . ? S6 Pd1 S5 176.07(18) . . ? S7 Pd1 S5 91.77(18) . . ? S4 Pd1 Pd1 91.52(15) . 7_655 ? S6 Pd1 Pd1 90.34(14) . 7_655 ? S7 Pd1 Pd1 92.05(14) . 7_655 ? S5 Pd1 Pd1 92.96(14) . 7_655 ? C1 S2 C2 97.0(9) . . ? C1 S3 C3 96.7(10) . . ? C2 S4 Pd1 101.4(6) . . ? C3 S5 Pd1 101.1(7) . . ? S1 C1 S3 124.0(13) . . ? S1 C1 S2 122.1(12) . . ? S3 C1 S2 113.9(11) . . ? C3 C2 S4 124.9(14) . . ? C3 C2 S2 115.2(14) . . ? S4 C2 S2 119.9(11) . . ? C2 C3 S5 122.9(15) . . ? C2 C3 S3 117.1(15) . . ? S5 C3 S3 120.0(11) . . ? C4 S6 Pd1 101.1(7) . . ? C5 S7 Pd1 101.2(7) . . ? C6 S8 C4 99.2(10) . . ? C5 S9 C6 97.8(10) . . ? C5 C4 S6 125.3(15) . . ? C5 C4 S8 114.5(15) . . ? S6 C4 S8 120.2(12) . . ? C4 C5 S7 122.1(15) . . ? C4 C5 S9 117.1(14) . . ? S7 C5 S9 120.8(12) . . ? S10 C6 S8 124.2(14) . . ? S10 C6 S9 124.4(13) . . ? S8 C6 S9 111.4(12) . . ? C8 C7 C12 111(5) . . ? C8 C7 H7A 109.5 . . ? C12 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C12 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 112(5) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 108(5) . . ? C8 C9 C14 108(4) . . ? C10 C9 C14 111(4) . . ? C8 C9 H9 110.3 . . ? C10 C9 H9 110.3 . . ? C14 C9 H9 110.3 . . ? C9 C10 C11 106(4) . . ? C9 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? C9 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 113(4) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 109(4) . . ? C11 C12 C7 111(5) . . ? C13 C12 C7 106(6) . . ? C11 C12 H12 110.1 . . ? C13 C12 H12 110.1 . . ? C7 C12 H12 110.1 . . ? C12 C13 C14 114(4) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C9 107(4) . . ? C13 C14 H14A 110.4 . . ? C9 C14 H14A 110.4 . . ? C13 C14 H14B 110.4 . . ? C9 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? 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 S6 Pd1 S4 C2 -176.3(6) . . . . ? S5 Pd1 S4 C2 0.5(6) . . . . ? Pd1 Pd1 S4 C2 93.4(6) 7_655 . . . ? S4 Pd1 S5 C3 0.1(6) . . . . ? S7 Pd1 S5 C3 176.4(6) . . . . ? Pd1 Pd1 S5 C3 -91.4(6) 7_655 . . . ? C3 S3 C1 S1 178.6(12) . . . . ? C3 S3 C1 S2 -2.1(11) . . . . ? C2 S2 C1 S1 -179.7(11) . . . . ? C2 S2 C1 S3 1.0(11) . . . . ? Pd1 S4 C2 C3 -1.3(17) . . . . ? Pd1 S4 C2 S2 -178.8(8) . . . . ? C1 S2 C2 C3 1.0(15) . . . . ? C1 S2 C2 S4 178.8(11) . . . . ? S4 C2 C3 S5 2(2) . . . . ? S2 C2 C3 S5 179.3(9) . . . . ? S4 C2 C3 S3 179.7(10) . . . . ? S2 C2 C3 S3 -2.7(19) . . . . ? Pd1 S5 C3 C2 -0.9(16) . . . . ? Pd1 S5 C3 S3 -178.9(9) . . . . ? C1 S3 C3 C2 2.9(16) . . . . ? C1 S3 C3 S5 -179.0(11) . . . . ? S4 Pd1 S6 C4 174.6(7) . . . . ? S7 Pd1 S6 C4 -1.9(7) . . . . ? Pd1 Pd1 S6 C4 -93.9(6) 7_655 . . . ? S6 Pd1 S7 C5 1.9(6) . . . . ? S5 Pd1 S7 C5 -174.7(6) . . . . ? Pd1 Pd1 S7 C5 92.3(6) 7_655 . . . ? Pd1 S6 C4 C5 1.5(18) . . . . ? Pd1 S6 C4 S8 -177.2(9) . . . . ? C6 S8 C4 C5 0.9(16) . . . . ? C6 S8 C4 S6 179.7(11) . . . . ? S6 C4 C5 S7 0(2) . . . . ? S8 C4 C5 S7 178.9(10) . . . . ? S6 C4 C5 S9 -179.4(10) . . . . ? S8 C4 C5 S9 -1(2) . . . . ? Pd1 S7 C5 C4 -1.7(17) . . . . ? Pd1 S7 C5 S9 177.8(9) . . . . ? C6 S9 C5 C4 0.1(16) . . . . ? C6 S9 C5 S7 -179.4(11) . . . . ? C4 S8 C6 S10 178.4(13) . . . . ? C4 S8 C6 S9 -0.8(12) . . . . ? C5 S9 C6 S10 -178.7(13) . . . . ? C5 S9 C6 S8 0.5(12) . . . . ? C12 C7 C8 C9 5(9) . . . . ? C7 C8 C9 C10 -63(7) . . . . ? C7 C8 C9 C14 56(7) . . . . ? C8 C9 C10 C11 59(6) . . . . ? C14 C9 C10 C11 -59(6) . . . . ? C9 C10 C11 C12 -1(7) . . . . ? C10 C11 C12 C13 59(6) . . . . ? C10 C11 C12 C7 -57(7) . . . . ? C8 C7 C12 C11 55(8) . . . . ? C8 C7 C12 C13 -63(8) . . . . ? C11 C12 C13 C14 -59(7) . . . . ? C7 C12 C13 C14 61(8) . . . . ? C12 C13 C14 C9 0(8) . . . . ? C8 C9 C14 C13 -58(6) . . . . ? C10 C9 C14 C13 60(6) . . . . ? # * Fraction theta max is twice value on next card because data C-centred _diffrn_measured_fraction_theta_max 0.408 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.408 # * Max density 1.54 Ang. from S5 _refine_diff_density_max 1.265 _refine_diff_density_min -1.477 _refine_diff_density_rms 0.299 #Least-squares planes (x,y,z in crystal coordinates) and deviations #from them (* indicates atom used to define plane). #Plane 1. # # 12.4201 (0.0151) x - 1.5061 (0.0137) y + 17.0608 (0.0561) z = 7.3738 (0.0124) #* -0.0056 (0.0054) S4 #* 0.0076 (0.0054) S5 #* -0.0130 (0.0133) C2 #* 0.0094 (0.0136) C3 #* 0.0135 (0.0051) S2 #* -0.0118 (0.0052) S3 # -0.0024 (0.0071) Pd1 # 0.0301 (0.0180) C1 # 0.0644 (0.0101) S1 #Rms deviation of fitted atoms = 0.0105 #Plane 2. # 13.0757 (0.0139) x - 1.7573 (0.0136) y + 12.6898 (0.0593) z = 7.8827 (0.0167) #Angle to previous plane (with approximate esd) = 7.70 ( 0.23 ) #* -0.0003 (0.0057) S6 #* -0.0075 (0.0056) S7 #* 0.0095 (0.0144) C4 #* 0.0055 (0.0141) C5 #* -0.0086 (0.0054) S8 #* 0.0014 (0.0053) S9 # -0.0804 (0.0071) Pd1 # 0.0017 (0.0200) C6 # 0.0289 (0.0110) S10 #Rms deviation of fitted atoms = 0.0065 # 'Linear' torsion angles excluded as per PLAT_713 level C alerts # S7 Pd1 S4 C2 -112(3) . . . . ? # S6 Pd1 S5 C3 55(3) . . . . ? # S5 Pd1 S6 C4 119(3) . . . . ? # S4 Pd1 S7 C5 -62(3) . . . . ? data_matlt _database_code_CSD 163764 # * this next for test purposes _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic ; Qinuclidinium bis(1,3-dithiol-2-thione-4,5-dithiolato)palladium at 150K ; _chemical_name_common ? _chemical_formula_moiety '(C7 H14 N), 2(C6 Pd S10)' _chemical_formula_sum 'C19 H14 N Pd2 S20' _chemical_formula_weight 1110.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.50(2) _cell_length_b 6.333(9) _cell_length_c 36.13(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.14(10) _cell_angle_gamma 90.00 _cell_volume 3318(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.55 _cell_measurement_theta_max 17.55 _exptl_crystal_description 'irregular platey needle' _exptl_crystal_colour black _exptl_crystal_size_max 1.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 2.364 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.317 _exptl_absorpt_process_details ; North, Phillips & Mathews, 1968 ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science MXC 18' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3600 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.62 _reflns_number_total 3416 _reflns_number_gt 2844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MXC System (Mac Science, Japan)' _computing_cell_refinement 'MXC System (Mac Science, Japan)' _computing_data_reduction 'MXC System (Mac Science, Japan)' _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Refinement based on same model as 298K structure but only Pd and S refined anisotropically to elliminate non-positive definite anisotropic thermal displacement ellipsoid tensors for a number of C atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+703.9433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3416 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.1247 _refine_ls_wR_factor_ref 0.3269 _refine_ls_wR_factor_gt 0.3151 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.65711(9) 0.3171(2) -0.01824(4) 0.0192(4) Uani 1 d . . . S1 S 0.4575(4) 0.6184(10) 0.15620(14) 0.0326(12) Uani 1 d . . . S2 S 0.4956(3) 0.3004(9) 0.09830(14) 0.0253(10) Uani 1 d . . . S3 S 0.5600(3) 0.7301(8) 0.08775(14) 0.0251(10) Uani 1 d . . . S4 S 0.5740(3) 0.1497(8) 0.02699(14) 0.0244(10) Uani 1 d . . . S5 S 0.6496(3) 0.6273(8) 0.01498(14) 0.0237(10) Uani 1 d . . . C1 C 0.5017(14) 0.547(3) 0.1164(6) 0.027(4) Uiso 1 d . . . C2 C 0.5559(12) 0.354(3) 0.0570(5) 0.020(4) Uiso 1 d . . . C3 C 0.5883(12) 0.552(3) 0.0523(5) 0.019(4) Uiso 1 d . . . S6 S 0.6535(3) 0.0078(8) -0.05169(13) 0.0217(10) Uani 1 d . . . S7 S 0.7318(3) 0.4843(8) -0.06627(14) 0.0217(10) Uani 1 d . . . S8 S 0.7149(3) -0.0953(8) -0.12854(14) 0.0260(11) Uani 1 d . . . S9 S 0.7852(3) 0.3264(9) -0.14161(14) 0.0273(11) Uani 1 d . . . S10 S 0.7992(5) -0.0056(12) -0.20072(17) 0.0488(18) Uani 1 d . . . C4 C 0.7033(12) 0.084(3) -0.0911(5) 0.021(4) Uiso 1 d . . . C5 C 0.7367(12) 0.283(3) -0.0984(5) 0.018(3) Uiso 1 d . . . C6 C 0.7693(13) 0.075(3) -0.1592(5) 0.023(4) Uiso 1 d . . . C7 C 0.929(3) 0.643(9) 0.2200(15) 0.041(11) Uiso 0.50 d P A -1 H7A H 0.9260 0.5732 0.1955 0.049 Uiso 0.50 calc PR A -1 H7B H 0.8908 0.7728 0.2190 0.049 Uiso 0.50 calc PR A -1 C8 C 0.893(4) 0.493(10) 0.2503(16) 0.049(13) Uiso 0.50 d P A -1 H8A H 0.8631 0.3685 0.2388 0.058 Uiso 0.50 calc PR A -1 H8B H 0.8462 0.5667 0.2656 0.058 Uiso 0.50 calc PR A -1 C9 C 0.974(3) 0.421(7) 0.2751(13) 0.036(9) Uiso 0.25 d P A -1 H9 H 0.9520 0.3161 0.2938 0.043 Uiso 0.50 calc PR A -1 N9 N 0.974(3) 0.421(7) 0.2751(13) 0.036(9) Uiso 0.25 d P B -1 C10 C 1.052(3) 0.309(9) 0.2485(14) 0.040(11) Uiso 0.50 d P A -1 H10A H 1.1030 0.2480 0.2633 0.048 Uiso 0.50 calc PR A -1 H10B H 1.0242 0.1960 0.2331 0.048 Uiso 0.50 calc PR A -1 C11 C 1.087(3) 0.499(7) 0.2235(12) 0.027(8) Uiso 0.50 d P A -1 H11A H 1.1527 0.5305 0.2296 0.032 Uiso 0.50 calc PR A -1 H11B H 1.0843 0.4584 0.1971 0.032 Uiso 0.50 calc PR A -1 C12 C 1.029(3) 0.699(7) 0.2297(11) 0.028(8) Uiso 0.25 d P A -1 H12 H 1.0506 0.8111 0.2124 0.034 Uiso 0.50 calc PR A -1 N12 N 1.029(3) 0.699(7) 0.2297(11) 0.028(8) Uiso 0.25 d P C -1 C13 C 1.036(3) 0.774(8) 0.2656(13) 0.037(10) Uiso 0.50 d P A -1 H13A H 0.9936 0.8955 0.2691 0.045 Uiso 0.50 calc PR A -1 H13B H 1.0995 0.8209 0.2708 0.045 Uiso 0.50 calc PR A -1 C14 C 1.008(4) 0.586(10) 0.2922(16) 0.050(13) Uiso 0.50 d P A -1 H14A H 1.0630 0.5426 0.3065 0.060 Uiso 0.50 calc PR A -1 H14B H 0.9614 0.6380 0.3100 0.060 Uiso 0.50 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0175(6) 0.0181(7) 0.0221(7) 0.0001(6) 0.0058(5) -0.0017(6) S1 0.034(3) 0.045(3) 0.019(2) -0.004(2) 0.0126(19) 0.006(2) S2 0.023(2) 0.028(3) 0.024(2) 0.001(2) 0.0115(17) -0.004(2) S3 0.029(2) 0.021(2) 0.024(2) -0.0042(19) 0.0083(18) 0.0010(19) S4 0.026(2) 0.019(2) 0.028(2) -0.0047(19) 0.0103(18) -0.0038(18) S5 0.025(2) 0.019(2) 0.027(2) -0.0013(19) 0.0089(18) -0.0038(18) S6 0.026(2) 0.018(2) 0.021(2) 0.0002(18) 0.0078(17) -0.0002(18) S7 0.023(2) 0.018(2) 0.025(2) -0.0002(19) 0.0097(17) 0.0000(18) S8 0.029(2) 0.027(3) 0.022(2) -0.005(2) 0.0105(18) 0.001(2) S9 0.029(2) 0.031(3) 0.023(2) -0.004(2) 0.0125(18) -0.004(2) S10 0.057(4) 0.061(4) 0.028(3) -0.019(3) 0.030(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S4 2.292(6) . ? Pd1 S6 2.302(6) . ? Pd1 S5 2.305(6) . ? Pd1 S7 2.305(5) . ? Pd1 Pd1 3.114(5) 7_655 ? S1 C1 1.64(2) . ? S2 C1 1.70(2) . ? S2 C2 1.762(19) . ? S3 C3 1.755(19) . ? S3 C1 1.77(2) . ? S4 C2 1.71(2) . ? S5 C3 1.685(19) . ? C2 C3 1.35(3) . ? S6 C4 1.671(19) . ? S7 C5 1.725(19) . ? S8 C6 1.74(2) . ? S8 C4 1.77(2) . ? S9 C6 1.73(2) . ? S9 C5 1.737(18) . ? S10 C6 1.64(2) . ? C4 C5 1.38(3) . ? C7 C12 1.53(6) . ? C7 C8 1.54(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.55(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.31(7) . ? C9 C10 1.64(6) . ? C9 H9 1.0000 . ? C10 C11 1.59(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.54(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.38(6) . ? C12 H12 1.0000 . ? C13 C14 1.58(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Pd1 S6 88.3(2) . . ? S4 Pd1 S5 89.8(2) . . ? S6 Pd1 S5 175.98(18) . . ? S4 Pd1 S7 176.0(2) . . ? S6 Pd1 S7 90.33(19) . . ? S5 Pd1 S7 91.3(2) . . ? S4 Pd1 Pd1 91.60(18) . 7_655 ? S6 Pd1 Pd1 90.48(15) . 7_655 ? S5 Pd1 Pd1 93.12(16) . 7_655 ? S7 Pd1 Pd1 92.11(16) . 7_655 ? C1 S2 C2 97.1(10) . . ? C3 S3 C1 96.8(10) . . ? C2 S4 Pd1 100.7(7) . . ? C3 S5 Pd1 101.6(7) . . ? S1 C1 S2 124.8(13) . . ? S1 C1 S3 121.4(13) . . ? S2 C1 S3 113.7(12) . . ? C3 C2 S4 124.6(15) . . ? C3 C2 S2 117.2(14) . . ? S4 C2 S2 118.1(11) . . ? C2 C3 S5 123.2(15) . . ? C2 C3 S3 115.0(14) . . ? S5 C3 S3 121.8(11) . . ? C4 S6 Pd1 101.1(7) . . ? C5 S7 Pd1 100.8(6) . . ? C6 S8 C4 97.7(9) . . ? C6 S9 C5 97.5(9) . . ? C5 C4 S6 125.5(15) . . ? C5 C4 S8 114.1(14) . . ? S6 C4 S8 120.4(11) . . ? C4 C5 S7 122.3(14) . . ? C4 C5 S9 117.3(14) . . ? S7 C5 S9 120.4(11) . . ? S10 C6 S9 125.8(12) . . ? S10 C6 S8 120.8(12) . . ? S9 C6 S8 113.4(11) . . ? C12 C7 C8 107(4) . . ? C12 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? C12 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? C7 C8 C9 109(4) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C14 C9 C8 108(5) . . ? C14 C9 C10 112(4) . . ? C8 C9 C10 108(4) . . ? C14 C9 H9 109.5 . . ? C8 C9 H9 109.5 . . ? C10 C9 H9 109.5 . . ? C11 C10 C9 103(4) . . ? C11 C10 H10A 111.1 . . ? C9 C10 H10A 111.1 . . ? C11 C10 H10B 111.1 . . ? C9 C10 H10B 111.1 . . ? H10A C10 H10B 109.1 . . ? C12 C11 C10 111(3) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C7 111(4) . . ? C13 C12 C11 113(4) . . ? C7 C12 C11 108(4) . . ? C13 C12 H12 108.5 . . ? C7 C12 H12 108.5 . . ? C11 C12 H12 108.5 . . ? C12 C13 C14 107(4) . . ? C12 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? C12 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C9 C14 C13 114(5) . . ? C9 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C9 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? 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 S6 Pd1 S4 C2 -175.7(7) . . . . ? S5 Pd1 S4 C2 0.8(7) . . . . ? Pd1 Pd1 S4 C2 93.9(6) 7_655 . . . ? S4 Pd1 S5 C3 -0.2(7) . . . . ? S7 Pd1 S5 C3 176.1(7) . . . . ? Pd1 Pd1 S5 C3 -91.8(7) 7_655 . . . ? C2 S2 C1 S1 179.6(14) . . . . ? C2 S2 C1 S3 0.5(13) . . . . ? C3 S3 C1 S1 179.2(13) . . . . ? C3 S3 C1 S2 -1.7(13) . . . . ? Pd1 S4 C2 C3 -1.5(17) . . . . ? Pd1 S4 C2 S2 -178.3(9) . . . . ? C1 S2 C2 C3 1.4(17) . . . . ? C1 S2 C2 S4 178.4(12) . . . . ? S4 C2 C3 S5 2(2) . . . . ? S2 C2 C3 S5 178.4(10) . . . . ? S4 C2 C3 S3 -179.5(10) . . . . ? S2 C2 C3 S3 -3(2) . . . . ? Pd1 S5 C3 C2 -0.7(17) . . . . ? Pd1 S5 C3 S3 -179.4(10) . . . . ? C1 S3 C3 C2 2.6(16) . . . . ? C1 S3 C3 S5 -178.6(12) . . . . ? S4 Pd1 S6 C4 174.7(7) . . . . ? S7 Pd1 S6 C4 -1.6(7) . . . . ? Pd1 Pd1 S6 C4 -93.7(7) 7_655 . . . ? S6 Pd1 S7 C5 1.8(6) . . . . ? S5 Pd1 S7 C5 -174.6(6) . . . . ? Pd1 Pd1 S7 C5 92.2(6) 7_655 . . . ? Pd1 S6 C4 C5 1.2(18) . . . . ? Pd1 S6 C4 S8 -177.7(10) . . . . ? C6 S8 C4 C5 1.0(16) . . . . ? C6 S8 C4 S6 -180.0(12) . . . . ? S6 C4 C5 S7 0(2) . . . . ? S8 C4 C5 S7 179.4(10) . . . . ? S6 C4 C5 S9 -179.7(11) . . . . ? S8 C4 C5 S9 -0.7(19) . . . . ? Pd1 S7 C5 C4 -1.7(16) . . . . ? Pd1 S7 C5 S9 178.4(9) . . . . ? C6 S9 C5 C4 0.0(16) . . . . ? C6 S9 C5 S7 180.0(11) . . . . ? C5 S9 C6 S10 179.8(14) . . . . ? C5 S9 C6 S8 0.7(12) . . . . ? C4 S8 C6 S10 179.9(12) . . . . ? C4 S8 C6 S9 -1.0(12) . . . . ? C12 C7 C8 C9 -10(6) . . . . ? C7 C8 C9 C14 64(6) . . . . ? C7 C8 C9 C10 -57(5) . . . . ? C14 C9 C10 C11 -53(5) . . . . ? C8 C9 C10 C11 66(5) . . . . ? C9 C10 C11 C12 -8(5) . . . . ? C8 C7 C12 C13 -53(6) . . . . ? C8 C7 C12 C11 71(5) . . . . ? C10 C11 C12 C13 64(5) . . . . ? C10 C11 C12 C7 -59(5) . . . . ? C7 C12 C13 C14 65(5) . . . . ? C11 C12 C13 C14 -56(5) . . . . ? C8 C9 C14 C13 -54(6) . . . . ? C10 C9 C14 C13 65(6) . . . . ? C12 C13 C14 C9 -9(6) . . . . ? # * fraction theta max is actually twice the value below because lattice # * absent reflections have been suppressed i.e. are, as they quite # * reasonably should be, missing from the .hkl file. _diffrn_measured_fraction_theta_max 0.406 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.406 # * this peak is 0.86 Ang. from Pd1 i.e. due to ripple caused by series # * termination _refine_diff_density_max 2.416 _refine_diff_density_min -3.291 _refine_diff_density_rms 0.429 #Least-squares planes (x,y,z in crystal coordinates) and deviations #from them (* indicates atom used to define plane). #Plane 1. # # 12.3186 (0.0263) x - 1.4920 (0.0142) y + 16.9770 (0.0633) z = 7.3085 (0.0179) #* -0.0028 (0.0057) S4 #* 0.0114 (0.0058) S5 #* -0.0199 (0.0144) C2 #* 0.0033 (0.0143) C3 #* 0.0172 (0.0054) S2 #* -0.0092 (0.0054) S3 # 0.0035 (0.0074) Pd1 # 0.0311 (0.0210) C1 # 0.0560 (0.0101) S1 #Rms deviation of fitted atoms = 0.0124 #Plane 2. # 12.9514 (0.0263) x - 1.7443 (0.0136) y + 12.7631 (0.0624) z = 7.7910 (0.0215) #Angle to previous plane (with approximate esd) = 7.49 ( 0.25 ) #* 0.0000 (0.0059) S6 #* -0.0045 (0.0056) S7 #* 0.0071 (0.0147) C4 #* 0.0014 (0.0139) C5 #* -0.0059 (0.0055) S8 #* 0.0019 (0.0053) S9 # -0.0664 (0.0072) Pd1 # 0.0096 (0.0196) C6 # 0.0080 (0.0115) S10 #Rms deviation of fitted atoms = 0.0043 # 'Linear' torsion angles excluded as per PLAT_713 level C alerts # S7 Pd1 S4 C2 -107(3) . . . . ? # S6 Pd1 S5 C3 62(3) . . . . ? # S5 Pd1 S6 C4 113(3) . . . . ? # S4 Pd1 S7 C5 -67(3) . . . . ?