Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_Me3Te[Ni(dmit)2]2 _database_code_CSD 184206 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C15 H9 Ni2 S20 Te ' _chemical_formula_moiety '?' _chemical_formula_weight 1075.44 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.473(2) _cell_length_b 36.11(1) _cell_length_c 6.482(2) _cell_angle_alpha 92.49(8) _cell_angle_beta 110.4(1) _cell_angle_gamma 95.36(4) _cell_volume 1626(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.025 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.196 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.334 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.920 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MAC Science DIP320S' _diffrn_reflns_number 4193 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 28.84 _diffrn_measured_fraction_theta_max 0.4928 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.4928 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 5 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4193 _reflns_number_gt 2827 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0540 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2827 _refine_ls_number_parameters 343 _refine_ls_goodness_of_fit_ref 1.378 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00076|Fo|^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 0.83 _refine_diff_density_min -0.70 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Te(1) Te -0.1095(1) 0.23813(1) 0.6558(1) 0.0503(2) Uani 1.00 d . . . Ni(1) Ni 0.2953(2) 0.52270(2) 0.8051(2) 0.0344(4) Uani 1.00 d . . . Ni(2) Ni 0.2376(2) 0.03217(2) 0.4744(2) 0.0372(4) Uani 1.00 d . . . S(1) S 0.3099(4) 0.55428(5) 1.1035(4) 0.0383(8) Uani 1.00 d . . . S(2) S 0.4133(4) 0.56926(5) 0.6838(4) 0.0405(8) Uani 1.00 d . . . S(3) S 0.1809(4) 0.47517(5) 0.9225(4) 0.0402(8) Uani 1.00 d . . . S(4) S 0.2690(4) 0.49233(5) 0.5003(4) 0.0412(8) Uani 1.00 d . . . S(5) S 0.4512(4) 0.63453(5) 1.2668(4) 0.0470(8) Uani 1.00 d . . . S(6) S 0.5482(4) 0.64826(5) 0.8831(4) 0.0473(8) Uani 1.00 d . . . S(7) S 0.0422(4) 0.39695(5) 0.7158(4) 0.0436(8) Uani 1.00 d . . . S(8) S 0.1248(4) 0.41324(5) 0.3243(4) 0.0416(8) Uani 1.00 d . . . S(9) S 0.6168(5) 0.70981(6) 1.2327(5) 0.066(1) Uani 1.00 d . . . S(10) S -0.0272(5) 0.33728(6) 0.3574(4) 0.064(1) Uani 1.00 d . . . S(11) S 0.2432(4) 0.08311(5) 0.6678(4) 0.0440(8) Uani 1.00 d . . . S(12) S 0.1941(4) 0.06090(5) 0.1763(4) 0.0462(8) Uani 1.00 d . . . S(13) S 0.2752(4) 0.00390(5) 0.7718(4) 0.0456(8) Uani 1.00 d . . . S(14) S 0.2361(4) -0.01933(5) 0.2857(4) 0.0442(8) Uani 1.00 d . . . S(15) S 0.2117(4) 0.16350(5) 0.5459(4) 0.0481(9) Uani 1.00 d . . . S(16) S 0.1513(4) 0.14327(5) 0.0900(4) 0.0490(9) Uani 1.00 d . . . S(17) S 0.3088(4) -0.07745(5) 0.8663(4) 0.0441(8) Uani 1.00 d . . . S(18) S 0.2747(4) -0.09925(5) 0.4195(4) 0.0477(9) Uani 1.00 d . . . S(19) S 0.1543(5) 0.22351(6) 0.2332(5) 0.066(1) Uani 1.00 d . . . S(20) S 0.3225(5) -0.15739(5) 0.7468(5) 0.0620(10) Uani 1.00 d . . . C(1) C 0.407(1) 0.5967(2) 1.073(1) 0.037(3) Uani 1.00 d . . . C(2) C 0.452(2) 0.6034(2) 0.891(1) 0.040(3) Uani 1.00 d . . . C(3) C 0.140(1) 0.4420(2) 0.716(1) 0.037(3) Uani 1.00 d . . . C(4) C 0.175(1) 0.4499(2) 0.528(1) 0.034(3) Uani 1.00 d . . . C(5) C 0.543(2) 0.6664(2) 1.128(2) 0.045(3) Uani 1.00 d . . . C(6) C 0.043(2) 0.3804(2) 0.463(2) 0.044(3) Uani 1.00 d . . . C(7) C 0.281(2) -0.0413(2) 0.690(2) 0.040(3) Uani 1.00 d . . . C(8) C 0.263(1) -0.0515(2) 0.476(1) 0.037(3) Uani 1.00 d . . . C(9) C 0.213(2) 0.1163(2) 0.476(2) 0.041(3) Uani 1.00 d . . . C(10) C 0.189(2) 0.1064(2) 0.263(2) 0.043(3) Uani 1.00 d . . . C(11) C 0.300(2) -0.1134(2) 0.679(2) 0.042(3) Uani 1.00 d . . . C(12) C 0.172(2) 0.1788(2) 0.290(2) 0.042(3) Uani 1.00 d . . . C(13) C -0.306(2) 0.2097(2) 0.771(2) 0.065(4) Uani 1.00 d . . . C(14) C -0.078(2) 0.2887(2) 0.846(2) 0.056(4) Uani 1.00 d . . . C(15) C -0.326(2) 0.2562(2) 0.371(2) 0.070(5) Uani 1.00 d . . . H(1) H -0.4220 0.2228 0.7384 0.0697 Uiso 1.00 calc . . . H(2) H -0.3463 0.1853 0.7054 0.0697 Uiso 1.00 calc . . . H(3) H -0.2553 0.2093 0.9289 0.0697 Uiso 1.00 calc . . . H(4) H 0.0130 0.2883 0.9934 0.0660 Uiso 1.00 calc . . . H(5) H -0.0438 0.3096 0.7811 0.0660 Uiso 1.00 calc . . . H(6) H -0.2013 0.2926 0.8656 0.0660 Uiso 1.00 calc . . . H(7) H -0.2756 0.2783 0.3272 0.0770 Uiso 1.00 calc . . . H(8) H -0.3659 0.2373 0.2544 0.0770 Uiso 1.00 calc . . . H(9) H -0.4346 0.2614 0.4097 0.0770 Uiso 1.00 calc . . . 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 Te(1) 0.0569(7) 0.0404(3) 0.0591(5) 0.0058(2) 0.0280(4) 0.0001(2) Ni(1) 0.038(1) 0.0293(5) 0.0371(7) 0.0028(4) 0.0152(6) 0.0018(4) Ni(2) 0.040(1) 0.0340(5) 0.0385(8) 0.0035(4) 0.0152(7) 0.0029(4) S(1) 0.045(2) 0.0348(9) 0.037(1) 0.0015(8) 0.017(1) 0.0016(7) S(2) 0.050(2) 0.0356(10) 0.039(2) -0.0013(8) 0.021(1) 0.0005(7) S(3) 0.053(2) 0.0354(9) 0.037(2) 0.0010(8) 0.024(1) 0.0014(7) S(4) 0.051(2) 0.0345(9) 0.041(1) -0.0012(8) 0.022(1) 0.0025(7) S(5) 0.056(2) 0.0364(10) 0.049(2) 0.0013(9) 0.021(1) -0.0063(8) S(6) 0.050(2) 0.0327(10) 0.059(2) 0.0002(8) 0.021(1) 0.0052(8) S(7) 0.053(2) 0.0356(10) 0.045(2) -0.0035(8) 0.023(1) 0.0044(8) S(8) 0.051(2) 0.0382(10) 0.034(1) -0.0022(8) 0.016(1) -0.0021(7) S(9) 0.062(3) 0.036(1) 0.099(2) -0.0044(10) 0.032(2) -0.016(1) S(10) 0.081(3) 0.041(1) 0.059(2) -0.017(1) 0.020(2) -0.0095(10) S(11) 0.061(2) 0.040(1) 0.035(2) 0.0095(9) 0.021(1) 0.0032(8) S(12) 0.059(2) 0.039(1) 0.041(2) 0.0018(9) 0.019(1) 0.0012(8) S(13) 0.063(2) 0.0357(10) 0.038(2) 0.0073(9) 0.018(1) 0.0015(8) S(14) 0.057(2) 0.038(1) 0.038(2) 0.0011(9) 0.018(1) -0.0005(8) S(15) 0.059(2) 0.037(1) 0.045(2) 0.0034(9) 0.016(1) 0.0002(8) S(16) 0.063(3) 0.044(1) 0.039(2) 0.0029(10) 0.019(2) 0.0093(8) S(17) 0.052(2) 0.040(1) 0.042(2) 0.0075(9) 0.018(1) 0.0064(8) S(18) 0.060(2) 0.0353(10) 0.049(2) 0.0021(9) 0.023(1) -0.0020(8) S(19) 0.082(3) 0.036(1) 0.071(2) 0.000(1) 0.018(2) 0.0111(10) S(20) 0.075(3) 0.035(1) 0.080(2) 0.0060(10) 0.032(2) 0.0106(10) C(1) 0.038(8) 0.031(4) 0.037(6) 0.004(3) 0.007(5) 0.001(3) C(2) 0.049(9) 0.032(4) 0.041(6) 0.005(3) 0.018(5) 0.007(3) C(3) 0.036(8) 0.030(4) 0.046(6) 0.003(3) 0.016(5) 0.004(3) C(4) 0.039(8) 0.031(4) 0.033(6) 0.003(3) 0.014(5) 0.003(3) C(5) 0.035(8) 0.033(4) 0.060(7) 0.003(3) 0.013(6) -0.007(3) C(6) 0.043(8) 0.031(4) 0.050(6) 0.000(3) 0.009(5) 0.002(3) C(7) 0.033(8) 0.038(4) 0.048(7) 0.000(3) 0.013(5) 0.005(3) C(8) 0.036(8) 0.040(4) 0.030(6) 0.000(3) 0.008(5) 0.002(3) C(9) 0.045(9) 0.035(4) 0.043(7) 0.002(3) 0.016(5) 0.002(3) C(10) 0.044(9) 0.037(4) 0.043(7) 0.006(3) 0.008(5) 0.009(3) C(11) 0.031(8) 0.041(4) 0.051(6) 0.000(3) 0.010(5) 0.004(3) C(12) 0.036(9) 0.042(4) 0.049(6) 0.005(3) 0.016(5) 0.010(3) C(13) 0.07(1) 0.056(5) 0.069(8) -0.012(5) 0.029(8) 0.010(4) C(14) 0.06(1) 0.035(4) 0.070(7) 0.002(4) 0.025(7) 0.000(4) C(15) 0.10(1) 0.054(6) 0.059(8) -0.003(5) 0.031(8) 0.006(4) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Te(1) C(13) 2.07(1) . . yes Te(1) C(14) 2.108(8) . . yes Te(1) C(15) 2.16(1) . . yes Ni(1) S(1) 2.166(2) . . yes Ni(1) S(2) 2.132(2) . . yes Ni(1) S(3) 2.133(2) . . yes Ni(1) S(4) 2.155(2) . . yes Ni(2) S(11) 2.169(2) . . yes Ni(2) S(12) 2.171(2) . . yes Ni(2) S(13) 2.164(2) . . yes Ni(2) S(14) 2.178(2) . . yes S(1) C(1) 1.683(7) . . yes S(2) C(2) 1.708(8) . . yes S(3) C(3) 1.683(8) . . yes S(4) C(4) 1.668(7) . . yes S(5) C(1) 1.742(8) . . yes S(5) C(5) 1.726(9) . . yes S(6) C(2) 1.721(7) . . yes S(6) C(5) 1.706(9) . . yes S(7) C(3) 1.718(7) . . yes S(7) C(6) 1.721(9) . . yes S(8) C(4) 1.745(7) . . yes S(8) C(6) 1.712(8) . . yes S(9) C(5) 1.644(7) . . yes S(10) C(6) 1.635(7) . . yes S(11) C(9) 1.738(8) . . yes S(12) C(10) 1.722(8) . . yes S(13) C(7) 1.705(8) . . yes S(14) C(8) 1.708(8) . . yes S(15) C(9) 1.746(7) . . yes S(15) C(12) 1.706(9) . . yes S(16) C(10) 1.757(8) . . yes S(16) C(12) 1.739(9) . . yes S(17) C(7) 1.751(8) . . yes S(17) C(11) 1.720(8) . . yes S(18) C(8) 1.763(7) . . yes S(18) C(11) 1.730(9) . . yes S(19) C(12) 1.679(7) . . yes S(20) C(11) 1.674(8) . . yes C(1) C(2) 1.36(1) . . yes C(3) C(4) 1.37(1) . . yes C(7) C(8) 1.37(1) . . yes C(9) C(10) 1.36(1) . . 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 C(13) Te(1) C(14) 96.0(4) . . . yes C(13) Te(1) C(15) 94.6(5) . . . yes C(14) Te(1) C(15) 93.0(4) . . . yes S(1) Ni(1) S(2) 93.54(8) . . . yes S(1) Ni(1) S(3) 87.71(8) . . . yes S(1) Ni(1) S(4) 177.4(1) . . . yes S(2) Ni(1) S(3) 178.5(1) . . . yes S(2) Ni(1) S(4) 86.04(8) . . . yes S(3) Ni(1) S(4) 92.75(8) . . . yes S(11) Ni(2) S(12) 92.52(8) . . . yes S(11) Ni(2) S(13) 86.87(8) . . . yes S(11) Ni(2) S(14) 178.9(1) . . . yes S(12) Ni(2) S(13) 178.8(1) . . . yes S(12) Ni(2) S(14) 88.36(8) . . . yes S(13) Ni(2) S(14) 92.27(8) . . . yes Ni(1) S(1) C(1) 101.8(3) . . . yes Ni(1) S(2) C(2) 101.6(3) . . . yes Ni(1) S(3) C(3) 102.5(3) . . . yes Ni(1) S(4) C(4) 102.4(3) . . . yes C(1) S(5) C(5) 96.5(4) . . . yes C(2) S(6) C(5) 98.0(4) . . . yes C(3) S(7) C(6) 97.6(4) . . . yes C(4) S(8) C(6) 96.0(4) . . . yes Ni(2) S(11) C(9) 102.6(3) . . . yes Ni(2) S(12) C(10) 102.9(3) . . . yes Ni(2) S(13) C(7) 103.2(3) . . . yes Ni(2) S(14) C(8) 102.6(3) . . . yes C(9) S(15) C(12) 97.5(4) . . . yes C(10) S(16) C(12) 97.5(4) . . . yes C(7) S(17) C(11) 98.0(4) . . . yes C(8) S(18) C(11) 97.6(4) . . . yes S(1) C(1) S(5) 122.5(5) . . . yes S(1) C(1) C(2) 121.2(5) . . . yes S(5) C(1) C(2) 116.3(5) . . . yes S(2) C(2) S(6) 122.7(5) . . . yes S(2) C(2) C(1) 121.8(5) . . . yes S(6) C(2) C(1) 115.5(6) . . . yes S(3) C(3) S(7) 123.8(5) . . . yes S(3) C(3) C(4) 121.1(5) . . . yes S(7) C(3) C(4) 115.0(5) . . . yes S(4) C(4) S(8) 121.9(5) . . . yes S(4) C(4) C(3) 121.2(5) . . . yes S(8) C(4) C(3) 116.9(5) . . . yes S(5) C(5) S(6) 113.7(4) . . . yes S(5) C(5) S(9) 120.7(6) . . . yes S(6) C(5) S(9) 125.6(6) . . . yes S(7) C(6) S(8) 114.4(4) . . . yes S(7) C(6) S(10) 124.5(5) . . . yes S(8) C(6) S(10) 121.1(6) . . . yes S(13) C(7) S(17) 123.4(6) . . . yes S(13) C(7) C(8) 120.9(6) . . . yes S(17) C(7) C(8) 115.8(6) . . . yes S(14) C(8) S(18) 123.6(5) . . . yes S(14) C(8) C(7) 121.2(6) . . . yes S(18) C(8) C(7) 115.2(5) . . . yes S(11) C(9) S(15) 122.2(6) . . . yes S(11) C(9) C(10) 120.8(6) . . . yes S(15) C(9) C(10) 117.0(6) . . . yes S(12) C(10) S(16) 124.3(6) . . . yes S(12) C(10) C(9) 121.1(6) . . . yes S(16) C(10) C(9) 114.6(6) . . . yes S(17) C(11) S(18) 113.5(4) . . . yes S(17) C(11) S(20) 122.5(6) . . . yes S(18) C(11) S(20) 124.0(5) . . . yes S(15) C(12) S(16) 113.4(4) . . . yes S(15) C(12) S(19) 124.0(5) . . . yes S(16) C(12) S(19) 122.6(5) . . . yes #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) S(5) 179.3(5) . . . . yes Ni(1) S(1) C(1) C(2) 0.8(9) . . . . yes Ni(1) S(2) C(2) S(6) 180.0(6) . . . . yes Ni(1) S(2) C(2) C(1) -0.4(10) . . . . yes Ni(1) S(3) C(3) S(7) -179.0(6) . . . . yes Ni(1) S(3) C(3) C(4) -1.8(9) . . . . yes Ni(1) S(4) C(4) S(8) -179.6(5) . . . . yes Ni(1) S(4) C(4) C(3) -1.4(9) . . . . yes Ni(2) S(11) C(9) S(15) -178.5(6) . . . . yes Ni(2) S(11) C(9) C(10) 1(1) . . . . yes Ni(2) S(12) C(10) S(16) -178.4(6) . . . . yes Ni(2) S(12) C(10) C(9) 1(1) . . . . yes Ni(2) S(13) C(7) S(17) -179.8(6) . . . . yes Ni(2) S(13) C(7) C(8) -0.2(10) . . . . yes Ni(2) S(14) C(8) S(18) -179.3(6) . . . . yes Ni(2) S(14) C(8) C(7) -0.8(10) . . . . yes S(1) Ni(1) S(2) C(2) 0.7(4) . . . . yes S(1) Ni(1) S(3) C(3) 178.1(4) . . . . yes S(1) Ni(1) S(4) C(4) -99(1) . . . . yes S(1) C(1) S(5) C(5) -179.2(7) . . . . yes S(1) C(1) C(2) S(2) 0(1) . . . . yes S(1) C(1) C(2) S(6) 179.4(6) . . . . yes S(2) Ni(1) S(1) C(1) -0.8(4) . . . . yes S(2) Ni(1) S(3) C(3) -35(4) . . . . yes S(2) Ni(1) S(4) C(4) 179.3(4) . . . . yes S(2) C(2) S(6) C(5) 179.1(7) . . . . yes S(2) C(2) C(1) S(5) -178.9(6) . . . . yes S(3) Ni(1) S(1) C(1) 178.4(4) . . . . yes S(3) Ni(1) S(2) C(2) -146(4) . . . . yes S(3) Ni(1) S(4) C(4) 0.2(4) . . . . yes S(3) C(3) S(7) C(6) 179.9(7) . . . . yes S(3) C(3) C(4) S(4) 2(1) . . . . yes S(3) C(3) C(4) S(8) -179.4(5) . . . . yes S(4) Ni(1) S(1) C(1) -81(2) . . . . yes S(4) Ni(1) S(2) C(2) 178.1(4) . . . . yes S(4) Ni(1) S(3) C(3) 0.7(4) . . . . yes S(4) C(4) S(8) C(6) 178.6(7) . . . . yes S(4) C(4) C(3) S(7) 179.7(5) . . . . yes S(5) C(1) C(2) S(6) 0(1) . . . . yes S(5) C(5) S(6) C(2) 0.1(7) . . . . yes S(6) C(5) S(5) C(1) 0.3(7) . . . . yes S(7) C(3) C(4) S(8) -1(1) . . . . yes S(7) C(6) S(8) C(4) 1.4(7) . . . . yes S(8) C(6) S(7) C(3) -2.3(7) . . . . yes S(9) C(5) S(5) C(1) -179.5(7) . . . . yes S(9) C(5) S(6) C(2) 179.8(7) . . . . yes S(10) C(6) S(7) C(3) 178.0(7) . . . . yes S(10) C(6) S(8) C(4) -178.9(7) . . . . yes S(11) Ni(2) S(12) C(10) -0.1(4) . . . . yes S(11) Ni(2) S(13) C(7) -179.5(4) . . . . yes S(11) Ni(2) S(14) C(8) 38(5) . . . . yes S(11) C(9) S(15) C(12) -178.7(7) . . . . yes S(11) C(9) C(10) S(12) -1(1) . . . . yes S(11) C(9) C(10) S(16) 177.7(6) . . . . yes S(12) Ni(2) S(11) C(9) -0.6(4) . . . . yes S(12) Ni(2) S(13) C(7) 120(4) . . . . yes S(12) Ni(2) S(14) C(8) -178.4(4) . . . . yes S(12) C(10) S(16) C(12) -178.5(7) . . . . yes S(12) C(10) C(9) S(15) 178.2(6) . . . . yes S(13) Ni(2) S(11) C(9) -179.5(4) . . . . yes S(13) Ni(2) S(12) C(10) 60(4) . . . . yes S(13) Ni(2) S(14) C(8) 0.5(4) . . . . yes S(13) C(7) S(17) C(11) 179.5(7) . . . . yes S(13) C(7) C(8) S(14) 0(1) . . . . yes S(13) C(7) C(8) S(18) 179.3(6) . . . . yes S(14) Ni(2) S(11) C(9) 142(5) . . . . yes S(14) Ni(2) S(12) C(10) -179.5(4) . . . . yes S(14) Ni(2) S(13) C(7) -0.2(4) . . . . yes S(14) C(8) S(18) C(11) -179.8(7) . . . . yes S(14) C(8) C(7) S(17) -179.6(6) . . . . yes S(15) C(9) C(10) S(16) -2(1) . . . . yes S(15) C(12) S(16) C(10) -1.1(7) . . . . yes S(16) C(12) S(15) C(9) 0.1(7) . . . . yes S(17) C(7) C(8) S(18) -1(1) . . . . yes S(17) C(11) S(18) C(8) -1.7(7) . . . . yes S(18) C(11) S(17) C(7) 1.2(7) . . . . yes S(19) C(12) S(15) C(9) -179.6(8) . . . . yes S(19) C(12) S(16) C(10) 178.7(7) . . . . yes S(20) C(11) S(17) C(7) 178.9(7) . . . . yes S(20) C(11) S(18) C(8) -179.3(7) . . . . yes C(1) C(2) S(6) C(5) -0.5(9) . . . . yes C(2) C(1) S(5) C(5) -0.7(9) . . . . yes C(3) C(4) S(8) C(6) 0.3(9) . . . . yes C(4) C(3) S(7) C(6) 2.5(9) . . . . yes C(7) C(8) S(18) C(11) 1.7(9) . . . . yes C(8) C(7) S(17) C(11) -0.1(9) . . . . yes C(9) C(10) S(16) C(12) 2.0(10) . . . . yes C(10) C(9) S(15) C(12) 1(1) . . . . yes C(10) C(9) S(15) C(12) 1(1) . . . . 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 S(1) S(4) 3.555(3) . 1_556 ? S(1) S(2) 3.572(3) . 1_556 ? S(2) S(8) 3.470(4) . 2_666 ? S(3) S(4) 3.584(3) . 1_556 ? S(4) S(4) 3.447(5) . 2_666 ? S(10) C(15) 3.54(1) . . ? S(10) C(14) 3.562(10) . 1_554 ? S(11) S(12) 3.559(3) . 1_556 ? S(12) S(13) 3.515(3) . 1_554 ? S(13) S(14) 3.572(3) . 1_556 ? S(14) S(17) 3.583(3) . 1_554 ? S(15) C(13) 3.59(1) . 1_655 ? S(17) C(10) 3.56(1) . 2_556 ? C(9) C(11) 3.60(2) . 2_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_Me3Te[Ni(dmit)2]3acetone _database_code_CSD 184207 _audit_creation_date 'Thu Jul 11 11:58:30 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H15 O Ni3 S30 Te ' _chemical_formula_moiety '?' _chemical_formula_weight 1584.88 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 38.01(2) _cell_length_b 11.955(2) _cell_length_c 11.173(2) _cell_angle_alpha 90 _cell_angle_beta 90.2(1) _cell_angle_gamma 90 _cell_volume 5077(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.025 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.926 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.929 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 7192 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 28.27 _diffrn_measured_fraction_theta_max 0.5449 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.5449 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6854 _reflns_number_gt 3163 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0490 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3163 _refine_ls_number_parameters 415 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]' _refine_ls_shift/su_max 0.0128 _refine_diff_density_max 1.15 _refine_diff_density_min -0.56 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Te(1) Te 0.25000(2) 0.10737(6) 0.15001(9) 0.0501(3) Uani 1.00 d . . . Ni(1) Ni 0.0000 0.0000 0.0000 0.0353(8) Uani 1.00 d S . . Ni(2) Ni -0.02675(3) 0.30779(9) -0.0003(1) 0.0317(5) Uani 1.00 d . . . Ni(3) Ni 0.02675(3) 0.19218(9) 0.5000(1) 0.0316(5) Uani 1.00 d . . . Ni(4) Ni 0.0000 0.5000 0.5000 0.0343(7) Uani 1.00 d S . . S(1) S 0.03524(6) 0.0770(2) 0.1297(3) 0.040(1) Uani 1.00 d . . . S(2) S 0.04102(6) -0.0158(2) -0.1342(3) 0.039(1) Uani 1.00 d . . . S(3) S 0.11210(7) 0.1464(2) 0.1087(3) 0.044(1) Uani 1.00 d . . . S(4) S 0.11775(6) 0.0549(2) -0.1321(3) 0.043(1) Uani 1.00 d . . . S(5) S 0.17932(7) 0.1725(3) -0.0290(4) 0.066(1) Uani 1.00 d . . . S(6) S 0.00678(6) 0.3888(2) 0.1293(3) 0.0374(10) Uani 1.00 d . . . S(7) S 0.01497(6) 0.2938(2) -0.1299(3) 0.038(1) Uani 1.00 d . . . S(8) S -0.06845(6) 0.3204(2) 0.1308(3) 0.039(1) Uani 1.00 d . . . S(9) S -0.06052(6) 0.2312(2) -0.1332(3) 0.039(1) Uani 1.00 d . . . S(10) S 0.08353(6) 0.4556(2) 0.1202(3) 0.043(1) Uani 1.00 d . . . S(11) S 0.09133(6) 0.3650(2) -0.1221(3) 0.040(1) Uani 1.00 d . . . S(12) S -0.14502(6) 0.2491(2) 0.1205(3) 0.046(1) Uani 1.00 d . . . S(13) S -0.13761(7) 0.1667(2) -0.1243(3) 0.047(1) Uani 1.00 d . . . S(14) S 0.15304(7) 0.4690(3) -0.0020(4) 0.063(1) Uani 1.00 d . . . S(15) S -0.20665(7) 0.1465(3) -0.0022(4) 0.074(1) Uani 1.00 d . . . S(16) S 0.06846(6) 0.1797(2) 0.6307(3) 0.039(1) Uani 1.00 d . . . S(17) S 0.06063(6) 0.2691(2) 0.3669(3) 0.038(1) Uani 1.00 d . . . S(18) S -0.00685(6) 0.1107(2) 0.6294(3) 0.0376(10) Uani 1.00 d . . . S(19) S -0.01504(6) 0.2063(2) 0.3698(3) 0.038(1) Uani 1.00 d . . . S(20) S 0.14494(6) 0.2513(2) 0.6210(3) 0.046(1) Uani 1.00 d . . . S(21) S 0.13759(6) 0.3330(2) 0.3758(3) 0.048(1) Uani 1.00 d . . . S(22) S -0.08367(6) 0.0448(2) 0.6199(3) 0.044(1) Uani 1.00 d . . . S(23) S -0.09136(6) 0.1350(2) 0.3776(3) 0.040(1) Uani 1.00 d . . . S(24) S 0.20657(7) 0.3535(3) 0.4980(4) 0.074(2) Uani 1.00 d . . . S(25) S -0.15301(7) 0.0313(3) 0.4979(4) 0.064(1) Uani 1.00 d . . . S(26) S 0.04105(6) 0.4839(2) 0.6338(3) 0.040(1) Uani 1.00 d . . . S(27) S 0.03525(6) 0.5767(2) 0.3706(3) 0.040(1) Uani 1.00 d . . . S(28) S 0.11765(6) 0.5551(2) 0.6321(3) 0.044(1) Uani 1.00 d . . . S(29) S 0.11207(7) 0.6460(2) 0.3915(3) 0.044(1) Uani 1.00 d . . . S(30) S 0.17938(7) 0.6727(3) 0.5294(4) 0.064(1) Uani 1.00 d . . . O(1) O 0.2501(4) -0.0048(10) 0.517(2) 0.142(8) Uani 1.00 d . . . C(1) C 0.0743(2) 0.0828(7) 0.049(1) 0.032(2) Uiso 1.00 d . . . C(2) C 0.0766(2) 0.0430(8) -0.062(1) 0.035(2) Uiso 1.00 d . . . C(3) C 0.1387(2) 0.1260(8) -0.015(1) 0.044(3) Uiso 1.00 d . . . C(4) C 0.0462(2) 0.3962(7) 0.059(1) 0.034(2) Uiso 1.00 d . . . C(5) C 0.0499(2) 0.3523(7) -0.058(1) 0.031(2) Uiso 1.00 d . . . C(6) C -0.1033(2) 0.2640(8) 0.057(1) 0.036(2) Uiso 1.00 d . . . C(7) C -0.0998(2) 0.2241(7) -0.057(1) 0.036(3) Uiso 1.00 d . . . C(8) C 0.1114(2) 0.4316(7) -0.001(1) 0.036(3) Uiso 1.00 d . . . C(9) C -0.1653(2) 0.1849(8) 0.000(1) 0.042(3) Uiso 1.00 d . . . C(10) C 0.1034(2) 0.2367(8) 0.556(1) 0.037(3) Uiso 1.00 d . . . C(11) C 0.0997(2) 0.2755(7) 0.440(1) 0.036(2) Uiso 1.00 d . . . C(12) C -0.0460(2) 0.1051(8) 0.557(1) 0.037(2) Uiso 1.00 d . . . C(13) C -0.0497(2) 0.1477(7) 0.442(1) 0.031(2) Uiso 1.00 d . . . C(14) C 0.1653(2) 0.3138(8) 0.497(1) 0.044(3) Uiso 1.00 d . . . C(15) C -0.1116(2) 0.0690(7) 0.499(1) 0.039(3) Uiso 1.00 d . . . C(16) C 0.0761(2) 0.5439(8) 0.562(1) 0.037(2) Uiso 1.00 d . . . C(17) C 0.0744(2) 0.5837(7) 0.451(1) 0.034(2) Uiso 1.00 d . . . C(18) C 0.1385(2) 0.6252(8) 0.518(1) 0.044(3) Uiso 1.00 d . . . C(19) C 0.2083(3) 0.072(1) 0.270(2) 0.083(4) Uiso 1.00 d . . . C(20) C 0.2497(4) 0.279(1) 0.173(2) 0.096(5) Uiso 1.00 d . . . C(21) C 0.2916(3) 0.073(1) 0.271(2) 0.080(4) Uiso 1.00 d . . . C(22) C 0.2497(4) -0.016(1) 0.622(2) 0.089(5) Uiso 1.00 d . . . C(23) C 0.2499(6) -0.120(2) 0.675(2) 0.159(7) Uiso 1.00 d . . . C(24) C 0.2497(7) 0.077(2) 0.707(3) 0.206(10) Uiso 1.00 d . . . H(1) H 0.2043 -0.0043 0.2734 0.0910 Uiso 1.00 calc . . . H(2) H 0.1882 0.1124 0.2470 0.0910 Uiso 1.00 calc . . . H(3) H 0.2155 0.0983 0.3495 0.0910 Uiso 1.00 calc . . . H(4) H 0.2330 0.3115 0.1222 0.1115 Uiso 1.00 calc . . . H(5) H 0.2457 0.2965 0.2533 0.1115 Uiso 1.00 calc . . . H(6) H 0.2729 0.3072 0.1507 0.1115 Uiso 1.00 calc . . . H(7) H 0.2857 0.0989 0.3458 0.0884 Uiso 1.00 calc . . . H(8) H 0.3122 0.1120 0.2414 0.0884 Uiso 1.00 calc . . . H(9) H 0.2961 -0.0043 0.2695 0.0884 Uiso 1.00 calc . . . H(10) H 0.2704 -0.1627 0.6539 0.1705 Uiso 1.00 calc . . . H(11) H 0.2495 -0.1246 0.7657 0.1705 Uiso 1.00 calc . . . H(12) H 0.2296 -0.1657 0.6525 0.1705 Uiso 1.00 calc . . . H(13) H 0.2490 0.0504 0.7984 0.2836 Uiso 1.00 calc . . . H(14) H 0.2699 0.1229 0.7080 0.2836 Uiso 1.00 calc . . . H(15) H 0.2291 0.1250 0.7068 0.2836 Uiso 1.00 calc . . . 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 Te(1) 0.0485(4) 0.0592(5) 0.0425(9) 0.0002(4) -0.0020(3) 0.0011(5) Ni(1) 0.040(1) 0.042(1) 0.024(2) -0.0009(7) -0.0030(9) 0.000(1) Ni(2) 0.0321(7) 0.0392(7) 0.024(1) -0.0002(5) -0.0008(5) -0.0002(7) Ni(3) 0.0316(7) 0.0384(7) 0.025(1) 0.0000(5) -0.0028(5) 0.0003(7) Ni(4) 0.041(1) 0.040(1) 0.023(2) -0.0012(7) -0.0014(9) 0.0012(10) S(1) 0.044(2) 0.049(2) 0.027(3) -0.005(1) 0.000(1) -0.006(1) S(2) 0.040(2) 0.052(2) 0.026(3) 0.000(1) -0.001(1) -0.006(1) S(3) 0.043(2) 0.052(2) 0.039(4) -0.004(1) -0.009(1) -0.001(2) S(4) 0.042(2) 0.052(2) 0.034(4) 0.003(1) -0.001(1) 0.000(2) S(5) 0.041(2) 0.088(2) 0.069(4) -0.006(1) -0.009(2) 0.009(2) S(6) 0.038(1) 0.051(2) 0.023(3) -0.002(1) 0.000(1) -0.006(2) S(7) 0.033(1) 0.050(2) 0.030(3) -0.0029(10) 0.000(1) -0.006(1) S(8) 0.036(2) 0.053(2) 0.028(3) -0.003(1) 0.002(1) -0.004(2) S(9) 0.036(2) 0.051(2) 0.029(3) -0.004(1) 0.001(1) -0.004(1) S(10) 0.040(2) 0.048(2) 0.041(4) -0.006(1) -0.009(1) -0.001(2) S(11) 0.035(1) 0.053(2) 0.033(3) -0.002(1) 0.003(1) 0.001(1) S(12) 0.035(2) 0.057(2) 0.047(4) -0.002(1) 0.004(1) -0.003(2) S(13) 0.040(2) 0.060(2) 0.041(4) -0.010(1) -0.006(1) -0.006(2) S(14) 0.039(2) 0.077(2) 0.073(4) -0.014(1) -0.009(2) -0.001(2) S(15) 0.036(2) 0.111(3) 0.073(5) -0.017(1) -0.001(2) -0.008(2) S(16) 0.036(1) 0.052(2) 0.030(3) -0.001(1) -0.004(1) 0.007(2) S(17) 0.039(2) 0.052(2) 0.023(3) -0.004(1) -0.005(1) 0.005(1) S(18) 0.038(1) 0.050(2) 0.025(3) -0.002(1) -0.003(1) 0.006(2) S(19) 0.034(1) 0.053(2) 0.027(3) -0.002(1) -0.002(1) 0.007(1) S(20) 0.035(2) 0.062(2) 0.039(3) -0.003(1) -0.008(1) 0.004(2) S(21) 0.036(2) 0.061(2) 0.045(4) -0.010(1) 0.003(1) 0.006(2) S(22) 0.040(2) 0.053(2) 0.038(3) -0.007(1) 0.004(1) 0.004(2) S(23) 0.036(1) 0.053(2) 0.032(3) -0.001(1) -0.007(1) 0.000(1) S(24) 0.035(2) 0.111(3) 0.077(5) -0.017(1) -0.004(2) 0.010(2) S(25) 0.037(2) 0.085(2) 0.069(4) -0.011(1) 0.000(1) 0.005(2) S(26) 0.042(2) 0.049(2) 0.027(3) 0.000(1) -0.003(1) 0.006(2) S(27) 0.045(2) 0.049(2) 0.027(3) -0.005(1) -0.003(1) 0.006(1) S(28) 0.040(2) 0.055(2) 0.036(4) 0.003(1) -0.002(1) 0.000(2) S(29) 0.046(2) 0.052(2) 0.034(4) -0.004(1) 0.004(1) 0.003(2) S(30) 0.042(2) 0.090(2) 0.059(4) -0.009(1) 0.005(1) -0.010(2) O(1) 0.18(1) 0.14(1) 0.11(2) 0.003(8) 0.00(1) 0.04(1) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Te(1) C(19) 2.13(2) . . yes Te(1) C(20) 2.07(1) . . yes Te(1) C(21) 2.11(2) . . yes Ni(1) S(1) 2.175(3) . . yes Ni(1) S(1) 2.175(3) . 3_555 yes Ni(1) S(2) 2.175(3) . . yes Ni(1) S(2) 2.175(3) . 3_555 yes Ni(2) S(6) 2.155(3) . . yes Ni(2) S(7) 2.158(3) . . yes Ni(2) S(8) 2.168(3) . . yes Ni(2) S(9) 2.164(3) . . yes Ni(3) S(16) 2.157(3) . . yes Ni(3) S(17) 2.175(3) . . yes Ni(3) S(18) 2.164(3) . . yes Ni(3) S(19) 2.157(3) . . yes Ni(4) S(26) 2.166(3) . . yes Ni(4) S(26) 2.166(3) . 3_566 yes Ni(4) S(27) 2.178(3) . . yes Ni(4) S(27) 2.178(3) . 3_566 yes S(1) C(1) 1.74(1) . . yes S(2) C(2) 1.72(1) . . yes S(3) C(1) 1.757(10) . . yes S(3) C(3) 1.74(1) . . yes S(4) C(2) 1.757(10) . . yes S(4) C(3) 1.75(1) . . yes S(5) C(3) 1.650(10) . . yes S(6) C(4) 1.696(9) . . yes S(7) C(5) 1.703(10) . . yes S(8) C(6) 1.70(1) . . yes S(9) C(7) 1.72(1) . . yes S(10) C(4) 1.727(10) . . yes S(10) C(8) 1.75(1) . . yes S(11) C(5) 1.740(9) . . yes S(11) C(8) 1.74(1) . . yes S(12) C(6) 1.747(10) . . yes S(12) C(9) 1.73(1) . . yes S(13) C(7) 1.76(1) . . yes S(13) C(9) 1.76(1) . . yes S(14) C(8) 1.643(9) . . yes S(15) C(9) 1.639(10) . . yes S(16) C(10) 1.71(1) . . yes S(17) C(11) 1.69(1) . . yes S(18) C(12) 1.693(10) . . yes S(19) C(13) 1.696(10) . . yes S(20) C(10) 1.74(1) . . yes S(20) C(14) 1.75(1) . . yes S(21) C(11) 1.75(1) . . yes S(21) C(14) 1.73(1) . . yes S(22) C(12) 1.755(10) . . yes S(22) C(15) 1.74(1) . . yes S(23) C(13) 1.743(10) . . yes S(23) C(15) 1.75(1) . . yes S(24) C(14) 1.640(10) . . yes S(25) C(15) 1.636(9) . . yes S(26) C(16) 1.72(1) . . yes S(27) C(17) 1.74(1) . . yes S(28) C(16) 1.76(1) . . yes S(28) C(18) 1.72(1) . . yes S(29) C(17) 1.750(10) . . yes S(29) C(18) 1.75(1) . . yes S(30) C(18) 1.658(10) . . yes O(1) C(22) 1.18(2) . . yes C(1) C(2) 1.33(2) . . yes C(4) C(5) 1.41(2) . . yes C(6) C(7) 1.38(2) . . yes C(10) C(11) 1.39(2) . . yes C(12) C(13) 1.39(2) . . yes C(16) C(17) 1.33(2) . . yes C(22) C(23) 1.37(2) . . yes C(22) C(24) 1.47(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 C(19) Te(1) C(20) 96.5(6) . . . yes C(19) Te(1) C(21) 96.7(6) . . . yes C(20) Te(1) C(21) 96.7(6) . . . yes S(1) Ni(1) S(1) 180.0 . . 3_555 yes S(1) Ni(1) S(2) 93.1(1) . . . yes S(1) Ni(1) S(2) 86.9(1) . . 3_555 yes S(1) Ni(1) S(2) 86.9(1) 3_555 . . yes S(1) Ni(1) S(2) 93.1(1) 3_555 . 3_555 yes S(2) Ni(1) S(2) 180.0 . . 3_555 yes S(6) Ni(2) S(7) 92.9(1) . . . yes S(6) Ni(2) S(8) 87.0(1) . . . yes S(6) Ni(2) S(9) 178.3(1) . . . yes S(7) Ni(2) S(8) 179.4(1) . . . yes S(7) Ni(2) S(9) 86.7(1) . . . yes S(8) Ni(2) S(9) 93.4(1) . . . yes S(16) Ni(3) S(17) 93.2(1) . . . yes S(16) Ni(3) S(18) 87.2(1) . . . yes S(16) Ni(3) S(19) 179.4(1) . . . yes S(17) Ni(3) S(18) 178.2(1) . . . yes S(17) Ni(3) S(19) 86.7(1) . . . yes S(18) Ni(3) S(19) 92.9(1) . . . yes S(26) Ni(4) S(26) 180.0 . . 3_566 yes S(26) Ni(4) S(27) 93.0(1) . . . yes S(26) Ni(4) S(27) 87.0(1) . . 3_566 yes S(26) Ni(4) S(27) 87.0(1) 3_566 . . yes S(26) Ni(4) S(27) 93.0(1) 3_566 . 3_566 yes S(27) Ni(4) S(27) 180.0 . . 3_566 yes Ni(1) S(1) C(1) 101.2(4) . . . yes Ni(1) S(2) C(2) 101.9(4) . . . yes C(1) S(3) C(3) 96.5(6) . . . yes C(2) S(4) C(3) 96.3(5) . . . yes Ni(2) S(6) C(4) 103.5(4) . . . yes Ni(2) S(7) C(5) 103.0(4) . . . yes Ni(2) S(8) C(6) 102.6(4) . . . yes Ni(2) S(9) C(7) 101.4(4) . . . yes C(4) S(10) C(8) 97.2(5) . . . yes C(5) S(11) C(8) 96.5(5) . . . yes C(6) S(12) C(9) 97.6(6) . . . yes C(7) S(13) C(9) 96.1(6) . . . yes Ni(3) S(16) C(10) 102.3(4) . . . yes Ni(3) S(17) C(11) 102.3(4) . . . yes Ni(3) S(18) C(12) 102.5(4) . . . yes Ni(3) S(19) C(13) 102.7(4) . . . yes C(10) S(20) C(14) 96.7(6) . . . yes C(11) S(21) C(14) 97.3(6) . . . yes C(12) S(22) C(15) 96.8(5) . . . yes C(13) S(23) C(15) 97.1(5) . . . yes Ni(4) S(26) C(16) 101.5(4) . . . yes Ni(4) S(27) C(17) 101.7(4) . . . yes C(16) S(28) C(18) 97.0(6) . . . yes C(17) S(29) C(18) 95.7(6) . . . yes S(1) C(1) S(3) 121.1(7) . . . yes S(1) C(1) C(2) 122.0(7) . . . yes S(3) C(1) C(2) 116.9(7) . . . yes S(2) C(2) S(4) 121.5(7) . . . yes S(2) C(2) C(1) 121.8(7) . . . yes S(4) C(2) C(1) 116.7(7) . . . yes S(3) C(3) S(4) 113.6(5) . . . yes S(3) C(3) S(5) 125.1(8) . . . yes S(4) C(3) S(5) 121.3(8) . . . yes S(6) C(4) S(10) 124.3(7) . . . yes S(6) C(4) C(5) 120.0(7) . . . yes S(10) C(4) C(5) 115.7(7) . . . yes S(7) C(5) S(11) 123.0(7) . . . yes S(7) C(5) C(4) 120.6(7) . . . yes S(11) C(5) C(4) 116.3(7) . . . yes S(8) C(6) S(12) 123.6(8) . . . yes S(8) C(6) C(7) 120.8(7) . . . yes S(12) C(6) C(7) 115.6(7) . . . yes S(9) C(7) S(13) 121.3(8) . . . yes S(9) C(7) C(6) 121.9(7) . . . yes S(13) C(7) C(6) 116.8(7) . . . yes S(10) C(8) S(11) 114.2(5) . . . yes S(10) C(8) S(14) 123.1(8) . . . yes S(11) C(8) S(14) 122.6(7) . . . yes S(12) C(9) S(13) 113.9(5) . . . yes S(12) C(9) S(15) 124.1(8) . . . yes S(13) C(9) S(15) 122.1(8) . . . yes S(16) C(10) S(20) 122.9(8) . . . yes S(16) C(10) C(11) 120.9(7) . . . yes S(20) C(10) C(11) 116.2(7) . . . yes S(17) C(11) S(21) 123.1(8) . . . yes S(17) C(11) C(10) 121.2(7) . . . yes S(21) C(11) C(10) 115.7(7) . . . yes S(18) C(12) S(22) 122.7(7) . . . yes S(18) C(12) C(13) 121.0(7) . . . yes S(22) C(12) C(13) 116.3(7) . . . yes S(19) C(13) S(23) 123.2(7) . . . yes S(19) C(13) C(12) 120.9(7) . . . yes S(23) C(13) C(12) 115.9(7) . . . yes S(20) C(14) S(21) 114.0(5) . . . yes S(20) C(14) S(24) 122.9(8) . . . yes S(21) C(14) S(24) 123.1(8) . . . yes S(22) C(15) S(23) 114.0(5) . . . yes S(22) C(15) S(25) 123.2(8) . . . yes S(23) C(15) S(25) 122.8(8) . . . yes S(26) C(16) S(28) 121.2(8) . . . yes S(26) C(16) C(17) 123.3(8) . . . yes S(28) C(16) C(17) 115.4(7) . . . yes S(27) C(17) S(29) 121.5(7) . . . yes S(27) C(17) C(16) 120.4(7) . . . yes S(29) C(17) C(16) 118.0(8) . . . yes S(28) C(18) S(29) 113.7(5) . . . yes S(28) C(18) S(30) 123.2(8) . . . yes S(29) C(18) S(30) 123.1(7) . . . yes O(1) C(22) C(23) 122(2) . . . yes O(1) C(22) C(24) 123(2) . . . yes C(23) C(22) C(24) 113(2) . . . yes #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) S(3) 176.3(5) . . . . yes Ni(1) S(1) C(1) C(2) -1.4(10) . . . . yes Ni(1) S(1) C(1) S(3) -176.3(5) . 3_555 3_555 3_555 yes Ni(1) S(1) C(1) C(2) 1.4(10) . 3_555 3_555 3_555 yes Ni(1) S(2) C(2) S(4) -178.8(5) . . . . yes Ni(1) S(2) C(2) C(1) 0.4(10) . . . . yes Ni(1) S(2) C(2) S(4) 178.8(5) . 3_555 3_555 3_555 yes Ni(1) S(2) C(2) C(1) -0.4(10) . 3_555 3_555 3_555 yes Ni(2) S(6) C(4) S(10) 179.2(5) . . . . yes Ni(2) S(6) C(4) C(5) -0.6(9) . . . . yes Ni(2) S(7) C(5) S(11) -179.3(5) . . . . yes Ni(2) S(7) C(5) C(4) -0.9(9) . . . . yes Ni(2) S(8) C(6) S(12) 178.9(5) . . . . yes Ni(2) S(8) C(6) C(7) 0.4(9) . . . . yes Ni(2) S(9) C(7) S(13) -179.6(5) . . . . yes Ni(2) S(9) C(7) C(6) 1.1(9) . . . . yes Ni(3) S(16) C(10) S(20) 178.8(5) . . . . yes Ni(3) S(16) C(10) C(11) -0.5(9) . . . . yes Ni(3) S(17) C(11) S(21) -178.9(5) . . . . yes Ni(3) S(17) C(11) C(10) -0.4(9) . . . . yes Ni(3) S(18) C(12) S(22) 179.3(5) . . . . yes Ni(3) S(18) C(12) C(13) 0.1(9) . . . . yes Ni(3) S(19) C(13) S(23) -179.5(5) . . . . yes Ni(3) S(19) C(13) C(12) -0.4(9) . . . . yes Ni(4) S(26) C(16) S(28) 179.3(5) . . . . yes Ni(4) S(26) C(16) C(17) -1(1) . . . . yes Ni(4) S(26) C(16) S(28) -179.3(5) . 3_566 3_566 3_566 yes Ni(4) S(26) C(16) C(17) 1(1) . 3_566 3_566 3_566 yes Ni(4) S(27) C(17) S(29) -176.8(5) . . . . yes Ni(4) S(27) C(17) C(16) 1.5(10) . . . . yes Ni(4) S(27) C(17) S(29) 176.8(5) . 3_566 3_566 3_566 yes Ni(4) S(27) C(17) C(16) -1.5(10) . 3_566 3_566 3_566 yes S(1) Ni(1) S(2) C(2) -1.0(4) . . . . yes S(1) Ni(1) S(2) C(2) -179.0(4) . . 3_555 3_555 yes S(1) C(1) S(3) C(3) -178.4(6) . . . . yes S(1) C(1) C(2) S(2) 0(1) . . . . yes S(1) C(1) C(2) S(4) 180.0(5) . . . . yes S(2) Ni(1) S(1) C(1) 1.3(3) . . . . yes S(2) Ni(1) S(1) C(1) 178.7(3) . . 3_555 3_555 yes S(2) C(2) S(4) C(3) 176.7(6) . . . . yes S(2) C(2) C(1) S(3) -177.1(5) . . . . yes S(3) C(1) C(2) S(4) 2(1) . . . . yes S(3) C(3) S(4) C(2) 2.0(6) . . . . yes S(4) C(3) S(3) C(1) -1.2(7) . . . . yes S(5) C(3) S(3) C(1) 176.0(7) . . . . yes S(5) C(3) S(4) C(2) -175.3(7) . . . . yes S(6) Ni(2) S(7) C(5) 0.4(3) . . . . yes S(6) Ni(2) S(8) C(6) 178.5(4) . . . . yes S(6) Ni(2) S(9) C(7) -103(3) . . . . yes S(6) C(4) S(10) C(8) -179.9(6) . . . . yes S(6) C(4) C(5) S(7) 1(1) . . . . yes S(6) C(4) C(5) S(11) 179.5(5) . . . . yes S(7) Ni(2) S(6) C(4) 0.0(3) . . . . yes S(7) Ni(2) S(8) C(6) -100(13) . . . . yes S(7) Ni(2) S(9) C(7) 178.9(3) . . . . yes S(7) C(5) S(11) C(8) 178.9(6) . . . . yes S(7) C(5) C(4) S(10) -178.7(5) . . . . yes S(8) Ni(2) S(6) C(4) 179.4(3) . . . . yes S(8) Ni(2) S(7) C(5) -80(13) . . . . yes S(8) Ni(2) S(9) C(7) -0.6(4) . . . . yes S(8) C(6) S(12) C(9) -178.5(7) . . . . yes S(8) C(6) C(7) S(9) -1(1) . . . . yes S(8) C(6) C(7) S(13) 179.6(5) . . . . yes S(9) Ni(2) S(6) C(4) -77(3) . . . . yes S(9) Ni(2) S(7) C(5) 178.8(3) . . . . yes S(9) Ni(2) S(8) C(6) 0.2(4) . . . . yes S(9) C(7) S(13) C(9) 179.2(6) . . . . yes S(9) C(7) C(6) S(12) -179.7(5) . . . . yes S(10) C(4) C(5) S(11) 0(1) . . . . yes S(10) C(8) S(11) C(5) -0.6(6) . . . . yes S(11) C(8) S(10) C(4) 0.5(6) . . . . yes S(12) C(6) C(7) S(13) 1(1) . . . . yes S(12) C(9) S(13) C(7) 1.5(7) . . . . yes S(13) C(9) S(12) C(6) -1.1(7) . . . . yes S(14) C(8) S(10) C(4) -179.7(6) . . . . yes S(14) C(8) S(11) C(5) 179.6(6) . . . . yes S(15) C(9) S(12) C(6) -179.7(7) . . . . yes S(15) C(9) S(13) C(7) -179.9(7) . . . . yes S(16) Ni(3) S(17) C(11) 0.1(4) . . . . yes S(16) Ni(3) S(18) C(12) 179.2(4) . . . . yes S(16) Ni(3) S(19) C(13) -99(13) . . . . yes S(16) C(10) S(20) C(14) -179.5(7) . . . . yes S(16) C(10) C(11) S(17) 0(1) . . . . yes S(16) C(10) C(11) S(21) 179.3(5) . . . . yes S(17) Ni(3) S(16) C(10) 0.2(4) . . . . yes S(17) Ni(3) S(18) C(12) -77(3) . . . . yes S(17) Ni(3) S(19) C(13) 178.6(3) . . . . yes S(17) C(11) S(21) C(14) 178.9(6) . . . . yes S(17) C(11) C(10) S(20) -178.7(5) . . . . yes S(18) Ni(3) S(16) C(10) 178.5(4) . . . . yes S(18) Ni(3) S(17) C(11) -103(3) . . . . yes S(18) Ni(3) S(19) C(13) 0.4(3) . . . . yes S(18) C(12) S(22) C(15) -179.9(6) . . . . yes S(18) C(12) C(13) S(19) 0(1) . . . . yes S(18) C(12) C(13) S(23) 179.4(5) . . . . yes S(19) Ni(3) S(16) C(10) -81(13) . . . . yes S(19) Ni(3) S(17) C(11) 179.5(4) . . . . yes S(19) Ni(3) S(18) C(12) -0.3(4) . . . . yes S(19) C(13) S(23) C(15) 179.6(6) . . . . yes S(19) C(13) C(12) S(22) -179.0(5) . . . . yes S(20) C(10) C(11) S(21) 0(1) . . . . yes S(20) C(14) S(21) C(11) -0.4(7) . . . . yes S(21) C(14) S(20) C(10) 0.4(7) . . . . yes S(22) C(12) C(13) S(23) 0(1) . . . . yes S(22) C(15) S(23) C(13) -0.9(6) . . . . yes S(23) C(15) S(22) C(12) 1.0(7) . . . . yes S(24) C(14) S(20) C(10) 178.8(7) . . . . yes S(24) C(14) S(21) C(11) -178.9(7) . . . . yes S(25) C(15) S(22) C(12) 179.8(7) . . . . yes S(25) C(15) S(23) C(13) -179.7(7) . . . . yes S(26) Ni(4) S(27) C(17) -1.8(3) . . . . yes S(26) Ni(4) S(27) C(17) -178.2(3) . . 3_566 3_566 yes S(26) C(16) S(28) C(18) -177.5(7) . . . . yes S(26) C(16) C(17) S(27) 0(1) . . . . yes S(26) C(16) C(17) S(29) 178.2(5) . . . . yes S(27) Ni(4) S(26) C(16) 1.7(4) . . . . yes S(27) Ni(4) S(26) C(16) 178.3(4) . . 3_566 3_566 yes S(27) C(17) S(29) C(18) 178.7(6) . . . . yes S(27) C(17) C(16) S(28) 179.3(5) . . . . yes S(28) C(16) C(17) S(29) -2(1) . . . . yes S(28) C(18) S(29) C(17) 1.8(7) . . . . yes S(29) C(18) S(28) C(16) -2.9(7) . . . . yes S(30) C(18) S(28) C(16) 175.1(7) . . . . yes S(30) C(18) S(29) C(17) -176.1(7) . . . . yes C(1) C(2) S(4) C(3) -2.6(9) . . . . yes C(2) C(1) S(3) C(3) -0.6(10) . . . . yes C(4) C(5) S(11) C(8) 0.5(8) . . . . yes C(5) C(4) S(10) C(8) -0.2(9) . . . . yes C(6) C(7) S(13) C(9) -1.5(9) . . . . yes C(7) C(6) S(12) C(9) 0.0(9) . . . . yes C(10) C(11) S(21) C(14) 0.3(9) . . . . yes C(11) C(10) S(20) C(14) -0.2(9) . . . . yes C(12) C(13) S(23) C(15) 0.5(9) . . . . yes C(13) C(12) S(22) C(15) -0.7(9) . . . . yes C(16) C(17) S(29) C(18) 0.4(10) . . . . yes C(17) C(16) S(28) C(18) 3.2(9) . . . . yes C(17) C(16) S(28) C(18) 3.2(9) . . . . 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 Te(1) S(5) 3.434(4) . . ? Te(1) S(30) 3.446(4) . 2_545 ? S(2) S(18) 3.541(4) . 1_554 ? S(4) S(16) 3.567(4) . 1_554 ? S(6) S(26) 3.559(4) . 3_566 ? S(6) S(19) 3.562(4) . . ? S(7) S(18) 3.563(4) . 1_554 ? S(8) S(28) 3.573(4) . 3_566 ? S(11) C(3) 3.58(1) . . ? S(14) C(21) 3.55(2) . 2_555 ? S(15) S(24) 3.299(4) . 4_454 ? S(23) C(18) 3.58(1) . 3_566 ? S(25) C(19) 3.56(2) . 3_556 ? O(1) C(19) 3.31(2) . . ? O(1) C(21) 3.31(2) . . ? O(1) C(20) 3.35(2) . 2_545 ? C(1) C(5) 3.56(1) . . ? C(2) C(7) 3.57(1) . 3_555 ? C(13) C(17) 3.55(1) . 3_566 ? #------------------------------------------------------------------------------ data_alpha-[MOT][Ni(dmit)2]2 _database_code_CSD 184208 _audit_creation_date 'Wed Jun 26 16:11:35 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H11 O Ni2 S20 Te ' _chemical_formula_moiety '?' _chemical_formula_weight 1117.47 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 37.695(7) _cell_length_b 7.097(1) _cell_length_c 12.589(2) _cell_angle_alpha 90 _cell_angle_beta 92.846(4) _cell_angle_gamma 90 _cell_volume 3363(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.045 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.232 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.865 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MAC Science DIP320S' _diffrn_reflns_number 7612 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 30.49 _diffrn_measured_fraction_theta_max 0.3975 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.3975 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4075 _reflns_number_gt 1627 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.1131 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1627 _refine_ls_number_parameters 280 _refine_ls_goodness_of_fit_ref 1.939 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00226|Fo|^2^]' _refine_ls_shift/su_max 0.0013 _refine_diff_density_max 1.34 _refine_diff_density_min -1.92 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Te(1) Te 0.23232(7) 0.9866(4) 0.2150(3) 0.091(1) Uani 1.00 d . . . Ni(1) Ni 0.02668(8) 0.3421(4) 0.2711(4) 0.022(1) Uani 1.00 d . . . Ni(2) Ni 0.47450(8) 0.3327(4) 0.2524(4) 0.023(1) Uani 1.00 d . . . S(1) S -0.0005(2) 0.341(1) 0.1183(8) 0.033(3) Uani 1.00 d . . . S(2) S -0.0219(2) 0.342(1) 0.3520(8) 0.033(3) Uani 1.00 d . . . S(3) S 0.0756(2) 0.341(1) 0.1887(8) 0.030(3) Uani 1.00 d . . . S(4) S 0.0539(2) 0.348(1) 0.4240(8) 0.033(3) Uani 1.00 d . . . S(5) S -0.0783(2) 0.348(1) 0.0519(8) 0.035(3) Uani 1.00 d . . . S(6) S -0.0983(2) 0.346(1) 0.2725(8) 0.031(3) Uani 1.00 d . . . S(7) S 0.1516(2) 0.348(1) 0.2714(7) 0.029(3) Uani 1.00 d . . . S(8) S 0.1324(2) 0.352(1) 0.4888(8) 0.034(3) Uani 1.00 d . . . S(9) S -0.1546(2) 0.355(1) 0.0980(8) 0.042(3) Uani 1.00 d . . . S(10) S 0.2083(2) 0.352(1) 0.4400(8) 0.043(3) Uani 1.00 d . . . S(11) S 0.4259(2) 0.329(1) 0.1537(8) 0.034(3) Uani 1.00 d . . . S(12) S 0.4471(2) 0.340(1) 0.3965(8) 0.037(3) Uani 1.00 d . . . S(13) S 0.5016(2) 0.330(1) 0.1088(8) 0.034(3) Uani 1.00 d . . . S(14) S 0.5231(2) 0.334(1) 0.3495(8) 0.037(3) Uani 1.00 d . . . S(15) S 0.3495(2) 0.341(1) 0.2141(8) 0.035(3) Uani 1.00 d . . . S(16) S 0.3684(2) 0.347(1) 0.4372(8) 0.034(3) Uani 1.00 d . . . S(17) S 0.5792(2) 0.336(1) 0.0626(8) 0.036(3) Uani 1.00 d . . . S(18) S 0.5997(2) 0.339(1) 0.2866(8) 0.037(3) Uani 1.00 d . . . S(19) S 0.2924(2) 0.348(1) 0.3651(8) 0.045(3) Uani 1.00 d . . . S(20) S 0.6551(2) 0.350(1) 0.1283(8) 0.042(3) Uani 1.00 d . . . O(1) O 0.2593(6) 0.630(3) 0.081(3) 0.074(8) Uiso 1.00 d . . . C(1) C -0.0433(6) 0.342(3) 0.148(3) 0.019(7) Uiso 1.00 d . . . C(2) C -0.0525(6) 0.337(3) 0.246(3) 0.022(7) Uiso 1.00 d . . . C(3) C 0.1063(6) 0.347(3) 0.295(3) 0.015(6) Uiso 1.00 d . . . C(4) C 0.0973(7) 0.347(4) 0.398(3) 0.030(8) Uiso 1.00 d . . . C(5) C -0.1126(6) 0.346(3) 0.138(3) 0.020(6) Uiso 1.00 d . . . C(6) C 0.1662(6) 0.350(3) 0.405(3) 0.022(7) Uiso 1.00 d . . . C(7) C 0.3948(6) 0.337(3) 0.246(3) 0.018(6) Uiso 1.00 d . . . C(8) C 0.4036(6) 0.344(3) 0.349(3) 0.028(7) Uiso 1.00 d . . . C(9) C 0.5447(6) 0.331(3) 0.147(3) 0.022(7) Uiso 1.00 d . . . C(10) C 0.5535(6) 0.330(3) 0.254(3) 0.020(7) Uiso 1.00 d . . . C(11) C 0.3355(6) 0.346(4) 0.341(3) 0.024(7) Uiso 1.00 d . . . C(12) C 0.6141(7) 0.345(4) 0.161(3) 0.029(7) Uiso 1.00 d . . . C(13) C 0.2063(8) 0.769(4) 0.156(3) 0.051(10) Uiso 1.00 d . . . C(14) C 0.2309(10) 0.592(5) 0.135(4) 0.07(1) Uiso 1.00 d . . . C(15) C 0.2851(10) 0.740(5) 0.128(4) 0.07(1) Uiso 1.00 d . . . C(16) C 0.2752(8) 0.942(4) 0.135(3) 0.045(9) Uiso 1.00 d . . . C(17) C 0.2472(7) 0.886(4) 0.358(3) 0.034(8) Uiso 1.00 d . . . H(1) H 0.1871 0.7329 0.1999 0.0453 Uiso 1.00 calc . . . H(2) H 0.1948 0.8005 0.0858 0.0453 Uiso 1.00 calc . . . H(3) H 0.2174 0.4911 0.1037 0.0692 Uiso 1.00 calc . . . H(4) H 0.2390 0.5454 0.2078 0.0692 Uiso 1.00 calc . . . H(5) H 0.2885 0.6951 0.2078 0.0863 Uiso 1.00 calc . . . H(6) H 0.3087 0.7226 0.1041 0.0863 Uiso 1.00 calc . . . H(7) H 0.2952 1.0200 0.1666 0.0684 Uiso 1.00 calc . . . H(8) H 0.2719 0.9882 0.0627 0.0684 Uiso 1.00 calc . . . H(9) H 0.2555 0.7561 0.3558 0.0474 Uiso 1.00 calc . . . H(10) H 0.2684 0.9556 0.3900 0.0474 Uiso 1.00 calc . . . H(11) H 0.2297 0.8935 0.4091 0.0474 Uiso 1.00 calc . . . 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 Te(1) 0.077(2) 0.105(2) 0.091(5) 0.008(2) -0.007(2) 0.001(2) Ni(1) 0.018(2) 0.023(2) 0.024(4) 0.000(2) 0.000(1) -0.001(2) Ni(2) 0.015(2) 0.026(2) 0.028(4) -0.001(2) 0.003(1) 0.004(2) S(1) 0.022(4) 0.050(5) 0.027(8) 0.005(4) -0.001(3) -0.001(5) S(2) 0.019(4) 0.052(5) 0.028(8) 0.001(4) 0.001(3) 0.005(5) S(3) 0.021(4) 0.047(5) 0.019(8) -0.001(3) -0.004(3) -0.003(5) S(4) 0.015(4) 0.047(5) 0.039(9) 0.002(3) 0.007(3) 0.002(5) S(5) 0.028(4) 0.054(5) 0.023(8) 0.001(4) -0.001(3) 0.004(5) S(6) 0.020(4) 0.051(5) 0.022(8) -0.001(4) 0.004(3) -0.003(5) S(7) 0.024(4) 0.046(5) 0.018(8) -0.004(3) 0.003(3) -0.008(5) S(8) 0.018(4) 0.050(5) 0.033(8) -0.001(3) 0.001(3) -0.004(5) S(9) 0.021(4) 0.056(5) 0.048(10) 0.004(4) -0.002(4) -0.011(5) S(10) 0.019(4) 0.070(6) 0.038(9) -0.004(4) -0.004(3) -0.011(6) S(11) 0.018(4) 0.052(5) 0.034(8) -0.002(3) 0.004(3) -0.006(5) S(12) 0.017(4) 0.060(6) 0.033(8) 0.000(4) -0.001(3) 0.002(5) S(13) 0.023(4) 0.055(5) 0.024(8) 0.004(3) 0.005(3) -0.009(5) S(14) 0.023(4) 0.062(5) 0.025(9) -0.001(4) 0.003(3) -0.003(5) S(15) 0.021(4) 0.058(5) 0.027(8) 0.000(4) 0.001(3) 0.003(5) S(16) 0.026(4) 0.054(5) 0.023(8) 0.002(4) 0.012(3) -0.006(5) S(17) 0.022(4) 0.057(5) 0.030(8) -0.003(4) 0.010(3) 0.002(5) S(18) 0.016(4) 0.056(5) 0.039(9) -0.002(4) -0.003(3) -0.005(5) S(19) 0.018(4) 0.063(6) 0.054(10) 0.002(4) 0.016(4) -0.004(6) S(20) 0.026(5) 0.054(5) 0.049(10) 0.002(4) 0.010(4) -0.003(6) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Te(1) C(13) 1.96(3) . . yes Te(1) C(16) 1.97(3) . . yes Te(1) C(17) 1.98(4) . . yes Ni(1) S(1) 2.135(9) . . yes Ni(1) S(2) 2.138(8) . . yes Ni(1) S(3) 2.160(9) . . yes Ni(1) S(4) 2.136(9) . . yes Ni(2) S(11) 2.161(8) . . yes Ni(2) S(12) 2.132(10) . . yes Ni(2) S(13) 2.120(9) . . yes Ni(2) S(14) 2.150(9) . . yes S(1) C(1) 1.67(3) . . yes S(2) C(2) 1.72(3) . . yes S(3) C(3) 1.73(3) . . yes S(4) C(4) 1.68(3) . . yes S(5) C(1) 1.75(3) . . yes S(5) C(5) 1.73(3) . . yes S(6) C(2) 1.78(3) . . yes S(6) C(5) 1.74(3) . . yes S(7) C(3) 1.75(2) . . yes S(7) C(6) 1.74(3) . . yes S(8) C(4) 1.70(3) . . yes S(8) C(6) 1.69(3) . . yes S(9) C(5) 1.64(2) . . yes S(10) C(6) 1.63(2) . . yes S(11) C(7) 1.70(3) . . yes S(12) C(8) 1.71(3) . . yes S(13) C(9) 1.67(3) . . yes S(14) C(10) 1.70(3) . . yes S(15) C(7) 1.74(2) . . yes S(15) C(11) 1.71(3) . . yes S(16) C(8) 1.77(3) . . yes S(16) C(11) 1.69(3) . . yes S(17) C(9) 1.72(3) . . yes S(17) C(12) 1.76(3) . . yes S(18) C(10) 1.77(2) . . yes S(18) C(12) 1.70(4) . . yes S(19) C(11) 1.67(3) . . yes S(20) C(12) 1.62(3) . . yes O(1) C(14) 1.32(4) . . yes O(1) C(15) 1.36(4) . . yes C(1) C(2) 1.30(4) . . yes C(3) C(4) 1.36(4) . . yes C(7) C(8) 1.32(4) . . yes C(9) C(10) 1.37(4) . . yes C(13) C(14) 1.59(4) . . yes C(15) C(16) 1.49(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 C(13) Te(1) C(16) 94(1) . . . yes C(13) Te(1) C(17) 100(1) . . . yes C(16) Te(1) C(17) 101(1) . . . yes S(1) Ni(1) S(2) 92.6(3) . . . yes S(1) Ni(1) S(3) 87.1(3) . . . yes S(1) Ni(1) S(4) 179.0(3) . . . yes S(2) Ni(1) S(3) 179.6(4) . . . yes S(2) Ni(1) S(4) 87.4(3) . . . yes S(3) Ni(1) S(4) 92.9(3) . . . yes S(11) Ni(2) S(12) 93.3(3) . . . yes S(11) Ni(2) S(13) 86.5(3) . . . yes S(11) Ni(2) S(14) 179.4(4) . . . yes S(12) Ni(2) S(13) 179.1(3) . . . yes S(12) Ni(2) S(14) 87.2(3) . . . yes S(13) Ni(2) S(14) 93.0(4) . . . yes Ni(1) S(1) C(1) 102(1) . . . yes Ni(1) S(2) C(2) 100(1) . . . yes Ni(1) S(3) C(3) 100(1) . . . yes Ni(1) S(4) C(4) 104(1) . . . yes C(1) S(5) C(5) 97(1) . . . yes C(2) S(6) C(5) 94(1) . . . yes C(3) S(7) C(6) 95(1) . . . yes C(4) S(8) C(6) 99(1) . . . yes Ni(2) S(11) C(7) 101(1) . . . yes Ni(2) S(12) C(8) 101(1) . . . yes Ni(2) S(13) C(9) 104(1) . . . yes Ni(2) S(14) C(10) 100(1) . . . yes C(7) S(15) C(11) 97(1) . . . yes C(8) S(16) C(11) 95(1) . . . yes C(9) S(17) C(12) 97(1) . . . yes C(10) S(18) C(12) 98(1) . . . yes C(14) O(1) C(15) 118(3) . . . yes S(1) C(1) S(5) 123(2) . . . yes S(1) C(1) C(2) 121(2) . . . yes S(5) C(1) C(2) 115(1) . . . yes S(2) C(2) S(6) 118(2) . . . yes S(2) C(2) C(1) 122(1) . . . yes S(6) C(2) C(1) 118(2) . . . yes S(3) C(3) S(7) 119(1) . . . yes S(3) C(3) C(4) 123(1) . . . yes S(7) C(3) C(4) 117(2) . . . yes S(4) C(4) S(8) 126(2) . . . yes S(4) C(4) C(3) 118(2) . . . yes S(8) C(4) C(3) 114(2) . . . yes S(5) C(5) S(6) 113(1) . . . yes S(5) C(5) S(9) 122(2) . . . yes S(6) C(5) S(9) 123(1) . . . yes S(7) C(6) S(8) 112(1) . . . yes S(7) C(6) S(10) 121(1) . . . yes S(8) C(6) S(10) 125(2) . . . yes S(11) C(7) S(15) 123(1) . . . yes S(11) C(7) C(8) 121(1) . . . yes S(15) C(7) C(8) 115(2) . . . yes S(12) C(8) S(16) 121(2) . . . yes S(12) C(8) C(7) 121(2) . . . yes S(16) C(8) C(7) 116(1) . . . yes S(13) C(9) S(17) 125(2) . . . yes S(13) C(9) C(10) 117(2) . . . yes S(17) C(9) C(10) 116(1) . . . yes S(14) C(10) S(18) 121(2) . . . yes S(14) C(10) C(9) 123(1) . . . yes S(18) C(10) C(9) 114(2) . . . yes S(15) C(11) S(16) 114(1) . . . yes S(15) C(11) S(19) 121(1) . . . yes S(16) C(11) S(19) 123(2) . . . yes S(17) C(12) S(18) 112(1) . . . yes S(17) C(12) S(20) 120(2) . . . yes S(18) C(12) S(20) 126(1) . . . yes Te(1) C(13) C(14) 113(2) . . . yes O(1) C(14) C(13) 114(2) . . . yes O(1) C(15) C(16) 113(2) . . . yes Te(1) C(16) C(15) 113(2) . . . yes #------------------------------------------------------------------------------ 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 Te(1) C(13) C(14) O(1) -49(4) . . . . yes Te(1) C(16) C(15) O(1) 59(4) . . . . yes Ni(1) S(1) C(1) S(5) 178(1) . . . . yes Ni(1) S(1) C(1) C(2) -2(2) . . . . yes Ni(1) S(2) C(2) S(6) -177(1) . . . . yes Ni(1) S(2) C(2) C(1) -2(2) . . . . yes Ni(1) S(3) C(3) S(7) 179(1) . . . . yes Ni(1) S(3) C(3) C(4) 1(2) . . . . yes Ni(1) S(4) C(4) S(8) 179(1) . . . . yes Ni(1) S(4) C(4) C(3) 1(2) . . . . yes Ni(2) S(11) C(7) S(15) 179(1) . . . . yes Ni(2) S(11) C(7) C(8) 0(2) . . . . yes Ni(2) S(12) C(8) S(16) 179(1) . . . . yes Ni(2) S(12) C(8) C(7) 1(2) . . . . yes Ni(2) S(13) C(9) S(17) -178(1) . . . . yes Ni(2) S(13) C(9) C(10) 0(2) . . . . yes Ni(2) S(14) C(10) S(18) 177(1) . . . . yes Ni(2) S(14) C(10) C(9) 1(2) . . . . yes S(1) Ni(1) S(2) C(2) 0.9(9) . . . . yes S(1) Ni(1) S(3) C(3) 178.9(8) . . . . yes S(1) Ni(1) S(4) C(4) -90(18) . . . . yes S(1) C(1) S(5) C(5) 179(1) . . . . yes S(1) C(1) C(2) S(2) 3(3) . . . . yes S(1) C(1) C(2) S(6) 178(1) . . . . yes S(2) Ni(1) S(1) C(1) 0.4(9) . . . . yes S(2) Ni(1) S(3) C(3) -143(49) . . . . yes S(2) Ni(1) S(4) C(4) 179.2(9) . . . . yes S(2) C(2) S(6) C(5) 177(1) . . . . yes S(2) C(2) C(1) S(5) -176(1) . . . . yes S(3) Ni(1) S(1) C(1) -179.9(9) . . . . yes S(3) Ni(1) S(2) C(2) -36(49) . . . . yes S(3) Ni(1) S(4) C(4) -0.6(9) . . . . yes S(3) C(3) S(7) C(6) -179(1) . . . . yes S(3) C(3) C(4) S(4) -1(3) . . . . yes S(3) C(3) C(4) S(8) 179(1) . . . . yes S(4) Ni(1) S(1) C(1) -89(18) . . . . yes S(4) Ni(1) S(2) C(2) 179.9(9) . . . . yes S(4) Ni(1) S(3) C(3) -0.1(8) . . . . yes S(4) C(4) S(8) C(6) -179(1) . . . . yes S(4) C(4) C(3) S(7) 179(1) . . . . yes S(5) C(1) C(2) S(6) -2(2) . . . . yes S(5) C(5) S(6) C(2) -2(1) . . . . yes S(6) C(5) S(5) C(1) 1(1) . . . . yes S(7) C(3) C(4) S(8) 0(2) . . . . yes S(7) C(6) S(8) C(4) 0(1) . . . . yes S(8) C(6) S(7) C(3) 0(1) . . . . yes S(9) C(5) S(5) C(1) 178(1) . . . . yes S(9) C(5) S(6) C(2) -179(1) . . . . yes S(10) C(6) S(7) C(3) 179(1) . . . . yes S(10) C(6) S(8) C(4) -179(1) . . . . yes S(11) Ni(2) S(12) C(8) -1.2(9) . . . . yes S(11) Ni(2) S(13) C(9) -179.6(9) . . . . yes S(11) Ni(2) S(14) C(10) 34(34) . . . . yes S(11) C(7) S(15) C(11) 179(1) . . . . yes S(11) C(7) C(8) S(12) -1(3) . . . . yes S(11) C(7) C(8) S(16) -178(1) . . . . yes S(12) Ni(2) S(11) C(7) 0.8(9) . . . . yes S(12) Ni(2) S(13) C(9) 103(19) . . . . yes S(12) Ni(2) S(14) C(10) -179.8(9) . . . . yes S(12) C(8) S(16) C(11) -178(1) . . . . yes S(12) C(8) C(7) S(15) 179(1) . . . . yes S(13) Ni(2) S(11) C(7) -178.3(9) . . . . yes S(13) Ni(2) S(12) C(8) 75(19) . . . . yes S(13) Ni(2) S(14) C(10) -0.7(9) . . . . yes S(13) C(9) S(17) C(12) 177(1) . . . . yes S(13) C(9) C(10) S(14) -1(3) . . . . yes S(13) C(9) C(10) S(18) -177(1) . . . . yes S(14) Ni(2) S(11) C(7) 146(33) . . . . yes S(14) Ni(2) S(12) C(8) 179.1(9) . . . . yes S(14) Ni(2) S(13) C(9) 0.0(9) . . . . yes S(14) C(10) S(18) C(12) -176(1) . . . . yes S(14) C(10) C(9) S(17) 177(1) . . . . yes S(15) C(7) C(8) S(16) 1(2) . . . . yes S(15) C(11) S(16) C(8) 0(1) . . . . yes S(16) C(11) S(15) C(7) 0(1) . . . . yes S(17) C(9) C(10) S(18) 1(2) . . . . yes S(17) C(12) S(18) C(10) 0(1) . . . . yes S(18) C(12) S(17) C(9) 1(1) . . . . yes S(19) C(11) S(15) C(7) -179(1) . . . . yes S(19) C(11) S(16) C(8) -179(1) . . . . yes S(20) C(12) S(17) C(9) 179(1) . . . . yes S(20) C(12) S(18) C(10) -178(1) . . . . yes C(1) C(2) S(6) C(5) 3(2) . . . . yes C(2) C(1) S(5) C(5) 0(2) . . . . yes C(3) C(4) S(8) C(6) -1(2) . . . . yes C(4) C(3) S(7) C(6) 0(2) . . . . yes C(7) C(8) S(16) C(11) -1(2) . . . . yes C(8) C(7) S(15) C(11) -1(2) . . . . yes C(9) C(10) S(18) C(12) 0(2) . . . . yes C(10) C(9) S(17) C(12) -1(2) . . . . yes C(13) Te(1) C(16) C(15) -40(3) . . . . yes C(13) C(14) O(1) C(15) 66(4) . . . . yes C(14) O(1) C(15) C(16) -72(4) . . . . yes C(14) C(13) Te(1) C(16) 35(3) . . . . yes C(14) C(13) Te(1) C(17) -67(2) . . . . yes C(15) C(16) Te(1) C(17) 60(3) . . . . yes C(15) C(16) Te(1) C(17) 60(3) . . . . 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 S(1) S(4) 3.53(1) . 4_554 ? S(9) C(6) 3.54(2) . 2_555 ? S(9) C(17) 3.57(3) . 2_545 ? S(10) S(19) 3.352(10) . . ? S(11) S(12) 3.58(1) . 4_554 ? S(12) S(13) 3.50(1) . 4_555 ? S(12) C(9) 3.54(2) . 2_655 ? S(13) S(14) 3.60(1) . 4_554 ? S(14) S(17) 3.55(1) . 4_555 ? S(18) C(7) 3.57(2) . 2_655 ? S(18) C(7) 3.59(2) . 2_645 ? S(20) C(11) 3.55(3) . 2_655 ? O(1) C(17) 2.84(5) . 4_564 ? C(14) C(17) 3.58(6) . 4_564 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_beta-[MOT][Ni(dmit)2]2 _database_code_CSD 184209 _audit_creation_date 'Wed Jun 26 16:40:48 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H11 O Ni2 S20 Te ' _chemical_formula_moiety '?' _chemical_formula_weight 1117.47 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.093(6) _cell_length_b 37.163(9) _cell_length_c 7.716(7) _cell_angle_alpha 90 _cell_angle_beta 105.51(5) _cell_angle_gamma 90 _cell_volume 3341(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'rod' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.221 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.253 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.937 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method ? _diffrn_reflns_number 5096 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 28.33 _diffrn_measured_fraction_theta_max 0.6077 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.6077 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5076 _reflns_number_gt 2485 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.1261 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2485 _refine_ls_number_parameters 365 _refine_ls_goodness_of_fit_ref 1.992 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00276|Fo|^2^]' _refine_ls_shift/su_max 0.0084 _refine_diff_density_max 1.42 _refine_diff_density_min -2.40 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Te(1) Te 0.5710(3) 0.25068(6) 0.1351(3) 0.103(1) Uani 1.00 d . . . Ni(1) Ni 0.5105(2) -0.02158(5) 0.3052(3) 0.0367(8) Uani 1.00 d . . . Ni(2) Ni -0.0142(2) 0.02047(5) 0.1997(3) 0.0368(8) Uani 1.00 d . . . S(1) S 0.6568(5) -0.0509(1) 0.4651(7) 0.043(2) Uani 1.00 d . . . S(2) S 0.3981(5) -0.0680(1) 0.2725(7) 0.041(2) Uani 1.00 d . . . S(3) S 0.6227(5) 0.0248(1) 0.3407(7) 0.047(2) Uani 1.00 d . . . S(4) S 0.3683(5) 0.0073(1) 0.1307(7) 0.046(2) Uani 1.00 d . . . S(5) S 0.6816(6) -0.1293(1) 0.5793(7) 0.048(2) Uani 1.00 d . . . S(6) S 0.4450(6) -0.1448(1) 0.4039(7) 0.050(2) Uani 1.00 d . . . S(7) S 0.5844(6) 0.0996(1) 0.1854(7) 0.048(2) Uani 1.00 d . . . S(8) S 0.3497(6) 0.0832(1) -0.0104(7) 0.048(2) Uani 1.00 d . . . S(9) S 0.5988(7) -0.2044(1) 0.5781(9) 0.064(2) Uani 1.00 d . . . S(10) S 0.4420(6) 0.1566(1) -0.0376(8) 0.061(2) Uani 1.00 d . . . S(11) S 0.1322(5) -0.0151(1) 0.2838(7) 0.046(2) Uani 1.00 d . . . S(12) S -0.1320(5) -0.0191(1) 0.2545(7) 0.046(2) Uani 1.00 d . . . S(13) S 0.0994(5) 0.0621(1) 0.1514(7) 0.040(2) Uani 1.00 d . . . S(14) S -0.1634(5) 0.0545(1) 0.1218(7) 0.043(2) Uani 1.00 d . . . S(15) S 0.1520(5) -0.0913(1) 0.4286(7) 0.046(2) Uani 1.00 d . . . S(16) S -0.0915(6) -0.0944(1) 0.4031(7) 0.047(2) Uani 1.00 d . . . S(17) S 0.0502(6) 0.1389(1) 0.0210(8) 0.051(2) Uani 1.00 d . . . S(18) S -0.1907(5) 0.1320(1) -0.0051(7) 0.047(2) Uani 1.00 d . . . S(19) S 0.0533(6) -0.1576(1) 0.5445(8) 0.060(2) Uani 1.00 d . . . S(20) S -0.1038(7) 0.2025(1) -0.0877(9) 0.067(2) Uani 1.00 d . . . O(1) O 0.785(2) 0.2509(4) 0.485(3) 0.085(5) Uiso 1.00 d . . . C(1) C 0.594(2) -0.0929(5) 0.469(3) 0.052(9) Uani 1.00 d . . . C(2) C 0.487(2) -0.1002(4) 0.388(2) 0.048(8) Uani 1.00 d . . . C(3) C 0.537(2) 0.0559(4) 0.218(3) 0.045(7) Uani 1.00 d . . . C(4) C 0.421(2) 0.0478(4) 0.115(3) 0.043(7) Uani 1.00 d . . . C(5) C 0.579(2) -0.1612(4) 0.523(3) 0.049(8) Uani 1.00 d . . . C(6) C 0.457(2) 0.1150(4) 0.044(2) 0.039(7) Uani 1.00 d . . . C(7) C 0.078(2) -0.0521(5) 0.345(3) 0.049(8) Uani 1.00 d . . . C(8) C -0.042(2) -0.0544(4) 0.332(2) 0.045(7) Uani 1.00 d . . . C(9) C 0.010(2) 0.0960(4) 0.081(3) 0.047(8) Uani 1.00 d . . . C(10) C -0.106(2) 0.0944(4) 0.067(2) 0.040(7) Uani 1.00 d . . . C(11) C 0.041(2) -0.1162(5) 0.456(2) 0.046(8) Uani 1.00 d . . . C(12) C -0.086(2) 0.1594(4) -0.024(3) 0.049(7) Uani 1.00 d . . . C(13) C 0.685(3) 0.2893(6) 0.259(4) 0.10(1) Uani 1.00 d . . . C(14) C 0.715(2) 0.2822(5) 0.454(3) 0.063(9) Uani 1.00 d . . . C(15) C 0.720(3) 0.2190(7) 0.464(3) 0.09(1) Uani 1.00 d . . . C(16) C 0.687(3) 0.2130(6) 0.273(6) 0.14(2) Uani 1.00 d . . . C(17) C 0.600(3) 0.2512(6) -0.118(5) 0.09(1) Uani 1.00 d . . . H(1) H 0.6549 0.3130 0.2221 0.1133 Uiso 1.00 calc . . . H(2) H 0.7545 0.2878 0.2081 0.1133 Uiso 1.00 calc . . . H(3) H 0.6498 0.2795 0.4949 0.0970 Uiso 1.00 calc . . . H(4) H 0.7601 0.3025 0.5211 0.0970 Uiso 1.00 calc . . . H(5) H 0.6517 0.2205 0.4990 0.1045 Uiso 1.00 calc . . . H(6) H 0.7630 0.1981 0.5219 0.1045 Uiso 1.00 calc . . . H(7) H 0.7563 0.2146 0.2095 0.1225 Uiso 1.00 calc . . . H(8) H 0.6575 0.1887 0.2199 0.1225 Uiso 1.00 calc . . . H(9) H 0.6812 0.2453 -0.0962 0.0967 Uiso 1.00 calc . . . H(10) H 0.5553 0.2340 -0.1850 0.0967 Uiso 1.00 calc . . . H(11) H 0.5873 0.2745 -0.1608 0.0967 Uiso 1.00 calc . . . 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 Te(1) 0.061(3) 0.131(2) 0.106(2) 0.002(1) 0.000(2) -0.012(1) Ni(1) 0.029(2) 0.032(1) 0.045(1) 0.0004(9) 0.002(1) 0.0006(9) Ni(2) 0.028(2) 0.033(1) 0.046(2) -0.0006(9) 0.004(1) -0.0002(9) S(1) 0.033(5) 0.037(2) 0.055(3) -0.002(2) 0.006(3) 0.003(2) S(2) 0.030(5) 0.035(2) 0.052(3) -0.003(2) -0.002(3) 0.002(2) S(3) 0.040(5) 0.035(2) 0.060(3) -0.004(2) 0.001(3) 0.006(2) S(4) 0.033(5) 0.037(2) 0.062(4) -0.004(2) 0.003(3) 0.005(2) S(5) 0.034(5) 0.041(3) 0.063(4) 0.004(2) 0.002(3) 0.009(2) S(6) 0.047(5) 0.034(2) 0.064(4) -0.005(2) 0.008(3) 0.003(2) S(7) 0.042(5) 0.037(2) 0.062(3) -0.007(2) 0.006(3) 0.001(2) S(8) 0.042(5) 0.041(3) 0.052(3) 0.005(2) -0.003(3) 0.005(2) S(9) 0.065(6) 0.038(3) 0.087(4) 0.007(2) 0.018(4) 0.015(2) S(10) 0.065(7) 0.041(3) 0.073(4) 0.005(2) 0.015(4) 0.009(2) S(11) 0.032(5) 0.041(3) 0.063(4) 0.003(2) 0.008(3) 0.009(2) S(12) 0.032(5) 0.037(2) 0.068(3) 0.002(2) 0.010(3) 0.008(2) S(13) 0.028(5) 0.040(2) 0.050(3) 0.000(2) 0.005(3) 0.003(2) S(14) 0.023(5) 0.036(2) 0.064(3) 0.000(2) 0.004(3) 0.005(2) S(15) 0.036(5) 0.041(3) 0.055(3) 0.008(2) 0.001(3) 0.007(2) S(16) 0.044(5) 0.039(3) 0.055(3) 0.003(2) 0.009(3) 0.006(2) S(17) 0.044(6) 0.038(3) 0.070(4) -0.003(2) 0.016(4) 0.009(2) S(18) 0.040(5) 0.034(2) 0.064(3) 0.004(2) 0.009(3) 0.003(2) S(19) 0.062(6) 0.040(3) 0.071(4) 0.007(2) 0.005(4) 0.008(2) S(20) 0.062(6) 0.039(3) 0.104(5) 0.008(3) 0.027(5) 0.020(3) C(1) 0.07(3) 0.04(1) 0.05(1) 0.00(1) 0.02(2) 0.010(9) C(2) 0.08(3) 0.033(9) 0.03(1) -0.02(1) 0.02(1) -0.001(8) C(3) 0.04(2) 0.037(10) 0.06(1) 0.000(8) 0.02(1) -0.004(8) C(4) 0.02(2) 0.04(1) 0.05(1) -0.006(8) -0.01(1) -0.009(8) C(5) 0.06(2) 0.036(10) 0.06(1) 0.008(9) 0.02(1) 0.011(8) C(6) 0.03(2) 0.041(10) 0.05(1) 0.013(8) 0.01(1) 0.012(8) C(7) 0.04(2) 0.04(1) 0.05(1) -0.001(9) 0.00(1) -0.001(8) C(8) 0.06(2) 0.035(10) 0.03(1) 0.007(9) -0.01(1) -0.002(7) C(9) 0.05(2) 0.04(1) 0.05(1) -0.023(9) 0.01(1) -0.005(8) C(10) 0.05(2) 0.033(9) 0.04(1) -0.010(8) 0.02(1) -0.002(7) C(11) 0.05(2) 0.05(1) 0.02(1) 0.016(10) -0.01(1) 0.003(8) C(12) 0.07(2) 0.032(9) 0.05(1) -0.003(9) 0.02(1) 0.003(7) C(13) 0.07(4) 0.05(1) 0.15(3) -0.01(1) 0.00(2) -0.01(1) C(14) 0.06(3) 0.05(1) 0.05(1) -0.01(1) -0.03(1) 0.008(9) C(15) 0.06(3) 0.10(2) 0.06(2) 0.03(2) -0.06(2) -0.01(1) C(16) 0.02(3) 0.03(1) 0.34(6) 0.02(1) 0.02(3) 0.04(2) C(17) 0.03(3) 0.09(2) 0.14(3) 0.00(1) 0.00(2) -0.02(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Te(1) C(13) 2.04(3) . . yes Te(1) C(16) 2.06(3) . . yes Te(1) C(17) 2.08(3) . . yes Ni(1) S(1) 2.162(6) . . yes Ni(1) S(2) 2.168(5) . . yes Ni(1) S(3) 2.166(6) . . yes Ni(1) S(4) 2.164(6) . . yes Ni(2) S(11) 2.166(6) . . yes Ni(2) S(12) 2.165(5) . . yes Ni(2) S(13) 2.168(5) . . yes Ni(2) S(14) 2.152(6) . . yes S(1) C(1) 1.74(2) . . yes S(2) C(2) 1.69(2) . . yes S(3) C(3) 1.67(2) . . yes S(4) C(4) 1.65(2) . . yes S(5) C(1) 1.79(2) . . yes S(5) C(5) 1.68(2) . . yes S(6) C(2) 1.75(2) . . yes S(6) C(5) 1.75(2) . . yes S(7) C(3) 1.76(2) . . yes S(7) C(6) 1.73(2) . . yes S(8) C(4) 1.72(2) . . yes S(8) C(6) 1.73(2) . . yes S(9) C(5) 1.66(2) . . yes S(10) C(6) 1.66(2) . . yes S(11) C(7) 1.65(2) . . yes S(12) C(8) 1.71(2) . . yes S(13) C(9) 1.65(2) . . yes S(14) C(10) 1.74(2) . . yes S(15) C(7) 1.74(2) . . yes S(15) C(11) 1.69(2) . . yes S(16) C(8) 1.75(2) . . yes S(16) C(11) 1.75(2) . . yes S(17) C(9) 1.77(2) . . yes S(17) C(12) 1.76(2) . . yes S(18) C(10) 1.74(2) . . yes S(18) C(12) 1.67(2) . . yes S(19) C(11) 1.67(2) . . yes S(20) C(12) 1.67(2) . . yes O(1) C(14) 1.42(3) . . yes O(1) C(15) 1.41(4) . . yes C(1) C(2) 1.31(3) . . yes C(3) C(4) 1.44(3) . . yes C(7) C(8) 1.43(3) . . yes C(9) C(10) 1.38(3) . . yes C(13) C(14) 1.48(4) . . yes C(15) C(16) 1.44(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 C(13) Te(1) C(16) 87(1) . . . yes C(13) Te(1) C(17) 99(1) . . . yes C(16) Te(1) C(17) 103(1) . . . yes S(1) Ni(1) S(2) 93.3(2) . . . yes S(1) Ni(1) S(3) 86.5(2) . . . yes S(1) Ni(1) S(4) 176.4(2) . . . yes S(2) Ni(1) S(3) 179.4(2) . . . yes S(2) Ni(1) S(4) 87.3(2) . . . yes S(3) Ni(1) S(4) 92.9(2) . . . yes S(11) Ni(2) S(12) 93.1(2) . . . yes S(11) Ni(2) S(13) 89.0(2) . . . yes S(11) Ni(2) S(14) 177.7(2) . . . yes S(12) Ni(2) S(13) 177.0(2) . . . yes S(12) Ni(2) S(14) 84.7(2) . . . yes S(13) Ni(2) S(14) 93.1(2) . . . yes Ni(1) S(1) C(1) 99.7(9) . . . yes Ni(1) S(2) C(2) 102.3(8) . . . yes Ni(1) S(3) C(3) 101.8(8) . . . yes Ni(1) S(4) C(4) 103.8(8) . . . yes C(1) S(5) C(5) 96(1) . . . yes C(2) S(6) C(5) 97(1) . . . yes C(3) S(7) C(6) 97(1) . . . yes C(4) S(8) C(6) 98(1) . . . yes Ni(2) S(11) C(7) 103.8(9) . . . yes Ni(2) S(12) C(8) 101.4(9) . . . yes Ni(2) S(13) C(9) 102.2(8) . . . yes Ni(2) S(14) C(10) 102.0(8) . . . yes C(7) S(15) C(11) 99(1) . . . yes C(8) S(16) C(11) 95(1) . . . yes C(9) S(17) C(12) 97(1) . . . yes C(10) S(18) C(12) 96(1) . . . yes C(14) O(1) C(15) 112(2) . . . yes S(1) C(1) S(5) 118(1) . . . yes S(1) C(1) C(2) 123(1) . . . yes S(5) C(1) C(2) 117(1) . . . yes S(2) C(2) S(6) 123(1) . . . yes S(2) C(2) C(1) 120(1) . . . yes S(6) C(2) C(1) 115(1) . . . yes S(3) C(3) S(7) 122(1) . . . yes S(3) C(3) C(4) 122(1) . . . yes S(7) C(3) C(4) 114(1) . . . yes S(4) C(4) S(8) 126(1) . . . yes S(4) C(4) C(3) 119(1) . . . yes S(8) C(4) C(3) 114(1) . . . yes S(5) C(5) S(6) 113.9(10) . . . yes S(5) C(5) S(9) 124(1) . . . yes S(6) C(5) S(9) 121(1) . . . yes S(7) C(6) S(8) 114.3(9) . . . yes S(7) C(6) S(10) 122(1) . . . yes S(8) C(6) S(10) 123(1) . . . yes S(11) C(7) S(15) 126(1) . . . yes S(11) C(7) C(8) 120(1) . . . yes S(15) C(7) C(8) 112(1) . . . yes S(12) C(8) S(16) 121(1) . . . yes S(12) C(8) C(7) 121(1) . . . yes S(16) C(8) C(7) 117(1) . . . yes S(13) C(9) S(17) 124(1) . . . yes S(13) C(9) C(10) 123(1) . . . yes S(17) C(9) C(10) 111(1) . . . yes S(14) C(10) S(18) 121(1) . . . yes S(14) C(10) C(9) 118(1) . . . yes S(18) C(10) C(9) 119(1) . . . yes S(15) C(11) S(16) 115.2(10) . . . yes S(15) C(11) S(19) 124(1) . . . yes S(16) C(11) S(19) 119(1) . . . yes S(17) C(12) S(18) 114.3(10) . . . yes S(17) C(12) S(20) 121(1) . . . yes S(18) C(12) S(20) 124(1) . . . yes Te(1) C(13) C(14) 107(1) . . . yes O(1) C(14) C(13) 106(1) . . . yes O(1) C(15) C(16) 103(2) . . . yes Te(1) C(16) C(15) 112(2) . . . yes #------------------------------------------------------------------------------ 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 Te(1) C(13) C(14) O(1) 71(2) . . . . yes Te(1) C(16) C(15) O(1) -68(3) . . . . yes Ni(1) S(1) C(1) S(5) 177.1(9) . . . . yes Ni(1) S(1) C(1) C(2) 0(1) . . . . yes Ni(1) S(2) C(2) S(6) -177.8(10) . . . . yes Ni(1) S(2) C(2) C(1) 0(1) . . . . yes Ni(1) S(3) C(3) S(7) -176.4(9) . . . . yes Ni(1) S(3) C(3) C(4) -3(1) . . . . yes Ni(1) S(4) C(4) S(8) 178(1) . . . . yes Ni(1) S(4) C(4) C(3) -3(1) . . . . yes Ni(2) S(11) C(7) S(15) -179(1) . . . . yes Ni(2) S(11) C(7) C(8) 0(1) . . . . yes Ni(2) S(12) C(8) S(16) 178.4(9) . . . . yes Ni(2) S(12) C(8) C(7) 0(1) . . . . yes Ni(2) S(13) C(9) S(17) 179(1) . . . . yes Ni(2) S(13) C(9) C(10) 1(1) . . . . yes Ni(2) S(14) C(10) S(18) -179.6(9) . . . . yes Ni(2) S(14) C(10) C(9) 0(1) . . . . yes S(1) Ni(1) S(2) C(2) 0.0(6) . . . . yes S(1) Ni(1) S(3) C(3) 177.1(6) . . . . yes S(1) Ni(1) S(4) C(4) -80(3) . . . . yes S(1) C(1) S(5) C(5) -175(1) . . . . yes S(1) C(1) C(2) S(2) -1(2) . . . . yes S(1) C(1) C(2) S(6) 177.4(10) . . . . yes S(2) Ni(1) S(1) C(1) -0.4(7) . . . . yes S(2) Ni(1) S(3) C(3) -113(25) . . . . yes S(2) Ni(1) S(4) C(4) -179.2(7) . . . . yes S(2) C(2) S(6) C(5) 175(1) . . . . yes S(2) C(2) C(1) S(5) -177.4(9) . . . . yes S(3) Ni(1) S(1) C(1) 179.1(7) . . . . yes S(3) Ni(1) S(2) C(2) -69(25) . . . . yes S(3) Ni(1) S(4) C(4) 1.3(7) . . . . yes S(3) C(3) S(7) C(6) 177(1) . . . . yes S(3) C(3) C(4) S(4) 4(2) . . . . yes S(3) C(3) C(4) S(8) -177.1(9) . . . . yes S(4) Ni(1) S(1) C(1) -99(3) . . . . yes S(4) Ni(1) S(2) C(2) 176.4(6) . . . . yes S(4) Ni(1) S(3) C(3) 0.7(6) . . . . yes S(4) C(4) S(8) C(6) 178(1) . . . . yes S(4) C(4) C(3) S(7) 178.6(9) . . . . yes S(5) C(1) C(2) S(6) 1(2) . . . . yes S(5) C(5) S(6) C(2) 3(1) . . . . yes S(6) C(5) S(5) C(1) -3(1) . . . . yes S(7) C(3) C(4) S(8) -3(1) . . . . yes S(7) C(6) S(8) C(4) 1(1) . . . . yes S(8) C(6) S(7) C(3) -3(1) . . . . yes S(9) C(5) S(5) C(1) 179(1) . . . . yes S(9) C(5) S(6) C(2) -178(1) . . . . yes S(10) C(6) S(7) C(3) 178(1) . . . . yes S(10) C(6) S(8) C(4) 179(1) . . . . yes S(11) Ni(2) S(12) C(8) 0.3(7) . . . . yes S(11) Ni(2) S(13) C(9) -179.8(7) . . . . yes S(11) Ni(2) S(14) C(10) 160(5) . . . . yes S(11) C(7) S(15) C(11) -179(1) . . . . yes S(11) C(7) C(8) S(12) 0(2) . . . . yes S(11) C(7) C(8) S(16) -178.9(9) . . . . yes S(12) Ni(2) S(11) C(7) -0.5(8) . . . . yes S(12) Ni(2) S(13) C(9) -43(5) . . . . yes S(12) Ni(2) S(14) C(10) 178.1(6) . . . . yes S(12) C(8) S(16) C(11) 179(1) . . . . yes S(12) C(8) C(7) S(15) 179.5(9) . . . . yes S(13) Ni(2) S(11) C(7) 177.4(7) . . . . yes S(13) Ni(2) S(12) C(8) -136(4) . . . . yes S(13) Ni(2) S(14) C(10) 0.1(6) . . . . yes S(13) C(9) S(17) C(12) -176(1) . . . . yes S(13) C(9) C(10) S(14) -1(2) . . . . yes S(13) C(9) C(10) S(18) 178.9(10) . . . . yes S(14) Ni(2) S(11) C(7) 17(6) . . . . yes S(14) Ni(2) S(12) C(8) -179.0(7) . . . . yes S(14) Ni(2) S(13) C(9) -0.6(7) . . . . yes S(14) C(10) S(18) C(12) 177(1) . . . . yes S(14) C(10) C(9) S(17) -179.5(9) . . . . yes S(15) C(7) C(8) S(16) 1(2) . . . . yes S(15) C(11) S(16) C(8) 2(1) . . . . yes S(16) C(11) S(15) C(7) -2(1) . . . . yes S(17) C(9) C(10) S(18) 0(2) . . . . yes S(17) C(12) S(18) C(10) 3(1) . . . . yes S(18) C(12) S(17) C(9) -2(1) . . . . yes S(19) C(11) S(15) C(7) -176(1) . . . . yes S(19) C(11) S(16) C(8) 177(1) . . . . yes S(20) C(12) S(17) C(9) 179(1) . . . . yes S(20) C(12) S(18) C(10) -178(1) . . . . yes C(1) C(2) S(6) C(5) -2(1) . . . . yes C(2) C(1) S(5) C(5) 1(1) . . . . yes C(3) C(4) S(8) C(6) 1(1) . . . . yes C(4) C(3) S(7) C(6) 3(1) . . . . yes C(7) C(8) S(16) C(11) -2(1) . . . . yes C(8) C(7) S(15) C(11) 0(1) . . . . yes C(9) C(10) S(18) C(12) -2(1) . . . . yes C(10) C(9) S(17) C(12) 1(1) . . . . yes C(13) Te(1) C(16) C(15) 54(2) . . . . yes C(13) C(14) O(1) C(15) -86(2) . . . . yes C(14) O(1) C(15) C(16) 82(2) . . . . yes C(14) C(13) Te(1) C(16) -52(2) . . . . yes C(14) C(13) Te(1) C(17) -155(2) . . . . yes C(15) C(16) Te(1) C(17) 153(2) . . . . yes C(15) C(16) Te(1) C(17) 153(2) . . . . 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 Te(1) O(1) 3.34(3) . 4_454 ? Ni(1) Ni(1) 3.475(4) . 3_656 ? Ni(1) S(3) 3.525(6) . 3_656 ? Ni(2) Ni(2) 3.536(4) . 3_555 ? S(1) S(12) 3.576(7) . 1_655 ? S(1) S(16) 3.590(8) . 1_655 ? S(1) S(4) 3.599(7) . 3_656 ? S(1) S(13) 3.600(8) . 3_656 ? S(2) S(3) 3.457(7) . 3_656 ? S(2) S(14) 3.598(8) . 3_555 ? S(3) S(11) 3.566(9) . 3_656 ? S(3) S(12) 3.599(8) . 1_655 ? S(4) S(11) 3.471(8) . . ? S(4) S(14) 3.553(8) . 3_555 ? S(4) S(12) 3.557(9) . 3_555 ? S(6) S(10) 3.480(7) . 3_655 ? S(9) S(20) 3.462(7) . 2_545 ? S(10) C(14) 3.55(2) . 4_454 ? S(11) S(14) 3.565(7) . 3_555 ? S(19) C(15) 3.58(3) . 3_656 ? C(1) C(3) 3.50(3) . 3_656 ? C(2) C(3) 3.54(2) . 3_656 ? C(7) C(9) 3.57(3) . 3_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_gamma-[MOT][Ni(dmit)2]2 _database_code_CSD 184210 _audit_creation_date 'Wed Jul 10 15:46:56 2002' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H11 O Ni2 S20 Te ' _chemical_formula_moiety 'C17 H11 O Ni2 S20 Te ' _chemical_formula_weight 1117.47 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.786(5) _cell_length_b 19.266(4) _cell_length_c 7.548(2) _cell_angle_alpha 92.54(2) _cell_angle_beta 101.78(3) _cell_angle_gamma 82.06(2) _cell_volume 1661.6(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 17.2 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.675 _exptl_crystal_size_mid 0.215 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.271 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 10368 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.11 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9696 _reflns_number_gt 7668 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1630 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7668 _refine_ls_number_parameters 365 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0901P)^2^+3.8203P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0080 _refine_diff_density_max 2.49 _refine_diff_density_min -1.95 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Te(1) Te 0.30370(4) -0.01326(2) 0.31775(6) 0.0385(1) Uani 0.65 d P . . Ni(1) Ni 0.37539(4) 0.48428(3) 0.61257(6) 0.0308(1) Uani 1.00 d . . . Ni(2) Ni 0.15875(4) 0.43370(3) 0.83918(6) 0.0310(1) Uani 1.00 d . . . S(1) S 0.51616(9) 0.40206(6) 0.7200(1) 0.0368(2) Uani 1.00 d . . . S(2) S 0.28221(9) 0.41296(5) 0.4269(1) 0.0374(2) Uani 1.00 d . . . S(3) S 0.46367(8) 0.55778(5) 0.7976(1) 0.0362(2) Uani 1.00 d . . . S(4) S 0.23560(8) 0.56410(5) 0.4970(1) 0.0358(2) Uani 1.00 d . . . S(5) S 0.55287(9) 0.24754(5) 0.6209(2) 0.0388(2) Uani 1.00 d . . . S(6) S 0.33687(9) 0.25817(5) 0.3559(1) 0.0372(2) Uani 1.00 d . . . S(7) S 0.40186(9) 0.71417(6) 0.8564(1) 0.0369(2) Uani 1.00 d . . . S(8) S 0.18789(9) 0.71871(6) 0.5858(2) 0.0382(2) Uani 1.00 d . . . S(9) S 0.4844(1) 0.12031(6) 0.4071(2) 0.0535(3) Uani 1.00 d . . . S(10) S 0.2447(1) 0.84958(6) 0.7829(2) 0.0537(3) Uani 1.00 d . . . S(11) S 0.29748(8) 0.35397(5) 0.9598(1) 0.0353(2) Uani 1.00 d . . . S(12) S 0.06828(9) 0.35991(6) 0.6564(1) 0.0380(2) Uani 1.00 d . . . S(13) S 0.24712(8) 0.50888(5) 1.0177(1) 0.0364(2) Uani 1.00 d . . . S(14) S 0.01354(9) 0.51130(6) 0.7343(1) 0.0393(2) Uani 1.00 d . . . S(15) S 0.3316(1) 0.19694(6) 0.8954(2) 0.0419(2) Uani 1.00 d . . . S(16) S 0.1256(1) 0.20309(6) 0.6101(2) 0.0400(2) Uani 1.00 d . . . S(17) S 0.17749(9) 0.66271(6) 1.0886(1) 0.0384(2) Uani 1.00 d . . . S(18) S -0.04031(9) 0.66452(6) 0.8257(2) 0.0385(2) Uani 1.00 d . . . S(19) S 0.2609(1) 0.06414(6) 0.7210(2) 0.0501(3) Uani 1.00 d . . . S(20) S 0.0157(1) 0.79561(6) 1.0221(2) 0.0519(3) Uani 1.00 d . . . O(1) O 0.0254(3) -0.0184(2) 0.2221(6) 0.0596(10) Uani 1.00 d . . . C(1) C 0.4732(3) 0.3313(2) 0.5966(5) 0.0309(7) Uani 1.00 d . . . C(2) C 0.3701(3) 0.3355(2) 0.4691(5) 0.0301(7) Uani 1.00 d . . . C(3) C 0.3747(3) 0.6345(2) 0.7481(5) 0.0313(7) Uani 1.00 d . . . C(4) C 0.2721(3) 0.6371(2) 0.6173(5) 0.0316(7) Uani 1.00 d . . . C(5) C 0.4589(3) 0.2043(2) 0.4609(6) 0.0366(8) Uani 1.00 d . . . C(6) C 0.2774(4) 0.7648(2) 0.7448(6) 0.0364(8) Uani 1.00 d . . . C(7) C 0.2559(3) 0.2799(2) 0.8456(5) 0.0323(7) Uani 1.00 d . . . C(8) C 0.1568(3) 0.2828(2) 0.7115(5) 0.0326(7) Uani 1.00 d . . . C(9) C 0.1534(3) 0.5834(2) 0.9781(5) 0.0320(7) Uani 1.00 d . . . C(10) C 0.0485(3) 0.5846(2) 0.8520(5) 0.0291(6) Uani 1.00 d . . . C(11) C 0.2404(4) 0.1502(2) 0.7406(6) 0.0376(8) Uani 1.00 d . . . C(12) C 0.0499(4) 0.7114(2) 0.9810(6) 0.0366(8) Uani 1.00 d . . . C(13) C 0.4010(5) -0.0418(3) 0.1436(7) 0.055(1) Uani 1.00 d . . . C(14) C 0.2132(4) -0.0921(3) 0.3016(7) 0.049(1) Uani 1.00 d . . . C(15) C 0.0951(4) -0.0663(3) 0.3482(7) 0.047(1) Uani 1.00 d . . . C(16) C 0.0653(4) 0.0488(3) 0.2368(9) 0.058(1) Uani 1.00 d . . . C(17) C 0.1775(3) 0.0483(2) 0.1676(6) 0.0408 Uani 1.00 d . . . H(1) H 0.4231 -0.0012 0.0992 0.0253 Uiso 1.00 calc . . . H(2) H 0.4659 -0.0723 0.1955 0.0253 Uiso 1.00 calc . . . H(3) H 0.3551 -0.0647 0.0424 0.0253 Uiso 1.00 calc . . . H(4) H 0.2556 -0.1275 0.3827 0.0253 Uiso 1.00 calc . . . H(5) H 0.2101 -0.1138 0.1725 0.0433 Uiso 1.00 calc . . . H(6) H 0.1072 -0.0457 0.4662 0.0253 Uiso 1.00 calc . . . H(7) H 0.0544 -0.1062 0.3498 0.0253 Uiso 1.00 calc . . . H(8) H 0.0785 0.0623 0.3593 0.0253 Uiso 1.00 calc . . . H(9) H 0.0060 0.0801 0.1673 0.0253 Uiso 1.00 calc . . . H(10) H 0.1969 0.0939 0.1713 0.0253 Uiso 1.00 calc . . . H(11) H 0.1666 0.0306 0.0447 0.0253 Uiso 1.00 calc . . . 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 Te(1) 0.0343(2) 0.0408(2) 0.0395(2) -0.0047(2) 0.0062(2) -0.0045(2) Ni(1) 0.0297(2) 0.0315(2) 0.0278(2) -0.0034(2) -0.0011(2) -0.0016(2) Ni(2) 0.0302(2) 0.0309(2) 0.0291(2) -0.0053(2) -0.0016(2) -0.0005(2) S(1) 0.0314(4) 0.0383(5) 0.0344(5) -0.0023(4) -0.0055(3) -0.0038(4) S(2) 0.0324(4) 0.0346(5) 0.0379(5) -0.0013(4) -0.0067(4) -0.0035(4) S(3) 0.0310(4) 0.0370(5) 0.0341(5) -0.0023(4) -0.0069(3) -0.0021(4) S(4) 0.0323(4) 0.0351(5) 0.0337(4) -0.0034(4) -0.0065(3) -0.0032(4) S(5) 0.0343(5) 0.0346(5) 0.0418(5) 0.0000(4) -0.0031(4) 0.0009(4) S(6) 0.0321(4) 0.0350(5) 0.0406(5) -0.0054(4) -0.0016(4) -0.0036(4) S(7) 0.0352(5) 0.0366(5) 0.0359(5) -0.0082(4) -0.0009(4) -0.0060(4) S(8) 0.0316(4) 0.0357(5) 0.0422(5) -0.0009(4) -0.0018(4) -0.0015(4) S(9) 0.0518(7) 0.0312(5) 0.0693(8) -0.0032(5) -0.0050(6) -0.0031(5) S(10) 0.0630(8) 0.0346(5) 0.0590(7) -0.0018(5) 0.0068(6) -0.0100(5) S(11) 0.0318(4) 0.0340(5) 0.0354(5) -0.0049(4) -0.0042(3) -0.0021(4) S(12) 0.0353(5) 0.0361(5) 0.0368(5) -0.0059(4) -0.0067(4) -0.0025(4) S(13) 0.0314(4) 0.0336(5) 0.0375(5) -0.0030(4) -0.0077(4) -0.0002(4) S(14) 0.0335(5) 0.0373(5) 0.0391(5) -0.0039(4) -0.0099(4) -0.0042(4) S(15) 0.0394(5) 0.0354(5) 0.0447(5) 0.0004(4) -0.0012(4) -0.0049(4) S(16) 0.0405(5) 0.0382(5) 0.0393(5) -0.0101(4) 0.0022(4) -0.0088(4) S(17) 0.0364(5) 0.0369(5) 0.0383(5) -0.0078(4) -0.0019(4) -0.0058(4) S(18) 0.0319(4) 0.0357(5) 0.0426(5) -0.0007(4) -0.0018(4) -0.0016(4) S(19) 0.0652(7) 0.0351(5) 0.0483(6) -0.0044(5) 0.0112(5) -0.0093(4) S(20) 0.0585(7) 0.0326(5) 0.0639(8) -0.0040(5) 0.0139(6) -0.0068(5) O(1) 0.037(2) 0.079(3) 0.060(2) -0.014(2) -0.003(2) 0.010(2) C(1) 0.029(2) 0.032(2) 0.030(2) -0.003(1) 0.002(1) 0.001(1) C(2) 0.028(2) 0.030(2) 0.030(2) -0.004(1) 0.001(1) -0.002(1) C(3) 0.025(1) 0.041(2) 0.026(2) -0.006(1) -0.001(1) 0.000(1) C(4) 0.027(2) 0.037(2) 0.027(2) -0.005(1) -0.001(1) -0.001(1) C(5) 0.031(2) 0.039(2) 0.040(2) -0.005(1) 0.006(1) 0.003(2) C(6) 0.036(2) 0.038(2) 0.035(2) -0.007(2) 0.008(1) -0.004(1) C(7) 0.030(2) 0.032(2) 0.032(2) -0.004(1) 0.002(1) -0.004(1) C(8) 0.031(2) 0.036(2) 0.030(2) -0.008(1) 0.002(1) -0.002(1) C(9) 0.028(2) 0.035(2) 0.030(2) -0.006(1) -0.001(1) 0.000(1) C(10) 0.028(1) 0.029(2) 0.030(2) -0.005(1) 0.001(1) 0.002(1) C(11) 0.041(2) 0.039(2) 0.034(2) -0.005(2) 0.013(2) -0.004(2) C(12) 0.035(2) 0.039(2) 0.036(2) -0.006(2) 0.009(1) 0.000(2) C(13) 0.043(2) 0.073(4) 0.050(3) -0.004(2) 0.015(2) -0.011(2) C(14) 0.046(2) 0.044(2) 0.059(3) -0.010(2) 0.013(2) -0.004(2) C(15) 0.042(2) 0.052(3) 0.052(3) -0.015(2) 0.010(2) 0.002(2) C(16) 0.034(2) 0.064(3) 0.072(3) 0.007(2) 0.008(2) 0.019(3) C(17) 0.0268 0.0456 0.0509 -0.0005 0.0083 0.0212 #------------------------------------------------------------------------------ _computing_data_collection 'AFC' _computing_cell_refinement 'AFC' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Te(1) C(13) 1.930(6) . . yes Te(1) C(14) 1.958(6) . . yes Te(1) C(17) 1.961(4) . . yes Ni(1) S(1) 2.181(1) . . yes Ni(1) S(2) 2.162(1) . . yes Ni(1) S(3) 2.163(1) . . yes Ni(1) S(4) 2.162(1) . . yes Ni(2) S(11) 2.164(1) . . yes Ni(2) S(12) 2.169(1) . . yes Ni(2) S(13) 2.161(1) . . yes Ni(2) S(14) 2.153(1) . . yes S(1) C(1) 1.694(4) . . yes S(2) C(2) 1.697(4) . . yes S(3) C(3) 1.698(4) . . yes S(4) C(4) 1.699(4) . . yes S(5) C(1) 1.748(4) . . yes S(5) C(5) 1.732(4) . . yes S(6) C(2) 1.737(4) . . yes S(6) C(5) 1.723(4) . . yes S(7) C(3) 1.745(4) . . yes S(7) C(6) 1.729(4) . . yes S(8) C(4) 1.737(4) . . yes S(8) C(6) 1.729(4) . . yes S(9) C(5) 1.652(4) . . yes S(10) C(6) 1.651(4) . . yes S(11) C(7) 1.713(4) . . yes S(12) C(8) 1.708(4) . . yes S(13) C(9) 1.685(4) . . yes S(14) C(10) 1.689(4) . . yes S(15) C(7) 1.735(4) . . yes S(15) C(11) 1.729(4) . . yes S(16) C(8) 1.737(4) . . yes S(16) C(11) 1.733(4) . . yes S(17) C(9) 1.737(4) . . yes S(17) C(12) 1.726(4) . . yes S(18) C(10) 1.733(4) . . yes S(18) C(12) 1.727(4) . . yes S(19) C(11) 1.647(4) . . yes S(20) C(12) 1.649(4) . . yes O(1) C(15) 1.407(6) . . yes O(1) C(16) 1.431(8) . . yes C(1) C(2) 1.382(5) . . yes C(3) C(4) 1.393(5) . . yes C(7) C(8) 1.377(5) . . yes C(9) C(10) 1.396(5) . . yes C(14) C(15) 1.518(7) . . yes C(16) C(17) 1.517(7) . . 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 C(13) Te(1) C(14) 101.2(3) . . . yes C(13) Te(1) C(17) 100.0(2) . . . yes C(14) Te(1) C(17) 94.4(2) . . . yes S(1) Ni(1) S(2) 93.03(5) . . . yes S(1) Ni(1) S(3) 88.61(4) . . . yes S(1) Ni(1) S(4) 178.03(4) . . . yes S(2) Ni(1) S(3) 178.25(4) . . . yes S(2) Ni(1) S(4) 85.41(4) . . . yes S(3) Ni(1) S(4) 92.97(4) . . . yes S(11) Ni(2) S(12) 93.53(4) . . . yes S(11) Ni(2) S(13) 87.53(4) . . . yes S(11) Ni(2) S(14) 175.68(5) . . . yes S(12) Ni(2) S(13) 178.86(5) . . . yes S(12) Ni(2) S(14) 86.38(4) . . . yes S(13) Ni(2) S(14) 92.60(5) . . . yes Ni(1) S(1) C(1) 101.6(1) . . . yes Ni(1) S(2) C(2) 102.4(1) . . . yes Ni(1) S(3) C(3) 102.5(1) . . . yes Ni(1) S(4) C(4) 102.7(1) . . . yes C(1) S(5) C(5) 97.9(2) . . . yes C(2) S(6) C(5) 97.6(2) . . . yes C(3) S(7) C(6) 97.5(2) . . . yes C(4) S(8) C(6) 97.5(2) . . . yes Ni(2) S(11) C(7) 101.9(1) . . . yes Ni(2) S(12) C(8) 101.8(1) . . . yes Ni(2) S(13) C(9) 102.9(1) . . . yes Ni(2) S(14) C(10) 103.1(1) . . . yes C(7) S(15) C(11) 97.6(2) . . . yes C(8) S(16) C(11) 97.5(2) . . . yes C(9) S(17) C(12) 97.1(2) . . . yes C(10) S(18) C(12) 96.9(2) . . . yes C(15) O(1) C(16) 112.7(4) . . . yes S(1) C(1) S(5) 123.4(2) . . . yes S(1) C(1) C(2) 121.9(3) . . . yes S(5) C(1) C(2) 114.7(3) . . . yes S(2) C(2) S(6) 122.5(2) . . . yes S(2) C(2) C(1) 121.0(3) . . . yes S(6) C(2) C(1) 116.5(3) . . . yes S(3) C(3) S(7) 123.6(2) . . . yes S(3) C(3) C(4) 121.1(3) . . . yes S(7) C(3) C(4) 115.3(3) . . . yes S(4) C(4) S(8) 123.4(2) . . . yes S(4) C(4) C(3) 120.7(3) . . . yes S(8) C(4) C(3) 115.9(3) . . . yes S(5) C(5) S(6) 113.4(2) . . . yes S(5) C(5) S(9) 124.0(2) . . . yes S(6) C(5) S(9) 122.6(2) . . . yes S(7) C(6) S(8) 113.8(2) . . . yes S(7) C(6) S(10) 124.1(2) . . . yes S(8) C(6) S(10) 122.1(2) . . . yes S(11) C(7) S(15) 122.8(2) . . . yes S(11) C(7) C(8) 121.2(3) . . . yes S(15) C(7) C(8) 116.0(3) . . . yes S(12) C(8) S(16) 122.7(2) . . . yes S(12) C(8) C(7) 121.5(3) . . . yes S(16) C(8) C(7) 115.7(3) . . . yes S(13) C(9) S(17) 123.8(2) . . . yes S(13) C(9) C(10) 120.8(3) . . . yes S(17) C(9) C(10) 115.4(3) . . . yes S(14) C(10) S(18) 123.3(2) . . . yes S(14) C(10) C(9) 120.6(3) . . . yes S(18) C(10) C(9) 116.1(3) . . . yes S(15) C(11) S(16) 113.2(2) . . . yes S(15) C(11) S(19) 123.1(2) . . . yes S(16) C(11) S(19) 123.7(3) . . . yes S(17) C(12) S(18) 114.5(2) . . . yes S(17) C(12) S(20) 123.3(2) . . . yes S(18) C(12) S(20) 122.3(2) . . . yes Te(1) C(14) C(15) 109.2(3) . . . yes O(1) C(15) C(14) 112.8(5) . . . yes O(1) C(16) C(17) 112.6(4) . . . yes Te(1) C(17) C(16) 109.5(3) . . . yes #------------------------------------------------------------------------------ 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 Te(1) C(14) C(15) O(1) 65.1(5) . . . . yes Te(1) C(17) C(16) O(1) -63.6(5) . . . . yes Ni(1) S(1) C(1) S(5) 179.6(2) . . . . yes Ni(1) S(1) C(1) C(2) -1.2(4) . . . . yes Ni(1) S(2) C(2) S(6) 179.8(2) . . . . yes Ni(1) S(2) C(2) C(1) -0.4(4) . . . . yes Ni(1) S(3) C(3) S(7) -179.9(2) . . . . yes Ni(1) S(3) C(3) C(4) 1.3(4) . . . . yes Ni(1) S(4) C(4) S(8) -178.5(2) . . . . yes Ni(1) S(4) C(4) C(3) 2.3(4) . . . . yes Ni(2) S(11) C(7) S(15) -176.2(2) . . . . yes Ni(2) S(11) C(7) C(8) 1.5(4) . . . . yes Ni(2) S(12) C(8) S(16) 178.3(2) . . . . yes Ni(2) S(12) C(8) C(7) 1.0(4) . . . . yes Ni(2) S(13) C(9) S(17) 178.8(2) . . . . yes Ni(2) S(13) C(9) C(10) -0.5(4) . . . . yes Ni(2) S(14) C(10) S(18) -178.7(2) . . . . yes Ni(2) S(14) C(10) C(9) 1.5(4) . . . . yes S(1) Ni(1) S(2) C(2) -0.2(2) . . . . yes S(1) Ni(1) S(3) C(3) 178.9(2) . . . . yes S(1) Ni(1) S(4) C(4) -144(1) . . . . yes S(1) C(1) S(5) C(5) 179.3(3) . . . . yes S(1) C(1) C(2) S(2) 1.2(5) . . . . yes S(1) C(1) C(2) S(6) -179.1(2) . . . . yes S(2) Ni(1) S(1) C(1) 0.7(2) . . . . yes S(2) Ni(1) S(3) C(3) -21(1) . . . . yes S(2) Ni(1) S(4) C(4) 178.2(2) . . . . yes S(2) C(2) S(6) C(5) 179.5(3) . . . . yes S(2) C(2) C(1) S(5) -179.6(2) . . . . yes S(3) Ni(1) S(1) C(1) -179.9(2) . . . . yes S(3) Ni(1) S(2) C(2) -159(1) . . . . yes S(3) Ni(1) S(4) C(4) -1.1(2) . . . . yes S(3) C(3) S(7) C(6) -178.2(3) . . . . yes S(3) C(3) C(4) S(4) -2.5(5) . . . . yes S(3) C(3) C(4) S(8) 178.2(2) . . . . yes S(4) Ni(1) S(1) C(1) -36(1) . . . . yes S(4) Ni(1) S(2) C(2) 178.6(2) . . . . yes S(4) Ni(1) S(3) C(3) 0.1(2) . . . . yes S(4) C(4) S(8) C(6) -178.9(3) . . . . yes S(4) C(4) C(3) S(7) 178.5(2) . . . . yes S(5) C(1) C(2) S(6) 0.2(4) . . . . yes S(5) C(5) S(6) C(2) 0.3(3) . . . . yes S(6) C(5) S(5) C(1) -0.2(3) . . . . yes S(7) C(3) C(4) S(8) -0.7(4) . . . . yes S(7) C(6) S(8) C(4) 0.2(3) . . . . yes S(8) C(6) S(7) C(3) -0.5(3) . . . . yes S(9) C(5) S(5) C(1) 177.8(3) . . . . yes S(9) C(5) S(6) C(2) -177.7(3) . . . . yes S(10) C(6) S(7) C(3) 179.7(3) . . . . yes S(10) C(6) S(8) C(4) -180.0(3) . . . . yes S(11) Ni(2) S(12) C(8) 0.0(2) . . . . yes S(11) Ni(2) S(13) C(9) -174.5(2) . . . . yes S(11) Ni(2) S(14) C(10) 90.2(6) . . . . yes S(11) C(7) S(15) C(11) 177.7(3) . . . . yes S(11) C(7) C(8) S(12) -1.8(5) . . . . yes S(11) C(7) C(8) S(16) -179.3(2) . . . . yes S(12) Ni(2) S(11) C(7) -0.6(2) . . . . yes S(12) Ni(2) S(13) C(9) 27(2) . . . . yes S(12) Ni(2) S(14) C(10) 179.1(2) . . . . yes S(12) C(8) S(16) C(11) -175.2(3) . . . . yes S(12) C(8) C(7) S(15) 176.1(2) . . . . yes S(13) Ni(2) S(11) C(7) 179.8(2) . . . . yes S(13) Ni(2) S(12) C(8) 158(2) . . . . yes S(13) Ni(2) S(14) C(10) -1.4(2) . . . . yes S(13) C(9) S(17) C(12) -180.0(3) . . . . yes S(13) C(9) C(10) S(14) -0.7(5) . . . . yes S(13) C(9) C(10) S(18) 179.5(2) . . . . yes S(14) Ni(2) S(11) C(7) 88.0(6) . . . . yes S(14) Ni(2) S(12) C(8) -175.7(2) . . . . yes S(14) Ni(2) S(13) C(9) 1.1(2) . . . . yes S(14) C(10) S(18) C(12) -179.4(3) . . . . yes S(14) C(10) C(9) S(17) 179.9(2) . . . . yes S(15) C(7) C(8) S(16) -1.4(5) . . . . yes S(15) C(11) S(16) C(8) -2.3(3) . . . . yes S(16) C(11) S(15) C(7) 1.7(3) . . . . yes S(17) C(9) C(10) S(18) 0.2(5) . . . . yes S(17) C(12) S(18) C(10) -0.8(3) . . . . yes S(18) C(12) S(17) C(9) 0.8(3) . . . . yes S(19) C(11) S(15) C(7) -177.9(3) . . . . yes S(19) C(11) S(16) C(8) 177.3(3) . . . . yes S(20) C(12) S(17) C(9) -179.3(3) . . . . yes S(20) C(12) S(18) C(10) 179.4(3) . . . . yes C(1) C(2) S(6) C(5) -0.3(4) . . . . yes C(2) C(1) S(5) C(5) 0.0(4) . . . . yes C(3) C(4) S(8) C(6) 0.3(4) . . . . yes C(4) C(3) S(7) C(6) 0.7(4) . . . . yes C(7) C(8) S(16) C(11) 2.3(4) . . . . yes C(8) C(7) S(15) C(11) -0.2(4) . . . . yes C(9) C(10) S(18) C(12) 0.4(4) . . . . yes C(10) C(9) S(17) C(12) -0.6(4) . . . . yes C(13) Te(1) C(14) C(15) -151.3(3) . . . . yes C(13) Te(1) C(17) C(16) 152.1(4) . . . . yes C(14) Te(1) C(17) C(16) 49.9(4) . . . . yes C(14) C(15) O(1) C(16) -73.1(6) . . . . yes C(15) O(1) C(16) C(17) 72.2(6) . . . . yes C(15) C(14) Te(1) C(17) -50.2(4) . . . . yes C(15) C(14) Te(1) C(17) -50.2(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 Te(1) S(9) 3.412(1) . 2_656 ? S(2) S(18) 3.563(2) . 2_566 ? S(2) S(14) 3.575(2) . 2_566 ? S(2) S(13) 3.591(2) . 1_554 ? S(3) S(13) 3.496(2) . 2_667 ? S(4) S(14) 3.555(2) . 2_566 ? S(4) S(17) 3.589(2) . 1_554 ? S(6) S(11) 3.499(1) . 1_554 ? S(14) S(14) 3.499(2) . 2_566 ? S(16) S(20) 3.514(2) . 2_567 ? S(20) C(16) 3.561(6) . 2_566 ? O(1) O(1) 3.373(8) . 2_555 ? O(1) C(16) 3.459(7) . 2_555 ? O(1) C(17) 3.473(6) . 2_555 ? C(1) C(3) 3.578(6) . 2_666 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------