Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_contact_author_name ' Kazuo Takimiya' _publ_contact_author_address ; Dr Kazuo Takimiya Department of Applied Chemistry Faculty of Engineering, Hiroshima University Higashi-Hiroshima 739-8527 JAPAN ; _publ_contact_author_email ' ktakimi@hiroshima-u.ac.jp ' _publ_contact_author_fax ' +81-824-22-7191 ' _publ_contact_author_phone ' +81-824-24-7734' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; Novel tellurium containing fulvalene-type electron donors, triselenatellurafulvalene (TSTeF) and diselenaditellurafulvalene (DSDTeF); synthesis, conductivities and crystal structures of their TCNQ complexes ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name 'Aso, Yoshio' 'Morikami, Atsushi' 'Otsubo, T.' 'Takimiya, Kazuo' _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. 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. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; data_TSTeF-TCNQ _database_code_CSD 164741 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jun 22 12:02:45 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source synthesized _chemical_name_common 'TSTeF-TCNQ' _chemical_formula_weight 644.77 _chemical_formula_analytical 'C18 H8 N4 Se3 Te1' _chemical_formula_sum 'C18 H8 N4 Se4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 12.633(3) _cell_length_b 3.901(3) _cell_length_c 18.557(2) _cell_angle_alpha 90 _cell_angle_beta 104.24(1) _cell_angle_gamma 90 _cell_volume 886.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 14.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560.00 _exptl_absorpt_coefficient_mu 8.289 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.47 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 0 6 0 0 4 -1 0 6 _diffrn_reflns_number 2110 _reflns_number_total 2022 _reflns_number_gt 1731 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.027 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05351 _diffrn_orient_matrix_UB_12 0.05405 _diffrn_orient_matrix_UB_13 0.03013 _diffrn_orient_matrix_UB_21 -0.06125 _diffrn_orient_matrix_UB_22 -0.01696 _diffrn_orient_matrix_UB_23 -0.04573 _diffrn_orient_matrix_UB_31 -0.00741 _diffrn_orient_matrix_UB_32 -0.25003 _diffrn_orient_matrix_UB_33 0.00961 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_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) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se(1) Se -0.15863(3) 0.1932(1) -0.09098(2) 0.0301(1) Uani 1.17 d P . . Se(2) Se 0.10376(3) 0.1958(1) -0.08162(2) 0.0287(1) Uani 1.10 d P . . N(1) N -0.6110(3) -0.079(1) -0.3107(2) 0.042(1) Uani 1.00 d . . . N(2) N -0.2591(3) -0.107(1) -0.3130(2) 0.040(1) Uani 1.00 d . . . C(1) C -0.0104(3) 0.073(1) -0.0339(2) 0.0226(10) Uani 1.00 d . . . C(2) C 0.0016(3) 0.359(1) -0.1683(2) 0.035(1) Uani 1.00 d . . . C(3) C -0.1033(3) 0.359(1) -0.1721(2) 0.036(1) Uani 1.00 d . . . C(4) C -0.6068(3) 0.6027(10) -0.5311(2) 0.0227(10) Uani 1.00 d . . . C(5) C -0.5859(3) 0.410(1) -0.4684(2) 0.0230(10) Uani 1.00 d . . . C(6) C -0.4773(3) 0.298(1) -0.4334(2) 0.0209(9) Uani 1.00 d . . . C(7) C -0.4548(3) 0.0974(10) -0.3693(2) 0.0228(10) Uani 1.00 d . . . C(8) C -0.5402(3) -0.001(1) -0.3353(2) 0.026(1) Uani 1.00 d . . . C(9) C -0.3466(3) -0.016(1) -0.3360(2) 0.025(1) Uani 1.00 d . . . H(1) H 0.0344 0.4307 -0.2042 0.0442 Uiso 1.00 calc . . . H(2) H -0.1498 0.4367 -0.2113 0.0446 Uiso 1.00 calc . . . H(3) H -0.6793 0.6782 -0.5571 0.0299 Uiso 1.00 calc . . . H(4) H -0.6411 0.3498 -0.4453 0.0297 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 Se(1) 0.0227(2) 0.0338(2) 0.0329(2) -0.0006(2) 0.0052(1) 0.0021(2) Se(2) 0.0226(2) 0.0326(2) 0.0308(2) 0.0018(2) 0.0066(1) 0.0036(2) N(1) 0.037(2) 0.056(3) 0.036(2) -0.008(2) 0.014(2) 0.005(2) N(2) 0.029(2) 0.053(3) 0.036(2) 0.007(2) 0.002(2) 0.006(2) C(1) 0.015(2) 0.026(2) 0.026(2) 0.001(2) 0.004(1) 0.003(2) C(2) 0.042(3) 0.040(3) 0.023(2) -0.002(2) 0.009(2) 0.004(2) C(3) 0.037(2) 0.039(3) 0.025(2) 0.005(2) -0.006(2) 0.003(2) C(4) 0.014(2) 0.026(2) 0.026(2) -0.001(2) 0.000(1) -0.001(2) C(5) 0.016(2) 0.030(2) 0.023(2) 0.000(2) 0.006(1) 0.002(2) C(6) 0.018(2) 0.024(2) 0.021(2) -0.002(2) 0.005(1) -0.003(2) C(7) 0.018(2) 0.025(2) 0.024(2) -0.001(2) 0.002(1) -0.002(2) C(8) 0.026(2) 0.030(2) 0.020(2) 0.003(2) 0.000(2) 0.003(2) C(9) 0.026(2) 0.028(2) 0.020(2) 0.000(2) 0.004(2) 0.002(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0080(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1731 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0215 _refine_ls_wR_factor_gt 0.0215 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.881 _refine_ls_shift/su_max 0.0177 _refine_ls_shift/su_mean 0.0039 _refine_diff_density_min -0.61 _refine_diff_density_max 0.47 #------------------------------------------------------------------------------ _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 Se(1) C(1) 1.967(3) 1_555 1_555 yes Se(1) C(3) 1.921(4) 1_555 1_555 yes Se(2) C(1) 1.929(3) 1_555 1_555 yes Se(2) C(2) 1.906(4) 1_555 1_555 yes N(1) C(8) 1.141(4) 1_555 1_555 yes N(2) C(9) 1.138(4) 1_555 1_555 yes C(1) C(1) 1.348(6) 1_555 3_555 yes C(2) C(3) 1.309(5) 1_555 1_555 yes C(2) H(1) 0.912 1_555 1_555 no C(3) H(2) 0.870 1_555 1_555 no C(4) C(5) 1.356(5) 1_555 1_555 yes C(4) C(6) 1.435(4) 1_555 3_464 yes C(4) H(3) 0.969 1_555 1_555 no C(5) C(6) 1.435(4) 1_555 1_555 yes C(5) H(4) 0.933 1_555 1_555 no C(6) C(7) 1.392(5) 1_555 1_555 yes C(7) C(8) 1.431(5) 1_555 1_555 yes C(7) C(9) 1.425(5) 1_555 1_555 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(1) Se(1) C(3) 91.2(1) 1_555 1_555 1_555 yes C(1) Se(2) C(2) 92.4(2) 1_555 1_555 1_555 yes Se(1) C(1) Se(2) 114.5(2) 1_555 1_555 1_555 yes Se(1) C(1) C(1) 123.0(3) 1_555 1_555 3_555 yes Se(2) C(1) C(1) 122.5(4) 1_555 1_555 3_555 yes Se(2) C(2) C(3) 120.8(3) 1_555 1_555 1_555 yes Se(2) C(2) H(1) 112.6(3) 1_555 1_555 1_555 no C(3) C(2) H(1) 126.5(4) 1_555 1_555 1_555 no Se(1) C(3) C(2) 121.0(3) 1_555 1_555 1_555 yes Se(1) C(3) H(2) 118.1(4) 1_555 1_555 1_555 no C(2) C(3) H(2) 120.9(4) 1_555 1_555 1_555 no C(5) C(4) C(6) 122.3(3) 1_555 1_555 3_464 yes C(5) C(4) H(3) 123.9(4) 1_555 1_555 1_555 no C(6) C(4) H(3) 113.8(3) 3_464 1_555 1_555 no C(4) C(5) C(6) 121.4(3) 1_555 1_555 1_555 yes C(4) C(5) H(4) 121.6(4) 1_555 1_555 1_555 no C(6) C(5) H(4) 117.0(3) 1_555 1_555 1_555 no C(4) C(6) C(5) 116.3(3) 3_464 1_555 1_555 yes C(4) C(6) C(7) 121.7(3) 3_464 1_555 1_555 yes C(5) C(6) C(7) 122.0(3) 1_555 1_555 1_555 yes C(6) C(7) C(8) 120.6(3) 1_555 1_555 1_555 yes C(6) C(7) C(9) 121.1(3) 1_555 1_555 1_555 yes C(8) C(7) C(9) 118.2(3) 1_555 1_555 1_555 yes N(1) C(8) C(7) 177.4(4) 1_555 1_555 1_555 yes N(2) C(9) C(7) 176.4(4) 1_555 1_555 1_555 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 Se(1) C(1) Se(2) C(2) -3.2(2) 1_555 1_555 1_555 1_555 yes Se(1) C(1) C(1) Se(1) 180.0 1_555 1_555 3_555 3_555 yes Se(1) C(1) C(1) Se(2) 1.9(7) 1_555 1_555 3_555 3_555 yes Se(1) C(3) C(2) Se(2) -0.5(6) 1_555 1_555 1_555 1_555 yes Se(2) C(1) Se(1) C(3) 3.0(2) 1_555 1_555 1_555 1_555 yes Se(2) C(1) C(1) Se(2) -180.0 1_555 1_555 3_555 3_555 yes N(1) C(8) C(7) C(6) 32(10) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(7) C(9) -147(10) 1_555 1_555 1_555 1_555 yes N(2) C(9) C(7) C(6) -30(7) 1_555 1_555 1_555 1_555 yes N(2) C(9) C(7) C(8) 148(7) 1_555 1_555 1_555 1_555 yes C(1) Se(1) C(3) C(2) -1.6(4) 1_555 1_555 1_555 1_555 yes C(1) Se(2) C(2) C(3) 2.3(4) 1_555 1_555 1_555 1_555 yes C(1) C(1) Se(1) C(3) 178.7(5) 1_555 3_555 3_555 3_555 yes C(1) C(1) Se(2) C(2) -178.5(5) 1_555 3_555 3_555 3_555 yes C(4) C(5) C(6) C(7) -179.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(6) C(7) C(8) 179.5(4) 1_555 3_464 3_464 3_464 yes C(4) C(6) C(7) C(9) -0.4(6) 1_555 3_464 3_464 3_464 yes C(5) C(4) C(6) C(7) -179.5(4) 1_555 1_555 3_464 3_464 yes C(5) C(6) C(7) C(8) -0.9(6) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(9) 179.0(4) 1_555 1_555 1_555 1_555 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 Se(1) N(1) 3.158(4) 1_555 2_454 ? Se(2) N(2) 3.187(3) 1_555 2_554 ? N(1) C(8) 3.339(5) 1_555 2_444 ? N(1) C(9) 3.365(5) 1_555 2_444 ? N(1) C(7) 3.476(5) 1_555 2_444 ? N(1) C(3) 3.552(5) 1_555 2_444 ? N(2) C(2) 3.359(5) 1_555 2_544 ? N(2) C(3) 3.390(5) 1_555 1_555 ? N(2) C(3) 3.539(5) 1_555 1_545 ? N(2) C(4) 3.545(5) 1_555 3_454 ? C(1) C(1) 3.544(8) 1_555 3_565 ? C(2) C(2) 3.599(6) 1_555 2_554 ? C(2) C(2) 3.599(6) 1_555 2_544 ? C(4) C(9) 3.309(5) 1_555 3_454 ? C(4) C(5) 3.345(5) 1_555 1_565 ? C(4) C(6) 3.444(5) 1_555 1_565 ? C(4) C(7) 3.491(5) 1_555 3_454 ? C(5) C(8) 3.319(5) 1_555 1_565 ? C(5) C(7) 3.438(5) 1_555 1_565 ? C(5) C(6) 3.506(5) 1_555 3_454 ? C(6) C(7) 3.325(5) 1_555 1_565 ? C(6) C(6) 3.338(7) 1_555 3_454 ? C(6) C(9) 3.418(5) 1_555 1_565 ? C(6) C(8) 3.485(5) 1_555 1_565 ? #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; All the chalcogen atoms were supposed to be Se, and the occupancies of Se atoms were included in the LS calculation under the constraint of the following equation. Se(2) occ = 2.265 - Se(1) occ ; #===END data_DSDTeF-TCNQ _database_code_CSD 164742 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jun 22 12:00:15 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source synthesized _chemical_name_common 'DSDTeF-TCNQ' _chemical_formula_weight 693.41 _chemical_formula_analytical 'C18 H8 N4 Se2 Te2' _chemical_formula_sum 'C18 H8 N4 Se2 Te2 ' _chemical_formula_moiety '?' _chemical_formula_structural 'C18 H8 N4 Se2 Te2' _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.271(3) _cell_length_b 16.735(9) _cell_length_c 3.876(2) _cell_angle_alpha 96.38(5) _cell_angle_beta 98.17(4) _cell_angle_gamma 87.04(4) _cell_volume 463.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 2.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316.00 _exptl_absorpt_coefficient_mu 7.083 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.949 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.68 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 1 1 0 0 1 -2 5 0 _diffrn_reflns_number 2266 _reflns_number_total 2107 _reflns_number_gt 1726 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_av_sigmaI/netI 0.038 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02709 _diffrn_orient_matrix_UB_12 0.05665 _diffrn_orient_matrix_UB_13 0.09801 _diffrn_orient_matrix_UB_21 -0.13434 _diffrn_orient_matrix_UB_22 0.01589 _diffrn_orient_matrix_UB_23 -0.05876 _diffrn_orient_matrix_UB_31 -0.02350 _diffrn_orient_matrix_UB_32 -0.01257 _diffrn_orient_matrix_UB_33 0.23588 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_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) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;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) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te(1) Te -0.2863(1) 0.38614(4) 0.2028(2) 0.0372(2) Uani 1.00 d . . . Se(1) Se -0.7490(2) 0.42156(7) 0.0536(3) 0.0357(3) Uani 1.00 d . . . N(1) N 0.951(1) 0.2484(5) 0.512(3) 0.049(3) Uani 1.00 d . . . N(2) N 1.476(1) 0.1224(6) 0.540(3) 0.050(3) Uani 1.00 d . . . C(1) C -0.509(1) 0.4623(5) 0.050(3) 0.029(3) Uani 1.00 d . . . C(2) C -0.479(2) 0.3021(6) 0.231(3) 0.042(4) Uani 1.00 d . . . C(3) C -0.654(2) 0.3200(7) 0.174(3) 0.042(3) Uani 1.00 d . . . C(4) C 0.884(1) 0.0666(6) 0.916(3) 0.030(3) Uani 1.00 d . . . C(5) C 1.074(1) 0.0621(5) 0.848(2) 0.025(3) Uani 1.00 d . . . C(6) C 1.184(1) -0.0066(6) 0.935(3) 0.027(3) Uani 1.00 d . . . C(7) C 1.143(1) 0.1238(6) 0.690(3) 0.029(3) Uani 1.00 d . . . C(8) C 1.031(1) 0.1930(6) 0.589(3) 0.033(3) Uani 1.00 d . . . C(9) C 1.329(1) 0.1219(6) 0.608(3) 0.032(3) Uani 1.00 d . . . H(1) H -0.4387 0.2507 0.2923 0.0549 Uiso 1.00 calc . . . H(2) H -0.7400 0.2798 0.1911 0.0495 Uiso 1.00 calc . . . H(3) H 0.8056 0.1113 0.8538 0.0357 Uiso 1.00 calc . . . H(4) H 1.3082 -0.0125 0.8876 0.0333 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) 0.0426(5) 0.0310(4) 0.0405(5) 0.0035(3) 0.0104(3) 0.0110(3) Se(1) 0.0358(7) 0.0343(6) 0.0399(7) -0.0026(5) 0.0074(5) 0.0134(5) N(1) 0.052(7) 0.030(5) 0.068(7) 0.011(5) 0.014(5) 0.019(5) N(2) 0.038(6) 0.048(6) 0.068(7) -0.001(5) 0.009(5) 0.021(5) C(1) 0.036(6) 0.023(5) 0.028(5) 0.009(4) 0.011(4) 0.006(4) C(2) 0.055(8) 0.026(6) 0.048(7) -0.006(5) 0.008(6) 0.014(5) C(3) 0.044(7) 0.039(7) 0.044(7) -0.016(5) 0.000(6) 0.009(5) C(4) 0.027(5) 0.021(5) 0.040(6) 0.002(4) -0.003(5) 0.008(4) C(5) 0.024(5) 0.022(5) 0.030(5) 0.001(4) 0.000(4) 0.007(4) C(6) 0.024(5) 0.025(5) 0.035(6) 0.002(4) 0.006(4) 0.010(4) C(7) 0.022(5) 0.034(6) 0.030(6) -0.002(4) -0.004(4) 0.012(4) C(8) 0.031(6) 0.024(5) 0.046(7) 0.000(5) 0.009(5) 0.009(5) C(9) 0.032(6) 0.029(6) 0.034(6) -0.001(5) -0.005(5) 0.012(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1726 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 4.118 _refine_ls_shift/su_max 3.4516 _refine_ls_shift/su_mean 0.0309 _refine_diff_density_min -1.37 _refine_diff_density_max 2.60 #------------------------------------------------------------------------------ _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(1) 2.069(10) 1_555 1_555 yes Te(1) C(2) 2.06(1) 1_555 1_555 yes Se(1) C(1) 1.91(1) 1_555 1_555 yes Se(1) C(3) 1.88(1) 1_555 1_555 yes N(1) C(8) 1.12(1) 1_555 1_555 yes N(2) C(9) 1.14(1) 1_555 1_555 yes C(1) C(1) 1.38(2) 1_555 2_465 yes C(2) C(3) 1.28(2) 1_555 1_555 yes C(2) H(1) 0.940 1_555 1_555 no C(3) H(2) 0.956 1_555 1_555 no C(4) C(5) 1.44(1) 1_555 1_555 yes C(4) C(6) 1.36(1) 1_555 2_757 yes C(4) H(3) 0.950 1_555 1_555 no C(5) C(6) 1.41(1) 1_555 1_555 yes C(5) C(7) 1.40(1) 1_555 1_555 yes C(6) H(4) 0.947 1_555 1_555 no C(7) C(8) 1.44(1) 1_555 1_555 yes C(7) C(9) 1.43(1) 1_555 1_555 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(1) Te(1) C(2) 86.8(4) 1_555 1_555 1_555 yes C(1) Se(1) C(3) 93.8(4) 1_555 1_555 1_555 yes Te(1) C(1) Se(1) 115.5(4) 1_555 1_555 1_555 yes Te(1) C(1) C(1) 123(1) 1_555 1_555 2_465 yes Se(1) C(1) C(1) 120(1) 1_555 1_555 2_465 yes Te(1) C(2) C(3) 120.5(8) 1_555 1_555 1_555 yes Te(1) C(2) H(1) 119.4(10) 1_555 1_555 1_555 no C(3) C(2) H(1) 120(1) 1_555 1_555 1_555 no Se(1) C(3) C(2) 123.1(9) 1_555 1_555 1_555 yes Se(1) C(3) H(2) 118.4(10) 1_555 1_555 1_555 no C(2) C(3) H(2) 118(1) 1_555 1_555 1_555 no C(5) C(4) C(6) 120.2(9) 1_555 1_555 2_757 yes C(5) C(4) H(3) 120.0(9) 1_555 1_555 1_555 no C(6) C(4) H(3) 119(1) 2_757 1_555 1_555 no C(4) C(5) C(6) 117.7(8) 1_555 1_555 1_555 yes C(4) C(5) C(7) 119.9(8) 1_555 1_555 1_555 yes C(6) C(5) C(7) 122.3(9) 1_555 1_555 1_555 yes C(4) C(6) C(5) 122.0(9) 2_757 1_555 1_555 yes C(4) C(6) H(4) 117.8(9) 2_757 1_555 1_555 no C(5) C(6) H(4) 120.1(9) 1_555 1_555 1_555 no C(5) C(7) C(8) 123.0(9) 1_555 1_555 1_555 yes C(5) C(7) C(9) 122.7(9) 1_555 1_555 1_555 yes C(8) C(7) C(9) 114.3(9) 1_555 1_555 1_555 yes N(1) C(8) C(7) 177(1) 1_555 1_555 1_555 yes N(2) C(9) C(7) 178(1) 1_555 1_555 1_555 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(1) Se(1) C(3) -4.4(6) 1_555 1_555 1_555 1_555 yes Te(1) C(1) C(1) Te(1) -180.0 1_555 1_555 2_465 2_465 yes Te(1) C(1) C(1) Se(1) 0(1) 1_555 1_555 2_465 2_465 yes Te(1) C(2) C(3) Se(1) 0(1) 1_555 1_555 1_555 1_555 yes Se(1) C(1) Te(1) C(2) 4.5(5) 1_555 1_555 1_555 1_555 yes Se(1) C(1) C(1) Se(1) 180.0 1_555 1_555 2_465 2_465 yes N(1) C(8) C(7) C(5) 150(25) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(7) C(9) -31(25) 1_555 1_555 1_555 1_555 yes N(2) C(9) C(7) C(5) -169(40) 1_555 1_555 1_555 1_555 yes N(2) C(9) C(7) C(8) 12(41) 1_555 1_555 1_555 1_555 yes C(1) Te(1) C(2) C(3) -3(1) 1_555 1_555 1_555 1_555 yes C(1) Se(1) C(3) C(2) 2(1) 1_555 1_555 1_555 1_555 yes C(1) C(1) Te(1) C(2) 175(1) 1_555 2_465 2_465 2_465 yes C(1) C(1) Se(1) C(3) -175(1) 1_555 2_465 2_465 2_465 yes C(4) C(5) C(7) C(8) 0(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(7) C(9) -178.3(9) 1_555 1_555 1_555 1_555 yes C(4) C(6) C(5) C(7) 179.1(10) 1_555 2_757 2_757 2_757 yes C(6) C(4) C(5) C(7) -179.2(10) 1_555 2_757 2_757 2_757 yes C(6) C(5) C(7) C(8) 177.7(10) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(7) C(9) 0(1) 1_555 1_555 1_555 1_555 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) N(1) 3.058(9) 1_555 1_455 ? N(1) C(2) 3.28(2) 1_555 1_655 ? N(2) C(4) 3.25(1) 1_555 1_655 ? N(2) C(2) 3.40(1) 1_555 1_755 ? N(2) C(6) 3.55(1) 1_555 1_554 ? C(1) C(1) 3.56(2) 1_555 2_466 ? C(3) C(8) 3.58(2) 1_555 1_354 ? C(4) C(8) 3.26(1) 1_555 1_556 ? C(4) C(6) 3.31(1) 1_555 2_756 ? C(4) C(7) 3.38(1) 1_555 1_556 ? C(4) C(5) 3.50(1) 1_555 2_756 ? C(5) C(7) 3.29(1) 1_555 1_556 ? C(5) C(5) 3.31(2) 1_555 2_756 ? C(5) C(9) 3.33(1) 1_555 1_556 ? C(5) C(6) 3.40(1) 1_555 2_756 ? C(5) C(8) 3.45(1) 1_555 1_556 ? C(6) C(9) 3.28(1) 1_555 1_556 ? C(6) C(7) 3.49(1) 1_555 1_556 ? #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #===END data_DSDTeF(neutral) _database_code_CSD 164743 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jun 22 11:53:57 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source synthesized _chemical_name_common DSDTeF _chemical_formula_weight 489.22 _chemical_formula_analytical 'C6 H4 Se2 Te2' _chemical_formula_sum 'C6 H4 Se2 Te2 ' _chemical_formula_moiety 'C6 H4 Se2 Te2' _chemical_formula_structural 'C6 H4 Se2 Te2' _chemical_melting_point 139-140C #------------------------------------------------------------------------------ _cell_length_a 9.088(3) _cell_length_b 10.845(3) _cell_length_c 8.875(3) _cell_angle_alpha 106.46(3) _cell_angle_beta 109.79(3) _cell_angle_gamma 104.14(3) _cell_volume 731.1(5) _cell_formula_units_Z 3 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 3.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636.00 _exptl_absorpt_coefficient_mu 13.385 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.707 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -5.69 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 -1 -2 2 -2 -1 2 -2 _diffrn_reflns_number 3527 _reflns_number_total 3318 _reflns_number_gt 2902 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03580 _diffrn_orient_matrix_UB_12 -0.03305 _diffrn_orient_matrix_UB_13 -0.12880 _diffrn_orient_matrix_UB_21 -0.09360 _diffrn_orient_matrix_UB_22 -0.08325 _diffrn_orient_matrix_UB_23 -0.02028 _diffrn_orient_matrix_UB_31 -0.07681 _diffrn_orient_matrix_UB_32 0.05249 _diffrn_orient_matrix_UB_33 -0.00951 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Te' 'Te' -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Se' 'Se' -0.093 2.226 ;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) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te(1) Te 0.57057(7) 0.82089(6) 0.42721(8) 0.0519(2) Uani 0.93 d P . . Te(2) Te 0.19728(8) 0.43640(7) 0.49062(9) 0.0510(2) Uani 0.89 d P . . Te(3) Te 0.84996(9) 1.16095(7) 1.47491(9) 0.0521(2) Uani 0.86 d P . . Se(1) Se 0.20139(9) 0.55492(8) 0.16331(9) 0.0501(2) Uani 1.11 d P . . Se(2) Se 0.5747(1) 0.70404(8) 0.76518(9) 0.0560(2) Uani 1.17 d P . . Se(3) Se 0.9381(1) 0.94055(9) 1.19542(10) 0.0639(3) Uani 1.22 d P . . C(1) C 0.3870(8) 0.6484(7) 0.3995(9) 0.035(2) Uani 1.00 d . . . C(2) C 0.245(1) 0.7235(9) 0.124(1) 0.054(2) Uani 1.00 d . . . C(3) C 0.389(1) 0.8313(8) 0.225(1) 0.052(2) Uani 1.00 d . . . C(4) C 0.3874(8) 0.6060(7) 0.5258(8) 0.032(2) Uani 1.00 d . . . C(5) C 0.439(1) 0.605(1) 0.856(1) 0.060(3) Uani 1.00 d . . . C(6) C 0.295(1) 0.504(1) 0.755(1) 0.060(3) Uani 1.00 d . . . C(7) C 0.9604(8) 1.0198(7) 1.4379(9) 0.034(2) Uani 1.00 d . . . C(8) C 0.818(2) 1.053(1) 1.124(1) 0.079(3) Uani 1.00 d . . . C(9) C 0.779(1) 1.136(1) 1.229(1) 0.075(3) Uani 1.00 d . . . H(1) H 0.1631 0.7313 0.0329 0.0666 Uiso 1.00 calc . . . H(2) H 0.4076 0.9132 0.2037 0.0632 Uiso 1.00 calc . . . H(3) H 0.4808 0.6340 0.9801 0.0703 Uiso 1.00 calc . . . H(4) H 0.2348 0.4589 0.8038 0.0786 Uiso 1.00 calc . . . H(5) H 0.7874 1.0498 1.0096 0.0947 Uiso 1.00 calc . . . H(6) H 0.7157 1.1866 1.1851 0.0901 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) 0.0446(3) 0.0484(3) 0.0622(4) 0.0128(3) 0.0176(3) 0.0330(3) Te(2) 0.0546(4) 0.0620(4) 0.0605(4) 0.0291(3) 0.0360(3) 0.0381(3) Te(3) 0.0599(4) 0.0562(4) 0.0616(4) 0.0309(3) 0.0354(3) 0.0347(3) Se(1) 0.0522(4) 0.0540(5) 0.0383(4) 0.0169(3) 0.0109(3) 0.0244(3) Se(2) 0.0659(5) 0.0693(5) 0.0408(4) 0.0359(4) 0.0221(3) 0.0259(4) Se(3) 0.0799(6) 0.0838(6) 0.0509(4) 0.0525(5) 0.0309(4) 0.0371(4) C(1) 0.029(3) 0.043(4) 0.036(4) 0.015(3) 0.012(3) 0.020(3) C(2) 0.070(6) 0.059(5) 0.046(4) 0.036(4) 0.020(4) 0.035(4) C(3) 0.064(5) 0.048(4) 0.047(4) 0.021(4) 0.018(4) 0.030(4) C(4) 0.037(3) 0.034(3) 0.030(3) 0.018(3) 0.015(3) 0.014(3) C(5) 0.088(7) 0.073(6) 0.041(4) 0.042(5) 0.039(5) 0.029(4) C(6) 0.081(6) 0.077(6) 0.054(5) 0.042(5) 0.045(5) 0.040(5) C(7) 0.037(3) 0.036(3) 0.038(4) 0.018(3) 0.020(3) 0.019(3) C(8) 0.115(9) 0.073(6) 0.052(6) 0.045(6) 0.021(6) 0.039(5) C(9) 0.094(8) 0.075(7) 0.068(6) 0.059(6) 0.023(6) 0.036(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00005|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0033(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2923 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_number_constraints 3 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0437 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.157 _refine_ls_shift/su_max 0.1420 _refine_ls_shift/su_mean 0.0354 _refine_diff_density_min -1.00 _refine_diff_density_max 1.24 #------------------------------------------------------------------------------ _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(1) 2.069(7) 1_555 1_555 yes Te(1) C(3) 2.040(8) 1_555 1_555 yes Te(2) C(4) 2.055(7) 1_555 1_555 yes Te(2) C(6) 2.031(9) 1_555 1_555 yes Te(3) C(7) 2.036(7) 1_555 1_555 yes Te(3) C(9) 1.97(1) 1_555 1_555 yes Se(1) C(1) 1.958(6) 1_555 1_555 yes Se(1) C(2) 1.928(8) 1_555 1_555 yes Se(2) C(4) 1.982(6) 1_555 1_555 yes Se(2) C(5) 1.963(9) 1_555 1_555 yes Se(3) C(7) 1.996(7) 1_555 1_555 yes Se(3) C(8) 1.92(1) 1_555 1_555 yes C(1) C(4) 1.326(9) 1_555 1_555 yes C(2) C(3) 1.32(1) 1_555 1_555 yes C(2) H(1) 0.938 1_555 1_555 no C(2) H(2) 1.974 1_555 1_555 no C(3) H(1) 1.946 1_555 1_555 no C(3) H(2) 0.948 1_555 1_555 no C(5) C(6) 1.29(1) 1_555 1_555 yes C(5) H(3) 0.956 1_555 1_555 no C(5) H(4) 1.930 1_555 1_555 no C(6) H(3) 1.946 1_555 1_555 no C(6) H(4) 0.938 1_555 1_555 no C(7) C(7) 1.34(1) 1_555 2_778 yes C(8) C(9) 1.30(1) 1_555 1_555 yes C(8) H(5) 0.948 1_555 1_555 no C(8) H(6) 1.950 1_555 1_555 no C(9) H(5) 1.941 1_555 1_555 no C(9) H(6) 0.952 1_555 1_555 no #------------------------------------------------------------------------------ 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(1) Te(1) C(3) 87.5(3) 1_555 1_555 1_555 yes C(4) Te(2) C(6) 87.9(3) 1_555 1_555 1_555 yes C(7) Te(3) C(9) 89.9(3) 1_555 1_555 1_555 yes C(1) Se(1) C(2) 91.9(3) 1_555 1_555 1_555 yes C(4) Se(2) C(5) 91.0(3) 1_555 1_555 1_555 yes C(7) Se(3) C(8) 91.7(4) 1_555 1_555 1_555 yes Te(1) C(1) Se(1) 112.3(3) 1_555 1_555 1_555 yes Te(1) C(1) C(4) 125.4(5) 1_555 1_555 1_555 yes Se(1) C(1) C(4) 122.3(5) 1_555 1_555 1_555 yes Se(1) C(2) C(3) 121.6(6) 1_555 1_555 1_555 yes Se(1) C(2) H(1) 120.3(7) 1_555 1_555 1_555 no Se(1) C(2) H(2) 146.1(4) 1_555 1_555 1_555 no C(3) C(2) H(1) 118.1(8) 1_555 1_555 1_555 no C(3) C(2) H(2) 24.5(4) 1_555 1_555 1_555 no H(1) C(2) H(2) 93.6(6) 1_555 1_555 1_555 no Te(1) C(3) C(2) 119.8(6) 1_555 1_555 1_555 yes Te(1) C(3) H(1) 145.0(4) 1_555 1_555 1_555 no Te(1) C(3) H(2) 120.0(7) 1_555 1_555 1_555 no C(2) C(3) H(1) 25.2(4) 1_555 1_555 1_555 no C(2) C(3) H(2) 120.2(8) 1_555 1_555 1_555 no H(1) C(3) H(2) 95.1(6) 1_555 1_555 1_555 no Te(2) C(4) Se(2) 115.0(3) 1_555 1_555 1_555 yes Te(2) C(4) C(1) 123.3(5) 1_555 1_555 1_555 yes Se(2) C(4) C(1) 121.7(5) 1_555 1_555 1_555 yes Se(2) C(5) C(6) 122.2(6) 1_555 1_555 1_555 yes Se(2) C(5) H(3) 118.3(8) 1_555 1_555 1_555 no Se(2) C(5) H(4) 147.3(5) 1_555 1_555 1_555 no C(6) C(5) H(3) 119.5(9) 1_555 1_555 1_555 no C(6) C(5) H(4) 25.1(4) 1_555 1_555 1_555 no H(3) C(5) H(4) 94.5(6) 1_555 1_555 1_555 no Te(2) C(6) C(5) 121.8(7) 1_555 1_555 1_555 yes Te(2) C(6) H(3) 147.1(5) 1_555 1_555 1_555 no Te(2) C(6) H(4) 118.8(8) 1_555 1_555 1_555 no C(5) C(6) H(3) 25.3(4) 1_555 1_555 1_555 no C(5) C(6) H(4) 119.4(9) 1_555 1_555 1_555 no H(3) C(6) H(4) 94.1(6) 1_555 1_555 1_555 no Te(3) C(7) Se(3) 113.9(3) 1_555 1_555 1_555 yes Te(3) C(7) C(7) 124.2(7) 1_555 1_555 2_778 yes Se(3) C(7) C(7) 121.8(7) 1_555 1_555 2_778 yes Se(3) C(8) C(9) 122.6(7) 1_555 1_555 1_555 yes Se(3) C(8) H(5) 119.0(9) 1_555 1_555 1_555 no Se(3) C(8) H(6) 147.9(6) 1_555 1_555 1_555 no C(9) C(8) H(5) 118(1) 1_555 1_555 1_555 no C(9) C(8) H(6) 25.3(5) 1_555 1_555 1_555 no H(5) C(8) H(6) 93.1(7) 1_555 1_555 1_555 no Te(3) C(9) C(8) 121.8(7) 1_555 1_555 1_555 yes Te(3) C(9) H(5) 147.1(5) 1_555 1_555 1_555 no Te(3) C(9) H(6) 119.3(8) 1_555 1_555 1_555 no C(8) C(9) H(5) 25.4(5) 1_555 1_555 1_555 no C(8) C(9) H(6) 118(1) 1_555 1_555 1_555 no H(5) C(9) H(6) 93.5(7) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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(1) Se(1) C(2) -25.2(4) 1_555 1_555 1_555 1_555 yes Te(1) C(1) C(4) Te(2) 178.3(3) 1_555 1_555 1_555 1_555 yes Te(1) C(1) C(4) Se(2) -1.6(9) 1_555 1_555 1_555 1_555 yes Te(1) C(3) C(2) Se(1) 0(1) 1_555 1_555 1_555 1_555 yes Te(2) C(4) Se(2) C(5) -13.8(4) 1_555 1_555 1_555 1_555 yes Te(2) C(4) C(1) Se(1) 0.9(8) 1_555 1_555 1_555 1_555 yes Te(2) C(6) C(5) Se(2) 0(1) 1_555 1_555 1_555 1_555 yes Te(3) C(7) Se(3) C(8) 1.1(5) 1_555 1_555 1_555 1_555 yes Te(3) C(7) C(7) Te(3) -180.0 1_555 1_555 2_778 2_778 yes Te(3) C(7) C(7) Se(3) -1(1) 1_555 1_555 2_778 2_778 yes Te(3) C(9) C(8) Se(3) 2(1) 1_555 1_555 1_555 1_555 yes Se(1) C(1) Te(1) C(3) 24.6(4) 1_555 1_555 1_555 1_555 yes Se(1) C(1) C(4) Se(2) -178.9(3) 1_555 1_555 1_555 1_555 yes Se(2) C(4) Te(2) C(6) 13.8(4) 1_555 1_555 1_555 1_555 yes Se(3) C(7) Te(3) C(9) -0.2(5) 1_555 1_555 1_555 1_555 yes Se(3) C(7) C(7) Se(3) 180.0 1_555 1_555 2_778 2_778 yes C(1) Te(1) C(3) C(2) -15.6(8) 1_555 1_555 1_555 1_555 yes C(1) Se(1) C(2) C(3) 16.0(8) 1_555 1_555 1_555 1_555 yes C(1) C(4) Te(2) C(6) -166.1(6) 1_555 1_555 1_555 1_555 yes C(1) C(4) Se(2) C(5) 166.1(6) 1_555 1_555 1_555 1_555 yes C(2) Se(1) C(1) C(4) 152.5(6) 1_555 1_555 1_555 1_555 yes C(3) Te(1) C(1) C(4) -153.0(7) 1_555 1_555 1_555 1_555 yes C(4) Te(2) C(6) C(5) -9.0(8) 1_555 1_555 1_555 1_555 yes C(4) Se(2) C(5) C(6) 8.4(9) 1_555 1_555 1_555 1_555 yes C(7) Te(3) C(9) C(8) -1(1) 1_555 1_555 1_555 1_555 yes C(7) Se(3) C(8) C(9) -2(1) 1_555 1_555 1_555 1_555 yes C(7) C(7) Te(3) C(9) 179.2(9) 1_555 2_778 2_778 2_778 yes C(7) C(7) Se(3) C(8) 179.9(9) 1_555 2_778 2_778 2_778 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(3) C(1) 3.556(7) 1_555 2_677 ? Se(1) Se(1) 3.457(2) 1_555 2_565 ? C(2) C(5) 3.56(1) 1_555 1_554 ? C(4) C(4) 3.47(1) 1_555 2_666 ? #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; The occupancies of Se and Te atoms were refined under the following constraints. Se(n) occ = [86 - 52 x Te(n) occ] / 34, n = 1, 2, 3 ; #===END