Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email GR@SOTON.AC.UK _publ_contact_author_name 'Dr Gillian Reid' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2003-01-20 _audit_creation_method 'by teXsan for Windows v1.06' _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; loop_ _publ_author_name G.Reid M.J.Hesford W.Levason M.L.Matthews S.D.Orchard data_tesn_1-thia-4-telluracyclohexane _database_code_CSD 206527 _audit_creation_method 'SHELXL-97 + hand edit' _chemical_name_systematic ; 1-thia-4-tellurocyclohexane ; _chemical_formula_moiety 'C4 H8 S Te' _chemical_formula_sum 'C4 H8 S Te' _chemical_formula_weight 215.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 7.020(2) _cell_length_b 5.6344(15) _cell_length_c 8.009(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.635(10) _cell_angle_gamma 90.00 _cell_volume 316.13(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1386 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 200 _exptl_absorpt_coefficient_mu 4.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'PLATON, A L Spek, Acta Cryst., Sect. A, 1990, 46, C34.' _exptl_absorpt_correction_T_min 0.2149 # shelxl 0.2576 _exptl_absorpt_correction_T_max 0.2794 # shelxl 0.4897 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1829 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.41 _reflns_number_total 706 _reflns_number_gt 650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Te1 and S1 are disordered on the same site and given the same adp values. H atoms in calc positions but at the end they were fixed and the common adp not refined (due to problems getting bond lengths etc). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.120P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 706 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.22738(3) 0.17201(4) 0.04746(3) 0.02871(17) Uani 0.50 d P . . Te1 Te 0.22738(3) 0.17201(4) 0.04746(3) 0.02871(17) Uani 0.50 d P . . C1 C -0.0133(5) 0.1831(4) 0.1609(4) 0.0366(7) Uani 1 d . . . C2 C 0.1912(4) -0.1495(5) -0.0505(4) 0.0363(7) Uani 1 d . . . H1A H -0.0090 0.0585 0.2483 0.059 Uiso 1 calc . . . H1B H -0.0211 0.3383 0.2179 0.059 Uiso 1 calc . . . H2A H 0.3024 -0.1862 -0.1163 0.059 Uiso 1 calc . . . H2B H 0.1908 -0.2661 0.0420 0.059 Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0243(2) 0.0256(2) 0.0363(2) -0.00355(9) 0.00278(15) -0.00492(8) Te1 0.0243(2) 0.0256(2) 0.0363(2) -0.00355(9) 0.00278(15) -0.00492(8) C1 0.062(2) 0.0236(14) 0.0240(14) -0.0076(9) -0.0016(14) 0.0039(11) C2 0.0291(16) 0.0402(16) 0.0408(17) 0.0056(12) 0.0105(13) 0.0152(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Te1 and S1 are disordered and occupy the same position. The bond lengths and angles involving Te1 and S1 are therefore some sort of average value. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.969(4) . ? S1 C2 1.984(3) . ? Te1 C1 1.969(4) . ? Te1 C2 1.984(3) . ? C1 C2 1.496(5) 3 ? C1 H1A 0.9898 . ? C1 H1B 0.9897 . ? C2 C1 1.496(5) 3 ? C2 H2A 0.9905 . ? C2 H2B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 96.86(12) . . ? C1 Te1 C2 96.86(12) . . ? C2 C1 S1 115.6(2) 3 . ? C2 C1 Te1 115.6(2) 3 . ? C2 C1 H1A 108.4 3 . ? S1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 3 . ? S1 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C1 C2 S1 115.48(18) 3 . ? C1 C2 Te1 115.48(18) 3 . ? C1 C2 H2A 108.4 3 . ? S1 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 3 . ? S1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? 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 C2 S1 C1 C2 -57.5(2) . . . 3 ? C1 S1 C2 C1 57.4(3) . . . 3 ? C2 Te1 C1 C2 -57.5(2) . . . 3 ? C1 Te1 C2 C1 57.4(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.538 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.137 # === END OF CIF ================================== data__02mlm003 _database_code_CSD 206528 _audit_creation_date 2002-10-24 _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 7.7448(3) _cell_length_b 5.5407(3) _cell_length_c 13.7720(4) _cell_angle_alpha 90 _cell_angle_beta 94.666(2) _cell_angle_gamma 90 _cell_volume 589.02(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour 'pale needle' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 317.96 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H18 S2 Te ' _chemical_formula_moiety 'C9 H18 S2 Te ' _chemical_formula_structural [12]aneS2Te _chemical_compound_source ? _exptl_crystal_F_000 312.00 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multiscan _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max. and min. transmission factors: 0.38029, 0.33757. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Mercury CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4147 _reflns_number_total 1479 _reflns_number_gt 1437 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04867 _diffrn_reflns_av_sigmaI/netI 0.069 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 18 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 36 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 4 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Te 0 2 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Te(1) -0.01102(3) -0.4999 -0.10715(2) 0.01870(9) 1.000 . Uani d ? S(1) -0.6179(2) -0.1567(3) -0.21978(10) 0.0257(3) 1.000 . Uani d ? S(2) -0.2066(2) -0.5185(4) -0.43352(8) 0.0215(3) 1.000 . Uani d ? C(1) -0.2612(7) -0.5989(11) -0.0601(3) 0.0235(13) 1.000 . Uani d ? C(2) -0.4151(6) -0.523(2) -0.1290(4) 0.0212(13) 1.000 . Uani d ? C(3) -0.4421(7) -0.2533(11) -0.1334(4) 0.0235(13) 1.000 . Uani d ? C(4) -0.5388(7) -0.2523(11) -0.3346(4) 0.0222(13) 1.000 . Uani d ? C(5) -0.3756(7) -0.1230(10) -0.3579(4) 0.0220(13) 1.000 . Uani d ? C(6) -0.2998(7) -0.2200(11) -0.4490(4) 0.026(1) 1.000 . Uani d ? C(7) -0.0041(6) -0.4466(9) -0.3633(3) 0.0182(13) 1.000 . Uani d ? C(8) 0.0721(6) -0.6705(11) -0.3127(4) 0.0227(13) 1.000 . Uani d ? C(9) -0.0246(7) -0.7527(11) -0.2258(4) 0.0225(13) 1.000 . Uani d ? H(1) -0.2640 -0.7680 -0.0500 0.031 1.000 . Uiso c ? H(2) -0.2728 -0.5215 0.0028 0.031 1.000 . Uiso c ? H(3) -0.3944 -0.5790 -0.1923 0.028 1.000 . Uiso c ? H(4) -0.5166 -0.5963 -0.1087 0.028 1.000 . Uiso c ? H(5) -0.3368 -0.1756 -0.1506 0.027 1.000 . Uiso c ? H(6) -0.4645 -0.1942 -0.0698 0.027 1.000 . Uiso c ? H(7) -0.5094 -0.4182 -0.3314 0.026 1.000 . Uiso c ? H(8) -0.6231 -0.2234 -0.3865 0.026 1.000 . Uiso c ? H(9) -0.4056 0.0473 -0.3679 0.024 1.000 . Uiso c ? H(10) -0.2930 -0.1320 -0.3036 0.024 1.000 . Uiso c ? H(11) -0.2108 -0.1138 -0.4685 0.033 1.000 . Uiso c ? H(12) -0.3887 -0.2275 -0.5022 0.033 1.000 . Uiso c ? H(13) 0.0797 -0.3834 -0.4042 0.020 1.000 . Uiso c ? H(14) -0.0216 -0.3282 -0.3141 0.020 1.000 . Uiso c ? H(15) 0.0669 -0.7987 -0.3598 0.032 1.000 . Uiso c ? H(16) 0.1893 -0.6430 -0.2905 0.032 1.000 . Uiso c ? H(17) 0.0237 -0.9047 -0.2022 0.028 1.000 . Uiso c ? H(18) -0.1437 -0.7807 -0.2472 0.028 1.000 . Uiso c ? 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) 0.0157(2) 0.0252(2) 0.0146(2) -0.0031(2) -0.00204(12) -0.0003(2) S(1) 0.0154(6) 0.0299(8) 0.0315(7) 0.0063(6) -0.0001(5) -0.0009(6) S(2) 0.0264(6) 0.0207(7) 0.0166(5) -0.0046(8) -0.0027(4) -0.0012(7) C(1) 0.017(2) 0.038(3) 0.017(2) -0.003(2) 0.002(2) 0.008(2) C(2) 0.011(2) 0.030(3) 0.022(2) -0.005(3) -0.001(2) 0.009(3) C(3) 0.018(3) 0.029(3) 0.022(3) 0.003(2) -0.002(2) -0.009(2) C(4) 0.020(3) 0.026(3) 0.019(2) -0.000(2) -0.009(2) 0.004(2) C(5) 0.025(3) 0.015(3) 0.024(2) -0.004(2) -0.010(2) 0.006(2) C(6) 0.028(3) 0.024(3) 0.026(3) -0.009(3) -0.003(2) 0.009(2) C(7) 0.017(2) 0.024(4) 0.015(2) -0.006(2) 0.006(2) -0.007(2) C(8) 0.017(3) 0.025(3) 0.026(3) -0.001(2) -0.000(2) -0.011(2) C(9) 0.023(3) 0.021(3) 0.021(2) 0.000(2) -0.007(2) -0.000(2) #============================================================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details Flack _refine_ls_abs_structure_Flack -0.0424(78) _refine_ls_number_reflns 1437 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_all 0.0380 _refine_ls_wR_factor_ref 0.0380 _refine_ls_goodness_of_fit_all 1.171 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0013 _refine_diff_density_min -0.93 _refine_diff_density_max 0.70 #============================================================================== # MOLECULAR GEOMETRY _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 TE1 C1 2.163(5) . . ? TE1 C9 2.148(6) . . ? S1 C3 1.814(6) . . ? S1 C4 1.820(6) . . ? S2 C6 1.810(7) . . ? S2 C7 1.818(5) . . ? C1 C2 1.521(8) . . ? C1 H1 0.95 . . no C1 H2 0.98 . . no C2 C3 1.511(10) . . ? C2 H3 0.95 . . no C2 H4 0.95 . . no C3 H5 0.97 . . no C3 H6 0.96 . . no C4 C5 1.510(8) . . ? C4 H7 0.95 . . no C4 H8 0.94 . . no C5 C6 1.525(9) . . ? C5 H9 0.98 . . no C5 H10 0.94 . . no C6 H11 0.96 . . no C6 H12 0.97 . . no C7 C8 1.518(8) . . ? C7 H13 0.96 . . no C7 H14 0.96 . . no C8 C9 1.533(8) . . ? C8 H15 0.96 . . no C8 H16 0.95 . . no C9 H17 0.97 . . no C9 H18 0.96 . . 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 C1 TE1 C9 94.2(2) . . . ? C3 S1 C4 101.3(2) . . . ? C6 S2 C7 100.4(3) . . . ? TE1 C1 C2 114.8(4) . . . ? TE1 C1 H1 109.0 . . . no TE1 C1 H2 107.6 . . . no C2 C1 H1 109.8 . . . no C2 C1 H2 108.0 . . . no H1 C1 H2 107.4 . . . no C1 C2 C3 113.3(6) . . . ? C1 C2 H3 107.5 . . . no C1 C2 H4 109.0 . . . no C3 C2 H3 108.6 . . . no C3 C2 H4 108.6 . . . no H3 C2 H4 109.8 . . . no S1 C3 C2 114.3(4) . . . ? S1 C3 H5 108.1 . . . no S1 C3 H6 108.3 . . . no C2 C3 H5 109.5 . . . no C2 C3 H6 109.6 . . . no H5 C3 H6 106.8 . . . no S1 C4 C5 113.1(4) . . . ? S1 C4 H7 109.8 . . . no S1 C4 H8 110.4 . . . no C5 C4 H7 105.5 . . . no C5 C4 H8 107.4 . . . no H7 C4 H8 110.5 . . . no C4 C5 C6 113.1(5) . . . ? C4 C5 H9 107.1 . . . no C4 C5 H10 109.4 . . . no C6 C5 H9 109.1 . . . no C6 C5 H10 110.5 . . . no H9 C5 H10 107.5 . . . no S2 C6 C5 113.7(4) . . . ? S2 C6 H11 107.7 . . . no S2 C6 H12 107.6 . . . no C5 C6 H11 110.4 . . . no C5 C6 H12 110.0 . . . no H11 C6 H12 107.3 . . . no S2 C7 C8 110.6(4) . . . ? S2 C7 H13 111.3 . . . no S2 C7 H14 111.1 . . . no C8 C7 H13 108.1 . . . no C8 C7 H14 107.8 . . . no H13 C7 H14 107.8 . . . no C7 C8 C9 113.9(5) . . . ? C7 C8 H15 107.5 . . . no C7 C8 H16 110.1 . . . no C9 C8 H15 108.1 . . . no C9 C8 H16 108.2 . . . no H15 C8 H16 108.9 . . . no TE1 C9 C8 113.8(4) . . . ? TE1 C9 H17 108.6 . . . no TE1 C9 H18 109.0 . . . no C8 C9 H17 108.7 . . . no C8 C9 H18 109.1 . . . no H17 C9 H18 107.4 . . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag TE1 C1 C2 C3 -68.6(6) . . . . yes TE1 C9 C8 C7 -65.0(5) . . . . yes S1 C3 C2 C1 177.0(3) . . . . yes C5 C6 S2 C7 -76.3(4) . . . . yes S1 C4 C5 C6 174.4(4) . . . . yes C6 S2 C7 C8 161.5(4) . . . . yes S2 C6 C5 C4 -70.3(5) . . . . yes S2 C7 C8 C9 -73.2(5) . . . . yes C1 TE1 C9 C8 149.6(4) . . . . yes C2 C1 TE1 C9 -69.8(5) . . . . yes C2 C3 S1 C4 -64.1(5) . . . . yes C3 S1 C4 C5 -64.1(5) . . . . yes data_02mlm021 _database_code_CSD 206529 #============================================================================== _computing_data_collection 'Nonius CCD Diffractometer Control' _computing_cell_refinement 'Nonius CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 10.4800(3) _cell_length_b 8.5703(3) _cell_length_c 16.6779(5) _cell_angle_alpha 90 _cell_angle_beta 94.309(2) _cell_angle_gamma 90 _cell_volume 1493.72(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; Crystals obtained by slow evaporation from a solution in CH2Cl2/CHCl3. ; _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.542 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 571.77 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H18 I2 S2 Te ' _chemical_formula_moiety 'C9 H18 I2 S2 Te ' _chemical_formula_structural [12]aneS2TeI2 _chemical_compound_source CH2Cl2/CHCl3 _exptl_crystal_F_000 1572.00 _exptl_absorpt_coefficient_mu 6.3749 _exptl_absorpt_correction_type multiscan _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. absorption correction: max and min transmission factors 0.30204, 0.21711 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'mercury CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method - _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 11927 _reflns_number_total 3494 _reflns_number_gt 2701 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06911 _diffrn_reflns_av_sigmaI/netI 0.119 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 54 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 108 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 12 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Te 0 6 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 12 -0.726 1.812 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom I(1) 0.53075(5) 0.13869(7) 0.22182(3) 0.0189(2) 1.000 . Uani d ? I(2) -0.00655(5) 0.00105(6) 0.13988(3) 0.0182(2) 1.000 . Uani d ? Te(1) 0.26313(5) 0.07552(6) 0.17695(3) 0.0117(1) 1.000 . Uani d ? S(1) 0.2507(2) 0.3487(2) -0.10307(11) 0.0164(5) 1.000 . Uani d ? S(2) 0.2543(2) 0.6545(2) 0.08937(11) 0.0149(5) 1.000 . Uani d ? C(1) 0.2780(8) 0.0918(10) 0.0470(4) 0.016(2) 1.000 . Uani d ? C(2) 0.3883(8) 0.1840(10) 0.0188(4) 0.018(2) 1.000 . Uani d ? C(3) 0.3736(8) 0.2064(10) -0.0723(4) 0.017(2) 1.000 . Uani d ? C(4) 0.3396(8) 0.5289(10) -0.0804(5) 0.017(2) 1.000 . Uani d ? C(5) 0.2484(7) 0.6661(9) -0.0766(4) 0.013(2) 1.000 . Uiso d ? C(6) 0.1628(7) 0.6542(10) -0.0075(5) 0.015(2) 1.000 . Uani d ? C(7) 0.1325(8) 0.5779(9) 0.1509(5) 0.016(2) 1.000 . Uani d ? C(8) 0.1195(8) 0.3989(9) 0.1459(5) 0.017(2) 1.000 . Uani d ? C(9) 0.2333(8) 0.3228(9) 0.1899(4) 0.014(2) 1.000 . Uani d ? H(1) 0.2014 0.1385 0.0242 0.020 1.000 . Uiso c ? H(2) 0.2846 -0.0114 0.0270 0.020 1.000 . Uiso c ? H(3) 0.3910 0.2833 0.0442 0.021 1.000 . Uiso c ? H(4) 0.4658 0.1296 0.0329 0.021 1.000 . Uiso c ? H(5) 0.3513 0.1091 -0.0969 0.021 1.000 . Uiso c ? H(6) 0.4530 0.2410 -0.0899 0.021 1.000 . Uiso c ? H(7) 0.3875 0.5183 -0.0300 0.021 1.000 . Uiso c ? H(8) 0.3963 0.5475 -0.1212 0.021 1.000 . Uiso c ? H(9) 0.2972 0.7593 -0.0704 0.016 1.000 . Uiso c ? H(10) 0.1959 0.6704 -0.1256 0.016 1.000 . Uiso c ? H(11) 0.1152 0.5599 -0.0128 0.018 1.000 . Uiso c ? H(12) 0.1057 0.7404 -0.0098 0.018 1.000 . Uiso c ? H(13) 0.0525 0.6233 0.1333 0.020 1.000 . Uiso c ? H(14) 0.1542 0.6062 0.2053 0.020 1.000 . Uiso c ? H(15) 0.0439 0.3676 0.1696 0.020 1.000 . Uiso c ? H(16) 0.1146 0.3675 0.0911 0.020 1.000 . Uiso c ? H(17) 0.2270 0.3421 0.2456 0.016 1.000 . Uiso c ? H(18) 0.3073 0.3733 0.1727 0.016 1.000 . Uiso c ? 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 I(1) 0.0205(3) 0.0168(3) 0.0197(3) 0.0033(2) 0.0026(2) 0.0028(2) I(2) 0.0203(3) 0.0126(3) 0.0225(3) -0.0014(2) 0.0064(2) 0.0011(2) Te(1) 0.0166(3) 0.0074(3) 0.0116(3) 0.0004(2) 0.0036(2) 0.0021(2) S(1) 0.0216(11) 0.0124(10) 0.0152(9) 0.0001(8) 0.0008(8) 0.0007(8) S(2) 0.0180(11) 0.0110(10) 0.0156(9) -0.0023(8) 0.0017(8) 0.0035(8) C(1) 0.026(5) 0.013(4) 0.010(4) -0.002(4) -0.002(3) -0.004(3) C(2) 0.022(5) 0.022(5) 0.009(3) 0.002(4) 0.008(3) 0.006(3) C(3) 0.024(4) 0.014(4) 0.016(4) 0.002(4) 0.015(3) -0.004(3) C(4) 0.014(4) 0.015(4) 0.022(4) 0.005(3) 0.003(3) -0.004(3) C(6) 0.009(4) 0.018(4) 0.018(4) 0.004(3) 0.002(3) 0.007(3) C(7) 0.026(5) 0.006(4) 0.018(4) 0.003(4) 0.008(3) -0.002(3) C(8) 0.021(5) 0.008(4) 0.023(4) 0.000(3) 0.013(3) 0.006(3) C(9) 0.021(4) 0.005(4) 0.015(4) -0.002(3) 0.005(3) -0.007(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; C(5) becomes npd when anisotropic (probably due to the presence of much heavier Te and I atoms), hence refined isotropically. Max and min residual electron density lies between Te and I atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _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 2701 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_all 0.0700 _refine_ls_wR_factor_ref 0.0700 _refine_ls_goodness_of_fit_all 1.505 _refine_ls_goodness_of_fit_ref 1.500 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.22 _refine_diff_density_max 1.96 #============================================================================== # MOLECULAR GEOMETRY 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 I1 TE1 2.8990(9) . . ? I2 TE1 2.9179(9) . . ? TE1 C1 2.189(9) . . ? TE1 C9 2.155(9) . . ? S1 C3 1.819(11) . . ? S1 C4 1.829(11) . . ? S2 C6 1.815(10) . . ? S2 C7 1.820(10) . . ? C1 C2 1.50(1) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C2 C3 1.528(12) . . ? C2 H3 0.95 . . no C2 H4 0.95 . . no C3 H5 0.95 . . no C3 H6 0.95 . . no C4 C5 1.52(1) . . ? C4 H7 0.95 . . no C4 H8 0.95 . . no C5 C6 1.516(12) . . ? C5 H9 0.95 . . no C5 H10 0.95 . . no C6 H11 0.95 . . no C6 H12 0.95 . . no C7 C8 1.54(1) . . ? C7 H13 0.95 . . no C7 H14 0.95 . . no C8 C9 1.50(1) . . ? C8 H15 0.95 . . no C8 H16 0.95 . . no C9 H17 0.95 . . no C9 H18 0.95 . . 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 I1 TE1 I2 176.77(3) . . . ? I1 TE1 C1 96.0(3) . . . ? I1 TE1 C9 86.3(3) . . . ? I2 TE1 C1 86.8(3) . . . ? I2 TE1 C9 95.2(3) . . . ? C1 TE1 C9 93.3(4) . . . ? C3 S1 C4 99.7(5) . . . ? C6 S2 C7 98.9(5) . . . ? TE1 C1 C2 117.2(6) . . . ? TE1 C1 H1 107.5 . . . no TE1 C1 H2 107.5 . . . no C2 C1 H1 107.5 . . . no C2 C1 H2 107.5 . . . no H1 C1 H2 109.5 . . . no C1 C2 C3 110.7(8) . . . ? C1 C2 H3 109.1 . . . no C1 C2 H4 109.1 . . . no C3 C2 H3 109.2 . . . no C3 C2 H4 109.2 . . . no H3 C2 H4 109.4 . . . no S1 C3 C2 112.4(6) . . . ? S1 C3 H5 108.8 . . . no S1 C3 H6 108.7 . . . no C2 C3 H5 108.7 . . . no C2 C3 H6 108.7 . . . no H5 C3 H6 109.5 . . . no S1 C4 C5 110.5(7) . . . ? S1 C4 H7 109.2 . . . no S1 C4 H8 109.2 . . . no C5 C4 H7 109.2 . . . no C5 C4 H8 109.2 . . . no H7 C4 H8 109.5 . . . no C4 C5 C6 112.9(8) . . . ? C4 C5 H9 108.6 . . . no C4 C5 H10 108.6 . . . no C6 C5 H9 108.6 . . . no C6 C5 H10 108.6 . . . no H9 C5 H10 109.4 . . . no S2 C6 C5 111.9(7) . . . ? S2 C6 H11 108.9 . . . no S2 C6 H12 108.9 . . . no C5 C6 H11 108.9 . . . no C5 C6 H12 108.9 . . . no H11 C6 H12 109.4 . . . no S2 C7 C8 113.1(6) . . . ? S2 C7 H13 108.6 . . . no S2 C7 H14 108.6 . . . no C8 C7 H13 108.6 . . . no C8 C7 H14 108.6 . . . no H13 C7 H14 109.4 . . . no C7 C8 C9 110.0(9) . . . ? C7 C8 H15 109.3 . . . no C7 C8 H16 109.3 . . . no C9 C8 H15 109.3 . . . no C9 C8 H16 109.3 . . . no H15 C8 H16 109.5 . . . no TE1 C9 C8 119.6(7) . . . ? TE1 C9 H17 106.9 . . . no TE1 C9 H18 106.9 . . . no C8 C9 H17 106.9 . . . no C8 C9 H18 106.9 . . . no H17 C9 H18 109.5 . . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag I1 TE1 C1 C2 . . . . -22.7(8) no I1 TE1 C9 C8 . . . . 156.3(7) no I2 TE1 C1 C2 . . . . 159.0(7) no I2 TE1 C9 C8 . . . . -26.6(7) no TE1 C1 C2 C3 . . . . -170.9(7) no TE1 C9 C8 C7 . . . . -168.9(6) no S1 C3 C2 C1 . . . . 74.0(10) no S1 C4 C5 C6 . . . . 65.6(9) no S2 C6 C5 C4 . . . . 62.2(10) no S2 C7 C8 C9 . . . . 72.0(9) no C1 TE1 C9 C8 . . . . 60.5(7) no C2 C1 TE1 C9 . . . . 63.9(8) no C2 C3 S1 C4 . . . . 78.8(8) no C3 S1 C4 C5 . . . . -162.8(7) no C5 C6 S2 C7 . . . . -162.8(7) no C6 S2 C7 C8 . . . . 80.6(8) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_Template_texray.inf _database_code_CSD 206530 _audit_creation_date 2002-10-24 _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 15.3529(4) _cell_length_b 12.6938(3) _cell_length_c 5.50550(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1072.95(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' 1/2-x,1/2+y,1/2+z '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 303.93 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H16 S2 Te ' _chemical_formula_moiety 'C8 H16 S2 Te ' _chemical_formula_structural [11]aneS2Te _chemical_compound_source ? _exptl_crystal_F_000 592.00 _exptl_absorpt_coefficient_mu 3.104 _exptl_absorpt_correction_type multiscan _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max. and min. transmission factors: 0.49812, 0.36152 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Mercury CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8858 _reflns_number_total 1452 _reflns_number_gt 1251 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06910 _diffrn_reflns_av_sigmaI/netI 0.076 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Te 0 4 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Te(1) 0.07457(2) 0.04837(2) 0.0091 0.01470(10) 1.000 . Uani d ? S(1) 0.22526(8) 0.34644(10) 0.5095(3) 0.0205(3) 1.000 . Uani d ? S(2) 0.02560(9) 0.38441(10) 0.2174(3) 0.0177(3) 1.000 . Uani d ? C(1) 0.1471(4) 0.1238(4) 0.2944(11) 0.0184(13) 1.000 . Uani d ? C(2) 0.2360(3) 0.1624(4) 0.2165(12) 0.0183(12) 1.000 . Uani d ? C(3) 0.2822(3) 0.2282(4) 0.4106(12) 0.0198(13) 1.000 . Uani d ? C(4) 0.2085(4) 0.4188(4) 0.2298(12) 0.0197(13) 1.000 . Uani d ? C(5) 0.1185(4) 0.4718(4) 0.223(1) 0.022(1) 1.000 . Uani d ? C(6) 0.0388(3) 0.3267(4) -0.0815(11) 0.0171(13) 1.000 . Uani d ? C(7) -0.0346(4) 0.2484(4) -0.1347(10) 0.020(1) 1.000 . Uani d ? C(8) -0.0364(3) 0.1524(4) 0.0307(13) 0.0180(12) 1.000 . Uani d ? H(1) 0.1138 0.1813 0.3575 0.024 1.000 . Uiso c ? H(2) 0.1548 0.0737 0.4261 0.024 1.000 . Uiso c ? H(3) 0.2715 0.1042 0.1740 0.023 1.000 . Uiso c ? H(4) 0.2287 0.2064 0.0761 0.023 1.000 . Uiso c ? H(5) 0.3383 0.2475 0.3465 0.025 1.000 . Uiso c ? H(6) 0.2916 0.1828 0.5470 0.025 1.000 . Uiso c ? H(7) 0.2534 0.4701 0.2142 0.024 1.000 . Uiso c ? H(8) 0.2128 0.3705 0.0967 0.024 1.000 . Uiso c ? H(9) 0.1155 0.5167 0.0798 0.028 1.000 . Uiso c ? H(10) 0.1131 0.5179 0.3615 0.028 1.000 . Uiso c ? H(11) 0.0385 0.3809 -0.2024 0.024 1.000 . Uiso c ? H(12) 0.0938 0.2909 -0.0906 0.024 1.000 . Uiso c ? H(13) -0.0886 0.2836 -0.1248 0.024 1.000 . Uiso c ? H(14) -0.0274 0.2219 -0.2983 0.024 1.000 . Uiso c ? H(15) -0.0884 0.1132 -0.0043 0.020 1.000 . Uiso c ? H(16) -0.0414 0.1785 0.1947 0.020 1.000 . Uiso c ? 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) 0.0134(2) 0.0141(2) 0.0166(2) 0.00030(10) 0.0010(2) -0.0008(2) S(1) 0.0196(6) 0.0252(6) 0.0168(6) -0.0021(5) -0.0002(8) -0.0028(10) S(2) 0.0164(6) 0.0167(6) 0.0200(6) -0.0003(5) 0.0020(7) -0.0026(6) C(1) 0.021(3) 0.018(3) 0.016(3) -0.004(2) 0.003(2) -0.000(2) C(2) 0.009(2) 0.019(3) 0.027(3) 0.001(2) 0.003(3) 0.000(3) C(3) 0.015(3) 0.021(3) 0.024(3) 0.000(2) -0.006(3) -0.002(3) C(4) 0.024(3) 0.019(2) 0.017(3) -0.008(2) -0.005(3) 0.002(3) C(5) 0.019(3) 0.019(2) 0.027(3) -0.008(2) 0.003(3) 0.001(3) C(6) 0.016(3) 0.017(3) 0.019(2) 0.004(2) 0.006(2) 0.001(2) C(7) 0.022(3) 0.019(3) 0.018(3) 0.004(2) -0.004(2) 0.001(2) C(8) 0.011(2) 0.021(2) 0.022(3) 0.003(2) 0.004(3) 0.002(3) #============================================================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details Flack _refine_ls_abs_structure_Flack 0.0017(27) _refine_ls_number_reflns 1251 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_all 0.0410 _refine_ls_wR_factor_ref 0.0410 _refine_ls_goodness_of_fit_all 1.243 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -1.42 _refine_diff_density_max 0.71 #============================================================================== # MOLECULAR GEOMETRY _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 TE1 C1 2.151(6) . . ? TE1 C8 2.158(5) . . ? S1 C3 1.821(6) . . ? S1 C4 1.812(7) . . ? S2 C5 1.807(6) . . ? S2 C6 1.813(7) . . ? C1 C2 1.512(8) . . ? C1 H1 0.96 . . no C1 H2 0.97 . . no C2 C3 1.530(9) . . ? C2 H3 0.95 . . no C2 H4 0.96 . . no C3 H5 0.96 . . no C3 H6 0.96 . . no C4 C5 1.536(9) . . ? C4 H7 0.95 . . no C4 H8 0.96 . . no C5 H9 0.97 . . no C5 H10 0.97 . . no C6 C7 1.531(8) . . ? C6 H11 0.96 . . no C6 H12 0.96 . . no C7 C8 1.521(9) . . ? C7 H13 0.94 . . no C7 H14 0.97 . . no C8 H15 0.96 . . no C8 H16 0.96 . . 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 C1 TE1 C8 95.5(2) . . . ? C3 S1 C4 103.4(3) . . . ? C5 S2 C6 100.1(3) . . . ? TE1 C1 C2 113.9(5) . . . ? TE1 C1 H1 109.1 . . . no TE1 C1 H2 108.4 . . . no C2 C1 H1 109.8 . . . no C2 C1 H2 108.4 . . . no H1 C1 H2 107.1 . . . no C1 C2 C3 113.4(6) . . . ? C1 C2 H3 109.6 . . . no C1 C2 H4 108.2 . . . no C3 C2 H3 109.3 . . . no C3 C2 H4 107.4 . . . no H3 C2 H4 108.8 . . . no S1 C3 C2 115.8(4) . . . ? S1 C3 H5 109.2 . . . no S1 C3 H6 109.5 . . . no C2 C3 H5 107.4 . . . no C2 C3 H6 106.8 . . . no H5 C3 H6 107.8 . . . no S1 C4 C5 111.8(5) . . . ? S1 C4 H7 108.7 . . . no S1 C4 H8 108.4 . . . no C5 C4 H7 110.4 . . . no C5 C4 H8 108.8 . . . no H7 C4 H8 108.6 . . . no S2 C5 C4 116.2(4) . . . ? S2 C5 H9 107.9 . . . no S2 C5 H10 108.5 . . . no C4 C5 H9 108.6 . . . no C4 C5 H10 108.8 . . . no H9 C5 H10 106.3 . . . no S2 C6 C7 110.7(4) . . . ? S2 C6 H11 109.9 . . . no S2 C6 H12 109.7 . . . no C7 C6 H11 109.2 . . . no C7 C6 H12 109.3 . . . no H11 C6 H12 108.0 . . . no C6 C7 C8 114.8(5) . . . ? C6 C7 H13 109.1 . . . no C6 C7 H14 108.7 . . . no C8 C7 H13 109.2 . . . no C8 C7 H14 106.4 . . . no H13 C7 H14 108.5 . . . no TE1 C8 C7 116.3(4) . . . ? TE1 C8 H15 109.2 . . . no TE1 C8 H16 109.0 . . . no C7 C8 H15 108.1 . . . no C7 C8 H16 106.6 . . . no H15 C8 H16 107.4 . . . no #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag TE1 C1 C2 C3 172.6(4) . . . . yes TE1 C8 C7 C6 -63.9(6) . . . . yes C4 C5 S2 C6 -67.9(6) . . . . yes S1 C3 C2 C1 -59.1(7) . . . . yes C5 S2 C6 C7 -179.2(4) . . . . yes S1 C4 C5 S2 -65.3(6) . . . . yes S2 C6 C7 C8 -64.2(6) . . . . yes C1 TE1 C8 C7 91.8(5) . . . . yes C2 C1 TE1 C8 -122.6(4) . . . . yes C2 C3 S1 C4 -56.4(5) . . . . yes C3 S1 C4 C5 140.7(4) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================