Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_ags2tebf_Ag{[11]aneS2Te}[BF4] _database_code_CSD 151895 _journal_coden_Cambridge 182 #------------------------------------------------------------------------------ _audit_creation_date '19100-10-16' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Chem. Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; _publ_contact_letter ; This is the CIF file for the structure of [Ag([11]andS2Te)]BF4 which is included in manuscript number B0083700 (Chem. Comm.). ; _publ_contact_author_phone ' 023 80 593609 ' _publ_contact_author_fax ' 023 80 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' loop_ _publ_author_name 'Levason, W.' 'Orchard, Simon D.' 'Reid, G' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. 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. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.885(2) _cell_length_b 17.329(3) _cell_length_c 9.018(2) _cell_angle_alpha 90 _cell_angle_beta 93.48(2) _cell_angle_gamma 90 _cell_volume 1386.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 16.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 498.61 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H16 B Ag F4 S2 Te ' _chemical_formula_moiety '?' _chemical_formula_structural [Ag([11]aneS2Re)]BF4 _chemical_compound_source ? _exptl_crystal_F_000 944.00 _exptl_absorpt_coefficient_mu 3.834 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.961 _exptl_special_details ; The scan width was (1.10+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -3 3 -1 -2 3 1 -5 2 _diffrn_reflns_number 2717 _reflns_number_total 2548 _reflns_number_gt 2022 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06623 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04373 _diffrn_orient_matrix_UB_12 -0.05319 _diffrn_orient_matrix_UB_13 -0.00133 _diffrn_orient_matrix_UB_21 0.09722 _diffrn_orient_matrix_UB_22 -0.02119 _diffrn_orient_matrix_UB_23 -0.03288 _diffrn_orient_matrix_UB_31 0.03673 _diffrn_orient_matrix_UB_32 -0.00723 _diffrn_orient_matrix_UB_33 0.10611 #------------------------------------------------------------------------------ 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, Tables 4.2.6.8 and 6.1.1.1) ; 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, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 4 -0.772 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ag 0 4 -1.085 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B 0 4 0.000 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 16 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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) 0.1869(1) 0.13367(5) 0.37308(9) 0.0191(2) 1.000 . Uani d ? Ag(1) 0.1451(1) 0.01403(6) 0.1878(1) 0.0297(3) 1.000 . Uani d ? S(1) 0.1295(3) 0.0691(2) 0.9151(3) 0.0161(7) 1.000 . Uani d ? S(2) -0.2482(4) 0.1211(2) 0.8267(4) 0.0222(8) 1.000 . Uani d ? F(1) 0.588(1) 0.1876(5) 0.201(1) 0.068(4) 1.000 . Uani d ? F(2) 0.7282(8) 0.0818(4) 0.2435(8) 0.030(2) 1.000 . Uani d ? F(3) 0.562(1) 0.1230(7) 0.412(1) 0.067(4) 1.000 . Uani d ? F(4) 0.477(1) 0.0705(6) 0.195(1) 0.064(3) 1.000 . Uani d ? C(1) 0.268(1) 0.0775(7) 0.568(1) 0.020(3) 1.000 . Uani d ? C(2) 0.311(1) 0.1336(7) 0.706(1) 0.022(3) 1.000 . Uani d ? C(3) 0.314(1) 0.0969(7) 0.853(2) 0.026(4) 1.000 . Uani d ? C(4) 0.048(1) 0.1642(7) 0.945(1) 0.022(3) 1.000 . Uani d ? C(5) -0.118(1) 0.1618(7) 0.973(1) 0.020(3) 1.000 . Uani d ? C(6) -0.198(1) 0.1714(7) 0.665(2) 0.025(4) 1.000 . Uani d ? C(7) -0.085(1) 0.1287(7) 0.562(1) 0.023(3) 1.000 . Uani d ? C(8) -0.021(1) 0.1794(7) 0.459(1) 0.021(3) 1.000 . Uani d ? B(1) 0.588(2) 0.1158(9) 0.257(2) 0.023(4) 1.000 . Uani d ? H(1) 0.1923 0.0428 0.5973 0.024 1.000 . Uiso c ? H(2) 0.3557 0.0493 0.5469 0.024 1.000 . Uiso c ? H(3) 0.4077 0.1546 0.6922 0.026 1.000 . Uiso c ? H(4) 0.2384 0.1740 0.7040 0.026 1.000 . Uiso c ? H(5) 0.3589 0.1321 0.9238 0.031 1.000 . Uiso c ? H(6) 0.3749 0.0518 0.8506 0.031 1.000 . Uiso c ? H(7) 0.1011 0.1873 1.0280 0.026 1.000 . Uiso c ? H(8) 0.0610 0.1947 0.8588 0.026 1.000 . Uiso c ? H(9) -0.1488 0.2133 0.9899 0.024 1.000 . Uiso c ? H(10) -0.1279 0.1321 1.0602 0.024 1.000 . Uiso c ? H(11) -0.2887 0.1813 0.6057 0.030 1.000 . Uiso c ? H(12) -0.1535 0.2190 0.6956 0.030 1.000 . Uiso c ? H(13) -0.0055 0.1068 0.6240 0.028 1.000 . Uiso c ? H(14) -0.1376 0.0889 0.5087 0.028 1.000 . Uiso c ? H(15) 0.0016 0.2272 0.5069 0.025 1.000 . Uiso c ? H(16) -0.0922 0.1875 0.3777 0.025 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) 0.0271(5) 0.0153(4) 0.0154(4) -0.0034(3) 0.0050(3) 0.0009(3) Ag(1) 0.0511(7) 0.0176(5) 0.0197(6) 0.0052(5) -0.0039(5) -0.0015(4) S(1) 0.018(2) 0.013(1) 0.017(2) 0.000(1) 0.001(1) 0.001(1) S(2) 0.019(2) 0.019(2) 0.029(2) 0.003(1) 0.005(1) 0.001(1) F(1) 0.098(9) 0.032(5) 0.080(8) 0.027(6) 0.041(6) 0.026(5) F(2) 0.029(4) 0.037(5) 0.024(4) 0.001(4) 0.004(3) 0.005(4) F(3) 0.028(5) 0.13(1) 0.048(6) -0.005(6) 0.011(4) 0.005(6) F(4) 0.030(5) 0.071(7) 0.089(8) -0.001(5) -0.011(5) -0.037(6) C(1) 0.019(7) 0.020(7) 0.020(7) -0.003(5) 0.002(5) -0.001(5) C(2) 0.021(7) 0.027(7) 0.017(7) -0.004(6) -0.001(5) 0.001(5) C(3) 0.012(6) 0.017(6) 0.047(9) -0.003(5) 0.000(6) -0.001(6) C(4) 0.033(8) 0.018(6) 0.014(6) 0.001(5) 0.004(5) 0.000(5) C(5) 0.037(8) 0.018(6) 0.004(6) 0.006(6) 0.000(5) 0.000(5) C(6) 0.024(7) 0.013(6) 0.037(8) 0.004(5) 0.000(6) 0.000(6) C(7) 0.023(7) 0.020(7) 0.027(7) 0.003(5) 0.000(6) -0.001(6) C(8) 0.031(7) 0.017(6) 0.014(6) 0.005(6) 0.001(5) 0.000(5) B(1) 0.031(9) 0.032(9) 0.008(7) -0.001(7) 0.000(6) 0.001(6) #------------------------------------------------------------------------------ _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) + 0.00000|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 2022 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_all 0.0709 _refine_ls_wR_factor_ref 0.0709 _refine_ls_goodness_of_fit_all 3.310 _refine_ls_goodness_of_fit_ref 3.310 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.15 _refine_diff_density_max 1.09 #------------------------------------------------------------------------------ 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) Ag(1) 2.674(1) . . yes Te(1) C(1) 2.10(1) . . yes Te(1) C(8) 2.19(1) . . yes Ag(1) S(1*) 2.634(3) . 1_554 yes Ag(1) S(2*) 2.521(3) . 3_556 yes S(1) C(3) 1.83(1) . . yes S(1) C(4) 1.82(1) . . yes S(2) C(5) 1.84(1) . . yes S(2) C(6) 1.78(1) . . yes F(1) B(1) 1.34(2) . . yes F(2) B(1) 1.39(2) . . yes F(3) B(1) 1.43(2) . . yes F(4) B(1) 1.36(2) . . yes C(1) C(2) 1.60(2) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) C(3) 1.48(2) . . yes C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) H(5) 0.95 . . no C(3) H(6) 0.95 . . no C(4) C(5) 1.51(2) . . yes C(4) H(7) 0.95 . . no C(4) H(8) 0.95 . . no C(5) H(9) 0.95 . . no C(5) H(10) 0.95 . . no C(6) C(7) 1.59(2) . . yes C(6) H(11) 0.95 . . no C(6) H(12) 0.95 . . no C(7) C(8) 1.42(2) . . yes C(7) H(13) 0.95 . . no C(7) H(14) 0.95 . . no C(8) H(15) 0.95 . . no C(8) H(16) 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 Ag(1) Te(1) C(1) 101.1(3) . . . yes Ag(1) Te(1) C(8) 114.4(3) . . . yes C(1) Te(1) C(8) 97.2(5) . . . yes Te(1) Ag(1) S(1*) 107.46(7) . . 1_554 yes Te(1) Ag(1) S(2*) 135.67(9) . . 3_556 yes S(1*) Ag(1) S(2*) 106.7(1) 1_554 . 3_556 yes Ag(1) S(1*) C(3*) 112.4(4) 1_556 . . yes Ag(1) S(1*) C(4*) 100.9(4) 1_556 . . yes C(3) S(1) C(4) 100.2(6) . . . yes Ag(1) S(2*) C(5*) 100.2(4) 3_556 . . yes Ag(1) S(2*) C(6*) 107.7(4) 3_556 . . yes C(5) S(2) C(6) 102.9(6) . . . yes Te(1) C(1) C(2) 114.8(8) . . . yes Te(1) C(1) H(1) 108.1 . . . no Te(1) C(1) H(2) 108.1 . . . no C(2) C(1) H(1) 108.1 . . . no C(2) C(1) H(2) 108.1 . . . no H(1) C(1) H(2) 109.5 . . . no C(1) C(2) C(3) 115(1) . . . yes C(1) C(2) H(3) 108.0 . . . no C(1) C(2) H(4) 108.0 . . . no C(3) C(2) H(3) 108.0 . . . no C(3) C(2) H(4) 108.0 . . . no H(3) C(2) H(4) 109.5 . . . no S(1) C(3) C(2) 114.6(9) . . . yes S(1) C(3) H(5) 108.2 . . . no S(1) C(3) H(6) 108.2 . . . no C(2) C(3) H(5) 108.2 . . . no C(2) C(3) H(6) 108.2 . . . no H(5) C(3) H(6) 109.5 . . . no S(1) C(4) C(5) 113.4(9) . . . yes S(1) C(4) H(7) 108.5 . . . no S(1) C(4) H(8) 108.5 . . . no C(5) C(4) H(7) 108.5 . . . no C(5) C(4) H(8) 108.5 . . . no H(7) C(4) H(8) 109.5 . . . no S(2) C(5) C(4) 117.9(8) . . . yes S(2) C(5) H(9) 107.3 . . . no S(2) C(5) H(10) 107.3 . . . no C(4) C(5) H(9) 107.3 . . . no C(4) C(5) H(10) 107.3 . . . no H(9) C(5) H(10) 109.5 . . . no S(2) C(6) C(7) 116.5(9) . . . yes S(2) C(6) H(11) 107.7 . . . no S(2) C(6) H(12) 107.7 . . . no C(7) C(6) H(11) 107.7 . . . no C(7) C(6) H(12) 107.7 . . . no H(11) C(6) H(12) 109.5 . . . no C(6) C(7) C(8) 113(1) . . . yes C(6) C(7) H(13) 108.7 . . . no C(6) C(7) H(14) 108.7 . . . no C(8) C(7) H(13) 108.7 . . . no C(8) C(7) H(14) 108.7 . . . no H(13) C(7) H(14) 109.5 . . . no Te(1) C(8) C(7) 112.7(9) . . . yes Te(1) C(8) H(15) 108.7 . . . no Te(1) C(8) H(16) 108.7 . . . no C(7) C(8) H(15) 108.7 . . . no C(7) C(8) H(16) 108.7 . . . no H(15) C(8) H(16) 109.5 . . . no F(1) B(1) F(2) 110(1) . . . yes F(1) B(1) F(3) 107(1) . . . yes F(1) B(1) F(4) 113(1) . . . yes F(2) B(1) F(3) 109(1) . . . yes F(2) B(1) F(4) 111(1) . . . yes F(3) B(1) F(4) 107(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 Te(1) F(4) 3.30(1) . . no Te(1) F(3) 3.337(9) . . no Ag(1) F(4) 3.103(9) . . no S(1) F(2) 3.271(8) . 3_656 no F(1) C(8) 3.28(2) . 4_554 no F(1) C(4) 3.41(2) . 4_554 no F(1) C(5) 3.46(2) . 1_654 no F(1) C(6) 3.53(2) . 4_554 no F(2) C(5) 3.19(1) . 1_654 no F(2) C(3) 3.23(1) . 3_656 no F(2) C(1) 3.24(1) . 3_656 no F(2) C(8) 3.33(1) . 1_655 no F(2) C(7) 3.33(1) . 1_655 no F(3) C(6) 3.14(2) . 1_655 no F(3) C(1) 3.15(1) . . no F(3) C(7) 3.34(2) . 1_655 no F(3) C(2) 3.57(2) . . no F(4) C(3) 3.35(2) . 1_554 no F(4) C(3) 3.48(2) . 3_656 no #------------------------------------------------------------------------------