Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data__01njh075new.inf _database_code_CSD 194426 _audit_creation_date '2002-09-19' _audit_creation_method 'by teXsan for Windows v1.06' _journal_coden_Cambridge 186 loop_ _publ_author_name 'Gillian Reid' 'Nicholas J. Hill' 'W. Levason' _publ_contact_author_name 'Dr Gillian Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'GR@SOTON.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structural Properties of the First Bismuth(III) Telluroether Complex ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_letter ; This is the CIF file for the crystal structure of [BiBr3(PhTeMe)]. ; _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 ; SHELX97 (Sheldrick, 1997) ; _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 8.4820(2) _cell_length_b 6.7592(2) _cell_length_c 22.5808(8) _cell_angle_alpha 90 _cell_angle_beta 100.6760(10) _cell_angle_gamma 90 _cell_volume 1272.18(6) _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/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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange-red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 3.490 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 668.43 _chemical_formula_analytical ? _chemical_formula_sum 'C7 H8 Bi Br3 Te ' _chemical_formula_moiety 'C7 H8 Bi Br3 Te ' _chemical_formula_structural [BiBr3(PhTeMe)] _chemical_compound_source ? _exptl_crystal_F_000 1160.00 _exptl_absorpt_coefficient_mu 25.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.' _exptl_absorpt_correction_T_min 0.02601 _exptl_absorpt_correction_T_max 0.05097 _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. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _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 5253 _reflns_number_total 2956 _reflns_number_gt 2144 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03036 _diffrn_reflns_av_sigmaI/netI 0.086 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.46 _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 28 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 12 -0.374 2.456 ;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) ; Bi 0 4 -4.861 10.559 ;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 Bi(1) 0.57122(3) 0.75630(4) 0.053171(12) 0.01946(9) 1.000 . Uani d ? Te(1) 0.88852(6) 0.54541(8) 0.09933(2) 0.0258(2) 1.000 . Uani d ? Br(1) 0.39043(10) 0.41568(12) 0.06972(3) 0.0263(2) 1.000 . Uani d ? Br(2) 0.56213(9) 0.88952(11) 0.16285(3) 0.0242(2) 1.000 . Uani d ? Br(3) 0.75461(9) 1.07715(11) 0.01902(3) 0.0231(2) 1.000 . Uani d ? C(1) 0.8023(10) 0.3757(12) 0.1637(4) 0.037(3) 1.000 . Uani d ? C(2) 0.9942(9) 0.7738(11) 0.1576(3) 0.022(2) 1.000 . Uani d ? C(3) 0.9720(8) 0.7842(11) 0.2172(3) 0.021(2) 1.000 . Uani d ? C(4) 1.0474(9) 0.9342(12) 0.2530(3) 0.026(2) 1.000 . Uani d ? C(5) 1.1394(9) 1.0724(11) 0.2309(4) 0.024(2) 1.000 . Uani d ? C(6) 1.1621(9) 1.0587(13) 0.1722(4) 0.033(3) 1.000 . Uani d ? C(7) 1.0880(9) 0.9103(12) 0.1346(3) 0.026(2) 1.000 . Uani d ? H(1) 0.8311 0.4368 0.2021 0.044 1.000 . Uiso c ? H(2) 0.6889 0.3663 0.1532 0.044 1.000 . Uiso c ? H(3) 0.8479 0.2471 0.1651 0.044 1.000 . Uiso c ? H(4) 0.9067 0.6903 0.2327 0.025 1.000 . Uiso c ? H(5) 1.0353 0.9418 0.2940 0.031 1.000 . Uiso c ? H(6) 1.1872 1.1775 0.2559 0.029 1.000 . Uiso c ? H(7) 1.2293 1.1517 0.1574 0.039 1.000 . Uiso c ? H(8) 1.1014 0.9027 0.0937 0.031 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 Bi(1) 0.0214(2) 0.0206(2) 0.0144(2) -0.00143(12) -0.00181(12) 0.00110(12) Te(1) 0.0246(3) 0.0277(3) 0.0225(3) 0.0024(2) -0.0026(2) -0.0042(2) Br(1) 0.0341(5) 0.0277(5) 0.0164(4) -0.0089(4) 0.0030(4) 0.0008(3) Br(2) 0.0264(5) 0.0269(5) 0.0194(4) 0.0011(3) 0.0046(3) -0.0026(3) Br(3) 0.0236(4) 0.0236(5) 0.0212(4) -0.0024(3) 0.0019(3) 0.0017(3) C(1) 0.033(5) 0.033(5) 0.039(6) -0.010(4) -0.004(4) 0.003(4) C(2) 0.015(4) 0.031(5) 0.017(4) 0.008(3) -0.001(3) -0.001(4) C(3) 0.016(4) 0.025(5) 0.021(4) 0.003(3) -0.000(3) 0.003(3) C(4) 0.020(4) 0.034(5) 0.023(5) 0.000(4) 0.004(4) -0.005(4) C(5) 0.015(4) 0.030(5) 0.026(5) -0.004(3) -0.002(4) -0.007(4) C(6) 0.023(5) 0.041(6) 0.037(5) -0.002(4) 0.011(4) 0.008(4) C(7) 0.024(5) 0.035(5) 0.019(4) -0.004(4) 0.006(4) -0.006(4) #============================================================================== # 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 ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2144 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_all 0.0370 _refine_ls_wR_factor_ref 0.0370 _refine_ls_goodness_of_fit_all 1.383 _refine_ls_goodness_of_fit_ref 1.380 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -2.60 _refine_diff_density_max 2.24 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; The symmetry operator for BI1a and BR1a is i: 1-x, 1-y, -z ; 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 BI1 TE1 3.0533(7) . . ? BI1 BR1 2.8291(9) . . ? BI1 BR1 3.0810(10) . 3 ? BI1 BR2 2.6497(9) . . ? BI1 BR3 2.8570(9) . . ? TE1 C1 2.088(10) . . ? TE1 C2 2.117(9) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C1 H3 0.95 . . no C2 C3 1.394(12) . . ? C2 C7 1.382(12) . . ? C3 C4 1.378(12) . . ? C3 H4 0.95 . . no C4 C5 1.370(12) . . ? C4 H5 0.95 . . no C5 C6 1.38(1) . . ? C5 H6 0.95 . . no C6 C7 1.388(13) . . ? C6 H7 0.95 . . no C7 H8 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 TE1 BI1 BR1 92.30(2) . . . ? TE1 BI1 BR1 84.14(2) . . 3 ? TE1 BI1 BR2 90.92(2) . . . ? TE1 BI1 BR3 87.53(2) . . . ? BR1 BI1 BR1 87.84(3) . . 3 ? BR1 BI1 BR2 92.45(3) . . . ? BR1 BI1 BR3 171.47(3) . . . ? BR1 BI1 BR2 175.05(3) 3_665 3_665 3_665 ? BR1 BI1 BR3 83.66(3) 3_665 3_665 3_665 ? BR2 BI1 BR3 96.08(3) . . . ? BI1 TE1 C1 95.4(3) . . . ? BI1 TE1 C2 96.7(2) . . . ? C1 TE1 C2 97.5(4) . . . ? BI1 BR1 BI1 92.16(3) . . . ? TE1 C1 H1 109.4 . . . no TE1 C1 H2 109.4 . . . no TE1 C1 H3 109.4 . . . no H1 C1 H2 109.6 . . . no H1 C1 H3 109.5 . . . no H2 C1 H3 109.5 . . . no TE1 C2 C3 121.3(6) . . . ? TE1 C2 C7 117.3(6) . . . ? C3 C2 C7 121.3(8) . . . ? C2 C3 C4 118.2(8) . . . ? C2 C3 H4 120.9 . . . no C4 C3 H4 120.9 . . . no C3 C4 C5 121.4(8) . . . ? C3 C4 H5 119.3 . . . no C5 C4 H5 119.3 . . . no C4 C5 C6 119.7(8) . . . ? C4 C5 H6 120.1 . . . no C6 C5 H6 120.1 . . . no C5 C6 C7 120.7(9) . . . ? C5 C6 H7 119.7 . . . no C7 C6 H7 119.6 . . . no C2 C7 C6 118.6(8) . . . ? C2 C7 H8 120.7 . . . no C6 C7 H8 120.7 . . . 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 C3 C5 3.585(12) . 2_745 no C4 C5 3.580(13) . 2_745 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 ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . 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 #==============================================================================