Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Gillian Reid' 'Nicholas J. Hill' 'W. Levason' 'Mark E. Light' _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 'Chemical Communications' _publ_section_title ; Synthesis and structural features of the first thallium(I) selenoether derivatives. ; data_Template_texray.inf _database_code_CSD 195979 #============================================================================== _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 7.3370(2) _cell_length_b 9.0243(3) _cell_length_c 17.8221(4) _cell_angle_alpha 90 _cell_angle_beta 92.311(2) _cell_angle_gamma 90 _cell_volume 1179.06(5) _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' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 3.185 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 565.38 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H10 F6 P Se2 Tl ' _chemical_formula_moiety '[Tl{MeSe(CH2)2SeMe}]PF6' _chemical_formula_structural ? _chemical_compound_source MeCN _exptl_crystal_F_000 1008.00 _exptl_absorpt_coefficient_mu 20.028 _exptl_absorpt_correction_type Scalepack _exptl_special_details ; Scalepack absorption correction Absorption correction: multi-scan (DENZO; Otwinowski & Minor, 1997) Maximum and minimum transmission coefficients: 0.3793, 0.1407. ; #============================================================================== # 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 'X-ray tube' _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 4352 _reflns_number_total 2828 _reflns_number_gt 2271 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03856 _diffrn_reflns_av_sigmaI/netI 0.065 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.96 _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 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 24 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 8 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Tl 0 4 -3.556 9.659 ;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 Tl(1) 0.08009(3) 0.06813(3) 0.347386(11) 0.01455(7) 1.000 . Uani d ? Se(1) -0.18303(8) -0.13336(7) 0.47175(3) 0.0147(2) 1.000 . Uani d ? Se(2) -0.66345(8) -0.20670(7) 0.29408(3) 0.0175(2) 1.000 . Uani d ? P(1) 0.1377(2) 0.2053(2) 0.85455(8) 0.0136(4) 1.000 . Uani d ? F(1) 0.0792(6) 0.0772(4) 0.9101(2) 0.0311(12) 1.000 . Uani d ? F(2) 0.2245(5) 0.2974(4) 0.9241(2) 0.0237(10) 1.000 . Uani d ? F(3) 0.3309(5) 0.1272(4) 0.8445(2) 0.0233(10) 1.000 . Uani d ? F(4) 0.1953(5) 0.3345(5) 0.7990(2) 0.0281(11) 1.000 . Uani d ? F(5) 0.0532(5) 0.1137(5) 0.7841(2) 0.0309(11) 1.000 . Uani d ? F(6) -0.0542(5) 0.2854(5) 0.8640(2) 0.0259(10) 1.000 . Uani d ? C(1) -0.1473(9) -0.3402(8) 0.4964(3) 0.023(2) 1.000 . Uani d ? C(2) -0.4296(8) -0.1476(7) 0.4260(3) 0.016(2) 1.000 . Uani d ? C(3) -0.4222(8) -0.2079(7) 0.3469(3) 0.016(2) 1.000 . Uani d ? C(4) -0.7885(9) -0.3545(9) 0.3531(4) 0.030(2) 1.000 . Uani d ? H(1) -0.1464 -0.3535 0.5492 0.028 1.000 . Uiso c ? H(2) -0.2422 -0.3980 0.4734 0.028 1.000 . Uiso c ? H(3) -0.0328 -0.3731 0.4783 0.028 1.000 . Uiso c ? H(4) -0.5029 -0.2106 0.4557 0.019 1.000 . Uiso c ? H(5) -0.4850 -0.0511 0.4244 0.019 1.000 . Uiso c ? H(6) -0.3774 -0.3083 0.3497 0.019 1.000 . Uiso c ? H(7) -0.3385 -0.1507 0.3196 0.019 1.000 . Uiso c ? H(8) -0.8043 -0.3179 0.4029 0.037 1.000 . Uiso c ? H(9) -0.9032 -0.3780 0.3306 0.037 1.000 . Uiso c ? H(10) -0.7158 -0.4431 0.3571 0.037 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 Tl(1) 0.0135(1) 0.0167(1) 0.01325(13) 0.00112(9) -0.00113(8) -0.00027(9) Se(1) 0.0135(3) 0.0180(3) 0.0123(3) -0.0040(3) -0.0035(2) 0.0002(2) Se(2) 0.0139(3) 0.0211(4) 0.0171(3) 0.0040(3) -0.0057(2) -0.0048(2) P(1) 0.0085(8) 0.0160(9) 0.0160(7) -0.0008(6) -0.0023(6) -0.0030(6) F(1) 0.028(2) 0.026(2) 0.039(2) -0.005(2) 0.005(2) 0.014(2) F(2) 0.021(2) 0.025(2) 0.025(2) -0.000(2) -0.006(2) -0.012(2) F(3) 0.012(2) 0.032(2) 0.027(2) 0.007(2) 0.001(1) -0.007(2) F(4) 0.029(2) 0.028(2) 0.027(2) -0.003(2) -0.003(2) 0.007(2) F(5) 0.023(2) 0.039(3) 0.030(2) 0.000(2) -0.005(2) -0.015(2) F(6) 0.013(2) 0.032(2) 0.032(2) 0.010(2) -0.002(2) -0.003(2) C(1) 0.024(4) 0.024(4) 0.020(3) 0.005(3) -0.007(3) 0.002(3) C(2) 0.012(3) 0.018(3) 0.017(3) -0.001(3) 0.001(2) 0.002(3) C(3) 0.014(3) 0.017(3) 0.017(3) 0.005(3) -0.003(2) -0.000(2) C(4) 0.019(4) 0.029(4) 0.041(4) -0.004(3) 0.008(3) -0.003(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _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 2271 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_all 0.0380 _refine_ls_wR_factor_ref 0.0380 _refine_ls_goodness_of_fit_all 1.648 _refine_ls_goodness_of_fit_ref 1.650 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_min -1.79 _refine_diff_density_max 1.59 #============================================================================== # 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 Tl(1) Se(1) 3.5058(8) . . ? Tl(1) Se(1) 3.3333(7) . 3_556 ? Tl(1) Se(2) 3.3142(8) . 1_655 ? Tl(1) Se(2) 3.2769(8) . 2 ? Tl(1) F(2) 3.231(5) . .4_454 ? Tl(1) F(3) 3.302(5) . 4_454 ? Tl(1) F(4) 3.048(5) . 4_454 ? Tl(1) F(5) 2.993(5) . 3_556 ? Tl(1) F(6) 2.995(5) . 4_454 ? Se(1) C(1) 1.933(9) . . ? Se(1) C(2) 1.959(8) . . ? Se(2) C(3) 1.971(7) . . ? Se(2) C(4) 1.950(9) . . ? P(1) F(1) 1.592(5) . . ? P(1) F(2) 1.603(5) . . ? P(1) F(3) 1.600(5) . . ? P(1) F(4) 1.597(5) . . ? P(1) F(5) 1.607(5) . . ? P(1) F(6) 1.598(5) . . ? C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.96 . . no C(2) C(3) 1.513(10) . . ? C(2) H(4) 0.96 . . no C(2) H(5) 0.96 . . no C(3) H(6) 0.96 . . no C(3) H(7) 0.95 . . no C(4) H(8) 0.96 . . no C(4) H(9) 0.94 . . no C(4) H(10) 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 Se(1) Tl(1) Se(1) 65.75(2) . . 3_556 ? Se(1) Tl(1) Se(2) 157.24(2) . . 1_655 ? Se(1) Tl(1) Se(2) 97.36(2) . . 2 ? Se(1) Tl(1) F(2) 56.80(8) . . 4_454 ? Se(1) Tl(1) F(4) 78.52(9) . . 4_454 ? Se(1) Tl(1) F(5) 92.28(10) . . 3_556 ? Se(1) Tl(1) F(6) 132.87(9) . . 4_454 ? Se(1) Tl(1) Se(2) 125.86(2) 3_556 3_556 3_556 ? Se(1) Tl(1) Se(2) 107.68(2) 3_556 3_556 3_556 ? Se(1) Tl(1) F(2) 71.31(8) 3_556 3_556 3_556 ? Se(1) Tl(1) F(4) 113.18(8) 3_556 3_556 3_556 ? Se(1) Tl(1) F(5) 155.26(11) 3_556 3_556 3_556 ? Se(1) Tl(1) F(6) 70.08(9) 3_556 3_556 3_556 ? Se(2) Tl(1) Se(2) 96.763(10) 2_455 2_455 2_455 ? Se(2) Tl(1) F(2) 105.59(8) 2_455 2_455 2_455 ? Se(2) Tl(1) F(4) 78.78(9) 2_455 2_455 2_455 ? Se(2) Tl(1) F(5) 78.75(11) 2_455 2_455 2_455 ? Se(2) Tl(1) F(6) 67.20(9) 2_455 2_455 2_455 ? Se(2) Tl(1) F(2) 152.87(8) 1_655 1_655 1_655 ? Se(2) Tl(1) F(4) 132.26(9) 1_655 1_655 1_655 ? Se(2) Tl(1) F(5) 62.05(10) 1_655 1_655 1_655 ? Se(2) Tl(1) F(6) 80.81(10) 1_655 1_655 1_655 ? F(2) Tl(1) F(4) 41.99(11) 4_454 4_454 4_454 ? F(2) Tl(1) F(5) 107.07(13) 4_454 4_454 4_454 ? F(2) Tl(1) F(6) 121.85(13) 4_454 4_454 4_454 ? F(4) Tl(1) F(5) 70.55(13) 4_454 4_454 4_454 ? F(4) Tl(1) F(6) 135.8(1) 4_454 4_454 4_454 ? F(5) Tl(1) F(6) 125.64(13) 3_556 3_556 3_556 ? Tl(1) Se(1) Tl(1) 114.25(2) . . . ? Tl(1) Se(1) C(1) 124.9(3) . . . ? Tl(1) Se(1) C(2) 107.1(2) . . . ? Tl(1) Se(1) C(1) 85.8(2) 3_556 3_556 3_556 ? Tl(1) Se(1) C(2) 125.7(2) 3_556 3_556 3_556 ? C(1) Se(1) C(2) 98.4(3) . . . ? Tl(1) Se(2) Tl(1) 144.13(2) 2_445 2_445 2_445 ? Tl(1) Se(2) C(3) 99.8(2) 2_445 2_445 2_445 ? Tl(1) Se(2) C(4) 95.5(3) 2_445 2_445 2_445 ? Tl(1) Se(2) C(3) 112.4(2) 1_455 1_455 1_455 ? Tl(1) Se(2) C(4) 94.2(3) 1_455 1_455 1_455 ? C(3) Se(2) C(4) 99.9(4) . . . ? F(1) P(1) F(2) 90.2(3) . . . ? F(1) P(1) F(3) 90.7(3) . . . ? F(1) P(1) F(4) 179.6(3) . . . ? F(1) P(1) F(5) 90.4(3) . . . ? F(1) P(1) F(6) 90.1(3) . . . ? F(2) P(1) F(3) 89.4(3) . . . ? F(2) P(1) F(4) 89.7(3) . . . ? F(2) P(1) F(5) 179.2(3) . . . ? F(2) P(1) F(6) 90.5(3) . . . ? F(3) P(1) F(4) 89.7(3) . . . ? F(3) P(1) F(5) 90.1(3) . . . ? F(3) P(1) F(6) 179.2(3) . . . ? F(4) P(1) F(5) 89.7(3) . . . ? F(4) P(1) F(6) 89.5(3) . . . ? F(5) P(1) F(6) 90.1(3) . . . ? Tl(1) F(2) P(1) 99.8(2) 4 4 4 ? Tl(1) F(4) P(1) 107.5(2) 4 4 4 ? Tl(1) F(5) P(1) 176.1(3) 3_556 3_556 3_556 ? Tl(1) F(6) P(1) 168.3(3) 4_455 4_455 4_455 ? Se(1) C(1) H(1) 110.1 . . . no Se(1) C(1) H(2) 110.0 . . . no Se(1) C(1) H(3) 109.6 . . . no H(1) C(1) H(2) 109.6 . . . no H(1) C(1) H(3) 108.8 . . . no H(2) C(1) H(3) 108.7 . . . no Se(1) C(2) C(3) 110.1(5) . . . ? Se(1) C(2) H(4) 109.8 . . . no Se(1) C(2) H(5) 109.6 . . . no C(3) C(2) H(4) 110.1 . . . no C(3) C(2) H(5) 109.2 . . . no H(4) C(2) H(5) 108.0 . . . no Se(2) C(3) C(2) 112.2(5) . . . ? Se(2) C(3) H(6) 109.1 . . . no Se(2) C(3) H(7) 109.7 . . . no C(2) C(3) H(6) 108.4 . . . no C(2) C(3) H(7) 109.3 . . . no H(6) C(3) H(7) 108.1 . . . no Se(2) C(4) H(8) 109.9 . . . no Se(2) C(4) H(9) 110.9 . . . no Se(2) C(4) H(10) 109.8 . . . no H(8) C(4) H(9) 109.4 . . . no H(8) C(4) H(10) 107.7 . . . no H(9) C(4) H(10) 109.2 . . . 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 Tl(1) F(5) 2.993(5) . 3_556 no Tl(1) F(6) 2.995(5) . 4_554 no Tl(1) F(4) 3.048(5) . 4_454 no Tl(1) F(2) 3.231(5) . 4_454 no Tl(1) F(3) 3.302(5) . 4_454 no Se(1) F(2) 3.213(5) . 4_454 no #------------------------------------------------------------------------------ # End of CIF data__02njh014.inf _database_code_CSD 195980 #============================================================================== _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 7.9081(3) _cell_length_b 7.9111(3) _cell_length_c 10.4005(4) _cell_angle_alpha 90 _cell_angle_beta 101.932(1) _cell_angle_gamma 90 _cell_volume 636.62(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 'C 2 ' _symmetry_Int_Tables_number 5 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y, -z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'colourless' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 3.022 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 579.40 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 F6 P Se2 Tl ' _chemical_formula_moiety 'C5 H12 F6 P Se2 Tl ' _chemical_formula_structural [Tl{MeSe(CH2)3SeMe}]PF6 _chemical_compound_source MeCN _exptl_crystal_F_000 520.00 _exptl_absorpt_coefficient_mu 18.551 _exptl_absorpt_correction_type multi-scan _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. Multi-scan - SORTAV ref Blessing, 1995; Max. and min. transmission factors: 0.0382, 0.0132 ; #============================================================================== # 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 Kappa CCD 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 2460 _reflns_number_total 1314 _reflns_number_gt 737 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04240 _diffrn_reflns_av_sigmaI/netI 0.077 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.53 _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 10 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 24 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 12 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 2 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 4 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Tl 0 2 -3.556 9.659 ;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 Tl(1) 0.0000 0.0098 0.0000 0.0322(2) 1.000 ST Uani d ? Se(1) 0.10459(12) 0.0094(3) 0.33295(9) 0.0317(3) 1.000 . Uani d ? P(1) -0.5000 0.0024(12) 0.0000 0.0281(8) 1.000 ST Uani d ? F(1) -0.605(2) -0.125(2) 0.078(2) 0.059(5) 0.750 S Uani d ? F(2) -0.610(3) 0.140(2) 0.054(3) 0.072(7) 0.750 S Uani d ? F(3) -0.346(2) 0.042(3) 0.1185(13) 0.080(5) 0.750 S Uani d ? F(4) -0.474(5) 0.158(5) -0.089(4) 0.039(9) 0.250 S Uiso d ? F(5) -0.568(4) -0.101(4) -0.117(3) 0.030(6) 0.250 S Uiso d ? F(6) -0.356(5) -0.138(5) 0.057(4) 0.048(8) 0.250 S Uiso d ? C(1) 0.294(2) -0.146(2) 0.338(1) 0.043(4) 1.000 . Uani d ? C(2) -0.065(2) -0.153(2) 0.375(2) 0.042(4) 1.000 . Uani d ? C(3) 0.0000 -0.254(2) 0.5000 0.032(4) 1.000 ST Uani d ? H(1) 0.3852 -0.0944 0.3069 0.055 1.000 . Uiso c ? H(2) 0.2538 -0.2426 0.2837 0.055 1.000 . Uiso c ? H(3) 0.3348 -0.1853 0.4257 0.055 1.000 . Uiso c ? H(4) -0.0981 -0.2286 0.3033 0.052 1.000 . Uiso c ? H(5) -0.1673 -0.0913 0.3856 0.052 1.000 . Uiso c ? H(6) 0.0909 -0.3266 0.4829 0.045 1.000 . Uiso c ? H(7) -0.0909 -0.3266 0.5171 0.045 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 Tl(1) 0.0307(3) 0.0335(3) 0.0320(3) 0.0000 0.0057(2) 0.0000 Se(1) 0.0321(6) 0.0332(6) 0.0296(5) 0.008(2) 0.0059(4) -0.006(2) P(1) 0.026(2) 0.031(2) 0.027(2) 0.0000 0.0054(13) 0.0000 F(1) 0.043(8) 0.093(13) 0.040(7) -0.004(7) 0.007(6) 0.042(8) F(2) 0.060(11) 0.024(8) 0.15(2) 0.003(7) 0.069(13) -0.007(8) F(3) 0.054(7) 0.11(2) 0.063(7) 0.013(9) -0.027(6) -0.032(10) C(1) 0.047(8) 0.047(9) 0.039(7) -0.008(6) 0.016(6) 0.003(6) C(2) 0.027(6) 0.043(8) 0.052(8) -0.013(6) -0.003(5) -0.012(7) C(3) 0.021(7) 0.018(7) 0.059(11) 0.0000 0.012(7) 0.0000 #============================================================================== # REFINEMENT DATA _refine_special_details ; PF6- disordered giving 2 components - major involving F(1)-F(3) (75%), minor F(4)-F(6) (25% occupancy). The minor component is not very well defined, but this model leads to improved thermal parameters and a better overall fit to data. All non-H atoms refined anisotropically except for the 25% occupied F's. ; _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 0.1035(99) _refine_ls_number_reflns 737 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_all 0.0530 _refine_ls_wR_factor_ref 0.0530 _refine_ls_goodness_of_fit_all 1.528 _refine_ls_goodness_of_fit_ref 1.530 _refine_ls_shift/su_max 0.0400 _refine_ls_shift/su_mean 0.0091 _refine_diff_density_min -2.03 _refine_diff_density_max 1.64 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Note that F1 - F3 belong to the major PF6- component (75% occupancy) while F4-F6 belong to the 25% component (less well defined). ; 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 TL1 SE1 3.390(1) 1 . . TL1 F4 2.95(5) 54503 . . TL1 F6 3.02(5) 3 . . TL1 F2 3.14(2) 54503 . . TL1 F1 3.16(3) 3 . . TL1 F2 3.19(3) 65501 . . TL1 F6 3.21(5) 1 . . TL1 F3 3.23(2) 1 . . TL1 F1 3.24(2) 65501 . . TL1 F5 3.31(3) 3 . . SE1 C1 1.93(2) . . ? SE1 C2 1.97(2) . . ? P1 F1 1.63(2) . . ? P1 F1 1.63(2) . . ? P1 F2 1.57(2) . . ? P1 F2 1.57(2) . . ? P1 F3 1.58(1) . . ? P1 F3 1.58(1) . . ? P1 F4 1.58(5) . . ? P1 F4 1.58(5) . . ? P1 F5 1.47(4) . . ? P1 F5 1.47(4) . . ? P1 F6 1.62(5) . . ? P1 F6 1.62(5) . . ? C1 H1 0.94 . . no C1 H2 0.97 . . no C1 H3 0.95 . . no C2 C3 1.52(2) . . ? C2 H4 0.95 . . no C2 H5 0.97 . . no C3 H6 0.96 . . no C3 H7 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 SE1 TL1 SE1 179.9(1) . . 2 ? C1 SE1 TL1 93.1(5) . . . ? C2 SE1 TL1 101.2(5) . . . ? C1 SE1 C2 97.9(8) . . . ? F1 P1 F1 103.5(20) . . . ? F1 P1 F2 82.6(8) . . . ? F1 P1 F2 171.0(17) . . . ? F1 P1 F3 97.3(11) . . . ? F1 P1 F3 96.7(10) . . . ? F2 P1 F2 92.1(17) . . . ? F2 P1 F3 88.9(14) . . . ? F2 P1 F3 75.3(14) . . . ? F3 P1 F3 157.3(18) . . . ? F4 P1 F4 77.6(37) . . . ? F4 P1 F5 91.1(22) . . . ? F4 P1 F5 148.0(18) . . . ? F4 P1 F6 125.8(24) . . . ? F4 P1 F6 119.2(24) . . . ? F5 P1 F5 112.4(28) . . . ? F5 P1 F6 91.8(22) . . . ? F5 P1 F6 37.1(20) . . . ? F6 P1 F6 93.0(33) . . . ? SE1 C1 H1 111.2 . . . no SE1 C1 H2 109.1 . . . no SE1 C1 H3 110.3 . . . no H1 C1 H2 108.4 . . . no H1 C1 H3 110.0 . . . no H2 C1 H3 107.7 . . . no SE1 C2 C3 114.1(9) . . . ? SE1 C2 H4 108.9 . . . no SE1 C2 H5 108.4 . . . no C3 C2 H4 109.4 . . . no C3 C2 H5 108.1 . . . no H4 C2 H5 107.7 . . . no C2 C3 C2 116.6(19) . . . ? C2 C3 H6 106.7 . . . no C2 C3 H7 109.6 . . . no C2 C3 H6 109.6 2_556 2_556 2_556 no C2 C3 H7 106.7 2_556 2_556 2_556 no H6 C3 H7 107.2 . . . 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 F1 C1 2.98(3) . 1_455 no F1 F2 3.02(3) . 4_345 no F1 F3 3.33(3) . 3_445 no F1 F4 3.52(6) . 3_445 no F2 F6 2.62(5) . 3_455 no F2 F5 3.43(4) . 4_355 no F3 C1 3.40(3) . 3_455 no F3 C2 3.46(2) . . no F4 F6 3.02(7) . 4_455 no F4 C2 3.40(5) . 4_455 no F4 C1 3.58(5) . 4_455 no F5 C1 3.49(4) . 2 no F5 C2 3.55(4) . 2_455 no C2 C2 2.59(4) . 2_556 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 #==============================================================================