Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Uruichi, M.' 'Mori, Takehiko' 'Nakamura, T.' 'Shirahata, Takashi' 'Takahashi, Kazuko' 'Yakushi, Kyuya' _publ_contact_author_name 'Dr M Uruichi' _publ_contact_author_address ; Institute for Molecular Science Graduate University of Advanced Studies Myodaiji Okazaki 444-8585 JAPAN ; _publ_contact_author_email 'URUICHI@IMS.AC.JP' _publ_section_title ; Structural phase transition in quasi-1D organic conductors (BDTFP)2X(PhCl)0.5 (X=PF6 amd AsF6) [BDTFP=5,7-bis(1,3-dithiol-2-ylidene)-5,7-dihydrofuro[3,4-b]pyrazine] ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; data_b2alt #(BDTFP)2AsF6(PhCl)0.5 at 100 K _database_code_CSD 181035 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 27 15:19:02 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H29 As2 Cl F12 N8 O4 S16 ' _chemical_formula_moiety '4(C12 H6 N2 O S4), C6 H5 Cl, 2(As F6)' _chemical_formula_weight 1780.11 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.252(4) _cell_length_b 16.083(5) _cell_length_c 6.8902(9) _cell_angle_alpha 100.22(2) _cell_angle_beta 98.09(2) _cell_angle_gamma 100.55(2) _cell_volume 1608.8(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 80 _cell_measurement_theta_min ? _cell_measurement_theta_max 25.6 _cell_measurement_temperature 100.0 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888.00 _exptl_absorpt_coefficient_mu 1.689 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 5459 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 25.67 _diffrn_measured_fraction_theta_max 0.8973 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.8973 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1826 _reflns_number_gt 4925 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.0870 _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 4925 _refine_ls_number_parameters 470 _refine_ls_goodness_of_fit_ref 1.725 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00123|Fo|^2^]' _refine_ls_shift/su_max 1.3176 _refine_diff_density_max 0.77 _refine_diff_density_min -1.05 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.056(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 As(1) As 0.18308(3) 0.69374(2) 0.47707(6) 0.0252(1) Uani 1.00 d . . . Cl(1) Cl -0.0066(2) -0.1202(2) 0.1783(4) 0.0595(7) Uani 0.50 d P . . S(1) S 0.10465(7) 0.25659(6) 0.2549(1) 0.0232(2) Uani 1.00 d . . . S(2) S 0.24463(7) 0.41370(6) 0.2935(1) 0.0213(2) Uani 1.00 d . . . S(3) S 0.20792(7) -0.03164(6) 0.1040(1) 0.0229(2) Uani 1.00 d . . . S(4) S 0.40523(7) -0.01495(6) 0.1338(1) 0.0217(2) Uani 1.00 d . . . S(5) S 0.11299(7) 0.34596(6) 0.7923(1) 0.0209(2) Uani 1.00 d . . . S(6) S 0.25165(7) 0.50136(6) 0.8244(1) 0.0222(2) Uani 1.00 d . . . S(7) S 0.22310(7) 0.06015(6) 0.6380(1) 0.0206(2) Uani 1.00 d . . . S(8) S 0.41912(7) 0.07824(6) 0.6615(1) 0.0208(2) Uani 1.00 d . . . F(1) F 0.2730(2) 0.7734(2) 0.4750(4) 0.0394(7) Uani 1.00 d . . . F(2) F 0.1330(2) 0.6987(2) 0.2418(4) 0.0553(9) Uani 1.00 d . . . F(3) F 0.1268(2) 0.7681(2) 0.5823(5) 0.0480(8) Uani 1.00 d . . . F(4) F 0.0928(2) 0.6127(1) 0.4813(3) 0.0310(6) Uani 1.00 d . . . F(5) F 0.2308(2) 0.6861(2) 0.7138(4) 0.0404(7) Uani 1.00 d . . . F(6) F 0.2392(2) 0.6178(2) 0.3769(5) 0.0492(8) Uani 1.00 d . . . O(1) O 0.2488(2) 0.1606(2) 0.1837(4) 0.0194(6) Uani 1.00 d . . . O(2) O 0.2612(2) 0.2514(2) 0.7222(4) 0.0184(6) Uani 1.00 d . . . N(1) N 0.4297(2) 0.3466(2) 0.2489(4) 0.0228(8) Uani 1.00 d . . . N(2) N 0.4899(2) 0.1857(2) 0.1990(4) 0.0224(8) Uani 1.00 d . . . N(3) N 0.4361(2) 0.4398(2) 0.7724(4) 0.0212(7) Uani 1.00 d . . . N(4) N 0.5002(2) 0.2805(2) 0.7169(4) 0.0222(8) Uani 1.00 d . . . C(1) C 0.0717(3) 0.3553(3) 0.3023(5) 0.0257(9) Uani 1.00 d . . . C(2) C 0.1348(3) 0.4260(2) 0.3195(5) 0.0241(9) Uani 1.00 d . . . C(3) C 0.2170(3) 0.3012(2) 0.2516(5) 0.0209(9) Uani 1.00 d . . . C(4) C 0.2786(3) 0.2502(2) 0.2200(5) 0.0187(8) Uani 1.00 d . . . C(5) C 0.3740(3) 0.2700(2) 0.2236(5) 0.0194(8) Uani 1.00 d . . . C(6) C 0.4035(3) 0.1913(2) 0.1996(5) 0.0193(8) Uani 1.00 d . . . C(7) C 0.3246(2) 0.1230(2) 0.1727(5) 0.0188(8) Uani 1.00 d . . . C(8) C 0.3138(2) 0.0366(2) 0.1407(5) 0.0187(8) Uani 1.00 d . . . C(9) C 0.5163(3) 0.3403(2) 0.2485(5) 0.0248(9) Uani 1.00 d . . . C(10) C 0.5459(3) 0.2629(3) 0.2242(5) 0.0244(9) Uani 1.00 d . . . C(11) C 0.2499(3) -0.1255(2) 0.0834(6) 0.0281(10) Uani 1.00 d . . . C(12) C 0.3389(3) -0.1175(2) 0.0990(6) 0.029(1) Uani 1.00 d . . . C(13) C 0.0805(3) 0.4445(2) 0.8425(5) 0.0234(9) Uani 1.00 d . . . C(14) C 0.1442(3) 0.5153(2) 0.8591(5) 0.0247(9) Uani 1.00 d . . . C(15) C 0.2241(3) 0.3903(2) 0.7852(5) 0.0202(8) Uani 1.00 d . . . C(16) C 0.2880(3) 0.3402(2) 0.7514(5) 0.0193(8) Uani 1.00 d . . . C(17) C 0.3816(3) 0.3620(2) 0.7499(5) 0.0193(8) Uani 1.00 d . . . C(18) C 0.4134(3) 0.2842(2) 0.7225(5) 0.0182(8) Uani 1.00 d . . . C(19) C 0.3374(3) 0.2160(2) 0.7031(5) 0.0191(8) Uani 1.00 d . . . C(20) C 0.3276(3) 0.1281(2) 0.6698(5) 0.0186(8) Uani 1.00 d . . . C(21) C 0.5215(3) 0.4356(3) 0.7629(5) 0.0266(10) Uani 1.00 d . . . C(22) C 0.5533(3) 0.3576(3) 0.7353(6) 0.0248(9) Uani 1.00 d . . . C(23) C 0.2652(3) -0.0336(2) 0.6127(5) 0.0216(9) Uani 1.00 d . . . C(24) C 0.3544(3) -0.0251(2) 0.6246(5) 0.0235(9) Uani 1.00 d . . . C(25) C 0.0023(6) -0.0421(6) 0.392(1) 0.034(2) Uani 0.50 d P . . C(26) C -0.0091(10) 0.0495(9) 0.390(2) 0.063(4) Uani 0.50 d P . . C(27) C -0.0026(6) 0.1020(6) 0.548(1) 0.038(2) Uani 0.50 d P . . C(28) C 0.0066(7) 0.0839(8) 0.730(1) 0.045(3) Uani 0.50 d P . . C(29) C 0.0172(7) -0.0002(8) 0.751(1) 0.048(3) Uani 0.50 d P . . C(30) C 0.0108(9) -0.0502(9) 0.606(2) 0.060(3) Uani 0.50 d P . . H(1) H 0.0104 0.3578 0.3152 0.0251 Uiso 1.00 calc . . . H(2) H 0.1205 0.4821 0.3492 0.0221 Uiso 1.00 calc . . . H(3) H 0.5624 0.3928 0.2742 0.0221 Uiso 1.00 calc . . . H(4) H 0.6095 0.2651 0.2214 0.0230 Uiso 1.00 calc . . . H(5) H 0.2096 -0.1804 0.0621 0.0268 Uiso 1.00 calc . . . H(6) H 0.3656 -0.1674 0.0899 0.0246 Uiso 1.00 calc . . . H(7) H 0.0196 0.4477 0.8643 0.0215 Uiso 1.00 calc . . . H(8) H 0.1327 0.5728 0.8884 0.0240 Uiso 1.00 calc . . . H(9) H 0.5638 0.4902 0.7770 0.0239 Uiso 1.00 calc . . . H(10) H 0.6171 0.3608 0.7290 0.0244 Uiso 1.00 calc . . . H(11) H 0.2253 -0.0896 0.5912 0.0181 Uiso 1.00 calc . . . H(12) H 0.3823 -0.0745 0.6129 0.0233 Uiso 1.00 calc . . . H(13) H -0.0182 0.0656 0.2610 0.1266 Uiso 0.50 calc P . . H(14) H -0.0146 0.1606 0.5351 0.0452 Uiso 0.50 calc P . . H(15) H 0.0046 0.1229 0.8361 0.0533 Uiso 0.50 calc P . . H(16) H 0.0298 -0.0116 0.8908 0.0450 Uiso 0.50 calc P . . H(17) H 0.0060 -0.1067 0.6326 0.1266 Uiso 0.50 calc P . . 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 As(1) 0.0237(2) 0.0160(2) 0.0369(2) 0.0056(2) 0.0076(2) 0.0048(2) Cl(1) 0.057(2) 0.035(1) 0.071(2) -0.017(1) 0.033(1) -0.018(1) S(1) 0.0242(5) 0.0198(4) 0.0290(4) 0.0084(4) 0.0090(4) 0.0068(3) S(2) 0.0281(5) 0.0158(4) 0.0214(4) 0.0073(3) 0.0066(4) 0.0035(3) S(3) 0.0239(5) 0.0192(4) 0.0250(4) 0.0029(4) 0.0047(4) 0.0043(3) S(4) 0.0254(5) 0.0181(4) 0.0242(4) 0.0101(3) 0.0070(3) 0.0034(3) S(5) 0.0236(5) 0.0189(4) 0.0211(4) 0.0064(3) 0.0064(3) 0.0033(3) S(6) 0.0287(5) 0.0144(4) 0.0250(4) 0.0068(3) 0.0078(4) 0.0033(3) S(7) 0.0224(5) 0.0155(4) 0.0238(4) 0.0037(3) 0.0046(3) 0.0034(3) S(8) 0.0234(5) 0.0164(4) 0.0238(4) 0.0078(3) 0.0051(3) 0.0033(3) F(1) 0.036(1) 0.022(1) 0.061(2) 0.001(1) 0.011(1) 0.015(1) F(2) 0.056(2) 0.059(2) 0.045(1) -0.002(2) -0.003(1) 0.021(1) F(3) 0.040(2) 0.021(1) 0.084(2) 0.015(1) 0.017(1) 0.000(1) F(4) 0.024(1) 0.021(1) 0.047(1) 0.0055(9) 0.013(1) -0.0006(10) F(5) 0.032(1) 0.041(1) 0.046(1) -0.002(1) 0.000(1) 0.019(1) F(6) 0.038(1) 0.026(1) 0.090(2) 0.008(1) 0.040(1) 0.005(1) O(1) 0.019(1) 0.015(1) 0.025(1) 0.0071(10) 0.0044(10) 0.0040(9) O(2) 0.017(1) 0.013(1) 0.026(1) 0.0033(9) 0.0060(10) 0.0032(9) N(1) 0.028(2) 0.019(1) 0.021(1) 0.003(1) 0.007(1) 0.004(1) N(2) 0.021(2) 0.023(2) 0.022(1) 0.006(1) 0.004(1) 0.000(1) N(3) 0.023(2) 0.016(1) 0.024(1) 0.002(1) 0.006(1) 0.003(1) N(4) 0.025(2) 0.021(1) 0.018(1) 0.004(1) 0.003(1) 0.000(1) C(1) 0.033(2) 0.029(2) 0.024(2) 0.021(2) 0.013(1) 0.006(1) C(2) 0.033(2) 0.024(2) 0.019(2) 0.016(2) 0.008(1) 0.004(1) C(3) 0.024(2) 0.022(2) 0.019(2) 0.009(1) 0.006(1) 0.007(1) C(4) 0.022(2) 0.013(2) 0.021(2) 0.006(1) 0.005(1) 0.002(1) C(5) 0.027(2) 0.020(2) 0.013(1) 0.008(1) 0.006(1) 0.002(1) C(6) 0.028(2) 0.018(2) 0.011(1) 0.007(1) 0.002(1) 0.002(1) C(7) 0.017(2) 0.017(2) 0.023(2) 0.006(1) 0.005(1) 0.002(1) C(8) 0.020(2) 0.020(2) 0.018(2) 0.007(1) 0.006(1) 0.003(1) C(9) 0.029(2) 0.023(2) 0.018(2) -0.003(2) 0.002(2) 0.003(1) C(10) 0.024(2) 0.026(2) 0.022(2) 0.005(2) 0.005(1) 0.003(1) C(11) 0.039(2) 0.017(2) 0.029(2) 0.006(2) 0.010(2) 0.002(1) C(12) 0.036(2) 0.015(2) 0.036(2) 0.008(2) 0.008(2) 0.002(1) C(13) 0.027(2) 0.025(2) 0.022(2) 0.013(2) 0.007(1) 0.005(1) C(14) 0.034(2) 0.027(2) 0.018(2) 0.019(2) 0.007(1) 0.006(1) C(15) 0.025(2) 0.017(2) 0.021(2) 0.007(1) 0.005(1) 0.003(1) C(16) 0.024(2) 0.015(2) 0.018(2) 0.005(1) 0.005(1) 0.001(1) C(17) 0.024(2) 0.015(2) 0.020(2) 0.005(1) 0.006(1) 0.004(1) C(18) 0.028(2) 0.015(2) 0.012(1) 0.007(1) 0.006(1) 0.000(1) C(19) 0.020(2) 0.019(2) 0.021(2) 0.008(1) 0.006(1) 0.005(1) C(20) 0.023(2) 0.014(2) 0.018(2) 0.003(1) 0.002(1) 0.004(1) C(21) 0.032(2) 0.022(2) 0.023(2) -0.002(2) 0.007(2) 0.002(1) C(22) 0.019(2) 0.026(2) 0.027(2) -0.001(2) 0.004(1) 0.004(1) C(23) 0.033(2) 0.011(2) 0.022(2) 0.005(1) 0.007(1) 0.003(1) C(24) 0.033(2) 0.015(2) 0.024(2) 0.010(1) 0.008(2) 0.003(1) C(25) 0.020(4) 0.025(4) 0.056(5) -0.005(3) 0.012(4) 0.014(4) C(26) 0.028(7) 0.074(7) 0.094(8) -0.007(6) -0.010(6) 0.070(5) C(27) 0.027(5) 0.038(5) 0.050(5) 0.005(4) 0.007(4) 0.014(4) C(28) 0.037(6) 0.062(7) 0.029(4) -0.001(5) 0.015(4) -0.005(4) C(29) 0.029(5) 0.081(8) 0.038(5) 0.011(5) 0.011(4) 0.018(5) C(30) 0.025(7) 0.076(7) 0.085(7) -0.011(6) -0.006(6) 0.068(5) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 As(1) F(1) 1.700(3) . . yes As(1) F(2) 1.713(3) . . yes As(1) F(3) 1.713(3) . . yes As(1) F(4) 1.721(2) . . yes As(1) F(5) 1.724(3) . . yes As(1) F(6) 1.718(3) . . yes Cl(1) C(25) 1.729(10) . . yes S(1) C(1) 1.741(4) . . yes S(1) C(3) 1.737(4) . . yes S(2) C(2) 1.753(4) . . yes S(2) C(3) 1.742(4) . . yes S(3) C(8) 1.736(4) . . yes S(3) C(11) 1.735(4) . . yes S(4) C(8) 1.750(4) . . yes S(4) C(12) 1.726(4) . . yes S(5) C(13) 1.737(4) . . yes S(5) C(15) 1.724(4) . . yes S(6) C(14) 1.737(4) . . yes S(6) C(15) 1.721(4) . . yes S(7) C(20) 1.722(4) . . yes S(7) C(23) 1.734(4) . . yes S(8) C(20) 1.735(4) . . yes S(8) C(24) 1.726(4) . . yes O(1) C(4) 1.395(4) . . yes O(1) C(7) 1.406(4) . . yes O(2) C(16) 1.381(4) . . yes O(2) C(19) 1.398(5) . . yes N(1) C(5) 1.330(5) . . yes N(1) C(9) 1.343(6) . . yes N(2) C(6) 1.337(5) . . yes N(2) C(10) 1.340(5) . . yes N(3) C(17) 1.340(4) . . yes N(3) C(21) 1.327(6) . . yes N(4) C(18) 1.342(5) . . yes N(4) C(22) 1.326(5) . . yes C(1) C(2) 1.324(6) . . yes C(3) C(4) 1.372(5) . . yes C(4) C(5) 1.427(6) . . yes C(5) C(6) 1.409(5) . . yes C(6) C(7) 1.439(5) . . yes C(7) C(8) 1.343(5) . . yes C(9) C(10) 1.390(6) . . yes C(11) C(12) 1.328(6) . . yes C(13) C(14) 1.332(6) . . yes C(15) C(16) 1.392(5) . . yes C(16) C(17) 1.408(6) . . yes C(17) C(18) 1.414(5) . . yes C(18) C(19) 1.414(5) . . yes C(19) C(20) 1.368(5) . . yes C(21) C(22) 1.418(6) . . yes C(23) C(24) 1.331(6) . . yes C(25) C(26) 1.52(2) . . yes C(25) C(30) 1.49(2) . . yes C(26) C(27) 1.23(2) . . yes C(27) C(28) 1.33(1) . . yes C(28) C(29) 1.42(2) . . yes C(29) C(30) 1.15(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) As(1) F(2) 91.6(1) . . . yes F(1) As(1) F(3) 91.1(1) . . . yes F(1) As(1) F(4) 179.3(1) . . . yes F(1) As(1) F(5) 90.1(1) . . . yes F(1) As(1) F(6) 89.8(1) . . . yes F(2) As(1) F(3) 90.6(2) . . . yes F(2) As(1) F(4) 89.0(1) . . . yes F(2) As(1) F(5) 178.3(1) . . . yes F(2) As(1) F(6) 90.7(2) . . . yes F(3) As(1) F(4) 89.1(1) . . . yes F(3) As(1) F(5) 89.5(1) . . . yes F(3) As(1) F(6) 178.5(1) . . . yes F(4) As(1) F(5) 89.3(1) . . . yes F(4) As(1) F(6) 90.0(1) . . . yes F(5) As(1) F(6) 89.2(1) . . . yes C(1) S(1) C(3) 95.2(2) . . . yes C(2) S(2) C(3) 94.4(2) . . . yes C(8) S(3) C(11) 94.5(2) . . . yes C(8) S(4) C(12) 94.3(2) . . . yes C(13) S(5) C(15) 95.2(2) . . . yes C(14) S(6) C(15) 94.9(2) . . . yes C(20) S(7) C(23) 94.6(2) . . . yes C(20) S(8) C(24) 94.6(2) . . . yes C(4) O(1) C(7) 108.1(3) . . . yes C(16) O(2) C(19) 108.0(3) . . . yes C(5) N(1) C(9) 112.7(3) . . . yes C(6) N(2) C(10) 113.0(3) . . . yes C(17) N(3) C(21) 113.0(3) . . . yes C(18) N(4) C(22) 113.0(3) . . . yes S(1) C(1) C(2) 117.1(3) . . . yes S(2) C(2) C(1) 117.9(3) . . . yes S(1) C(3) S(2) 115.3(2) . . . yes S(1) C(3) C(4) 121.3(3) . . . yes S(2) C(3) C(4) 123.3(3) . . . yes O(1) C(4) C(3) 118.6(3) . . . yes O(1) C(4) C(5) 108.9(3) . . . yes C(3) C(4) C(5) 132.5(3) . . . yes N(1) C(5) C(4) 129.3(3) . . . yes N(1) C(5) C(6) 123.2(4) . . . yes C(4) C(5) C(6) 107.5(3) . . . yes N(2) C(6) C(5) 123.8(3) . . . yes N(2) C(6) C(7) 129.0(3) . . . yes C(5) C(6) C(7) 107.2(3) . . . yes O(1) C(7) C(6) 108.2(3) . . . yes O(1) C(7) C(8) 119.7(3) . . . yes C(6) C(7) C(8) 132.1(4) . . . yes S(3) C(8) S(4) 115.4(2) . . . yes S(3) C(8) C(7) 122.2(3) . . . yes S(4) C(8) C(7) 122.4(3) . . . yes N(1) C(9) C(10) 124.5(3) . . . yes N(2) C(10) C(9) 123.0(4) . . . yes S(3) C(11) C(12) 117.7(3) . . . yes S(4) C(12) C(11) 118.1(3) . . . yes S(5) C(13) C(14) 116.8(3) . . . yes S(6) C(14) C(13) 117.4(3) . . . yes S(5) C(15) S(6) 115.7(2) . . . yes S(5) C(15) C(16) 122.6(3) . . . yes S(6) C(15) C(16) 121.7(3) . . . yes O(2) C(16) C(15) 118.6(3) . . . yes O(2) C(16) C(17) 109.0(3) . . . yes C(15) C(16) C(17) 132.4(3) . . . yes N(3) C(17) C(16) 129.7(3) . . . yes N(3) C(17) C(18) 122.7(4) . . . yes C(16) C(17) C(18) 107.5(3) . . . yes N(4) C(18) C(17) 123.9(3) . . . yes N(4) C(18) C(19) 129.2(3) . . . yes C(17) C(18) C(19) 106.8(3) . . . yes O(2) C(19) C(18) 108.6(3) . . . yes O(2) C(19) C(20) 118.9(3) . . . yes C(18) C(19) C(20) 132.4(4) . . . yes S(7) C(20) S(8) 115.8(2) . . . yes S(7) C(20) C(19) 121.7(3) . . . yes S(8) C(20) C(19) 122.5(3) . . . yes N(3) C(21) C(22) 124.2(3) . . . yes N(4) C(22) C(21) 123.1(4) . . . yes S(7) C(23) C(24) 117.5(3) . . . yes S(8) C(24) C(23) 117.5(3) . . . yes Cl(1) C(25) C(26) 123.9(8) . . . yes Cl(1) C(25) C(30) 129.7(8) . . . yes C(26) C(25) C(30) 106.0(10) . . . yes C(25) C(26) C(27) 120(1) . . . yes C(26) C(27) C(28) 125(1) . . . yes C(27) C(28) C(29) 118.9(10) . . . yes C(28) C(29) C(30) 116(1) . . . yes C(25) C(30) C(29) 131(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 Cl(1) S(1) 3.343(3) . 2_555 ? Cl(1) S(3) 3.467(3) . . ? S(2) F(6) 3.249(3) . . ? S(2) C(15) 3.418(4) . 1_554 ? S(2) C(15) 3.525(4) . . ? S(2) C(16) 3.579(4) . . ? S(3) C(23) 3.498(4) . . ? S(4) S(8) 3.263(2) . 2_656 ? S(4) C(24) 3.453(4) . 1_554 ? S(4) C(24) 3.599(4) . . ? S(5) C(1) 3.381(4) . . ? S(5) C(2) 3.579(4) . 1_556 ? S(5) C(3) 3.586(4) . 1_556 ? S(6) F(5) 3.255(3) . . ? S(6) C(2) 3.566(4) . . ? S(7) C(30) 3.35(1) . . ? S(7) C(29) 3.35(1) . . ? S(7) C(25) 3.370(9) . 2_556 ? S(7) C(26) 3.38(1) . 2_556 ? S(7) C(25) 3.507(8) . . ? S(7) C(28) 3.52(1) . . ? F(1) C(23) 3.110(4) . 1_565 ? F(1) C(24) 3.176(4) . 1_565 ? F(1) C(11) 3.398(5) . 1_565 ? F(1) C(10) 3.417(5) . 2_666 ? F(1) C(12) 3.536(5) . 1_565 ? F(2) C(11) 3.488(5) . 1_565 ? F(2) C(13) 3.534(5) . 2_566 ? F(3) C(27) 3.22(1) . 2_566 ? F(3) C(23) 3.441(4) . 1_565 ? F(3) C(1) 3.575(5) . 2_566 ? F(4) C(13) 3.087(4) . 2_566 ? F(4) C(1) 3.169(5) . 2_566 ? F(4) C(2) 3.223(4) . . ? F(4) C(14) 3.341(4) . . ? F(5) C(14) 3.211(5) . . ? F(5) C(10) 3.301(5) . 2_666 ? F(5) C(11) 3.533(5) . 1_566 ? F(6) C(2) 3.130(5) . . ? F(6) C(22) 3.332(5) . 2_666 ? O(1) C(19) 3.535(4) . . ? O(1) C(20) 3.557(4) . . ? O(2) C(4) 3.407(4) . 1_556 ? O(2) C(3) 3.480(4) . . ? O(2) C(4) 3.504(4) . . ? O(2) C(5) 3.572(4) . 1_556 ? N(1) C(21) 3.464(5) . 2_666 ? N(1) C(17) 3.476(5) . 1_554 ? N(1) C(18) 3.548(4) . 1_554 ? N(1) C(21) 3.553(4) . . ? N(1) C(22) 3.564(5) . . ? N(2) N(4) 3.593(4) . . ? N(3) C(21) 3.369(4) . 2_667 ? N(3) N(3) 3.483(6) . 2_667 ? N(3) C(9) 3.510(5) . 2_666 ? N(4) C(10) 3.534(5) . . ? N(4) C(10) 3.538(5) . 1_556 ? N(4) C(9) 3.556(5) . . ? N(4) C(9) 3.579(4) . 1_556 ? N(4) C(6) 3.587(4) . . ? C(2) C(13) 3.354(5) . 1_554 ? C(2) C(15) 3.491(5) . . ? C(3) C(16) 3.370(5) . . ? C(4) C(19) 3.490(5) . . ? C(5) C(18) 3.364(5) . . ? C(5) C(19) 3.476(5) . 1_554 ? C(6) C(19) 3.540(5) . 1_554 ? C(6) C(20) 3.572(4) . 1_554 ? C(7) C(20) 3.405(5) . . ? C(7) C(20) 3.487(5) . 1_554 ? C(8) C(23) 3.541(5) . 1_554 ? C(9) C(22) 3.275(5) . . ? C(9) C(21) 3.587(5) . . ? C(10) C(22) 3.557(5) . . ? C(29) C(29) 3.54(2) . 2_557 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_b2art #(BDTFP)2AsF6(PhCl)0.5 at RT _database_code_CSD 181036 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Oct 31 12:47:24 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H29 As2 Cl F12 N8 O4 S16 ' _chemical_formula_moiety '4(C12 H6 N2 O S4), C6 H5 Cl, 2(As F6)' _chemical_formula_weight 1780.11 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.628(3) _cell_length_b 16.285(7) _cell_length_c 6.9693(7) _cell_angle_alpha 100.28(2) _cell_angle_beta 102.86(1) _cell_angle_gamma 97.13(3) _cell_volume 1676.4(8) _cell_formula_units_Z 1 _cell_measurement_reflns_used 80 _cell_measurement_theta_min ? _cell_measurement_theta_max 25.5 _cell_measurement_temperature 290.0 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888.00 _exptl_absorpt_coefficient_mu 1.621 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 5352 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_max 25.56 _diffrn_measured_fraction_theta_max 0.8533 _diffrn_reflns_theta_full 25.56 _diffrn_measured_fraction_theta_full 0.8533 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5352 _reflns_number_gt 4320 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.1030 _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 4320 _refine_ls_number_parameters 443 _refine_ls_goodness_of_fit_ref 1.941 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00123|Fo|^2^]' _refine_ls_shift/su_max 1.1739 _refine_diff_density_max 0.60 _refine_diff_density_min -0.88 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.122(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 As(1) As 0.68552(4) 0.20492(3) 0.33343(10) 0.0765(2) Uani 1.00 d . . . Cl(1) Cl 0.5002(6) 0.3839(4) 0.725(1) 0.219(3) Uani 0.50 d P . . S(1) S 0.38312(10) 0.14515(8) 0.3663(2) 0.0640(4) Uani 1.00 d . . . S(2) S 0.2435(1) -0.00410(8) 0.2716(2) 0.0700(4) Uani 1.00 d . . . S(3) S 0.27207(9) 0.43230(8) 0.4407(2) 0.0595(3) Uani 1.00 d . . . S(4) S 0.07853(9) 0.42166(8) 0.3594(2) 0.0597(3) Uani 1.00 d . . . S(5) S 0.3951(1) 0.23068(10) 0.9118(2) 0.0782(4) Uani 1.00 d . . . S(6) S 0.2571(1) 0.07887(9) 0.8016(2) 0.0792(4) Uani 1.00 d . . . S(7) S 0.28624(10) 0.51680(9) 0.9820(2) 0.0641(4) Uani 1.00 d . . . S(8) S 0.09254(10) 0.50584(9) 0.8916(2) 0.0644(4) Uani 1.00 d . . . F(1) F 0.7440(3) 0.1324(3) 0.405(1) 0.178(2) Uani 1.00 d . . . F(2) F 0.5942(4) 0.1376(3) 0.299(1) 0.241(3) Uani 1.00 d . . . F(3) F 0.6869(8) 0.2379(7) 0.563(1) 0.320(5) Uani 1.00 d . . . F(4) F 0.6269(4) 0.2768(3) 0.247(1) 0.167(2) Uani 1.00 d . . . F(5) F 0.7790(4) 0.2734(3) 0.382(1) 0.178(2) Uani 1.00 d . . . F(6) F 0.6953(7) 0.1755(5) 0.1084(9) 0.245(4) Uani 1.00 d . . . O(1) O 0.2347(2) 0.2442(2) 0.3575(4) 0.0524(8) Uani 1.00 d . . . O(2) O 0.2474(2) 0.3282(2) 0.8954(5) 0.0591(9) Uani 1.00 d . . . N(1) N 0.0600(3) 0.0633(3) 0.2409(7) 0.072(1) Uani 1.00 d . . . N(2) N -0.0031(3) 0.2239(3) 0.2620(6) 0.066(1) Uani 1.00 d . . . N(3) N 0.0708(4) 0.1478(3) 0.7630(7) 0.075(1) Uani 1.00 d . . . N(4) N 0.0093(3) 0.3093(3) 0.7897(6) 0.070(1) Uani 1.00 d . . . C(1) C 0.4162(4) 0.0471(4) 0.3389(9) 0.077(2) Uani 1.00 d . . . C(2) C 0.3504(4) -0.0208(3) 0.2961(8) 0.077(2) Uani 1.00 d . . . C(3) C 0.2710(4) 0.1057(3) 0.3194(6) 0.056(1) Uani 1.00 d . . . C(4) C 0.2078(4) 0.1564(3) 0.3192(7) 0.056(1) Uani 1.00 d . . . C(5) C 0.1144(4) 0.1390(3) 0.2804(7) 0.058(1) Uani 1.00 d . . . C(6) C 0.0830(3) 0.2172(3) 0.2920(6) 0.053(1) Uani 1.00 d . . . C(7) C 0.1591(3) 0.2824(3) 0.3417(6) 0.051(1) Uani 1.00 d . . . C(8) C 0.1690(3) 0.3685(3) 0.3772(6) 0.050(1) Uani 1.00 d . . . C(9) C 0.2306(4) 0.5260(3) 0.4562(8) 0.068(2) Uani 1.00 d . . . C(10) C 0.1434(4) 0.5218(3) 0.4173(7) 0.067(2) Uani 1.00 d . . . C(11) C -0.0244(5) 0.0714(4) 0.2115(9) 0.082(2) Uani 1.00 d . . . C(12) C -0.0569(4) 0.1480(4) 0.2228(9) 0.078(2) Uani 1.00 d . . . C(13) C 0.4313(5) 0.1332(4) 0.8846(9) 0.086(2) Uani 1.00 d . . . C(14) C 0.3656(5) 0.0639(4) 0.8364(8) 0.087(2) Uani 1.00 d . . . C(15) C 0.2839(4) 0.1886(3) 0.8542(7) 0.065(1) Uani 1.00 d . . . C(16) C 0.2196(4) 0.2401(3) 0.8517(7) 0.062(1) Uani 1.00 d . . . C(17) C 0.1255(4) 0.2228(3) 0.8064(7) 0.060(1) Uani 1.00 d . . . C(18) C 0.0950(4) 0.3016(3) 0.8226(6) 0.060(1) Uani 1.00 d . . . C(19) C 0.1720(3) 0.3669(3) 0.8776(6) 0.053(1) Uani 1.00 d . . . C(20) C 0.1827(3) 0.4526(3) 0.9117(6) 0.054(1) Uani 1.00 d . . . C(21) C 0.2444(5) 0.6107(4) 0.9972(9) 0.079(2) Uani 1.00 d . . . C(22) C 0.1585(5) 0.6058(4) 0.9510(9) 0.084(2) Uani 1.00 d . . . C(23) C -0.0147(5) 0.1569(4) 0.7300(9) 0.088(2) Uani 1.00 d . . . C(24) C -0.0464(4) 0.2340(4) 0.7409(9) 0.083(2) Uani 1.00 d . . . C(25) C 0.5012(7) 0.4542(9) 0.623(3) 0.242(6) Uani 1.00 d . . . C(26) C 0.5003(9) 0.406(1) 0.471(5) 0.40(1) Uani 1.00 d . . . C(27) C 0.4911(7) 0.5402(9) 0.662(2) 0.218(4) Uani 1.00 d . . . H(1) H 0.4794 0.0378 0.3449 0.0760 Uiso 1.00 calc . . . H(2) H 0.3613 -0.0786 0.2742 0.0793 Uiso 1.00 calc . . . H(3) H 0.2699 0.5804 0.4833 0.0689 Uiso 1.00 calc . . . H(4) H 0.1171 0.5722 0.4194 0.0675 Uiso 1.00 calc . . . H(5) H -0.0668 0.0222 0.1939 0.0746 Uiso 1.00 calc . . . H(6) H -0.1216 0.1461 0.1892 0.0828 Uiso 1.00 calc . . . H(7) H 0.4931 0.1246 0.8948 0.0842 Uiso 1.00 calc . . . H(8) H 0.3767 0.0056 0.8103 0.0813 Uiso 1.00 calc . . . H(9) H 0.2832 0.6645 1.0427 0.0761 Uiso 1.00 calc . . . H(10) H 0.1321 0.6549 0.9503 0.0852 Uiso 1.00 calc . . . H(11) H -0.0593 0.1072 0.7057 0.0845 Uiso 1.00 calc . . . H(12) H -0.1106 0.2286 0.7080 0.0844 Uiso 1.00 calc . . . H(13) H 0.5134 0.3621 0.3970 0.1801 Uiso 1.00 calc . . . H(14) H 0.4949 0.5556 0.8006 0.1552 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0743(4) 0.0435(3) 0.1098(4) 0.0077(3) 0.0199(3) 0.0175(3) Cl(1) 0.214(8) 0.156(5) 0.246(7) -0.068(5) -0.001(6) 0.081(4) S(1) 0.0715(8) 0.0572(7) 0.0690(7) 0.0160(6) 0.0205(6) 0.0207(5) S(2) 0.0877(10) 0.0442(6) 0.0825(8) 0.0150(6) 0.0285(7) 0.0138(5) S(3) 0.0605(8) 0.0488(6) 0.0657(6) 0.0029(6) 0.0128(6) 0.0114(5) S(4) 0.0647(8) 0.0497(6) 0.0649(6) 0.0164(5) 0.0132(6) 0.0121(5) S(5) 0.094(1) 0.0623(8) 0.0819(8) 0.0241(7) 0.0232(8) 0.0149(6) S(6) 0.131(1) 0.0462(7) 0.0622(7) 0.0161(8) 0.0276(7) 0.0122(5) S(7) 0.0623(8) 0.0566(7) 0.0706(7) 0.0022(6) 0.0164(6) 0.0118(5) S(8) 0.0675(8) 0.0613(7) 0.0691(7) 0.0197(6) 0.0205(6) 0.0159(5) F(1) 0.101(4) 0.100(3) 0.330(6) 0.010(3) -0.004(4) 0.119(3) F(2) 0.076(3) 0.144(4) 0.515(10) -0.002(3) 0.019(5) 0.183(4) F(3) 0.40(1) 0.37(1) 0.170(5) 0.00(1) 0.155(6) -0.036(7) F(4) 0.111(3) 0.110(3) 0.311(6) 0.047(3) 0.055(4) 0.105(3) F(5) 0.112(4) 0.077(3) 0.310(7) -0.016(3) -0.024(4) 0.070(3) F(6) 0.36(1) 0.248(8) 0.126(4) 0.109(7) 0.073(5) -0.013(4) O(1) 0.058(2) 0.041(2) 0.059(2) 0.010(1) 0.015(1) 0.012(1) O(2) 0.068(2) 0.044(2) 0.063(2) 0.010(2) 0.013(2) 0.012(1) N(1) 0.077(3) 0.052(2) 0.084(3) 0.001(2) 0.027(2) 0.007(2) N(2) 0.059(3) 0.056(2) 0.081(3) 0.010(2) 0.019(2) 0.004(2) N(3) 0.090(4) 0.057(3) 0.072(2) -0.005(2) 0.020(2) 0.011(2) N(4) 0.066(3) 0.073(3) 0.063(2) 0.000(2) 0.010(2) 0.005(2) C(1) 0.085(4) 0.072(3) 0.091(3) 0.034(3) 0.030(3) 0.034(3) C(2) 0.106(4) 0.056(3) 0.085(3) 0.036(3) 0.034(3) 0.026(2) C(3) 0.074(3) 0.046(2) 0.051(2) 0.014(2) 0.015(2) 0.015(2) C(4) 0.069(3) 0.044(2) 0.055(2) 0.008(2) 0.019(2) 0.012(2) C(5) 0.074(3) 0.046(2) 0.053(2) 0.006(2) 0.022(2) 0.005(2) C(6) 0.059(3) 0.049(2) 0.051(2) 0.008(2) 0.014(2) 0.007(2) C(7) 0.058(3) 0.047(2) 0.049(2) 0.011(2) 0.016(2) 0.009(2) C(8) 0.056(3) 0.044(2) 0.050(2) 0.011(2) 0.015(2) 0.012(2) C(9) 0.087(4) 0.037(2) 0.072(3) 0.001(2) 0.015(3) 0.006(2) C(10) 0.098(4) 0.040(2) 0.068(3) 0.017(2) 0.025(3) 0.011(2) C(11) 0.089(4) 0.059(3) 0.089(3) -0.010(3) 0.032(3) -0.003(3) C(12) 0.062(3) 0.069(4) 0.091(4) 0.001(3) 0.017(3) -0.002(3) C(13) 0.115(5) 0.078(4) 0.078(3) 0.047(3) 0.034(3) 0.021(3) C(14) 0.140(6) 0.066(3) 0.065(3) 0.041(3) 0.033(3) 0.020(2) C(15) 0.100(4) 0.048(2) 0.050(2) 0.014(3) 0.019(2) 0.016(2) C(16) 0.088(4) 0.042(2) 0.055(2) 0.008(2) 0.019(2) 0.010(2) C(17) 0.081(4) 0.051(3) 0.046(2) 0.002(2) 0.017(2) 0.005(2) C(18) 0.073(3) 0.054(3) 0.047(2) 0.004(2) 0.012(2) 0.009(2) C(19) 0.056(3) 0.053(2) 0.052(2) 0.012(2) 0.017(2) 0.011(2) C(20) 0.059(3) 0.052(2) 0.053(2) 0.007(2) 0.015(2) 0.014(2) C(21) 0.090(4) 0.054(3) 0.086(3) -0.002(3) 0.017(3) 0.012(3) C(22) 0.121(5) 0.049(3) 0.088(3) 0.020(3) 0.034(3) 0.015(2) C(23) 0.097(5) 0.074(4) 0.085(4) -0.021(3) 0.029(3) 0.010(3) C(24) 0.070(4) 0.091(4) 0.077(3) -0.017(3) 0.021(3) 0.007(3) C(25) 0.084(7) 0.15(1) 0.40(2) -0.036(7) -0.077(9) 0.02(1) C(26) 0.070(8) 0.26(2) 0.67(4) 0.014(10) -0.04(1) -0.22(2) C(27) 0.087(6) 0.256(10) 0.215(7) -0.016(7) 0.042(5) -0.175(6) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 As(1) F(1) 1.659(4) . . yes As(1) F(2) 1.631(5) . . yes As(1) F(3) 1.590(7) . . yes As(1) F(4) 1.687(5) . . yes As(1) F(5) 1.653(5) . . yes As(1) F(6) 1.603(6) . . yes Cl(1) C(25) 1.45(2) . . yes S(1) C(1) 1.731(6) . . yes S(1) C(3) 1.726(6) . . yes S(2) C(2) 1.702(7) . . yes S(2) C(3) 1.740(5) . . yes S(3) C(8) 1.724(5) . . yes S(3) C(9) 1.726(6) . . yes S(4) C(8) 1.740(5) . . yes S(4) C(10) 1.739(5) . . yes S(5) C(13) 1.744(6) . . yes S(5) C(15) 1.717(6) . . yes S(6) C(14) 1.714(8) . . yes S(6) C(15) 1.737(5) . . yes S(7) C(20) 1.731(5) . . yes S(7) C(21) 1.732(7) . . yes S(8) C(20) 1.737(5) . . yes S(8) C(22) 1.742(6) . . yes O(1) C(4) 1.398(5) . . yes O(1) C(7) 1.395(6) . . yes O(2) C(16) 1.403(6) . . yes O(2) C(19) 1.397(6) . . yes N(1) C(5) 1.355(6) . . yes N(1) C(11) 1.315(8) . . yes N(2) C(6) 1.337(7) . . yes N(2) C(12) 1.352(7) . . yes N(3) C(17) 1.344(7) . . yes N(3) C(23) 1.336(9) . . yes N(4) C(18) 1.333(7) . . yes N(4) C(24) 1.353(7) . . yes C(1) C(2) 1.354(8) . . yes C(3) C(4) 1.363(7) . . yes C(4) C(5) 1.406(8) . . yes C(5) C(6) 1.416(7) . . yes C(6) C(7) 1.426(7) . . yes C(7) C(8) 1.363(6) . . yes C(9) C(10) 1.319(9) . . yes C(11) C(12) 1.401(9) . . yes C(13) C(14) 1.365(9) . . yes C(15) C(16) 1.385(8) . . yes C(16) C(17) 1.414(8) . . yes C(17) C(18) 1.418(7) . . yes C(18) C(19) 1.435(7) . . yes C(19) C(20) 1.355(7) . . yes C(21) C(22) 1.299(10) . . yes C(23) C(24) 1.402(10) . . yes C(25) C(26) 1.20(3) . . yes C(25) C(27) 1.41(2) . . yes C(26) C(27) 1.40(4) . 2_666 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) As(1) F(2) 89.1(3) . . . yes F(1) As(1) F(3) 88.2(5) . . . yes F(1) As(1) F(4) 176.6(3) . . . yes F(1) As(1) F(5) 89.7(2) . . . yes F(1) As(1) F(6) 89.6(4) . . . yes F(2) As(1) F(3) 91.3(5) . . . yes F(2) As(1) F(4) 91.2(3) . . . yes F(2) As(1) F(5) 176.8(4) . . . yes F(2) As(1) F(6) 94.4(5) . . . yes F(3) As(1) F(4) 95.3(5) . . . yes F(3) As(1) F(5) 85.8(5) . . . yes F(3) As(1) F(6) 173.9(5) . . . yes F(4) As(1) F(5) 90.1(2) . . . yes F(4) As(1) F(6) 86.9(4) . . . yes F(5) As(1) F(6) 88.6(5) . . . yes C(1) S(1) C(3) 95.3(3) . . . yes C(2) S(2) C(3) 94.8(3) . . . yes C(8) S(3) C(9) 94.8(3) . . . yes C(8) S(4) C(10) 94.4(3) . . . yes C(13) S(5) C(15) 95.3(3) . . . yes C(14) S(6) C(15) 94.3(3) . . . yes C(20) S(7) C(21) 94.8(3) . . . yes C(20) S(8) C(22) 94.1(3) . . . yes C(4) O(1) C(7) 108.6(4) . . . yes C(16) O(2) C(19) 108.5(4) . . . yes C(5) N(1) C(11) 112.1(5) . . . yes C(6) N(2) C(12) 112.7(5) . . . yes C(17) N(3) C(23) 111.9(5) . . . yes C(18) N(4) C(24) 113.2(5) . . . yes S(1) C(1) C(2) 115.9(5) . . . yes S(2) C(2) C(1) 118.7(4) . . . yes S(1) C(3) S(2) 115.3(3) . . . yes S(1) C(3) C(4) 122.9(4) . . . yes S(2) C(3) C(4) 121.8(4) . . . yes O(1) C(4) C(3) 118.7(5) . . . yes O(1) C(4) C(5) 108.4(4) . . . yes C(3) C(4) C(5) 132.8(4) . . . yes N(1) C(5) C(4) 129.0(5) . . . yes N(1) C(5) C(6) 123.2(5) . . . yes C(4) C(5) C(6) 107.8(4) . . . yes N(2) C(6) C(5) 123.7(4) . . . yes N(2) C(6) C(7) 129.2(5) . . . yes C(5) C(6) C(7) 107.2(4) . . . yes O(1) C(7) C(6) 108.0(4) . . . yes O(1) C(7) C(8) 119.2(4) . . . yes C(6) C(7) C(8) 132.8(5) . . . yes S(3) C(8) S(4) 115.4(3) . . . yes S(3) C(8) C(7) 122.3(4) . . . yes S(4) C(8) C(7) 122.3(4) . . . yes S(3) C(9) C(10) 118.1(4) . . . yes S(4) C(10) C(9) 117.2(4) . . . yes N(1) C(11) C(12) 125.7(5) . . . yes N(2) C(12) C(11) 122.7(6) . . . yes S(5) C(13) C(14) 115.3(6) . . . yes S(6) C(14) C(13) 118.8(5) . . . yes S(5) C(15) S(6) 116.4(3) . . . yes S(5) C(15) C(16) 121.3(4) . . . yes S(6) C(15) C(16) 122.3(5) . . . yes O(2) C(16) C(15) 118.3(5) . . . yes O(2) C(16) C(17) 108.7(4) . . . yes C(15) C(16) C(17) 132.9(5) . . . yes N(3) C(17) C(16) 129.2(5) . . . yes N(3) C(17) C(18) 123.2(5) . . . yes C(16) C(17) C(18) 107.5(4) . . . yes N(4) C(18) C(17) 124.0(5) . . . yes N(4) C(18) C(19) 128.7(5) . . . yes C(17) C(18) C(19) 107.3(5) . . . yes O(2) C(19) C(18) 108.0(4) . . . yes O(2) C(19) C(20) 118.9(4) . . . yes C(18) C(19) C(20) 133.1(5) . . . yes S(7) C(20) S(8) 115.2(3) . . . yes S(7) C(20) C(19) 122.9(4) . . . yes S(8) C(20) C(19) 121.9(4) . . . yes S(7) C(21) C(22) 117.7(5) . . . yes S(8) C(22) C(21) 118.2(5) . . . yes N(3) C(23) C(24) 125.7(6) . . . yes N(4) C(24) C(23) 122.0(6) . . . yes Cl(1) C(25) C(26) 88(1) . . . yes Cl(1) C(25) C(27) 137(1) . . . yes C(26) C(25) C(27) 132(2) . . . yes C(25) C(26) C(27) 102(1) . . 2_666 yes C(25) C(27) C(26) 123(1) . . 2_666 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 Cl(1) S(5) 3.420(7) . . ? Cl(1) S(7) 3.517(7) . 2_667 ? S(1) F(2) 3.448(7) . . ? S(1) C(13) 3.568(6) . . ? S(1) C(13) 3.578(7) . 1_554 ? S(2) F(1) 3.328(6) . 2_656 ? S(3) C(25) 3.47(1) . . ? S(3) C(27) 3.52(1) . . ? S(4) S(8) 3.323(2) . 2_566 ? S(6) F(1) 3.480(5) . 2_656 ? S(6) C(3) 3.510(4) . 1_556 ? S(6) C(3) 3.516(5) . . ? S(7) C(9) 3.583(6) . 1_556 ? S(8) C(10) 3.527(5) . 1_556 ? S(8) S(8) 3.549(3) . 2_567 ? F(1) C(14) 3.379(8) . 2_656 ? F(1) C(2) 3.447(9) . 2_656 ? F(1) C(24) 3.580(8) . 1_655 ? F(2) C(1) 3.075(9) . . ? F(2) C(13) 3.382(10) . 1_554 ? F(2) C(14) 3.423(9) . 2_656 ? F(3) C(21) 3.435(10) . 2_667 ? F(4) C(26) 3.46(2) . . ? F(4) C(21) 3.466(9) . 2_666 ? F(5) C(9) 3.294(7) . 2_666 ? F(5) C(10) 3.335(7) . 2_666 ? F(5) C(24) 3.478(9) . 1_655 ? F(5) C(21) 3.491(9) . 2_666 ? F(5) C(22) 3.516(9) . 2_666 ? F(6) C(2) 3.305(8) . 2_655 ? O(1) C(16) 3.468(6) . 1_554 ? O(1) C(16) 3.516(6) . . ? N(1) C(11) 3.392(7) . 2_555 ? N(1) N(1) 3.579(9) . 2_555 ? N(2) C(24) 3.530(8) . . ? N(2) C(24) 3.581(8) . 1_554 ? N(3) C(5) 3.550(6) . 1_556 ? N(3) C(5) 3.559(7) . . ? N(3) C(11) 3.597(8) . 2_556 ? C(1) C(14) 3.483(8) . 1_554 ? C(4) C(15) 3.573(6) . . ? C(6) C(17) 3.481(6) . . ? C(7) C(17) 3.584(6) . 1_554 ? C(8) C(19) 3.482(6) . . ? C(8) C(19) 3.489(6) . 1_554 ? C(11) C(23) 3.596(8) . . ? C(12) C(23) 3.421(9) . . ? C(12) C(24) 3.592(8) . . ? #------------------------------------------------------------------------------ data_b2plt #(BDTFP)2PF6(PhCl)0.5 at 90 K _database_code_CSD 181037 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 27 16:37:56 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H29 Cl F12 N8 O4 P2 S16 ' _chemical_formula_moiety '4(C12 H6 N2 O S4), C6 H5 Cl, 2(F6 P)' _chemical_formula_weight 1692.22 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.159(4) _cell_length_b 16.159(3) _cell_length_c 13.749(2) _cell_angle_alpha 103.585(10) _cell_angle_beta 99.92(2) _cell_angle_gamma 78.70(2) _cell_volume 3181.9(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 80 _cell_measurement_theta_min ? _cell_measurement_theta_max 25.9 _cell_measurement_temperature 90.0 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704.00 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 7682 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 25.90 _diffrn_measured_fraction_theta_max 0.6129 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.6129 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2529 _reflns_number_gt 3947 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0668 _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 3947 _refine_ls_number_parameters 875 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_shift/su_max 1.6423 _refine_diff_density_max 0.47 _refine_diff_density_min -0.53 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00360(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cl(1) Cl 0.5019(3) 0.3832(2) 0.0643(3) 0.052(1) Uani 1.00 d . . . S(1) S 0.7352(2) 0.4289(2) 0.7457(2) 0.0185(7) Uani 1.00 d . . . S(2) S 0.9330(2) 0.4257(2) 0.7893(2) 0.0163(7) Uani 1.00 d . . . S(3) S 0.6320(2) 0.1341(2) 0.6296(2) 0.0191(7) Uani 1.00 d . . . S(4) S 0.7780(2) -0.0168(2) 0.6083(2) 0.0205(8) Uani 1.00 d . . . S(5) S 0.7059(2) 0.5322(2) 0.5212(2) 0.0192(7) Uani 1.00 d . . . S(6) S 0.9054(2) 0.5047(2) 0.5548(2) 0.0180(7) Uani 1.00 d . . . S(7) S 0.5707(2) 0.2410(2) 0.3964(2) 0.0216(8) Uani 1.00 d . . . S(8) S 0.7088(2) 0.0836(2) 0.3792(2) 0.0203(8) Uani 1.00 d . . . S(9) S 0.7216(2) 0.4505(2) 0.2522(2) 0.0170(7) Uani 1.00 d . . . S(10) S 0.9194(2) 0.4389(2) 0.2869(2) 0.0180(7) Uani 1.00 d . . . S(11) S 0.6079(2) 0.1523(2) 0.1336(2) 0.0174(7) Uani 1.00 d . . . S(12) S 0.7543(2) 0.0047(2) 0.1081(2) 0.0196(7) Uani 1.00 d . . . S(13) S 0.7061(2) 0.5058(2) 0.0139(2) 0.0183(7) Uani 1.00 d . . . S(14) S 0.9021(2) 0.4978(2) 0.0544(2) 0.0199(8) Uani 1.00 d . . . S(15) S 0.5981(2) 0.2108(2) -0.1076(2) 0.0208(8) Uani 1.00 d . . . S(16) S 0.7396(2) 0.0591(2) -0.1254(2) 0.0223(8) Uani 1.00 d . . . P(1) P 0.3027(2) 0.2124(2) 0.1671(2) 0.0231(8) Uani 1.00 d . . . P(2) P 0.3280(2) 0.1998(2) 0.6940(2) 0.0245(9) Uani 1.00 d . . . F(1) F 0.3051(5) 0.1690(4) 0.2607(5) 0.043(2) Uani 1.00 d . . . F(2) F 0.3564(5) 0.2837(4) 0.2394(6) 0.049(2) Uani 1.00 d . . . F(3) F 0.3978(4) 0.1516(4) 0.1452(5) 0.031(2) Uani 1.00 d . . . F(4) F 0.3001(5) 0.2544(5) 0.0739(5) 0.061(2) Uani 1.00 d . . . F(5) F 0.2483(5) 0.1369(5) 0.0998(6) 0.046(2) Uani 1.00 d . . . F(6) F 0.2081(4) 0.2720(4) 0.1902(5) 0.031(2) Uani 1.00 d . . . F(7) F 0.3298(5) 0.1454(5) 0.7767(6) 0.060(2) Uani 1.00 d . . . F(8) F 0.3890(5) 0.2604(5) 0.7741(7) 0.063(3) Uani 1.00 d . . . F(9) F 0.4189(4) 0.1382(4) 0.6597(5) 0.039(2) Uani 1.00 d . . . F(10) F 0.3294(6) 0.2521(5) 0.6113(5) 0.062(2) Uani 1.00 d . . . F(11) F 0.2675(5) 0.1367(6) 0.6160(7) 0.069(3) Uani 1.00 d . . . F(12) F 0.2378(4) 0.2615(4) 0.7282(5) 0.037(2) Uani 1.00 d . . . O(1) O 0.7800(5) 0.2390(4) 0.6923(5) 0.015(2) Uani 1.00 d . . . O(2) O 0.7291(5) 0.3371(4) 0.4595(5) 0.018(2) Uani 1.00 d . . . O(3) O 0.7602(4) 0.2586(4) 0.1930(5) 0.013(2) Uani 1.00 d . . . O(4) O 0.7477(5) 0.3120(4) -0.0427(5) 0.015(2) Uani 1.00 d . . . N(1) N 1.0233(6) 0.2264(5) 0.7469(6) 0.018(2) Uani 1.00 d . . . N(2) N 0.9651(6) 0.0589(5) 0.6684(7) 0.020(2) Uani 1.00 d . . . N(3) N 0.9739(6) 0.3061(5) 0.5107(6) 0.020(3) Uani 1.00 d . . . N(4) N 0.9031(7) 0.1467(6) 0.4382(7) 0.025(3) Uani 1.00 d . . . N(5) N 1.0035(6) 0.2389(6) 0.2386(6) 0.018(2) Uani 1.00 d . . . N(6) N 0.9383(6) 0.0750(5) 0.1666(6) 0.014(2) Uani 1.00 d . . . N(7) N 0.9894(6) 0.2993(6) 0.0062(7) 0.020(3) Uani 1.00 d . . . N(8) N 0.9300(6) 0.1329(6) -0.0610(6) 0.023(3) Uani 1.00 d . . . C(1) C 0.7740(7) 0.5267(7) 0.7845(8) 0.020(3) Uani 1.00 d . . . C(2) C 0.8620(8) 0.5263(7) 0.8036(8) 0.024(3) Uani 1.00 d . . . C(3) C 0.8427(7) 0.3680(6) 0.7528(8) 0.012(3) Uani 1.00 d . . . C(4) C 0.8569(7) 0.2815(7) 0.7258(8) 0.019(3) Uani 1.00 d . . . C(5) C 0.9361(7) 0.2158(6) 0.7208(8) 0.012(3) Uani 1.00 d . . . C(6) C 0.9073(7) 0.1345(7) 0.6839(8) 0.018(3) Uani 1.00 d . . . C(7) C 0.8102(7) 0.1487(6) 0.6685(8) 0.015(3) Uani 1.00 d . . . C(8) C 0.7472(7) 0.0953(7) 0.6370(8) 0.017(3) Uani 1.00 d . . . C(9) C 1.0791(7) 0.1509(7) 0.7315(8) 0.021(3) Uani 1.00 d . . . C(10) C 1.0520(7) 0.0700(7) 0.6940(9) 0.024(3) Uani 1.00 d . . . C(11) C 0.6008(8) 0.0327(7) 0.5921(8) 0.020(3) Uani 1.00 d . . . C(12) C 0.6657(7) -0.0354(7) 0.5849(7) 0.017(3) Uani 1.00 d . . . C(13) C 0.7600(8) 0.6226(7) 0.5590(8) 0.024(3) Uani 1.00 d . . . C(14) C 0.8490(8) 0.6106(7) 0.5768(9) 0.022(3) Uani 1.00 d . . . C(15) C 0.8056(7) 0.4594(7) 0.5207(8) 0.016(3) Uani 1.00 d . . . C(16) C 0.8102(7) 0.3740(7) 0.4931(8) 0.021(3) Uani 1.00 d . . . C(17) C 0.8858(7) 0.3013(7) 0.4866(8) 0.015(3) Uani 1.00 d . . . C(18) C 0.8473(8) 0.2246(7) 0.4509(8) 0.020(3) Uani 1.00 d . . . C(19) C 0.7530(7) 0.2463(7) 0.4370(8) 0.017(3) Uani 1.00 d . . . C(20) C 0.6861(7) 0.1961(7) 0.4084(8) 0.020(3) Uani 1.00 d . . . C(21) C 1.0266(7) 0.2255(7) 0.4980(8) 0.026(3) Uani 1.00 d . . . C(22) C 0.9901(8) 0.1501(7) 0.4625(9) 0.025(3) Uani 1.00 d . . . C(23) C 0.5328(8) 0.1423(7) 0.3621(8) 0.022(3) Uani 1.00 d . . . C(24) C 0.5938(7) 0.0700(7) 0.3540(8) 0.018(3) Uani 1.00 d . . . C(25) C 0.7657(8) 0.5474(7) 0.2955(9) 0.026(3) Uani 1.00 d . . . C(26) C 0.8555(8) 0.5420(7) 0.3113(8) 0.022(3) Uani 1.00 d . . . C(27) C 0.8268(7) 0.3854(6) 0.2506(8) 0.013(3) Uani 1.00 d . . . C(28) C 0.8369(7) 0.2971(6) 0.2223(8) 0.014(3) Uani 1.00 d . . . C(29) C 0.9150(7) 0.2328(6) 0.2181(7) 0.013(3) Uani 1.00 d . . . C(30) C 0.8828(7) 0.1522(6) 0.1823(7) 0.012(3) Uani 1.00 d . . . C(31) C 0.7863(8) 0.1694(7) 0.1672(8) 0.018(3) Uani 1.00 d . . . C(32) C 0.7216(7) 0.1142(7) 0.1399(8) 0.013(3) Uani 1.00 d . . . C(33) C 1.0580(7) 0.1641(7) 0.2254(8) 0.015(3) Uani 1.00 d . . . C(34) C 1.0257(7) 0.0825(6) 0.1896(8) 0.015(3) Uani 1.00 d . . . C(35) C 0.5770(7) 0.0513(7) 0.0962(8) 0.023(3) Uani 1.00 d . . . C(36) C 0.6450(7) -0.0169(7) 0.0863(8) 0.021(3) Uani 1.00 d . . . C(37) C 0.7477(8) 0.6008(7) 0.0551(8) 0.020(3) Uani 1.00 d . . . C(38) C 0.8369(8) 0.5988(7) 0.0751(8) 0.018(3) Uani 1.00 d . . . C(39) C 0.8124(7) 0.4428(6) 0.0152(7) 0.013(3) Uani 1.00 d . . . C(40) C 0.8226(7) 0.3534(7) -0.0115(8) 0.016(3) Uani 1.00 d . . . C(41) C 0.9022(7) 0.2893(7) -0.0166(8) 0.017(3) Uani 1.00 d . . . C(42) C 0.8728(7) 0.2091(7) -0.0491(8) 0.017(3) Uani 1.00 d . . . C(43) C 0.7755(7) 0.2214(7) -0.0657(8) 0.018(3) Uani 1.00 d . . . C(44) C 0.7104(8) 0.1715(7) -0.0950(8) 0.021(3) Uani 1.00 d . . . C(45) C 1.0472(7) 0.2225(7) -0.0056(8) 0.021(3) Uani 1.00 d . . . C(46) C 1.0164(8) 0.1449(7) -0.0372(8) 0.024(3) Uani 1.00 d . . . C(47) C 0.5610(8) 0.1105(7) -0.1480(8) 0.019(3) Uani 1.00 d . . . C(48) C 0.6269(8) 0.0409(7) -0.1548(8) 0.025(3) Uani 1.00 d . . . C(49) C 0.4949(8) 0.4581(7) 0.1773(8) 0.024(3) Uani 1.00 d . . . C(50) C 0.5005(8) 0.5433(7) 0.1804(8) 0.029(3) Uani 1.00 d . . . C(51) C 0.4990(9) 0.6005(8) 0.275(1) 0.055(4) Uani 1.00 d . . . C(52) C 0.4922(8) 0.5741(9) 0.3612(9) 0.037(4) Uani 1.00 d . . . C(53) C 0.4861(8) 0.4881(9) 0.3547(9) 0.034(4) Uani 1.00 d . . . C(54) C 0.4882(7) 0.4307(7) 0.2638(9) 0.035(3) Uani 1.00 d . . . H(1) H 0.7321 0.5815 0.7910 0.0260 Uiso 1.00 calc . . . H(2) H 0.8873 0.5799 0.8246 0.0220 Uiso 1.00 calc . . . H(3) H 1.1440 0.1512 0.7494 0.0234 Uiso 1.00 calc . . . H(4) H 1.0985 0.0193 0.6855 0.0198 Uiso 1.00 calc . . . H(5) H 0.5364 0.0274 0.5779 0.0256 Uiso 1.00 calc . . . H(6) H 0.6516 -0.0937 0.5666 0.0145 Uiso 1.00 calc . . . H(7) H 0.7253 0.6807 0.5696 0.0246 Uiso 1.00 calc . . . H(8) H 0.8825 0.6585 0.5999 0.0239 Uiso 1.00 calc . . . H(9) H 1.0919 0.2201 0.5141 0.0185 Uiso 1.00 calc . . . H(10) H 1.0324 0.0971 0.4564 0.0250 Uiso 1.00 calc . . . H(11) H 0.4679 0.1389 0.3480 0.0184 Uiso 1.00 calc . . . H(12) H 0.5765 0.0128 0.3360 0.0162 Uiso 1.00 calc . . . H(13) H 0.7239 0.6016 0.3096 0.0221 Uiso 1.00 calc . . . H(14) H 0.8840 0.5941 0.3330 0.0246 Uiso 1.00 calc . . . H(15) H 1.1223 0.1641 0.2430 0.0125 Uiso 1.00 calc . . . H(16) H 1.0720 0.0319 0.1829 0.0110 Uiso 1.00 calc . . . H(17) H 0.5131 0.0451 0.0842 0.0203 Uiso 1.00 calc . . . H(18) H 0.6317 -0.0748 0.0675 0.0215 Uiso 1.00 calc . . . H(19) H 0.7068 0.6550 0.0659 0.0230 Uiso 1.00 calc . . . H(20) H 0.8638 0.6515 0.1037 0.0161 Uiso 1.00 calc . . . H(21) H 1.1133 0.2230 0.0069 0.0227 Uiso 1.00 calc . . . H(22) H 1.0623 0.0933 -0.0397 0.0245 Uiso 1.00 calc . . . H(23) H 0.4975 0.1063 -0.1617 0.0178 Uiso 1.00 calc . . . H(24) H 0.6120 -0.0183 -0.1776 0.0249 Uiso 1.00 calc . . . H(25) H 0.5062 0.5617 0.1202 0.0217 Uiso 1.00 calc . . . H(26) H 0.5034 0.6610 0.2793 0.0410 Uiso 1.00 calc . . . H(27) H 0.4915 0.6128 0.4244 0.0388 Uiso 1.00 calc . . . H(28) H 0.4833 0.4665 0.4130 0.0308 Uiso 1.00 calc . . . H(29) H 0.4841 0.3708 0.2596 0.0248 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.058(2) 0.047(2) 0.031(2) 0.025(2) 0.006(2) -0.001(2) S(1) 0.018(2) 0.015(1) 0.020(1) 0.000(1) 0.002(1) 0.003(1) S(2) 0.016(1) 0.013(1) 0.018(1) -0.003(1) 0.001(1) -0.001(1) S(3) 0.020(2) 0.021(1) 0.017(1) -0.005(1) 0.004(1) 0.003(1) S(4) 0.021(2) 0.018(1) 0.022(2) -0.006(1) 0.002(1) 0.002(1) S(5) 0.017(1) 0.019(1) 0.021(2) 0.000(1) 0.003(1) 0.005(1) S(6) 0.017(1) 0.021(1) 0.017(1) -0.006(1) 0.000(1) 0.004(1) S(7) 0.024(2) 0.016(1) 0.025(2) -0.005(1) 0.003(1) 0.003(1) S(8) 0.028(2) 0.018(1) 0.016(1) -0.006(1) 0.005(1) 0.001(1) S(9) 0.014(1) 0.015(1) 0.020(1) 0.001(1) 0.003(1) 0.004(1) S(10) 0.015(1) 0.021(1) 0.019(1) -0.004(1) 0.002(1) 0.003(1) S(11) 0.017(2) 0.018(1) 0.015(1) -0.003(1) 0.001(1) -0.001(1) S(12) 0.017(1) 0.019(1) 0.022(2) -0.003(1) 0.002(1) 0.002(1) S(13) 0.017(2) 0.018(1) 0.018(1) 0.002(1) 0.004(1) 0.003(1) S(14) 0.019(2) 0.023(2) 0.017(1) -0.004(1) 0.003(1) 0.002(1) S(15) 0.022(2) 0.017(1) 0.022(2) -0.002(1) 0.005(1) 0.001(1) S(16) 0.032(2) 0.016(1) 0.019(2) 0.000(1) 0.008(1) 0.003(1) P(1) 0.019(2) 0.014(2) 0.033(2) 0.002(1) 0.003(1) 0.003(1) P(2) 0.023(2) 0.016(2) 0.033(2) -0.001(1) 0.010(1) 0.001(1) F(1) 0.034(4) 0.049(4) 0.052(4) -0.001(3) 0.011(3) 0.025(3) F(2) 0.026(4) 0.020(4) 0.090(6) -0.010(3) 0.002(4) -0.013(4) F(3) 0.018(4) 0.023(4) 0.047(4) 0.004(3) 0.008(3) -0.002(3) F(4) 0.062(5) 0.082(5) 0.051(4) 0.016(4) 0.022(4) 0.049(3) F(5) 0.029(4) 0.033(5) 0.053(5) 0.002(4) -0.002(4) -0.023(4) F(6) 0.019(4) 0.019(4) 0.051(4) 0.005(3) 0.004(3) 0.003(3) F(7) 0.064(5) 0.066(5) 0.062(5) 0.010(4) 0.030(4) 0.037(4) F(8) 0.043(5) 0.061(6) 0.073(6) -0.031(4) 0.019(4) -0.036(5) F(9) 0.028(4) 0.033(4) 0.057(5) 0.008(3) 0.018(3) 0.010(3) F(10) 0.079(6) 0.056(5) 0.057(4) 0.035(4) 0.042(4) 0.033(3) F(11) 0.032(5) 0.070(6) 0.075(7) -0.020(4) 0.016(4) -0.059(5) F(12) 0.028(4) 0.022(4) 0.061(5) 0.004(3) 0.020(3) 0.002(3) O(1) 0.016(4) 0.014(4) 0.018(4) 0.001(3) 0.005(3) 0.006(3) O(2) 0.024(4) 0.011(4) 0.017(4) -0.004(3) 0.004(3) 0.001(3) O(3) 0.007(4) 0.014(4) 0.015(4) -0.007(3) -0.002(3) -0.004(3) O(4) 0.014(4) 0.008(3) 0.023(4) -0.003(3) 0.005(3) 0.000(3) N(1) 0.016(5) 0.010(4) 0.028(5) 0.006(4) 0.009(4) 0.009(4) N(2) 0.019(5) 0.017(5) 0.020(5) 0.002(4) 0.002(4) 0.003(4) N(3) 0.029(6) 0.014(5) 0.016(5) 0.000(4) 0.003(4) 0.004(4) N(4) 0.035(6) 0.023(5) 0.020(5) -0.004(5) 0.010(4) 0.005(4) N(5) 0.012(5) 0.021(5) 0.021(5) -0.001(4) 0.000(4) 0.005(4) N(6) 0.017(5) 0.006(4) 0.021(5) 0.000(4) 0.008(4) 0.000(4) N(7) 0.017(5) 0.024(5) 0.021(5) -0.006(4) 0.002(4) 0.006(4) N(8) 0.024(5) 0.027(5) 0.019(5) 0.005(4) 0.008(4) 0.012(4) C(1) 0.018(6) 0.020(6) 0.026(6) -0.004(5) -0.002(5) 0.014(5) C(2) 0.034(7) 0.011(6) 0.028(7) -0.005(5) 0.008(6) 0.001(5) C(3) 0.016(6) 0.009(5) 0.011(5) -0.002(5) 0.005(4) 0.004(4) C(4) 0.013(6) 0.026(6) 0.018(6) -0.008(5) 0.002(5) 0.001(5) C(5) 0.013(6) 0.007(5) 0.019(5) -0.002(5) 0.000(4) 0.007(4) C(6) 0.010(6) 0.026(6) 0.020(6) 0.000(5) 0.004(5) 0.010(5) C(7) 0.025(6) 0.010(5) 0.010(6) -0.010(5) 0.000(5) -0.002(4) C(8) 0.014(6) 0.025(6) 0.016(5) 0.003(5) 0.009(4) 0.010(4) C(9) 0.012(6) 0.030(6) 0.022(6) -0.010(5) -0.003(5) 0.007(5) C(10) 0.011(6) 0.030(7) 0.024(6) 0.005(5) -0.005(5) 0.004(5) C(11) 0.023(6) 0.029(6) 0.011(6) -0.018(5) -0.002(5) -0.001(5) C(12) 0.015(6) 0.027(6) 0.015(5) -0.010(5) 0.001(4) 0.012(4) C(13) 0.028(7) 0.014(6) 0.024(7) -0.002(5) 0.001(5) -0.003(5) C(14) 0.023(7) 0.017(6) 0.019(6) 0.001(5) 0.006(5) -0.010(5) C(15) 0.010(6) 0.021(6) 0.018(6) 0.004(5) 0.007(5) 0.005(5) C(16) 0.013(6) 0.039(7) 0.014(6) -0.016(5) 0.001(5) 0.005(5) C(17) 0.016(6) 0.015(5) 0.012(6) -0.001(5) 0.004(5) -0.001(4) C(18) 0.022(6) 0.026(6) 0.012(5) 0.004(5) 0.010(5) 0.008(5) C(19) 0.030(7) 0.016(5) 0.010(5) -0.015(5) -0.005(5) 0.007(4) C(20) 0.028(6) 0.012(6) 0.017(6) 0.002(5) 0.001(5) 0.001(5) C(21) 0.014(6) 0.037(7) 0.027(7) -0.008(5) -0.010(5) 0.014(5) C(22) 0.021(6) 0.022(6) 0.034(7) 0.006(5) 0.012(5) 0.012(5) C(23) 0.036(7) 0.015(6) 0.012(6) -0.003(5) 0.002(5) -0.002(5) C(24) 0.022(6) 0.021(6) 0.017(6) -0.010(5) 0.007(5) 0.006(4) C(25) 0.026(7) 0.021(6) 0.027(7) 0.006(6) 0.008(5) 0.002(5) C(26) 0.024(7) 0.029(6) 0.014(6) -0.004(5) 0.006(5) 0.008(5) C(27) 0.020(6) 0.013(5) 0.007(5) -0.002(5) 0.003(4) 0.004(4) C(28) 0.010(6) 0.012(5) 0.023(6) 0.001(5) 0.000(5) 0.009(4) C(29) 0.014(6) 0.016(5) 0.011(6) -0.005(5) 0.001(4) 0.004(4) C(30) 0.010(6) 0.015(5) 0.010(5) 0.001(5) 0.000(4) 0.003(4) C(31) 0.025(6) 0.014(6) 0.013(6) 0.001(5) 0.009(5) 0.000(4) C(32) 0.016(6) 0.016(5) 0.004(5) 0.004(5) 0.005(4) 0.002(4) C(33) 0.009(6) 0.017(5) 0.021(6) 0.001(5) 0.006(5) 0.006(4) C(34) 0.017(6) 0.009(5) 0.018(6) 0.004(5) 0.004(5) 0.002(4) C(35) 0.016(6) 0.037(7) 0.020(6) -0.008(5) 0.000(5) 0.010(5) C(36) 0.019(6) 0.027(7) 0.015(6) -0.005(5) 0.007(5) -0.005(5) C(37) 0.023(6) 0.012(5) 0.025(6) -0.002(5) 0.008(5) 0.004(4) C(38) 0.025(6) 0.016(6) 0.015(6) -0.008(5) 0.008(5) -0.002(5) C(39) 0.010(6) 0.017(5) 0.012(6) -0.001(5) 0.002(4) 0.002(4) C(40) 0.016(6) 0.017(5) 0.012(6) -0.002(5) 0.003(5) -0.001(4) C(41) 0.020(6) 0.016(6) 0.009(5) 0.010(5) 0.002(5) 0.002(4) C(42) 0.028(6) 0.016(6) 0.011(6) -0.001(5) 0.007(5) 0.009(5) C(43) 0.018(6) 0.019(6) 0.013(6) 0.005(5) 0.005(5) 0.002(5) C(44) 0.037(7) 0.018(6) 0.010(5) -0.003(5) 0.001(5) 0.008(4) C(45) 0.015(6) 0.025(7) 0.013(6) 0.008(5) 0.000(5) -0.002(5) C(46) 0.038(8) 0.015(6) 0.014(6) 0.004(6) 0.002(5) 0.002(5) C(47) 0.029(7) 0.020(6) 0.011(5) -0.008(5) 0.006(5) 0.001(4) C(48) 0.034(7) 0.025(6) 0.017(6) -0.010(6) 0.002(5) 0.005(5) C(49) 0.023(6) 0.038(7) 0.013(6) -0.003(5) 0.005(5) 0.007(5) C(50) 0.035(7) 0.031(7) 0.025(6) 0.005(6) 0.013(5) 0.015(5) C(51) 0.023(7) 0.028(7) 0.12(1) -0.010(6) -0.005(8) 0.028(7) C(52) 0.024(7) 0.055(9) 0.022(7) -0.001(7) -0.007(6) -0.002(7) C(53) 0.020(7) 0.064(9) 0.017(6) -0.006(6) 0.002(5) 0.009(6) C(54) 0.015(6) 0.044(6) 0.064(7) 0.001(5) 0.010(5) 0.047(5) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl(1) C(49) 1.74(1) . . yes S(1) C(1) 1.73(1) . . yes S(1) C(3) 1.73(1) . . yes S(2) C(2) 1.75(1) . . yes S(2) C(3) 1.74(1) . . yes S(3) C(8) 1.73(1) . . yes S(3) C(11) 1.73(1) . . yes S(4) C(8) 1.75(1) . . yes S(4) C(12) 1.75(1) . . yes S(5) C(13) 1.75(1) . . yes S(5) C(15) 1.724(10) . . yes S(6) C(14) 1.74(1) . . yes S(6) C(15) 1.75(1) . . yes S(7) C(20) 1.75(1) . . yes S(7) C(23) 1.73(1) . . yes S(8) C(20) 1.74(1) . . yes S(8) C(24) 1.76(1) . . yes S(9) C(25) 1.76(1) . . yes S(9) C(27) 1.73(1) . . yes S(10) C(26) 1.74(1) . . yes S(10) C(27) 1.73(1) . . yes S(11) C(32) 1.71(1) . . yes S(11) C(35) 1.72(1) . . yes S(12) C(32) 1.71(1) . . yes S(12) C(36) 1.72(1) . . yes S(13) C(37) 1.71(1) . . yes S(13) C(39) 1.73(1) . . yes S(14) C(38) 1.72(1) . . yes S(14) C(39) 1.71(1) . . yes S(15) C(44) 1.69(1) . . yes S(15) C(47) 1.76(1) . . yes S(16) C(44) 1.75(1) . . yes S(16) C(48) 1.75(1) . . yes P(1) F(1) 1.597(7) . . yes P(1) F(2) 1.591(8) . . yes P(1) F(3) 1.610(7) . . yes P(1) F(4) 1.576(7) . . yes P(1) F(5) 1.621(8) . . yes P(1) F(6) 1.598(7) . . yes P(2) F(7) 1.584(7) . . yes P(2) F(8) 1.588(9) . . yes P(2) F(9) 1.606(7) . . yes P(2) F(10) 1.573(7) . . yes P(2) F(11) 1.595(9) . . yes P(2) F(12) 1.597(7) . . yes O(1) C(4) 1.42(1) . . yes O(1) C(7) 1.42(1) . . yes O(2) C(16) 1.43(1) . . yes O(2) C(19) 1.41(1) . . yes O(3) C(28) 1.38(1) . . yes O(3) C(31) 1.39(1) . . yes O(4) C(40) 1.38(1) . . yes O(4) C(43) 1.42(1) . . yes N(1) C(5) 1.34(1) . . yes N(1) C(9) 1.34(1) . . yes N(2) C(6) 1.35(1) . . yes N(2) C(10) 1.34(1) . . yes N(3) C(17) 1.33(1) . . yes N(3) C(21) 1.38(1) . . yes N(4) C(18) 1.36(1) . . yes N(4) C(22) 1.31(1) . . yes N(5) C(29) 1.34(1) . . yes N(5) C(33) 1.32(1) . . yes N(6) C(30) 1.35(1) . . yes N(6) C(34) 1.33(1) . . yes N(7) C(41) 1.34(1) . . yes N(7) C(45) 1.37(1) . . yes N(8) C(42) 1.35(1) . . yes N(8) C(46) 1.34(1) . . yes C(1) C(2) 1.31(2) . . yes C(3) C(4) 1.34(1) . . yes C(4) C(5) 1.44(1) . . yes C(5) C(6) 1.42(1) . . yes C(6) C(7) 1.43(1) . . yes C(7) C(8) 1.36(2) . . yes C(9) C(10) 1.40(2) . . yes C(11) C(12) 1.32(1) . . yes C(13) C(14) 1.31(2) . . yes C(15) C(16) 1.33(1) . . yes C(16) C(17) 1.47(1) . . yes C(17) C(18) 1.42(2) . . yes C(18) C(19) 1.40(2) . . yes C(19) C(20) 1.37(2) . . yes C(21) C(22) 1.38(2) . . yes C(23) C(24) 1.34(1) . . yes C(25) C(26) 1.33(2) . . yes C(27) C(28) 1.37(1) . . yes C(28) C(29) 1.41(1) . . yes C(29) C(30) 1.43(1) . . yes C(30) C(31) 1.42(1) . . yes C(31) C(32) 1.40(2) . . yes C(33) C(34) 1.44(1) . . yes C(35) C(36) 1.35(1) . . yes C(37) C(38) 1.33(2) . . yes C(39) C(40) 1.39(1) . . yes C(40) C(41) 1.43(1) . . yes C(41) C(42) 1.40(2) . . yes C(42) C(43) 1.44(2) . . yes C(43) C(44) 1.35(2) . . yes C(45) C(46) 1.37(2) . . yes C(47) C(48) 1.35(1) . . yes C(49) C(50) 1.39(2) . . yes C(49) C(54) 1.39(1) . . yes C(50) C(51) 1.41(2) . . yes C(51) C(52) 1.38(2) . . yes C(52) C(53) 1.39(2) . . yes C(53) C(54) 1.37(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(3) 94.3(5) . . . yes C(2) S(2) C(3) 93.6(5) . . . yes C(8) S(3) C(11) 94.4(5) . . . yes C(8) S(4) C(12) 93.7(5) . . . yes C(13) S(5) C(15) 94.3(5) . . . yes C(14) S(6) C(15) 94.4(5) . . . yes C(20) S(7) C(23) 94.7(5) . . . yes C(20) S(8) C(24) 95.1(5) . . . yes C(25) S(9) C(27) 94.7(5) . . . yes C(26) S(10) C(27) 95.4(5) . . . yes C(32) S(11) C(35) 94.4(5) . . . yes C(32) S(12) C(36) 94.1(5) . . . yes C(37) S(13) C(39) 94.0(5) . . . yes C(38) S(14) C(39) 95.5(5) . . . yes C(44) S(15) C(47) 96.4(5) . . . yes C(44) S(16) C(48) 94.4(5) . . . yes F(1) P(1) F(2) 89.4(4) . . . yes F(1) P(1) F(3) 88.2(4) . . . yes F(1) P(1) F(4) 179.4(5) . . . yes F(1) P(1) F(5) 86.8(4) . . . yes F(1) P(1) F(6) 90.9(4) . . . yes F(2) P(1) F(3) 89.6(4) . . . yes F(2) P(1) F(4) 91.2(5) . . . yes F(2) P(1) F(5) 176.2(5) . . . yes F(2) P(1) F(6) 90.5(4) . . . yes F(3) P(1) F(4) 91.6(4) . . . yes F(3) P(1) F(5) 90.2(4) . . . yes F(3) P(1) F(6) 179.0(4) . . . yes F(4) P(1) F(5) 92.6(5) . . . yes F(4) P(1) F(6) 89.3(4) . . . yes F(5) P(1) F(6) 89.6(4) . . . yes F(7) P(2) F(8) 89.0(5) . . . yes F(7) P(2) F(9) 89.2(4) . . . yes F(7) P(2) F(10) 178.1(4) . . . yes F(7) P(2) F(11) 89.1(5) . . . yes F(7) P(2) F(12) 91.0(4) . . . yes F(8) P(2) F(9) 89.0(4) . . . yes F(8) P(2) F(10) 90.6(5) . . . yes F(8) P(2) F(11) 178.1(5) . . . yes F(8) P(2) F(12) 90.8(4) . . . yes F(9) P(2) F(10) 88.9(4) . . . yes F(9) P(2) F(11) 90.5(4) . . . yes F(9) P(2) F(12) 179.7(4) . . . yes F(10) P(2) F(11) 91.2(5) . . . yes F(10) P(2) F(12) 90.9(4) . . . yes F(11) P(2) F(12) 89.7(4) . . . yes C(4) O(1) C(7) 108.9(8) . . . yes C(16) O(2) C(19) 108.6(8) . . . yes C(28) O(3) C(31) 109.0(8) . . . yes C(40) O(4) C(43) 110.2(8) . . . yes C(5) N(1) C(9) 111.4(9) . . . yes C(6) N(2) C(10) 112.1(9) . . . yes C(17) N(3) C(21) 111.7(9) . . . yes C(18) N(4) C(22) 115(1) . . . yes C(29) N(5) C(33) 114.2(9) . . . yes C(30) N(6) C(34) 112.6(9) . . . yes C(41) N(7) C(45) 112.5(10) . . . yes C(42) N(8) C(46) 111.1(10) . . . yes S(1) C(1) C(2) 118.4(8) . . . yes S(2) C(2) C(1) 117.5(9) . . . yes S(1) C(3) S(2) 116.1(6) . . . yes S(1) C(3) C(4) 122.5(9) . . . yes S(2) C(3) C(4) 121.3(8) . . . yes O(1) C(4) C(3) 118.2(9) . . . yes O(1) C(4) C(5) 107.1(9) . . . yes C(3) C(4) C(5) 134(1) . . . yes N(1) C(5) C(4) 127.6(10) . . . yes N(1) C(5) C(6) 124.1(9) . . . yes C(4) C(5) C(6) 108.3(9) . . . yes N(2) C(6) C(5) 123.5(10) . . . yes N(2) C(6) C(7) 128(1) . . . yes C(5) C(6) C(7) 108.0(9) . . . yes O(1) C(7) C(6) 107.8(9) . . . yes O(1) C(7) C(8) 118.6(9) . . . yes C(6) C(7) C(8) 133.6(10) . . . yes S(3) C(8) S(4) 116.1(6) . . . yes S(3) C(8) C(7) 122.0(8) . . . yes S(4) C(8) C(7) 121.8(8) . . . yes N(1) C(9) C(10) 125.3(10) . . . yes N(2) C(10) C(9) 123.6(10) . . . yes S(3) C(11) C(12) 118.2(9) . . . yes S(4) C(12) C(11) 117.5(9) . . . yes S(5) C(13) C(14) 118.5(9) . . . yes S(6) C(14) C(13) 117.3(10) . . . yes S(5) C(15) S(6) 115.5(6) . . . yes S(5) C(15) C(16) 124.4(9) . . . yes S(6) C(15) C(16) 120.1(8) . . . yes O(2) C(16) C(15) 120.2(9) . . . yes O(2) C(16) C(17) 106.2(9) . . . yes C(15) C(16) C(17) 133(1) . . . yes N(3) C(17) C(16) 126.6(10) . . . yes N(3) C(17) C(18) 126.3(9) . . . yes C(16) C(17) C(18) 107.1(9) . . . yes N(4) C(18) C(17) 119(1) . . . yes N(4) C(18) C(19) 131(1) . . . yes C(17) C(18) C(19) 109.0(9) . . . yes O(2) C(19) C(18) 109.0(9) . . . yes O(2) C(19) C(20) 119.6(9) . . . yes C(18) C(19) C(20) 131(1) . . . yes S(7) C(20) S(8) 115.1(6) . . . yes S(7) C(20) C(19) 121.9(8) . . . yes S(8) C(20) C(19) 123.0(8) . . . yes N(3) C(21) C(22) 122(1) . . . yes N(4) C(22) C(21) 124.8(10) . . . yes S(7) C(23) C(24) 118.9(9) . . . yes S(8) C(24) C(23) 116.1(9) . . . yes S(9) C(25) C(26) 117.4(9) . . . yes S(10) C(26) C(25) 116.9(9) . . . yes S(9) C(27) S(10) 115.6(6) . . . yes S(9) C(27) C(28) 122.6(8) . . . yes S(10) C(27) C(28) 121.8(8) . . . yes O(3) C(28) C(27) 118.9(9) . . . yes O(3) C(28) C(29) 109.4(8) . . . yes C(27) C(28) C(29) 131(1) . . . yes N(5) C(29) C(28) 131.1(10) . . . yes N(5) C(29) C(30) 122.8(9) . . . yes C(28) C(29) C(30) 106.1(9) . . . yes N(6) C(30) C(29) 123.5(9) . . . yes N(6) C(30) C(31) 128(1) . . . yes C(29) C(30) C(31) 107.9(9) . . . yes O(3) C(31) C(30) 107.5(9) . . . yes O(3) C(31) C(32) 120.9(9) . . . yes C(30) C(31) C(32) 131.4(10) . . . yes S(11) C(32) S(12) 117.3(6) . . . yes S(11) C(32) C(31) 122.0(8) . . . yes S(12) C(32) C(31) 120.6(8) . . . yes N(5) C(33) C(34) 123.2(10) . . . yes N(6) C(34) C(33) 123.7(9) . . . yes S(11) C(35) C(36) 116.9(9) . . . yes S(12) C(36) C(35) 117.3(9) . . . yes S(13) C(37) C(38) 119.1(8) . . . yes S(14) C(38) C(37) 115.8(9) . . . yes S(13) C(39) S(14) 115.6(6) . . . yes S(13) C(39) C(40) 121.3(8) . . . yes S(14) C(39) C(40) 123.1(8) . . . yes O(4) C(40) C(39) 120.9(9) . . . yes O(4) C(40) C(41) 108.2(9) . . . yes C(39) C(40) C(41) 130(1) . . . yes N(7) C(41) C(40) 129(1) . . . yes N(7) C(41) C(42) 124.1(9) . . . yes C(40) C(41) C(42) 106.7(10) . . . yes N(8) C(42) C(41) 123(1) . . . yes N(8) C(42) C(43) 126(1) . . . yes C(41) C(42) C(43) 109.8(9) . . . yes O(4) C(43) C(42) 105.1(9) . . . yes O(4) C(43) C(44) 117.7(9) . . . yes C(42) C(43) C(44) 137(1) . . . yes S(15) C(44) S(16) 116.0(7) . . . yes S(15) C(44) C(43) 123.7(9) . . . yes S(16) C(44) C(43) 120.3(9) . . . yes N(7) C(45) C(46) 122(1) . . . yes N(8) C(46) C(45) 126.8(10) . . . yes S(15) C(47) C(48) 115.7(9) . . . yes S(16) C(48) C(47) 117.5(9) . . . yes Cl(1) C(49) C(50) 119.3(8) . . . yes Cl(1) C(49) C(54) 119.4(9) . . . yes C(50) C(49) C(54) 121(1) . . . yes C(49) C(50) C(51) 116(1) . . . yes C(50) C(51) C(52) 122(1) . . . yes C(51) C(52) C(53) 118(1) . . . yes C(52) C(53) C(54) 120(1) . . . yes C(49) C(54) C(53) 120(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 Cl(1) S(13) 3.440(4) . 2_665 ? Cl(1) S(15) 3.460(4) . . ? S(1) C(52) 3.51(1) . 2_666 ? S(1) C(53) 3.53(1) . 2_666 ? S(2) S(14) 3.241(4) . 2_766 ? S(3) F(9) 3.312(7) . . ? S(3) C(47) 3.54(1) . 1_556 ? S(4) F(11) 3.274(9) . 2_656 ? S(5) C(25) 3.45(1) . . ? S(6) S(10) 3.262(4) . 2_766 ? S(6) S(6) 3.424(6) . 2_766 ? S(6) C(26) 3.471(10) . . ? S(6) C(2) 3.52(1) . . ? S(8) C(8) 3.46(1) . . ? S(8) C(32) 3.48(1) . . ? S(8) F(11) 3.522(10) . 2_656 ? S(9) C(49) 3.40(1) . . ? S(9) C(50) 3.47(1) . . ? S(9) S(13) 3.552(4) . . ? S(10) S(14) 3.498(4) . . ? S(11) F(3) 3.218(7) . . ? S(11) C(23) 3.57(1) . . ? S(12) F(5) 3.214(8) . 2_655 ? S(12) S(16) 3.483(4) . . ? S(13) C(1) 3.59(1) . 1_554 ? S(14) C(2) 3.52(1) . 1_554 ? S(14) S(14) 3.564(6) . 2_765 ? S(14) C(26) 3.60(1) . . ? S(15) F(8) 3.343(8) . 1_554 ? S(16) F(5) 3.235(8) . 2_655 ? S(16) C(8) 3.475(10) . 1_554 ? S(16) C(32) 3.59(1) . . ? F(1) C(12) 3.29(1) . 2_656 ? F(1) C(48) 3.39(1) . 2_655 ? F(1) C(23) 3.48(1) . . ? F(2) C(54) 3.32(1) . . ? F(2) C(1) 3.36(1) . 2_666 ? F(2) C(13) 3.43(1) . 2_666 ? F(3) C(35) 2.97(1) . . ? F(3) C(48) 3.24(1) . 2_655 ? F(3) C(23) 3.33(1) . . ? F(3) C(36) 3.45(1) . 2_655 ? F(4) C(37) 3.16(1) . 2_665 ? F(5) C(36) 3.28(1) . 2_655 ? F(5) C(48) 3.29(1) . 2_655 ? F(5) C(45) 3.33(1) . 1_455 ? F(5) C(33) 3.52(1) . 1_455 ? F(6) C(2) 3.21(1) . 2_666 ? F(6) C(1) 3.25(1) . 2_666 ? F(6) C(33) 3.28(1) . 1_455 ? F(6) C(45) 3.37(1) . 1_455 ? F(6) N(5) 3.45(1) . 1_455 ? F(6) C(13) 3.47(1) . 2_666 ? F(6) C(14) 3.47(1) . 2_666 ? F(7) C(36) 3.05(1) . 2_656 ? F(7) C(47) 3.45(1) . 1_556 ? F(7) C(24) 3.59(1) . 2_656 ? F(8) C(51) 3.32(2) . 2_666 ? F(8) C(47) 3.41(1) . 1_556 ? F(8) C(37) 3.50(1) . 2_666 ? F(9) C(11) 3.11(1) . . ? F(9) C(47) 3.17(1) . 1_556 ? F(9) C(24) 3.37(1) . 2_656 ? F(9) C(12) 3.53(1) . 2_656 ? F(10) C(25) 3.33(1) . 2_666 ? F(10) C(13) 3.39(1) . 2_666 ? F(11) C(12) 3.09(1) . 2_656 ? F(11) C(9) 3.44(1) . 1_455 ? F(12) C(25) 3.17(1) . 2_666 ? F(12) C(37) 3.28(1) . 2_666 ? F(12) C(9) 3.28(1) . 1_455 ? F(12) C(38) 3.30(1) . 2_666 ? F(12) C(26) 3.34(1) . 2_666 ? F(12) N(1) 3.47(1) . 1_455 ? O(1) C(43) 3.42(1) . 1_556 ? O(1) C(19) 3.49(1) . . ? O(1) C(18) 3.58(1) . . ? O(3) C(19) 3.43(1) . . ? O(3) C(43) 3.51(1) . . ? O(3) O(4) 3.511(9) . . ? N(1) C(45) 3.37(1) . 1_556 ? N(1) C(21) 3.43(1) . . ? N(1) C(46) 3.54(1) . 1_556 ? N(1) N(7) 3.58(1) . 1_556 ? N(2) C(34) 3.31(1) . 2_756 ? N(2) C(22) 3.43(1) . 2_756 ? N(2) N(6) 3.45(1) . 2_756 ? N(2) C(22) 3.59(1) . . ? N(4) C(6) 3.42(1) . . ? N(4) C(30) 3.50(1) . . ? N(4) C(10) 3.54(1) . 2_756 ? N(5) C(45) 3.47(1) . . ? N(5) N(7) 3.52(1) . . ? N(5) C(21) 3.58(1) . . ? N(6) C(10) 3.33(1) . 2_756 ? N(6) N(8) 3.45(1) . . ? N(6) C(46) 3.57(1) . 2_755 ? N(8) C(30) 3.47(1) . . ? N(8) C(6) 3.47(1) . 1_554 ? N(8) C(34) 3.51(1) . 2_755 ? N(8) C(5) 3.58(1) . 1_554 ? C(3) C(40) 3.37(1) . 1_556 ? C(3) C(16) 3.54(1) . . ? C(3) C(41) 3.60(1) . 1_556 ? C(4) C(41) 3.47(1) . 1_556 ? C(4) C(17) 3.49(1) . . ? C(4) C(42) 3.51(1) . 1_556 ? C(5) C(42) 3.49(1) . 1_556 ? C(6) C(22) 3.57(2) . . ? C(9) C(46) 3.50(2) . 1_556 ? C(9) C(21) 3.60(1) . . ? C(11) C(48) 3.41(1) . 1_556 ? C(11) C(24) 3.45(1) . . ? C(13) C(25) 3.55(2) . . ? C(14) C(26) 3.57(2) . . ? C(16) C(27) 3.44(1) . . ? C(17) C(28) 3.57(1) . . ? C(18) C(29) 3.56(1) . . ? C(18) C(28) 3.57(1) . . ? C(24) C(35) 3.46(1) . . ? C(25) C(37) 3.56(2) . . ? C(26) C(38) 3.53(1) . . ? C(27) C(40) 3.51(1) . . ? C(27) C(39) 3.53(1) . . ? C(28) C(40) 3.50(1) . . ? C(28) C(41) 3.56(1) . . ? C(29) C(41) 3.52(1) . . ? C(29) C(42) 3.56(1) . . ? C(30) C(42) 3.48(1) . . ? C(31) C(43) 3.47(1) . . ? C(31) C(44) 3.60(1) . . ? C(32) C(44) 3.53(1) . . ? C(33) C(45) 3.49(1) . . ? C(33) C(46) 3.51(1) . . ? C(34) C(46) 3.47(1) . . ? C(35) C(35) 3.54(2) . 2_655 ? #------------------------------------------------------------------------------ data_b2prt #(BDTFP)2PF6(PhCl)0.5 at RT _database_code_CSD 181038 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Dec 22 14:35:58 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? # CHEMICAL DATA _chemical_formula_sum 'C54 H29 Cl F12 N8 O4 P2 S16 ' _chemical_formula_moiety '4(C12 H6 N2 O S4), C6 H5 Cl, 2(F6 P)' _chemical_formula_weight 1692.22 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.438(5) _cell_length_b 16.147(2) _cell_length_c 6.9811(8) _cell_angle_alpha 100.911(9) _cell_angle_beta 101.81(2) _cell_angle_gamma 97.25(2) _cell_volume 1647.7(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 80 _cell_measurement_theta_min ? _cell_measurement_theta_max 25.5 _cell_measurement_temperature 290.0 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852.00 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 4506 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 25.57 _diffrn_measured_fraction_theta_max 0.7226 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 0.7226 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1482 _reflns_number_gt 2850 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0502 _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 2850 _refine_ls_number_parameters 443 _refine_ls_goodness_of_fit_ref 1.656 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_shift/su_max 4.2515 _refine_diff_density_max 0.41 _refine_diff_density_min -0.46 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0223(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cl(1) Cl -0.0032(4) 0.3820(4) 0.7187(9) 0.173(2) Uani 0.50 d P . . S(1) S 0.77214(9) 0.43543(10) 0.4395(2) 0.0510(4) Uani 1.00 d . . . S(2) S 0.57738(9) 0.42570(10) 0.3592(2) 0.0515(4) Uani 1.00 d . . . S(3) S 0.88245(10) 0.1450(1) 0.3701(2) 0.0561(5) Uani 1.00 d . . . S(4) S 0.7415(1) -0.0050(1) 0.2713(2) 0.0610(5) Uani 1.00 d . . . S(5) S 0.78919(9) 0.5190(1) 0.9820(2) 0.0572(5) Uani 1.00 d . . . S(6) S 0.59446(9) 0.5065(1) 0.8928(2) 0.0557(5) Uani 1.00 d . . . S(7) S 0.9020(1) 0.2300(1) 0.9216(2) 0.0693(5) Uani 1.00 d . . . S(8) S 0.7641(1) 0.0768(1) 0.8051(2) 0.0695(5) Uani 1.00 d . . . P(1) P 0.1853(1) 0.2043(1) 0.3419(3) 0.0721(6) Uani 1.00 d . . . F(1) F 0.2751(3) 0.2657(3) 0.3685(8) 0.142(2) Uani 1.00 d . . . F(2) F 0.1308(3) 0.2703(3) 0.2676(9) 0.162(2) Uani 1.00 d . . . F(3) F 0.0975(3) 0.1440(3) 0.3256(9) 0.157(2) Uani 1.00 d . . . F(4) F 0.2393(3) 0.1347(3) 0.4021(9) 0.160(2) Uani 1.00 d . . . F(5) F 0.1863(4) 0.2440(5) 0.5582(8) 0.239(3) Uani 1.00 d . . . F(6) F 0.1855(4) 0.1681(4) 0.1251(7) 0.197(3) Uani 1.00 d . . . O(1) O 0.7340(2) 0.2460(2) 0.3578(5) 0.044(1) Uani 1.00 d . . . O(2) O 0.7520(2) 0.3281(2) 0.8967(5) 0.050(1) Uani 1.00 d . . . N(1) N 0.4938(3) 0.2270(3) 0.2589(7) 0.057(1) Uani 1.00 d . . . N(2) N 0.5565(3) 0.0646(3) 0.2377(6) 0.059(2) Uani 1.00 d . . . N(3) N 0.5117(3) 0.3089(3) 0.7887(6) 0.058(2) Uani 1.00 d . . . N(4) N 0.5750(3) 0.1468(3) 0.7606(6) 0.064(2) Uani 1.00 d . . . C(1) C 0.7306(4) 0.5309(4) 0.4589(8) 0.057(2) Uani 1.00 d . . . C(2) C 0.6428(4) 0.5277(3) 0.4228(8) 0.055(2) Uani 1.00 d . . . C(3) C 0.6682(3) 0.3721(3) 0.3764(6) 0.039(1) Uani 1.00 d . . . C(4) C 0.6578(3) 0.2852(3) 0.3425(7) 0.042(2) Uani 1.00 d . . . C(5) C 0.5808(3) 0.2190(4) 0.2903(7) 0.047(2) Uani 1.00 d . . . C(6) C 0.6115(3) 0.1405(3) 0.2792(7) 0.046(2) Uani 1.00 d . . . C(7) C 0.7069(4) 0.1577(3) 0.3195(7) 0.045(2) Uani 1.00 d . . . C(8) C 0.7689(3) 0.1056(4) 0.3210(7) 0.047(2) Uani 1.00 d . . . C(9) C 0.9151(4) 0.0446(4) 0.3419(8) 0.062(2) Uani 1.00 d . . . C(10) C 0.8502(4) -0.0224(4) 0.2984(8) 0.061(2) Uani 1.00 d . . . C(11) C 0.4390(4) 0.1502(4) 0.2141(9) 0.068(2) Uani 1.00 d . . . C(12) C 0.4708(4) 0.0731(4) 0.2076(9) 0.066(2) Uani 1.00 d . . . C(13) C 0.7459(4) 0.6130(4) 0.9935(9) 0.070(2) Uani 1.00 d . . . C(14) C 0.6579(4) 0.6078(4) 0.9507(8) 0.065(2) Uani 1.00 d . . . C(15) C 0.6858(3) 0.4527(4) 0.9107(7) 0.046(2) Uani 1.00 d . . . C(16) C 0.6761(3) 0.3667(4) 0.8770(7) 0.046(2) Uani 1.00 d . . . C(17) C 0.5988(3) 0.3010(4) 0.8241(7) 0.047(2) Uani 1.00 d . . . C(18) C 0.6302(4) 0.2223(4) 0.8088(7) 0.056(2) Uani 1.00 d . . . C(19) C 0.7251(4) 0.2390(4) 0.8536(7) 0.049(2) Uani 1.00 d . . . C(20) C 0.7890(4) 0.1879(4) 0.8598(7) 0.053(2) Uani 1.00 d . . . C(21) C 0.9380(4) 0.1318(4) 0.8949(9) 0.073(2) Uani 1.00 d . . . C(22) C 0.8752(4) 0.0624(4) 0.8413(8) 0.074(2) Uani 1.00 d . . . C(23) C 0.4577(4) 0.2336(5) 0.7409(9) 0.076(2) Uani 1.00 d . . . C(24) C 0.4882(4) 0.1540(5) 0.7265(9) 0.079(2) Uani 1.00 d . . . C(25) C 0.0006(6) 0.4475(8) 0.621(2) 0.172(5) Uani 1.00 d . . . C(26) C 0.0076(6) 0.4133(7) 0.426(2) 0.225(5) Uani 1.00 d . . . C(27) C -0.0062(5) 0.5305(8) 0.679(1) 0.170(4) Uani 1.00 d . . . H(1) H 0.7728 0.5847 0.4927 0.0608 Uiso 1.00 calc . . . H(2) H 0.6180 0.5786 0.4288 0.0623 Uiso 1.00 calc . . . H(3) H 0.9790 0.0382 0.3578 0.0676 Uiso 1.00 calc . . . H(4) H 0.8651 -0.0820 0.2800 0.0565 Uiso 1.00 calc . . . H(5) H 0.3736 0.1497 0.1924 0.0624 Uiso 1.00 calc . . . H(6) H 0.4253 0.0224 0.1805 0.0615 Uiso 1.00 calc . . . H(7) H 0.7868 0.6691 1.0386 0.0738 Uiso 1.00 calc . . . H(8) H 0.6292 0.6596 0.9587 0.0747 Uiso 1.00 calc . . . H(9) H 1.0018 0.1247 0.9110 0.0871 Uiso 1.00 calc . . . H(10) H 0.8888 0.0048 0.8205 0.0956 Uiso 1.00 calc . . . H(11) H 0.3907 0.2309 0.7240 0.0783 Uiso 1.00 calc . . . H(12) H 0.4424 0.1033 0.6799 0.0834 Uiso 1.00 calc . . . H(13) H 0.0105 0.3457 0.4194 0.0778 Uiso 1.00 calc . . . H(14) H -0.0055 0.5445 0.8326 0.0778 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.152(5) 0.137(5) 0.199(5) -0.057(4) -0.013(4) 0.072(4) S(1) 0.0471(8) 0.0437(9) 0.0580(8) 0.0004(7) 0.0084(7) 0.0100(7) S(2) 0.0509(8) 0.0448(9) 0.0596(8) 0.0140(7) 0.0101(7) 0.0128(7) S(3) 0.0571(9) 0.052(1) 0.0616(9) 0.0113(8) 0.0132(7) 0.0183(8) S(4) 0.072(1) 0.0393(9) 0.0748(10) 0.0115(8) 0.0217(8) 0.0136(8) S(5) 0.0505(9) 0.051(1) 0.0673(9) 0.0003(8) 0.0128(7) 0.0125(8) S(6) 0.0539(9) 0.057(1) 0.0611(9) 0.0169(8) 0.0159(7) 0.0182(8) S(7) 0.079(1) 0.056(1) 0.076(1) 0.0197(9) 0.0207(8) 0.0150(9) S(8) 0.112(1) 0.043(1) 0.0546(9) 0.0137(9) 0.0221(9) 0.0119(8) P(1) 0.064(1) 0.038(1) 0.111(1) 0.0044(9) 0.0161(10) 0.0145(10) F(1) 0.091(3) 0.071(3) 0.261(6) -0.008(2) 0.015(3) 0.068(3) F(2) 0.092(3) 0.096(4) 0.327(7) 0.046(3) 0.045(4) 0.101(4) F(3) 0.067(3) 0.100(4) 0.315(6) -0.002(3) 0.035(3) 0.092(4) F(4) 0.096(3) 0.091(3) 0.307(6) 0.009(3) 0.017(4) 0.113(4) F(5) 0.292(7) 0.274(9) 0.118(4) -0.017(6) 0.086(4) -0.040(5) F(6) 0.252(6) 0.207(7) 0.119(4) 0.061(5) 0.043(4) -0.009(4) O(1) 0.043(2) 0.039(2) 0.051(2) 0.009(2) 0.008(2) 0.013(2) O(2) 0.054(2) 0.040(2) 0.057(2) 0.010(2) 0.012(2) 0.010(2) N(1) 0.047(3) 0.052(3) 0.072(3) 0.007(2) 0.014(2) 0.013(3) N(2) 0.065(3) 0.036(3) 0.072(3) 0.000(3) 0.021(2) 0.006(2) N(3) 0.054(3) 0.056(3) 0.055(3) -0.004(3) 0.009(2) 0.006(2) N(4) 0.086(4) 0.043(3) 0.057(3) -0.008(3) 0.017(3) 0.010(2) C(1) 0.065(4) 0.042(4) 0.061(3) -0.001(3) 0.015(3) 0.014(3) C(2) 0.078(4) 0.033(3) 0.058(3) 0.014(3) 0.015(3) 0.015(3) C(3) 0.049(3) 0.040(3) 0.028(2) 0.010(3) 0.008(2) 0.007(2) C(4) 0.045(3) 0.039(3) 0.046(3) 0.010(3) 0.011(2) 0.013(3) C(5) 0.051(3) 0.040(4) 0.049(3) 0.002(3) 0.014(2) 0.006(3) C(6) 0.057(3) 0.038(3) 0.043(3) 0.004(3) 0.018(2) 0.004(3) C(7) 0.058(3) 0.037(3) 0.042(3) 0.008(3) 0.015(2) 0.009(3) C(8) 0.057(3) 0.039(3) 0.049(3) 0.007(3) 0.013(3) 0.019(3) C(9) 0.070(4) 0.066(4) 0.063(4) 0.031(3) 0.024(3) 0.022(3) C(10) 0.080(4) 0.044(4) 0.073(4) 0.029(3) 0.028(3) 0.027(3) C(11) 0.049(3) 0.066(5) 0.084(4) 0.002(3) 0.021(3) 0.001(4) C(12) 0.065(4) 0.044(4) 0.083(4) -0.005(3) 0.024(3) 0.003(3) C(13) 0.091(5) 0.042(4) 0.072(4) -0.001(4) 0.022(3) 0.003(3) C(14) 0.081(4) 0.043(4) 0.073(4) 0.018(3) 0.025(3) 0.010(3) C(15) 0.041(3) 0.049(4) 0.045(3) 0.005(3) 0.008(2) 0.011(3) C(16) 0.052(3) 0.044(4) 0.038(3) 0.004(3) 0.006(2) 0.006(3) C(17) 0.057(3) 0.046(4) 0.033(3) -0.003(3) 0.009(2) 0.006(3) C(18) 0.073(4) 0.046(4) 0.042(3) -0.005(3) 0.007(3) 0.008(3) C(19) 0.064(4) 0.040(3) 0.044(3) 0.004(3) 0.014(3) 0.009(3) C(20) 0.079(4) 0.042(4) 0.043(3) 0.013(3) 0.021(3) 0.012(3) C(21) 0.101(5) 0.067(5) 0.063(4) 0.037(4) 0.026(3) 0.018(3) C(22) 0.116(5) 0.063(4) 0.051(3) 0.044(4) 0.027(3) 0.007(3) C(23) 0.063(4) 0.083(5) 0.070(4) -0.017(4) 0.009(3) 0.014(4) C(24) 0.081(5) 0.073(5) 0.066(4) -0.032(4) 0.011(3) 0.009(4) C(25) 0.062(6) 0.16(1) 0.23(1) -0.006(7) -0.027(7) -0.013(9) C(26) 0.066(6) 0.16(1) 0.35(2) 0.043(6) -0.039(8) -0.108(10) C(27) 0.060(5) 0.22(1) 0.160(7) 0.025(6) 0.004(5) -0.112(6) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl(1) C(25) 1.36(1) . . yes S(1) C(1) 1.736(6) . . yes S(1) C(3) 1.715(5) . . yes S(2) C(2) 1.747(6) . . yes S(2) C(3) 1.733(5) . . yes S(3) C(8) 1.727(5) . . yes S(3) C(9) 1.745(7) . . yes S(4) C(8) 1.732(6) . . yes S(4) C(10) 1.716(6) . . yes S(5) C(13) 1.728(7) . . yes S(5) C(15) 1.727(5) . . yes S(6) C(14) 1.726(6) . . yes S(6) C(15) 1.743(6) . . yes S(7) C(20) 1.724(6) . . yes S(7) C(21) 1.736(7) . . yes S(8) C(20) 1.737(6) . . yes S(8) C(22) 1.733(7) . . yes P(1) F(1) 1.555(4) . . yes P(1) F(2) 1.539(5) . . yes P(1) F(3) 1.537(4) . . yes P(1) F(4) 1.552(5) . . yes P(1) F(5) 1.521(5) . . yes P(1) F(6) 1.517(5) . . yes O(1) C(4) 1.400(6) . . yes O(1) C(7) 1.393(6) . . yes O(2) C(16) 1.390(6) . . yes O(2) C(19) 1.404(6) . . yes N(1) C(5) 1.343(6) . . yes N(1) C(11) 1.353(7) . . yes N(2) C(6) 1.345(6) . . yes N(2) C(12) 1.325(7) . . yes N(3) C(17) 1.343(6) . . yes N(3) C(23) 1.327(7) . . yes N(4) C(18) 1.338(7) . . yes N(4) C(24) 1.337(8) . . yes C(1) C(2) 1.319(7) . . yes C(3) C(4) 1.362(7) . . yes C(4) C(5) 1.429(7) . . yes C(5) C(6) 1.403(8) . . yes C(6) C(7) 1.422(7) . . yes C(7) C(8) 1.352(7) . . yes C(9) C(10) 1.320(8) . . yes C(11) C(12) 1.392(9) . . yes C(13) C(14) 1.318(8) . . yes C(15) C(16) 1.347(8) . . yes C(16) C(17) 1.428(7) . . yes C(17) C(18) 1.411(8) . . yes C(18) C(19) 1.413(7) . . yes C(19) C(20) 1.362(8) . . yes C(21) C(22) 1.324(9) . . yes C(23) C(24) 1.416(10) . . yes C(25) C(26) 1.40(2) . . yes C(25) C(27) 1.35(1) . . yes C(26) C(27) 1.27(2) . 2_566 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(3) 94.5(3) . . . yes C(2) S(2) C(3) 94.8(3) . . . yes C(8) S(3) C(9) 95.1(3) . . . yes C(8) S(4) C(10) 95.2(3) . . . yes C(13) S(5) C(15) 95.1(3) . . . yes C(14) S(6) C(15) 95.5(3) . . . yes C(20) S(7) C(21) 95.5(3) . . . yes C(20) S(8) C(22) 95.0(3) . . . yes F(1) P(1) F(2) 91.2(3) . . . yes F(1) P(1) F(3) 177.5(3) . . . yes F(1) P(1) F(4) 89.5(3) . . . yes F(1) P(1) F(5) 87.9(3) . . . yes F(1) P(1) F(6) 90.5(3) . . . yes F(2) P(1) F(3) 89.9(3) . . . yes F(2) P(1) F(4) 176.2(3) . . . yes F(2) P(1) F(5) 90.7(4) . . . yes F(2) P(1) F(6) 87.9(4) . . . yes F(3) P(1) F(4) 89.6(3) . . . yes F(3) P(1) F(5) 89.8(3) . . . yes F(3) P(1) F(6) 91.8(3) . . . yes F(4) P(1) F(5) 93.1(4) . . . yes F(4) P(1) F(6) 88.3(3) . . . yes F(5) P(1) F(6) 177.9(4) . . . yes C(4) O(1) C(7) 108.8(4) . . . yes C(16) O(2) C(19) 109.0(4) . . . yes C(5) N(1) C(11) 112.0(5) . . . yes C(6) N(2) C(12) 112.1(5) . . . yes C(17) N(3) C(23) 112.2(6) . . . yes C(18) N(4) C(24) 113.3(6) . . . yes S(1) C(1) C(2) 118.6(4) . . . yes S(2) C(2) C(1) 116.3(5) . . . yes S(1) C(3) S(2) 115.8(3) . . . yes S(1) C(3) C(4) 122.0(4) . . . yes S(2) C(3) C(4) 122.2(4) . . . yes O(1) C(4) C(3) 119.2(4) . . . yes O(1) C(4) C(5) 107.6(5) . . . yes C(3) C(4) C(5) 133.1(5) . . . yes N(1) C(5) C(4) 128.2(5) . . . yes N(1) C(5) C(6) 124.1(5) . . . yes C(4) C(5) C(6) 107.6(5) . . . yes N(2) C(6) C(5) 123.4(5) . . . yes N(2) C(6) C(7) 128.8(5) . . . yes C(5) C(6) C(7) 107.8(5) . . . yes O(1) C(7) C(6) 108.1(5) . . . yes O(1) C(7) C(8) 119.8(5) . . . yes C(6) C(7) C(8) 132.0(5) . . . yes S(3) C(8) S(4) 114.8(3) . . . yes S(3) C(8) C(7) 122.0(4) . . . yes S(4) C(8) C(7) 123.1(4) . . . yes S(3) C(9) C(10) 116.5(5) . . . yes S(4) C(10) C(9) 118.4(5) . . . yes N(1) C(11) C(12) 123.1(5) . . . yes N(2) C(12) C(11) 125.3(5) . . . yes S(5) C(13) C(14) 118.3(5) . . . yes S(6) C(14) C(13) 116.8(5) . . . yes S(5) C(15) S(6) 114.3(3) . . . yes S(5) C(15) C(16) 123.1(4) . . . yes S(6) C(15) C(16) 122.5(4) . . . yes O(2) C(16) C(15) 119.4(4) . . . yes O(2) C(16) C(17) 108.2(5) . . . yes C(15) C(16) C(17) 132.4(5) . . . yes N(3) C(17) C(16) 128.7(5) . . . yes N(3) C(17) C(18) 124.4(5) . . . yes C(16) C(17) C(18) 106.9(5) . . . yes N(4) C(18) C(17) 122.7(5) . . . yes N(4) C(18) C(19) 128.8(6) . . . yes C(17) C(18) C(19) 108.6(5) . . . yes O(2) C(19) C(18) 107.4(5) . . . yes O(2) C(19) C(20) 119.1(5) . . . yes C(18) C(19) C(20) 133.5(6) . . . yes S(7) C(20) S(8) 114.9(3) . . . yes S(7) C(20) C(19) 121.7(4) . . . yes S(8) C(20) C(19) 123.4(4) . . . yes S(7) C(21) C(22) 117.0(5) . . . yes S(8) C(22) C(21) 117.7(5) . . . yes N(3) C(23) C(24) 124.0(6) . . . yes N(4) C(24) C(23) 123.3(6) . . . yes Cl(1) C(25) C(26) 107(1) . . . yes Cl(1) C(25) C(27) 131(1) . . . yes C(26) C(25) C(27) 121(1) . . . yes C(25) C(26) C(27) 111(1) . . 2_566 yes C(25) C(27) C(26) 127(1) . . 2_566 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 Cl(1) S(7) 3.381(6) . 1_455 ? Cl(1) S(5) 3.524(5) . 2_667 ? S(1) C(25) 3.463(9) . 1_655 ? S(1) C(27) 3.496(8) . 1_655 ? S(2) S(6) 3.298(2) . 2_666 ? S(3) F(3) 3.398(4) . 1_655 ? S(3) C(21) 3.568(6) . 1_554 ? S(4) F(4) 3.371(6) . 2_656 ? S(6) S(6) 3.542(3) . 2_667 ? S(6) C(2) 3.563(5) . 1_556 ? S(6) C(2) 3.578(6) . . ? S(8) F(4) 3.437(5) . 2_656 ? S(8) C(8) 3.512(5) . . ? S(8) C(8) 3.527(5) . 1_556 ? F(1) C(1) 3.296(7) . 2_666 ? F(1) C(2) 3.346(7) . 2_666 ? F(1) C(13) 3.468(9) . 2_666 ? F(1) C(14) 3.513(8) . 2_666 ? F(1) C(11) 3.548(8) . . ? F(1) C(23) 3.585(8) . . ? F(2) C(26) 3.34(1) . . ? F(2) C(13) 3.509(8) . 2_666 ? F(2) C(1) 3.579(7) . 2_666 ? F(3) C(9) 3.094(7) . 1_455 ? F(3) C(22) 3.425(8) . 2_656 ? F(3) C(21) 3.429(8) . 1_454 ? F(3) C(10) 3.589(8) . 2_656 ? F(4) C(22) 3.384(8) . 2_656 ? F(4) C(10) 3.399(8) . 2_656 ? F(4) C(11) 3.589(8) . . ? F(5) C(13) 3.397(7) . 2_667 ? F(6) C(10) 3.310(7) . 2_655 ? O(1) C(19) 3.474(6) . 1_554 ? O(1) C(19) 3.514(6) . . ? N(1) C(23) 3.506(8) . . ? N(1) C(23) 3.569(8) . 1_554 ? N(2) C(12) 3.375(6) . 2_655 ? N(2) N(2) 3.536(8) . 2_655 ? N(2) C(24) 3.576(9) . 2_656 ? N(2) N(4) 3.580(6) . . ? N(4) C(6) 3.505(7) . . ? N(4) C(6) 3.571(7) . 1_556 ? N(4) C(12) 3.589(8) . 2_656 ? C(3) C(16) 3.490(7) . . ? C(3) C(16) 3.499(7) . 1_554 ? C(4) C(18) 3.592(7) . 1_554 ? C(5) C(18) 3.533(7) . . ? C(9) C(22) 3.496(8) . 1_554 ? C(11) C(24) 3.489(9) . . ? C(12) C(24) 3.553(8) . . ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------