# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/259 data_(BEDT-ATD)2AsF6(THF),297K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:04:20 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1498.87 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H36 As F6 N4 O S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.990(3) _cell_length_b 7.946(2) _cell_length_c 13.357(1) _cell_angle_alpha 90 _cell_angle_beta 103.415(9) _cell_angle_gamma 90 _cell_volume 2889.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 297.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1518.00 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 297.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4193 _reflns_number_total 4193 _reflns_number_observed 2573 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.136 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; As 0 2 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags As1 0.0000 0.0000 0.0000 0.0680(6) Uani d . 0.50 S S1 0.11417(9) 0.1536(4) 0.2705(2) 0.0647(9) Uani d . 1.00 . S2 0.24252(8) 0.3176(3) 0.1795(2) 0.0496(8) Uani d . 1.00 . S3 0.33116(8) 0.4030(3) 0.3338(2) 0.0484(8) Uani d . 1.00 . S4 0.27391(10) 0.4650(4) 0.0037(2) 0.071(1) Uani d . 1.00 . S5 0.38258(9) 0.5670(4) 0.1913(2) 0.0588(9) Uani d . 1.00 . S6 0.09503(8) 0.3559(3) 0.5545(2) 0.0491(8) Uani d . 1.00 . S7 0.18025(8) 0.4231(3) 0.7221(2) 0.0480(7) Uani d . 1.00 . S8 0.02268(9) 0.5104(4) 0.6542(2) 0.0618(9) Uani d . 1.00 . S9 0.12559(9) 0.5848(4) 0.8597(2) 0.0584(9) Uani d . 1.00 . F1 -0.0051(3) -0.011(1) 0.1220(5) 0.139(4) Uani d . 1.00 . F2 0.0596(2) -0.059(1) 0.0366(6) 0.132(4) Uani d . 1.00 . F3 0.0180(3) 0.202(1) 0.0157(9) 0.177(5) Uani d . 1.00 . O1 0.0445(6) -0.039(2) 0.600(2) 0.100(7) Uani d . 0.50 . N1 0.1717(3) 0.179(1) 0.2643(5) 0.054(3) Uani d . 1.00 . N2 0.1204(3) 0.196(1) 0.3927(5) 0.056(3) Uani d . 1.00 . C1 0.1972(3) 0.222(1) 0.3580(6) 0.043(3) Uani d . 1.00 . C2 0.2483(3) 0.262(1) 0.3854(6) 0.037(2) Uani d . 1.00 . C3 0.2714(3) 0.319(1) 0.3101(6) 0.039(3) Uani d . 1.00 . C4 0.2720(3) 0.248(1) 0.4969(6) 0.039(3) Uani d . 1.00 . C5 0.3214(3) 0.220(1) 0.5306(7) 0.048(3) Uani d . 1.00 . C6 0.3447(3) 0.195(1) 0.6355(7) 0.047(3) Uani d . 1.00 . C7 0.3961(3) 0.167(1) 0.6694(8) 0.061(3) Uani d . 1.00 . C8 0.4162(4) 0.134(2) 0.7739(8) 0.075(4) Uani d . 1.00 . C9 0.3861(4) 0.130(2) 0.8435(7) 0.078(4) Uani d . 1.00 . C10 0.3384(3) 0.161(1) 0.8135(7) 0.061(4) Uani d . 1.00 . C11 0.3155(3) 0.197(1) 0.7086(7) 0.048(3) Uani d . 1.00 . C12 0.2658(3) 0.224(1) 0.6730(6) 0.044(3) Uani d . 1.00 . C13 0.2420(3) 0.253(1) 0.5713(7) 0.042(3) Uani d . 1.00 . C14 0.1885(3) 0.277(1) 0.5373(6) 0.040(3) Uani d . 1.00 . C15 0.1588(3) 0.340(1) 0.5988(6) 0.039(3) Uani d . 1.00 . C16 0.1679(3) 0.230(1) 0.4329(6) 0.041(3) Uani d . 1.00 . C17 0.2881(3) 0.429(1) 0.1366(7) 0.049(3) Uani d . 1.00 . C18 0.3289(3) 0.468(1) 0.2079(7) 0.048(3) Uani d . 1.00 . C19 0.3342(4) 0.508(1) -0.0137(8) 0.069(4) Uani d . 1.00 . C20 0.3614(4) 0.639(1) 0.0595(8) 0.073(4) Uani d . 1.00 . C21 0.0849(3) 0.465(1) 0.6616(7) 0.046(3) Uani d . 1.00 . C22 0.1237(3) 0.494(1) 0.7393(7) 0.045(3) Uani d . 1.00 . C23 0.0289(4) 0.649(2) 0.7635(8) 0.072(4) Uani d . 1.00 . C24 0.0609(4) 0.583(2) 0.8583(8) 0.082(4) Uani d . 1.00 . C25 -0.0031(5) 0.011(2) 0.589(1) 0.097(5) Uani d . 1.00 . C26 0.0356(5) -0.085(2) 0.501(1) 0.108(6) Uani d . 1.00 . H1 0.3412 0.2167 0.4802 0.0579 Uiso calc . 1.00 . H2 0.4168 0.1708 0.6208 0.0744 Uiso calc . 1.00 . H3 0.4503 0.1154 0.7976 0.0921 Uiso calc . 1.00 . H4 0.3991 0.1050 0.9151 0.0950 Uiso calc . 1.00 . H5 0.3183 0.1569 0.8637 0.0759 Uiso calc . 1.00 . H6 0.2457 0.2224 0.7235 0.0518 Uiso calc . 1.00 . H7 0.3520 0.4074 -0.0033 0.0825 Uiso calc . 1.00 . H8 0.3308 0.5485 -0.0812 0.0825 Uiso calc . 1.00 . H9 0.3400 0.7322 0.0607 0.0882 Uiso calc . 1.00 . H10 0.3889 0.6735 0.0361 0.0882 Uiso calc . 1.00 . H11 0.0421 0.7530 0.7459 0.0855 Uiso calc . 1.00 . H12 -0.0023 0.6665 0.7757 0.0855 Uiso calc . 1.00 . H13 0.0523 0.4725 0.8667 0.0976 Uiso calc . 1.00 . H14 0.0570 0.6526 0.9127 0.0976 Uiso calc . 1.00 . H15 -0.0200 -0.0875 0.6027 0.1137 Uiso calc . 1.00 . H16 -0.0016 0.0885 0.6450 0.1137 Uiso calc . 1.00 . H17 0.0679 -0.0901 0.4843 0.1278 Uiso calc . 1.00 . H18 0.0252 -0.2041 0.4997 0.1278 Uiso calc . 1.00 . 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) 0.0560(9) 0.081(1) 0.072(1) 0.0198(9) 0.0251(8) -0.0062(10) S(1) 0.050(1) 0.092(3) 0.054(2) -0.017(2) 0.015(1) -0.017(2) S(2) 0.047(1) 0.058(2) 0.046(1) -0.005(1) 0.015(1) 0.000(1) S(3) 0.046(1) 0.049(2) 0.053(1) -0.005(1) 0.018(1) -0.007(1) S(4) 0.066(2) 0.093(3) 0.057(2) -0.005(2) 0.021(1) 0.017(2) S(5) 0.059(2) 0.054(2) 0.071(2) -0.011(1) 0.031(1) -0.002(1) S(6) 0.044(1) 0.058(2) 0.049(1) -0.004(1) 0.019(1) -0.008(1) S(7) 0.045(1) 0.050(2) 0.050(1) -0.002(1) 0.013(1) -0.008(1) S(8) 0.047(1) 0.075(2) 0.067(2) 0.005(1) 0.020(1) -0.014(2) S(9) 0.067(2) 0.055(2) 0.055(2) 0.001(1) 0.019(1) -0.014(1) F(1) 0.134(7) 0.22(1) 0.076(5) 0.039(7) 0.054(5) 0.005(6) F(2) 0.077(5) 0.172(9) 0.155(7) 0.049(5) 0.045(5) 0.037(6) F(3) 0.163(9) 0.083(8) 0.31(1) -0.019(6) 0.096(9) -0.035(8) O(1) 0.08(1) 0.10(2) 0.12(2) -0.01(1) 0.02(1) 0.02(1) N(1) 0.043(4) 0.075(7) 0.046(5) -0.007(4) 0.014(4) -0.009(5) N(2) 0.048(5) 0.069(7) 0.052(5) -0.011(4) 0.018(4) -0.008(5) C(1) 0.045(5) 0.046(7) 0.041(5) -0.004(5) 0.014(5) 0.001(5) C(2) 0.040(5) 0.030(6) 0.040(5) 0.001(4) 0.011(4) -0.001(4) C(3) 0.037(5) 0.043(6) 0.039(5) 0.003(4) 0.016(4) -0.004(4) C(4) 0.039(5) 0.038(6) 0.042(5) -0.003(4) 0.014(4) -0.002(4) C(5) 0.050(5) 0.045(7) 0.053(6) 0.004(5) 0.018(5) -0.002(5) C(6) 0.048(5) 0.044(7) 0.050(6) 0.000(5) 0.011(5) -0.010(5) C(7) 0.052(6) 0.070(9) 0.061(7) 0.011(6) 0.010(5) -0.008(6) C(8) 0.052(6) 0.11(1) 0.055(7) 0.018(7) -0.008(5) -0.014(7) C(9) 0.094(9) 0.09(1) 0.042(6) 0.009(8) 0.003(6) -0.011(7) C(10) 0.047(6) 0.082(9) 0.051(6) 0.002(6) 0.005(5) 0.000(6) C(11) 0.049(5) 0.040(7) 0.058(6) -0.005(5) 0.022(5) -0.005(5) C(12) 0.051(6) 0.046(7) 0.035(5) 0.001(5) 0.011(5) 0.010(5) C(13) 0.041(5) 0.040(6) 0.048(5) -0.001(4) 0.013(4) -0.002(5) C(14) 0.048(5) 0.036(6) 0.038(5) -0.005(4) 0.015(4) 0.006(4) C(15) 0.045(5) 0.033(6) 0.043(5) -0.006(4) 0.018(4) 0.000(4) C(16) 0.038(5) 0.046(6) 0.041(5) -0.007(4) 0.015(4) -0.004(4) C(17) 0.047(5) 0.055(7) 0.054(6) 0.006(5) 0.031(5) 0.002(5) C(18) 0.055(6) 0.045(7) 0.052(6) 0.000(5) 0.030(5) 0.001(5) C(19) 0.078(7) 0.074(9) 0.064(7) 0.005(7) 0.033(6) 0.019(7) C(20) 0.105(9) 0.066(9) 0.063(7) -0.023(7) 0.048(7) -0.006(6) C(21) 0.052(5) 0.048(7) 0.044(5) 0.003(5) 0.025(5) -0.002(5) C(22) 0.053(5) 0.038(6) 0.052(6) -0.004(5) 0.026(5) -0.006(5) C(23) 0.068(7) 0.09(1) 0.062(7) 0.027(7) 0.022(6) -0.012(7) C(24) 0.089(8) 0.10(1) 0.068(7) 0.038(8) 0.037(7) -0.001(7) C(25) 0.093(10) 0.10(1) 0.10(1) 0.014(9) 0.021(8) 0.004(9) C(26) 0.13(1) 0.09(1) 0.086(10) -0.013(9) -0.011(10) 0.011(10) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0036(7) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2573 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0620 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0730 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.728 _refine_ls_shift/esd_max 0.3750 _refine_ls_shift/esd_mean 0.0400 _refine_diff_density_min -0.45 _refine_diff_density_max 0.44 #------------------------------------------------------------------------------ _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) 1.671(6) 1_555 1_555 yes As(1) F(1) 1.671(6) 1_555 3_555 yes As(1) F(2) 1.693(6) 1_555 1_555 yes As(1) F(2) 1.693(6) 1_555 3_555 yes As(1) F(3) 1.684(9) 1_555 1_555 yes As(1) F(3) 1.684(9) 1_555 3_555 yes S(1) N(1) 1.643(7) 1_555 1_555 yes S(1) N(2) 1.635(7) 1_555 1_555 yes S(2) C(3) 1.745(8) 1_555 1_555 yes S(2) C(17) 1.755(8) 1_555 1_555 yes S(3) C(3) 1.759(8) 1_555 1_555 yes S(3) C(18) 1.745(9) 1_555 1_555 yes S(4) C(17) 1.750(9) 1_555 1_555 yes S(4) C(19) 1.788(10) 1_555 1_555 yes S(5) C(18) 1.756(9) 1_555 1_555 yes S(5) C(20) 1.82(1) 1_555 1_555 yes S(6) C(15) 1.751(8) 1_555 1_555 yes S(6) C(21) 1.751(8) 1_555 1_555 yes S(7) C(15) 1.745(8) 1_555 1_555 yes S(7) C(22) 1.747(8) 1_555 1_555 yes S(8) C(21) 1.760(9) 1_555 1_555 yes S(8) C(23) 1.80(1) 1_555 1_555 yes S(9) C(22) 1.751(9) 1_555 1_555 yes S(9) C(24) 1.81(1) 1_555 1_555 yes O(1) C(25) 1.36(2) 1_555 1_555 yes O(1) C(26) 1.34(2) 1_555 1_555 yes N(1) C(1) 1.33(1) 1_555 1_555 yes N(2) C(16) 1.340(10) 1_555 1_555 yes C(1) C(2) 1.43(1) 1_555 1_555 yes C(1) C(16) 1.433(10) 1_555 1_555 yes C(2) C(3) 1.39(1) 1_555 1_555 yes C(2) C(4) 1.49(1) 1_555 1_555 yes C(4) C(5) 1.37(1) 1_555 1_555 yes C(4) C(13) 1.44(1) 1_555 1_555 yes C(5) C(6) 1.42(1) 1_555 1_555 yes C(6) C(7) 1.42(1) 1_555 1_555 yes C(6) C(11) 1.41(1) 1_555 1_555 yes C(7) C(8) 1.40(1) 1_555 1_555 yes C(8) C(9) 1.39(1) 1_555 1_555 yes C(9) C(10) 1.33(1) 1_555 1_555 yes C(10) C(11) 1.43(1) 1_555 1_555 yes C(11) C(12) 1.38(1) 1_555 1_555 yes C(12) C(13) 1.39(1) 1_555 1_555 yes C(13) C(14) 1.47(1) 1_555 1_555 yes C(14) C(15) 1.39(1) 1_555 1_555 yes C(14) C(16) 1.43(1) 1_555 1_555 yes C(17) C(18) 1.34(1) 1_555 1_555 yes C(19) C(20) 1.51(1) 1_555 1_555 yes C(21) C(22) 1.34(1) 1_555 1_555 yes C(23) C(24) 1.47(1) 1_555 1_555 yes C(25) C(26) 1.44(2) 1_555 3_556 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(1) 180.0 1_555 1_555 3_555 yes F(1) As(1) F(2) 90.3(4) 1_555 1_555 1_555 yes F(1) As(1) F(2) 89.7(4) 1_555 1_555 3_555 yes F(1) As(1) F(3) 91.1(5) 1_555 1_555 1_555 yes F(1) As(1) F(3) 88.9(5) 1_555 1_555 3_555 yes F(1) As(1) F(2) 89.7(4) 3_555 1_555 1_555 yes F(1) As(1) F(2) 90.3(4) 3_555 1_555 3_555 yes F(1) As(1) F(3) 88.9(5) 3_555 1_555 1_555 yes F(1) As(1) F(3) 91.1(5) 3_555 1_555 3_555 yes F(2) As(1) F(2) 180.0 1_555 1_555 3_555 yes F(2) As(1) F(3) 89.0(5) 1_555 1_555 1_555 yes F(2) As(1) F(3) 91.0(5) 1_555 1_555 3_555 yes F(2) As(1) F(3) 91.0(5) 3_555 1_555 1_555 yes F(2) As(1) F(3) 89.0(5) 3_555 1_555 3_555 yes F(3) As(1) F(3) 180.0 1_555 1_555 3_555 yes N(1) S(1) N(2) 98.4(4) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.8(4) 1_555 1_555 1_555 yes C(3) S(3) C(18) 96.8(4) 1_555 1_555 1_555 yes C(17) S(4) C(19) 99.5(4) 1_555 1_555 1_555 yes C(18) S(5) C(20) 99.7(5) 1_555 1_555 1_555 yes C(15) S(6) C(21) 95.9(4) 1_555 1_555 1_555 yes C(15) S(7) C(22) 97.1(4) 1_555 1_555 1_555 yes C(21) S(8) C(23) 99.9(5) 1_555 1_555 1_555 yes C(22) S(9) C(24) 99.9(5) 1_555 1_555 1_555 yes C(25) O(1) C(26) 91(1) 1_555 1_555 1_555 yes S(1) N(1) C(1) 107.5(5) 1_555 1_555 1_555 yes S(1) N(2) C(16) 107.9(6) 1_555 1_555 1_555 yes N(1) C(1) C(2) 125.7(7) 1_555 1_555 1_555 yes N(1) C(1) C(16) 113.4(7) 1_555 1_555 1_555 yes C(2) C(1) C(16) 120.9(8) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.6(8) 1_555 1_555 1_555 yes C(1) C(2) C(4) 115.3(7) 1_555 1_555 1_555 yes C(3) C(2) C(4) 125.0(7) 1_555 1_555 1_555 yes S(2) C(3) S(3) 112.6(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 122.3(6) 1_555 1_555 1_555 yes S(3) C(3) C(2) 125.1(6) 1_555 1_555 1_555 yes C(2) C(4) C(5) 121.5(7) 1_555 1_555 1_555 yes C(2) C(4) C(13) 119.5(7) 1_555 1_555 1_555 yes C(5) C(4) C(13) 118.9(8) 1_555 1_555 1_555 yes C(4) C(5) C(6) 123.1(8) 1_555 1_555 1_555 yes C(4) C(5) H(1) 118.2(9) 1_555 1_555 1_555 no C(6) C(5) H(1) 118.8(9) 1_555 1_555 1_555 no C(5) C(6) C(7) 122.4(8) 1_555 1_555 1_555 yes C(5) C(6) C(11) 118.4(8) 1_555 1_555 1_555 yes C(7) C(6) C(11) 119.2(9) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.2(9) 1_555 1_555 1_555 yes C(6) C(7) H(2) 120.2(10) 1_555 1_555 1_555 no C(8) C(7) H(2) 120.6(9) 1_555 1_555 1_555 no C(7) C(8) C(9) 120.2(9) 1_555 1_555 1_555 yes C(7) C(8) H(3) 120(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 119(1) 1_555 1_555 1_555 no C(8) C(9) C(10) 121.1(10) 1_555 1_555 1_555 yes C(8) C(9) H(4) 121(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 117(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 121.8(9) 1_555 1_555 1_555 yes C(9) C(10) H(5) 119(1) 1_555 1_555 1_555 no C(11) C(10) H(5) 118.9(9) 1_555 1_555 1_555 no C(6) C(11) C(10) 118.4(8) 1_555 1_555 1_555 yes C(6) C(11) C(12) 117.6(9) 1_555 1_555 1_555 yes C(10) C(11) C(12) 123.9(8) 1_555 1_555 1_555 yes C(11) C(12) C(13) 125.6(8) 1_555 1_555 1_555 yes C(11) C(12) H(6) 117.2(8) 1_555 1_555 1_555 no C(13) C(12) H(6) 117.2(8) 1_555 1_555 1_555 no C(4) C(13) C(12) 116.5(8) 1_555 1_555 1_555 yes C(4) C(13) C(14) 120.2(8) 1_555 1_555 1_555 yes C(12) C(13) C(14) 123.2(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 124.5(8) 1_555 1_555 1_555 yes C(13) C(14) C(16) 114.8(7) 1_555 1_555 1_555 yes C(15) C(14) C(16) 120.7(8) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.1(4) 1_555 1_555 1_555 yes S(6) C(15) C(14) 121.8(7) 1_555 1_555 1_555 yes S(7) C(15) C(14) 125.0(6) 1_555 1_555 1_555 yes N(2) C(16) C(1) 112.8(8) 1_555 1_555 1_555 yes N(2) C(16) C(14) 125.5(7) 1_555 1_555 1_555 yes C(1) C(16) C(14) 121.6(7) 1_555 1_555 1_555 yes S(2) C(17) S(4) 113.7(5) 1_555 1_555 1_555 yes S(2) C(17) C(18) 116.6(7) 1_555 1_555 1_555 yes S(4) C(17) C(18) 129.6(7) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.4(6) 1_555 1_555 1_555 yes S(3) C(18) C(17) 116.8(7) 1_555 1_555 1_555 yes S(5) C(18) C(17) 128.7(7) 1_555 1_555 1_555 yes S(4) C(19) C(20) 113.4(7) 1_555 1_555 1_555 yes S(4) C(19) H(7) 107.7(8) 1_555 1_555 1_555 no S(4) C(19) H(8) 107.5(8) 1_555 1_555 1_555 no C(20) C(19) H(7) 108(1) 1_555 1_555 1_555 no C(20) C(19) H(8) 107.9(10) 1_555 1_555 1_555 no H(7) C(19) H(8) 111(1) 1_555 1_555 1_555 no S(5) C(20) C(19) 114.3(7) 1_555 1_555 1_555 yes S(5) C(20) H(9) 107.0(7) 1_555 1_555 1_555 no S(5) C(20) H(10) 107.8(9) 1_555 1_555 1_555 no C(19) C(20) H(9) 108(1) 1_555 1_555 1_555 no C(19) C(20) H(10) 108.5(9) 1_555 1_555 1_555 no H(9) C(20) H(10) 110(1) 1_555 1_555 1_555 no S(6) C(21) S(8) 113.6(5) 1_555 1_555 1_555 yes S(6) C(21) C(22) 117.8(7) 1_555 1_555 1_555 yes S(8) C(21) C(22) 128.5(7) 1_555 1_555 1_555 yes S(7) C(22) S(9) 114.7(5) 1_555 1_555 1_555 yes S(7) C(22) C(21) 116.0(6) 1_555 1_555 1_555 yes S(9) C(22) C(21) 129.2(7) 1_555 1_555 1_555 yes S(8) C(23) C(24) 114.1(8) 1_555 1_555 1_555 yes S(8) C(23) H(11) 107.3(7) 1_555 1_555 1_555 no S(8) C(23) H(12) 108.3(9) 1_555 1_555 1_555 no C(24) C(23) H(11) 108(1) 1_555 1_555 1_555 no C(24) C(23) H(12) 108.2(9) 1_555 1_555 1_555 no H(11) C(23) H(12) 109(1) 1_555 1_555 1_555 no S(9) C(24) C(23) 114.6(8) 1_555 1_555 1_555 yes S(9) C(24) H(13) 107.0(8) 1_555 1_555 1_555 no S(9) C(24) H(14) 106.5(10) 1_555 1_555 1_555 no C(23) C(24) H(13) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(14) 107(1) 1_555 1_555 1_555 no H(13) C(24) H(14) 112(1) 1_555 1_555 1_555 no O(1) C(25) C(26) 128(1) 1_555 1_555 3_556 yes O(1) C(25) H(15) 104(1) 1_555 1_555 1_555 no O(1) C(25) H(16) 103(1) 1_555 1_555 1_555 no C(26) C(25) H(15) 104(1) 3_556 1_555 1_555 no C(26) C(25) H(16) 107(1) 3_556 1_555 1_555 no H(15) C(25) H(16) 107(1) 1_555 1_555 1_555 no O(1) C(26) C(25) 129(1) 1_555 1_555 3_556 yes O(1) C(26) H(17) 105(1) 1_555 1_555 1_555 no O(1) C(26) H(18) 105(1) 1_555 1_555 1_555 no C(25) C(26) H(17) 105(1) 3_556 1_555 1_555 no C(25) C(26) H(18) 104(1) 3_556 1_555 1_555 no H(17) C(26) H(18) 103(1) 1_555 1_555 1_555 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 S(1) F(2) 3.569(10) 1_555 1_555 ? S(2) C(10) 3.56(1) 1_555 2_556 ? S(3) O(1) 3.42(2) 1_555 2_556 ? S(3) C(14) 3.539(9) 1_555 2_556 ? S(3) C(15) 3.586(9) 1_555 2_556 ? S(5) O(1) 3.16(2) 1_555 2_556 ? S(5) F(1) 3.505(7) 1_555 4_555 ? S(5) C(22) 3.536(10) 1_555 2_556 ? S(6) O(1) 3.55(2) 1_555 1_555 ? S(7) C(3) 3.492(9) 1_555 2_556 ? S(9) C(18) 3.499(10) 1_555 2_556 ? F(1) C(23) 3.40(1) 1_555 3_566 ? F(2) C(19) 3.11(1) 1_555 2_545 ? F(2) C(9) 3.14(1) 1_555 2_546 ? F(2) C(20) 3.22(1) 1_555 2_545 ? F(2) C(8) 3.46(1) 1_555 2_546 ? F(3) C(24) 3.51(1) 1_555 3_566 ? O(1) C(23) 3.40(2) 1_555 1_545 ? N(1) C(19) 3.58(1) 1_555 2_545 ? C(3) C(12) 3.40(1) 1_555 2_556 ? C(5) C(15) 3.58(1) 1_555 2_546 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2BF4(THF),90K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:10:46 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1396.77 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H36 B F4 N4 O S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.67(1) _cell_length_b 7.601(1) _cell_length_c 13.342(3) _cell_angle_alpha 90 _cell_angle_beta 102.05(3) _cell_angle_gamma 90 _cell_volume 2744.0701 _cell_formula_units_Z 2 _cell_measurement_temperature 90.0 _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 a ' _symmetry_Int_Tables_number 7 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x, -y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.690 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1426.00 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 90.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4508 _reflns_number_total 4508 _reflns_number_observed 3525 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.127 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B 0 2 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 8 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S11 0.1575(9) -0.0723(4) 0.122(2) 0.0367(10) Uani d . 1.00 . S12 0.2893(10) 0.0687(4) 0.028(2) 0.0327(9) Uani d . 1.00 . S13 0.3237(10) 0.2234(4) -0.147(2) 0.041(1) Uani d . 1.00 . S14 0.4360(10) 0.2861(4) 0.038(2) 0.0356(9) Uani d . 1.00 . S15 0.3793(9) 0.1348(4) 0.180(2) 0.0318(9) Uani d . 1.00 . S16 0.2207(10) 0.2039(4) 0.570(2) 0.0324(9) Uani d . 1.00 . S17 0.1638(10) 0.3688(4) 0.710(2) 0.0361(9) Uani d . 1.00 . S18 0.0619(10) 0.2821(4) 0.506(2) 0.0360(9) Uani d . 1.00 . S19 0.1369(10) 0.1341(4) 0.405(2) 0.0337(9) Uani d . 1.00 . S21 0.9283(10) 0.5826(4) 0.574(2) 0.038(1) Uani d . 1.00 . S22 0.7993(10) 0.4002(4) 0.662(2) 0.0326(9) Uani d . 1.00 . S23 0.7671(9) 0.2535(5) 0.839(2) 0.0404(10) Uani d . 1.00 . S24 0.6563(10) 0.1562(4) 0.659(2) 0.0358(9) Uani d . 1.00 . S25 0.7097(10) 0.3201(4) 0.511(2) 0.0323(9) Uani d . 1.00 . S26 0.8691(10) 0.3393(4) 0.115(2) 0.0326(9) Uani d . 1.00 . S27 0.9277(10) 0.1981(4) -0.026(2) 0.0358(9) Uani d . 1.00 . S28 1.0283(10) 0.2580(4) 0.185(2) 0.0362(9) Uani d . 1.00 . S29 0.9522(10) 0.4021(4) 0.286(2) 0.0336(9) Uani d . 1.00 . F1 0.5983(10) 0.286(1) 0.874(2) 0.064(3) Uani d . 1.00 . F2 0.536(1) 0.219(2) 0.948(2) 0.116(5) Uani d . 1.00 . F3 0.520(1) 0.333(2) 0.785(2) 0.105(4) Uani d . 1.00 . F4 0.552(1) 0.054(1) 0.817(2) 0.127(5) Uani d . 1.00 . O1 0.586(1) 0.259(1) 0.449(2) 0.047(3) Uani d . 1.00 . N11 0.215(1) -0.057(1) 0.115(2) 0.039(3) Uani d . 1.00 . N12 0.164(1) -0.022(1) 0.245(2) 0.036(2) Uani d . 1.00 . N21 0.871(1) 0.548(1) 0.583(2) 0.035(2) Uani d . 1.00 . N22 0.924(1) 0.546(1) 0.452(2) 0.040(2) Uani d . 1.00 . C1 0.845(1) 0.512(1) 0.481(2) 0.031(3) Uani d . 1.00 . C2 0.877(1) 0.514(1) 0.412(2) 0.029(3) Uani d . 1.00 . C3 0.856(1) 0.466(1) 0.303(2) 0.031(3) Uani d . 1.00 . C4 0.804(1) 0.487(1) 0.272(2) 0.028(3) Uani d . 1.00 . C5 0.795(1) 0.463(1) 0.456(2) 0.030(3) Uani d . 1.00 . C6 0.772(1) 0.482(1) 0.347(2) 0.029(3) Uani d . 1.00 . C7 0.721(1) 0.502(2) 0.311(2) 0.032(3) Uani d . 1.00 . C8 0.700(1) 0.528(1) 0.208(2) 0.031(3) Uani d . 1.00 . C9 0.730(1) 0.543(1) 0.135(2) 0.029(3) Uani d . 1.00 . C10 0.782(1) 0.519(2) 0.171(2) 0.030(3) Uani d . 1.00 . C11 0.887(1) 0.414(1) 0.240(2) 0.030(2) Uani d . 1.00 . C12 0.649(1) 0.546(2) 0.173(2) 0.036(3) Uani d . 1.00 . C13 0.628(1) 0.574(2) 0.070(2) 0.037(3) Uani d . 1.00 . C14 0.658(1) 0.587(2) 0.002(2) 0.041(4) Uani d . 1.00 . C15 0.707(1) 0.568(2) 0.029(2) 0.037(3) Uani d . 1.00 . C16 0.928(1) 0.274(1) 0.098(2) 0.031(2) Uani d . 1.00 . C17 0.964(1) 0.299(2) 0.176(2) 0.034(2) Uani d . 1.00 . C18 0.994(1) 0.215(2) -0.024(2) 0.043(3) Uani d . 1.00 . C19 1.025(1) 0.123(2) 0.069(2) 0.042(4) Uani d . 1.00 . C20 0.201(1) 0.121(1) 0.446(2) 0.032(2) Uani d . 1.00 . C21 0.231(1) 0.052(1) 0.390(2) 0.028(3) Uani d . 1.00 . C22 0.318(1) 0.062(2) 0.158(2) 0.037(2) Uani d . 1.00 . C23 0.293(1) 0.010(1) 0.231(2) 0.030(3) Uani d . 1.00 . C24 0.285(1) 0.025(2) 0.419(2) 0.032(3) Uani d . 1.00 . C25 0.315(1) -0.002(2) 0.344(2) 0.031(3) Uani d . 1.00 . C26 0.211(1) 0.002(1) 0.285(2) 0.033(3) Uani d . 1.00 . C27 0.309(1) 0.011(2) 0.527(2) 0.033(3) Uani d . 1.00 . C28 0.359(1) -0.020(2) 0.555(2) 0.032(3) Uani d . 1.00 . C29 0.364(1) -0.033(1) 0.374(2) 0.031(3) Uani d . 1.00 . C30 0.338(1) 0.172(2) -0.013(2) 0.038(3) Uani d . 1.00 . C31 0.380(1) 0.204(1) 0.054(2) 0.032(2) Uani d . 1.00 . C32 0.772(1) 0.401(1) 0.535(2) 0.028(2) Uani d . 1.00 . C33 0.125(1) 0.244(2) 0.514(2) 0.034(2) Uani d . 1.00 . C34 0.163(1) 0.273(1) 0.590(2) 0.030(2) Uani d . 1.00 . C35 0.376(1) 0.362(2) -0.154(2) 0.041(3) Uani d . 1.00 . C36 0.712(1) 0.246(1) 0.638(2) 0.033(2) Uani d . 1.00 . C37 0.753(1) 0.288(2) 0.707(2) 0.038(3) Uani d . 1.00 . C38 0.679(1) 0.074(2) 0.792(2) 0.045(3) Uani d . 1.00 . C39 0.705(1) 0.216(2) 0.862(2) 0.040(3) Uani d . 1.00 . C40 0.425(1) 0.279(2) -0.100(2) 0.048(3) Uani d . 1.00 . C42 0.066(1) 0.431(2) 0.615(2) 0.037(3) Uani d . 1.00 . C43 0.382(1) -0.033(2) 0.664(2) 0.039(3) Uani d . 1.00 . C44 0.432(1) -0.054(1) 0.689(2) 0.036(3) Uani d . 1.00 . C47 0.098(1) 0.355(2) 0.711(2) 0.038(3) Uani d . 1.00 . C48 0.537(1) 0.223(2) 0.448(2) 0.046(3) Uani d . 1.00 . C49 0.513(1) 0.147(2) 0.343(2) 0.046(4) Uani d . 1.00 . C50 0.547(1) 0.220(2) 0.271(3) 0.053(4) Uani d . 1.00 . C51 0.586(1) 0.325(2) 0.346(2) 0.056(4) Uani d . 1.00 . C52 0.240(1) -0.026(1) 0.206(2) 0.032(3) Uani d . 1.00 . C53 0.389(1) -0.038(2) 0.481(2) 0.032(3) Uani d . 1.00 . C54 0.440(1) -0.074(2) 0.516(3) 0.038(3) Uani d . 1.00 . C55 0.461(1) -0.076(2) 0.620(2) 0.039(4) Uani d . 1.00 . B1 0.552(1) 0.214(3) 0.854(3) 0.076(5) Uani d . 1.00 . H1 0.7021 0.5020 0.3679 0.0327 Uiso calc . 1.00 . H2 0.8032 0.5277 0.1269 0.0279 Uiso calc . 1.00 . H3 0.6290 0.5440 0.2272 0.0332 Uiso calc . 1.00 . H4 0.5942 0.5815 0.0545 0.0370 Uiso calc . 1.00 . H5 0.6458 0.6033 -0.0625 0.0431 Uiso calc . 1.00 . H6 0.7286 0.5624 -0.0147 0.0408 Uiso calc . 1.00 . H7 0.2913 0.0212 0.5846 0.0310 Uiso calc . 1.00 . H8 0.3873 -0.0434 0.3326 0.0355 Uiso calc . 1.00 . H9 0.3647 -0.0161 0.7242 0.0392 Uiso calc . 1.00 . H10 0.4483 -0.0632 0.7675 0.0388 Uiso calc . 1.00 . H11 0.4609 -0.0986 0.4705 0.0439 Uiso calc . 1.00 . H12 0.4979 -0.0901 0.6501 0.0391 Uiso calc . 1.00 . H13 1.0014 0.1626 -0.0775 0.0571 Uiso calc . 1.00 . H14 1.0042 0.3343 -0.0137 0.0571 Uiso calc . 1.00 . H15 1.0613 0.1058 0.0647 0.0498 Uiso calc . 1.00 . H16 1.0156 0.0058 0.0859 0.0498 Uiso calc . 1.00 . H17 0.3786 0.3835 -0.2189 0.0439 Uiso calc . 1.00 . H18 0.3737 0.4764 -0.1180 0.0439 Uiso calc . 1.00 . H19 0.6549 0.0169 0.8234 0.0520 Uiso calc . 1.00 . H20 0.7049 -0.0262 0.7939 0.0520 Uiso calc . 1.00 . H21 0.7111 0.1802 0.9430 0.0424 Uiso calc . 1.00 . H22 0.6892 0.3216 0.8624 0.0424 Uiso calc . 1.00 . H23 0.4526 0.3398 -0.1143 0.0561 Uiso calc . 1.00 . H24 0.4257 0.1609 -0.1139 0.0561 Uiso calc . 1.00 . H25 0.0841 0.5404 0.6082 0.0357 Uiso calc . 1.00 . H26 0.0366 0.4607 0.6343 0.0357 Uiso calc . 1.00 . H27 0.0903 0.2332 0.7228 0.0369 Uiso calc . 1.00 . H28 0.0931 0.4141 0.7776 0.0369 Uiso calc . 1.00 . H29 0.5370 0.1348 0.5091 0.0510 Uiso calc . 1.00 . H30 0.5220 0.3240 0.4715 0.0510 Uiso calc . 1.00 . H31 0.5139 0.0214 0.3508 0.0410 Uiso calc . 1.00 . H32 0.4813 0.1887 0.3291 0.0410 Uiso calc . 1.00 . H33 0.5640 0.1273 0.2450 0.0543 Uiso calc . 1.00 . H34 0.5312 0.2939 0.2228 0.0543 Uiso calc . 1.00 . H35 0.5803 0.4497 0.3504 0.0598 Uiso calc . 1.00 . H36 0.6206 0.3136 0.3388 0.0598 Uiso calc . 1.00 . 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 S(11) 0.044(2) 0.049(2) 0.017(2) -0.005(1) 0.007(2) -0.005(1) S(12) 0.039(2) 0.044(2) 0.015(2) 0.000(1) 0.007(2) 0.000(1) S(13) 0.049(2) 0.060(2) 0.013(2) -0.004(2) 0.007(2) 0.006(2) S(14) 0.041(2) 0.045(2) 0.021(2) -0.003(1) 0.007(2) -0.002(1) S(15) 0.036(2) 0.041(2) 0.019(2) -0.003(1) 0.007(2) -0.002(1) S(16) 0.038(2) 0.039(2) 0.021(2) -0.001(1) 0.008(2) -0.002(1) S(17) 0.043(2) 0.042(2) 0.023(2) 0.004(1) 0.006(2) -0.005(1) S(18) 0.037(2) 0.049(2) 0.022(2) 0.001(1) 0.006(2) -0.003(1) S(19) 0.040(2) 0.042(2) 0.019(2) 0.000(1) 0.006(2) 0.000(1) S(21) 0.041(2) 0.055(2) 0.018(2) -0.007(1) 0.004(2) -0.007(1) S(22) 0.038(2) 0.043(2) 0.016(2) 0.001(1) 0.005(2) 0.000(1) S(23) 0.043(2) 0.057(2) 0.020(2) 0.002(1) 0.006(2) 0.005(2) S(24) 0.047(2) 0.041(2) 0.022(2) -0.004(1) 0.013(2) -0.004(1) S(25) 0.038(2) 0.039(2) 0.019(2) -0.003(1) 0.006(2) -0.003(1) S(26) 0.041(2) 0.042(2) 0.015(2) -0.005(1) 0.005(2) 0.002(1) S(27) 0.046(2) 0.046(2) 0.016(2) 0.003(1) 0.007(2) -0.005(1) S(28) 0.037(2) 0.048(2) 0.024(2) 0.001(1) 0.006(2) -0.002(1) S(29) 0.037(2) 0.044(2) 0.020(2) 0.000(1) 0.006(2) -0.001(1) F(1) 0.060(5) 0.076(5) 0.059(6) -0.009(4) 0.017(5) -0.008(5) F(2) 0.060(7) 0.21(1) 0.077(8) 0.028(7) 0.016(7) 0.082(9) F(3) 0.098(9) 0.17(1) 0.058(7) 0.039(7) 0.040(7) 0.078(7) F(4) 0.13(1) 0.093(7) 0.13(1) -0.035(7) -0.057(10) -0.005(8) O(1) 0.062(5) 0.062(5) 0.019(5) 0.002(5) 0.015(5) 0.006(4) N(11) 0.047(4) 0.047(6) 0.026(6) -0.004(5) 0.016(5) -0.014(5) N(12) 0.046(5) 0.047(5) 0.018(4) -0.006(5) 0.008(5) -0.002(5) N(21) 0.040(4) 0.052(6) 0.012(5) 0.002(5) 0.004(5) -0.002(5) N(22) 0.046(6) 0.055(6) 0.012(3) -0.011(5) -0.009(5) 0.011(5) C(1) 0.044(6) 0.035(6) 0.014(5) -0.002(5) 0.006(5) -0.006(5) C(2) 0.042(5) 0.032(5) 0.013(6) -0.005(5) 0.005(4) -0.008(5) C(3) 0.041(6) 0.040(6) 0.012(6) 0.002(5) 0.006(5) 0.000(5) C(4) 0.040(6) 0.028(5) 0.013(5) -0.003(5) 0.000(5) -0.002(5) C(5) 0.039(5) 0.043(6) 0.009(5) 0.009(5) 0.008(5) -0.002(5) C(6) 0.037(5) 0.035(6) 0.013(6) 0.002(5) -0.003(4) -0.001(5) C(7) 0.038(5) 0.043(6) 0.014(6) 0.008(5) 0.001(5) -0.008(5) C(8) 0.049(6) 0.036(6) 0.010(5) 0.009(5) 0.014(4) -0.004(5) C(9) 0.027(5) 0.043(6) 0.017(6) -0.003(5) 0.003(4) 0.003(5) C(10) 0.028(5) 0.044(6) 0.014(6) -0.005(5) -0.002(5) -0.002(5) C(11) 0.036(3) 0.034(5) 0.020(4) -0.007(5) 0.006(4) -0.009(5) C(12) 0.047(6) 0.052(7) 0.010(6) -0.008(6) 0.010(5) -0.006(6) C(13) 0.012(6) 0.067(8) 0.022(6) 0.018(5) -0.016(5) 0.003(6) C(14) 0.042(6) 0.071(9) 0.005(7) 0.009(6) -0.006(5) -0.005(6) C(15) 0.041(6) 0.060(8) 0.012(6) 0.002(6) 0.007(5) -0.001(6) C(16) 0.047(4) 0.031(6) 0.018(4) 0.000(5) 0.010(4) -0.005(5) C(17) 0.038(3) 0.039(6) 0.027(6) 0.004(5) 0.008(4) -0.008(5) C(18) 0.046(4) 0.060(8) 0.028(7) 0.004(6) 0.016(6) -0.008(6) C(19) 0.049(9) 0.047(7) 0.032(6) 0.007(6) 0.014(7) -0.011(4) C(20) 0.040(3) 0.034(6) 0.020(4) -0.008(5) 0.004(4) 0.003(4) C(21) 0.032(5) 0.031(6) 0.019(6) -0.005(4) -0.003(5) 0.013(5) C(22) 0.027(4) 0.060(7) 0.020(3) 0.006(5) -0.002(4) 0.005(6) C(23) 0.043(6) 0.030(5) 0.017(6) 0.009(5) 0.004(5) 0.006(5) C(24) 0.031(5) 0.052(7) 0.010(6) -0.007(5) 0.001(4) 0.010(5) C(25) 0.040(5) 0.041(6) 0.014(6) 0.003(5) 0.009(5) -0.001(5) C(26) 0.045(6) 0.036(6) 0.018(6) -0.005(5) 0.008(5) 0.004(5) C(27) 0.044(6) 0.049(7) 0.008(6) 0.000(5) 0.006(5) 0.015(5) C(28) 0.043(6) 0.046(6) 0.006(5) -0.004(5) 0.004(4) -0.003(5) C(29) 0.040(5) 0.040(6) 0.017(6) -0.007(5) 0.011(5) -0.007(5) C(30) 0.039(6) 0.060(8) 0.016(3) 0.010(5) 0.013(4) 0.016(6) C(31) 0.042(5) 0.036(6) 0.022(4) 0.005(5) 0.014(5) 0.001(5) C(32) 0.036(4) 0.032(5) 0.016(3) -0.003(4) 0.005(4) -0.002(5) C(33) 0.039(3) 0.042(6) 0.022(5) 0.010(5) 0.013(4) 0.005(4) C(34) 0.043(4) 0.020(5) 0.029(5) 0.000(4) 0.012(4) -0.009(4) C(35) 0.068(6) 0.038(6) 0.016(7) -0.010(4) 0.009(6) 0.013(5) C(36) 0.051(5) 0.031(6) 0.024(4) 0.004(4) 0.022(5) 0.005(5) C(37) 0.047(6) 0.047(7) 0.024(3) 0.010(5) 0.013(4) 0.024(6) C(38) 0.057(9) 0.058(7) 0.022(5) -0.003(6) 0.011(6) 0.006(5) C(39) 0.048(5) 0.048(7) 0.028(8) 0.008(5) 0.020(6) 0.005(5) C(40) 0.064(8) 0.060(8) 0.018(3) -0.001(6) 0.007(6) -0.003(6) C(42) 0.046(8) 0.043(6) 0.018(5) 0.026(6) 0.000(6) 0.007(4) C(43) 0.052(6) 0.060(8) 0.003(5) 0.014(6) 0.002(5) -0.004(6) C(44) 0.051(6) 0.033(6) 0.025(8) 0.010(5) 0.008(6) 0.007(5) C(47) 0.044(3) 0.064(8) 0.008(6) 0.000(6) 0.007(5) 0.019(6) C(48) 0.059(6) 0.043(7) 0.031(7) -0.008(6) -0.002(7) -0.014(6) C(49) 0.08(1) 0.041(7) 0.020(7) -0.001(6) 0.011(7) -0.006(5) C(50) 0.053(9) 0.052(8) 0.05(1) 0.001(6) 0.012(7) 0.020(7) C(51) 0.09(1) 0.057(8) 0.017(6) 0.006(7) 0.010(7) 0.006(6) C(52) 0.043(6) 0.032(6) 0.023(6) 0.009(5) 0.010(5) 0.010(5) C(53) 0.030(6) 0.046(6) 0.020(6) -0.001(5) 0.006(4) -0.005(5) C(54) 0.032(6) 0.058(7) 0.024(6) 0.011(6) 0.005(6) 0.007(6) C(55) 0.05(1) 0.041(6) 0.022(6) 0.002(6) 0.007(6) -0.005(6) B(1) 0.064(8) 0.086(8) 0.09(1) -0.022(8) 0.038(9) 0.041(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0146(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3525 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0805 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0847 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.249 _refine_ls_shift/esd_max 0.2960 _refine_ls_shift/esd_mean 0.0170 _refine_diff_density_min -0.97 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _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 S(11) N(11) 1.63(2) 1_555 1_555 yes S(11) N(12) 1.65(2) 1_555 1_555 yes S(12) C(22) 1.74(2) 1_555 1_555 yes S(12) C(30) 1.75(2) 1_555 1_555 yes S(13) C(30) 1.79(2) 1_555 1_555 yes S(13) C(35) 1.81(2) 1_555 1_555 yes S(14) C(31) 1.74(2) 1_555 1_555 yes S(14) C(40) 1.79(2) 1_555 1_555 yes S(15) C(22) 1.76(2) 1_555 1_555 yes S(15) C(31) 1.76(2) 1_555 1_555 yes S(16) C(20) 1.75(2) 1_555 1_555 yes S(16) C(34) 1.75(2) 1_555 1_555 yes S(17) C(34) 1.76(2) 1_555 1_555 yes S(17) C(47) 1.83(2) 1_555 1_555 yes S(18) C(33) 1.75(2) 1_555 1_555 yes S(18) C(42) 1.83(2) 1_555 1_555 yes S(19) C(20) 1.74(2) 1_555 1_555 yes S(19) C(33) 1.77(2) 1_555 1_555 yes S(21) N(21) 1.64(2) 1_555 1_555 yes S(21) N(22) 1.64(2) 1_555 1_555 yes S(22) C(32) 1.71(2) 1_555 1_555 yes S(22) C(37) 1.76(2) 1_555 1_555 yes S(23) C(37) 1.75(2) 1_555 1_555 yes S(23) C(39) 1.82(2) 1_555 1_555 yes S(24) C(36) 1.76(2) 1_555 1_555 yes S(24) C(38) 1.86(2) 1_555 1_555 yes S(25) C(32) 1.79(2) 1_555 1_555 yes S(25) C(36) 1.77(2) 1_555 1_555 yes S(26) C(11) 1.74(2) 1_555 1_555 yes S(26) C(16) 1.75(2) 1_555 1_555 yes S(27) C(16) 1.76(2) 1_555 1_555 yes S(27) C(18) 1.82(2) 1_555 1_555 yes S(28) C(17) 1.79(2) 1_555 1_555 yes S(28) C(19) 1.84(2) 1_555 1_555 yes S(29) C(11) 1.78(2) 1_555 1_555 yes S(29) C(17) 1.75(2) 1_555 1_555 yes F(1) B(1) 1.36(4) 1_555 1_555 yes F(2) B(1) 1.42(4) 1_555 1_555 yes F(3) B(1) 1.46(4) 1_555 1_555 yes F(4) B(1) 1.31(4) 1_555 1_555 yes O(1) C(48) 1.38(3) 1_555 1_555 yes O(1) C(51) 1.46(3) 1_555 1_555 yes N(11) C(52) 1.29(3) 1_555 1_555 yes N(12) C(26) 1.33(3) 1_555 1_555 yes N(21) C(1) 1.43(3) 1_555 1_555 yes N(22) C(2) 1.31(3) 1_555 1_555 yes C(1) C(2) 1.42(3) 1_555 1_555 yes C(1) C(5) 1.40(3) 1_555 1_555 yes C(2) C(3) 1.49(3) 1_555 1_555 yes C(3) C(4) 1.43(3) 1_555 1_555 yes C(3) C(11) 1.37(3) 1_555 1_555 yes C(4) C(6) 1.46(3) 1_555 1_555 yes C(4) C(10) 1.39(3) 1_555 1_555 yes C(5) C(6) 1.47(3) 1_555 1_555 yes C(5) C(32) 1.42(3) 1_555 1_555 yes C(6) C(7) 1.41(3) 1_555 1_555 yes C(7) C(8) 1.39(3) 1_555 1_555 yes C(8) C(9) 1.40(2) 1_555 1_555 yes C(8) C(12) 1.38(3) 1_555 1_555 yes C(9) C(10) 1.43(3) 1_555 1_555 yes C(9) C(15) 1.44(3) 1_555 1_555 yes C(12) C(13) 1.39(3) 1_555 1_555 yes C(13) C(14) 1.37(3) 1_555 1_555 yes C(14) C(15) 1.32(3) 1_555 1_555 yes C(16) C(17) 1.30(3) 1_555 1_555 yes C(18) C(19) 1.53(3) 1_555 1_555 yes C(20) C(21) 1.34(3) 1_555 1_555 yes C(21) C(24) 1.48(3) 1_555 1_555 yes C(21) C(26) 1.44(3) 1_555 1_555 yes C(22) C(23) 1.36(3) 1_555 1_555 yes C(23) C(25) 1.51(3) 1_555 1_555 yes C(23) C(52) 1.46(3) 1_555 1_555 yes C(24) C(25) 1.44(2) 1_555 1_555 yes C(24) C(27) 1.47(3) 1_555 1_555 yes C(25) C(29) 1.35(3) 1_555 1_555 yes C(26) C(52) 1.47(3) 1_555 1_555 yes C(27) C(28) 1.36(3) 1_555 1_555 yes C(28) C(43) 1.47(3) 1_555 1_555 yes C(28) C(53) 1.43(2) 1_555 1_555 yes C(29) C(53) 1.45(3) 1_555 1_555 yes C(30) C(31) 1.32(3) 1_555 1_555 yes C(33) C(34) 1.32(3) 1_555 1_555 yes C(35) C(40) 1.54(3) 1_555 1_555 yes C(36) C(37) 1.34(3) 1_555 1_555 yes C(38) C(39) 1.52(3) 1_555 1_555 yes C(42) C(47) 1.50(3) 1_555 1_555 yes C(43) C(44) 1.36(3) 1_555 1_555 yes C(44) C(55) 1.34(3) 1_555 1_555 yes C(48) C(49) 1.53(3) 1_555 1_555 yes C(49) C(50) 1.59(3) 1_555 1_555 yes C(50) C(51) 1.52(4) 1_555 1_555 yes C(53) C(54) 1.41(3) 1_555 1_555 yes C(54) C(55) 1.39(3) 1_555 1_555 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 N(11) S(11) N(12) 98.1(10) 1_555 1_555 1_555 yes C(22) S(12) C(30) 96(1) 1_555 1_555 1_555 yes C(30) S(13) C(35) 99(1) 1_555 1_555 1_555 yes C(31) S(14) C(40) 98(1) 1_555 1_555 1_555 yes C(22) S(15) C(31) 97(1) 1_555 1_555 1_555 yes C(20) S(16) C(34) 97.5(10) 1_555 1_555 1_555 yes C(34) S(17) C(47) 99.1(10) 1_555 1_555 1_555 yes C(33) S(18) C(42) 98.8(10) 1_555 1_555 1_555 yes C(20) S(19) C(33) 96.9(10) 1_555 1_555 1_555 yes N(21) S(21) N(22) 99.6(9) 1_555 1_555 1_555 yes C(32) S(22) C(37) 97(1) 1_555 1_555 1_555 yes C(37) S(23) C(39) 99(1) 1_555 1_555 1_555 yes C(36) S(24) C(38) 98.6(10) 1_555 1_555 1_555 yes C(32) S(25) C(36) 95(1) 1_555 1_555 1_555 yes C(11) S(26) C(16) 97.2(10) 1_555 1_555 1_555 yes C(16) S(27) C(18) 99(1) 1_555 1_555 1_555 yes C(17) S(28) C(19) 99.9(10) 1_555 1_555 1_555 yes C(11) S(29) C(17) 95.0(9) 1_555 1_555 1_555 yes C(48) O(1) C(51) 103(1) 1_555 1_555 1_555 yes S(11) N(11) C(52) 106(1) 1_555 1_555 1_555 yes S(11) N(12) C(26) 109(1) 1_555 1_555 1_555 yes S(21) N(21) C(1) 105(1) 1_555 1_555 1_555 yes S(21) N(22) C(2) 107(1) 1_555 1_555 1_555 yes N(21) C(1) C(2) 111(1) 1_555 1_555 1_555 yes N(21) C(1) C(5) 123(1) 1_555 1_555 1_555 yes C(2) C(1) C(5) 124(1) 1_555 1_555 1_555 yes N(22) C(2) C(1) 115(1) 1_555 1_555 1_555 yes N(22) C(2) C(3) 125(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 118(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 114(1) 1_555 1_555 1_555 yes C(2) C(3) C(11) 120(1) 1_555 1_555 1_555 yes C(4) C(3) C(11) 125(1) 1_555 1_555 1_555 yes C(3) C(4) C(6) 121(1) 1_555 1_555 1_555 yes C(3) C(4) C(10) 120(1) 1_555 1_555 1_555 yes C(6) C(4) C(10) 117(1) 1_555 1_555 1_555 yes C(1) C(5) C(6) 114(1) 1_555 1_555 1_555 yes C(1) C(5) C(32) 118(1) 1_555 1_555 1_555 yes C(6) C(5) C(32) 126(1) 1_555 1_555 1_555 yes C(4) C(6) C(5) 119(1) 1_555 1_555 1_555 yes C(4) C(6) C(7) 117(1) 1_555 1_555 1_555 yes C(5) C(6) C(7) 122(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 123(1) 1_555 1_555 1_555 yes C(6) C(7) H(1) 112(3) 1_555 1_555 1_555 no C(8) C(7) H(1) 124(3) 1_555 1_555 1_555 no C(7) C(8) C(9) 120(1) 1_555 1_555 1_555 yes C(7) C(8) C(12) 122(1) 1_555 1_555 1_555 yes C(9) C(8) C(12) 117(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 117(1) 1_555 1_555 1_555 yes C(8) C(9) C(15) 119(1) 1_555 1_555 1_555 yes C(10) C(9) C(15) 123(1) 1_555 1_555 1_555 yes C(4) C(10) C(9) 123(1) 1_555 1_555 1_555 yes C(4) C(10) H(2) 115(3) 1_555 1_555 1_555 no C(9) C(10) H(2) 121(3) 1_555 1_555 1_555 no S(26) C(11) S(29) 112(1) 1_555 1_555 1_555 yes S(26) C(11) C(3) 126(1) 1_555 1_555 1_555 yes S(29) C(11) C(3) 121(1) 1_555 1_555 1_555 yes C(8) C(12) C(13) 122(1) 1_555 1_555 1_555 yes C(8) C(12) H(3) 115(3) 1_555 1_555 1_555 no C(13) C(12) H(3) 121(3) 1_555 1_555 1_555 no C(12) C(13) C(14) 118(1) 1_555 1_555 1_555 yes C(12) C(13) H(4) 116(3) 1_555 1_555 1_555 no C(14) C(13) H(4) 125(3) 1_555 1_555 1_555 no C(13) C(14) C(15) 122(1) 1_555 1_555 1_555 yes C(13) C(14) H(5) 119(3) 1_555 1_555 1_555 no C(15) C(14) H(5) 117(3) 1_555 1_555 1_555 no C(9) C(15) C(14) 120(1) 1_555 1_555 1_555 yes C(9) C(15) H(6) 114(3) 1_555 1_555 1_555 no C(14) C(15) H(6) 125(3) 1_555 1_555 1_555 no S(26) C(16) S(27) 113(1) 1_555 1_555 1_555 yes S(26) C(16) C(17) 116(1) 1_555 1_555 1_555 yes S(27) C(16) C(17) 130(1) 1_555 1_555 1_555 yes S(28) C(17) S(29) 112(1) 1_555 1_555 1_555 yes S(28) C(17) C(16) 128(1) 1_555 1_555 1_555 yes S(29) C(17) C(16) 119(1) 1_555 1_555 1_555 yes S(27) C(18) C(19) 112(1) 1_555 1_555 1_555 yes S(27) C(18) H(13) 111(3) 1_555 1_555 1_555 no S(27) C(18) H(14) 110(2) 1_555 1_555 1_555 no C(19) C(18) H(13) 104(2) 1_555 1_555 1_555 no C(19) C(18) H(14) 102(3) 1_555 1_555 1_555 no H(13) C(18) H(14) 115(4) 1_555 1_555 1_555 no S(28) C(19) C(18) 110(1) 1_555 1_555 1_555 yes S(28) C(19) H(15) 104(2) 1_555 1_555 1_555 no S(28) C(19) H(16) 106(2) 1_555 1_555 1_555 no C(18) C(19) H(15) 114(2) 1_555 1_555 1_555 no C(18) C(19) H(16) 117(3) 1_555 1_555 1_555 no H(15) C(19) H(16) 102(2) 1_555 1_555 1_555 no S(16) C(20) S(19) 112(1) 1_555 1_555 1_555 yes S(16) C(20) C(21) 123(1) 1_555 1_555 1_555 yes S(19) C(20) C(21) 123(1) 1_555 1_555 1_555 yes C(20) C(21) C(24) 128(1) 1_555 1_555 1_555 yes C(20) C(21) C(26) 119(1) 1_555 1_555 1_555 yes C(24) C(21) C(26) 111(1) 1_555 1_555 1_555 yes S(12) C(22) S(15) 112(1) 1_555 1_555 1_555 yes S(12) C(22) C(23) 122(1) 1_555 1_555 1_555 yes S(15) C(22) C(23) 125(1) 1_555 1_555 1_555 yes C(22) C(23) C(25) 125(1) 1_555 1_555 1_555 yes C(22) C(23) C(52) 121(1) 1_555 1_555 1_555 yes C(25) C(23) C(52) 113(1) 1_555 1_555 1_555 yes C(21) C(24) C(25) 122(1) 1_555 1_555 1_555 yes C(21) C(24) C(27) 119(1) 1_555 1_555 1_555 yes C(25) C(24) C(27) 117(1) 1_555 1_555 1_555 yes C(23) C(25) C(24) 120(1) 1_555 1_555 1_555 yes C(23) C(25) C(29) 118(1) 1_555 1_555 1_555 yes C(24) C(25) C(29) 120(1) 1_555 1_555 1_555 yes N(12) C(26) C(21) 125(1) 1_555 1_555 1_555 yes N(12) C(26) C(52) 108(1) 1_555 1_555 1_555 yes C(21) C(26) C(52) 126(1) 1_555 1_555 1_555 yes C(24) C(27) C(28) 120(1) 1_555 1_555 1_555 yes C(24) C(27) H(7) 123(3) 1_555 1_555 1_555 no C(28) C(27) H(7) 116(2) 1_555 1_555 1_555 no C(27) C(28) C(43) 119(1) 1_555 1_555 1_555 yes C(27) C(28) C(53) 122(1) 1_555 1_555 1_555 yes C(43) C(28) C(53) 118(1) 1_555 1_555 1_555 yes C(25) C(29) C(53) 122(1) 1_555 1_555 1_555 yes C(25) C(29) H(8) 127(3) 1_555 1_555 1_555 no C(53) C(29) H(8) 110(3) 1_555 1_555 1_555 no S(12) C(30) S(13) 112(1) 1_555 1_555 1_555 yes S(12) C(30) C(31) 119(1) 1_555 1_555 1_555 yes S(13) C(30) C(31) 128(1) 1_555 1_555 1_555 yes S(14) C(31) S(15) 114(1) 1_555 1_555 1_555 yes S(14) C(31) C(30) 130(1) 1_555 1_555 1_555 yes S(15) C(31) C(30) 114(1) 1_555 1_555 1_555 yes S(22) C(32) S(25) 112(1) 1_555 1_555 1_555 yes S(22) C(32) C(5) 123(1) 1_555 1_555 1_555 yes S(25) C(32) C(5) 123(1) 1_555 1_555 1_555 yes S(18) C(33) S(19) 112(1) 1_555 1_555 1_555 yes S(18) C(33) C(34) 130(1) 1_555 1_555 1_555 yes S(19) C(33) C(34) 117(1) 1_555 1_555 1_555 yes S(16) C(34) S(17) 114(1) 1_555 1_555 1_555 yes S(16) C(34) C(33) 116(1) 1_555 1_555 1_555 yes S(17) C(34) C(33) 128(1) 1_555 1_555 1_555 yes S(13) C(35) C(40) 111(1) 1_555 1_555 1_555 yes S(13) C(35) H(17) 112(2) 1_555 1_555 1_555 no S(13) C(35) H(18) 110(2) 1_555 1_555 1_555 no C(40) C(35) H(17) 107(3) 1_555 1_555 1_555 no C(40) C(35) H(18) 105(3) 1_555 1_555 1_555 no H(17) C(35) H(18) 109(2) 1_555 1_555 1_555 no S(24) C(36) S(25) 114(1) 1_555 1_555 1_555 yes S(24) C(36) C(37) 128(1) 1_555 1_555 1_555 yes S(25) C(36) C(37) 115(1) 1_555 1_555 1_555 yes S(22) C(37) S(23) 113(1) 1_555 1_555 1_555 yes S(22) C(37) C(36) 116(1) 1_555 1_555 1_555 yes S(23) C(37) C(36) 129(1) 1_555 1_555 1_555 yes S(24) C(38) C(39) 111(1) 1_555 1_555 1_555 yes S(24) C(38) H(19) 116(3) 1_555 1_555 1_555 no S(24) C(38) H(20) 111(2) 1_555 1_555 1_555 no C(39) C(38) H(19) 109(2) 1_555 1_555 1_555 no C(39) C(38) H(20) 105(2) 1_555 1_555 1_555 no H(19) C(38) H(20) 101(2) 1_555 1_555 1_555 no S(23) C(39) C(38) 110(1) 1_555 1_555 1_555 yes S(23) C(39) H(21) 104(2) 1_555 1_555 1_555 no S(23) C(39) H(22) 109(2) 1_555 1_555 1_555 no C(38) C(39) H(21) 112(1) 1_555 1_555 1_555 no C(38) C(39) H(22) 116(3) 1_555 1_555 1_555 no H(21) C(39) H(22) 100(3) 1_555 1_555 1_555 no S(14) C(40) C(35) 114(1) 1_555 1_555 1_555 yes S(14) C(40) H(23) 103(3) 1_555 1_555 1_555 no S(14) C(40) H(24) 103(3) 1_555 1_555 1_555 no C(35) C(40) H(23) 111(2) 1_555 1_555 1_555 no C(35) C(40) H(24) 110(3) 1_555 1_555 1_555 no H(23) C(40) H(24) 112(3) 1_555 1_555 1_555 no S(18) C(42) C(47) 111(1) 1_555 1_555 1_555 yes S(18) C(42) H(25) 113(2) 1_555 1_555 1_555 no S(18) C(42) H(26) 116(2) 1_555 1_555 1_555 no C(47) C(42) H(25) 101(3) 1_555 1_555 1_555 no C(47) C(42) H(26) 104(3) 1_555 1_555 1_555 no H(25) C(42) H(26) 107(1) 1_555 1_555 1_555 no C(28) C(43) C(44) 117(1) 1_555 1_555 1_555 yes C(28) C(43) H(9) 126(3) 1_555 1_555 1_555 no C(44) C(43) H(9) 116(3) 1_555 1_555 1_555 no C(43) C(44) C(55) 124(2) 1_555 1_555 1_555 yes C(43) C(44) H(10) 116(2) 1_555 1_555 1_555 no C(55) C(44) H(10) 118(2) 1_555 1_555 1_555 no S(17) C(47) C(42) 112(1) 1_555 1_555 1_555 yes S(17) C(47) H(27) 108(2) 1_555 1_555 1_555 no S(17) C(47) H(28) 106(2) 1_555 1_555 1_555 no C(42) C(47) H(27) 113(3) 1_555 1_555 1_555 no C(42) C(47) H(28) 113(2) 1_555 1_555 1_555 no H(27) C(47) H(28) 101(3) 1_555 1_555 1_555 no O(1) C(48) C(49) 109(1) 1_555 1_555 1_555 yes O(1) C(48) H(29) 106(2) 1_555 1_555 1_555 no O(1) C(48) H(30) 109(2) 1_555 1_555 1_555 no C(49) C(48) H(29) 113(2) 1_555 1_555 1_555 no C(49) C(48) H(30) 117(3) 1_555 1_555 1_555 no H(29) C(48) H(30) 100(3) 1_555 1_555 1_555 no C(48) C(49) C(50) 102(1) 1_555 1_555 1_555 yes C(48) C(49) H(31) 106(3) 1_555 1_555 1_555 no C(48) C(49) H(32) 105(2) 1_555 1_555 1_555 no C(50) C(49) H(31) 114(2) 1_555 1_555 1_555 no C(50) C(49) H(32) 115(2) 1_555 1_555 1_555 no H(31) C(49) H(32) 111(3) 1_555 1_555 1_555 no C(49) C(50) C(51) 102(2) 1_555 1_555 1_555 yes C(49) C(50) H(33) 111(2) 1_555 1_555 1_555 no C(49) C(50) H(34) 112(3) 1_555 1_555 1_555 no C(51) C(50) H(33) 107(3) 1_555 1_555 1_555 no C(51) C(50) H(34) 108(2) 1_555 1_555 1_555 no H(33) C(50) H(34) 114(5) 1_555 1_555 1_555 no O(1) C(51) C(50) 107(1) 1_555 1_555 1_555 yes O(1) C(51) H(35) 104(3) 1_555 1_555 1_555 no O(1) C(51) H(36) 103(3) 1_555 1_555 1_555 no C(50) C(51) H(35) 117(3) 1_555 1_555 1_555 no C(50) C(51) H(36) 116(2) 1_555 1_555 1_555 no H(35) C(51) H(36) 104(3) 1_555 1_555 1_555 no N(11) C(52) C(23) 124(1) 1_555 1_555 1_555 yes N(11) C(52) C(26) 116(1) 1_555 1_555 1_555 yes C(23) C(52) C(26) 118(1) 1_555 1_555 1_555 yes C(28) C(53) C(29) 116(1) 1_555 1_555 1_555 yes C(28) C(53) C(54) 118(1) 1_555 1_555 1_555 yes C(29) C(53) C(54) 124(1) 1_555 1_555 1_555 yes C(53) C(54) C(55) 120(1) 1_555 1_555 1_555 yes C(53) C(54) H(11) 121(3) 1_555 1_555 1_555 no C(55) C(54) H(11) 117(3) 1_555 1_555 1_555 no C(44) C(55) C(54) 120(2) 1_555 1_555 1_555 yes C(44) C(55) H(12) 116(3) 1_555 1_555 1_555 no C(54) C(55) H(12) 123(3) 1_555 1_555 1_555 no F(1) B(1) F(2) 106(3) 1_555 1_555 1_555 yes F(1) B(1) F(3) 107(1) 1_555 1_555 1_555 yes F(1) B(1) F(4) 112(2) 1_555 1_555 1_555 yes F(2) B(1) F(3) 105(2) 1_555 1_555 1_555 yes F(2) B(1) F(4) 112(2) 1_555 1_555 1_555 yes F(3) B(1) F(4) 112(3) 1_555 1_555 1_555 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 S(12) S(23) 3.474(7) 1_555 2_454 ? S(12) C(39) 3.58(2) 1_555 2_454 ? S(12) C(15) 3.58(2) 1_555 2_465 ? S(14) F(2) 3.28(2) 1_555 1_554 ? S(14) C(16) 3.46(2) 1_555 2_465 ? S(15) C(11) 3.52(2) 1_555 2_465 ? S(15) C(3) 3.57(2) 1_555 2_465 ? S(16) C(32) 3.39(2) 1_555 2_465 ? S(16) C(36) 3.56(2) 1_555 2_455 ? S(16) S(24) 3.600(6) 1_555 2_455 ? S(17) C(36) 3.44(2) 1_555 2_465 ? S(17) C(38) 3.53(2) 1_555 2_455 ? S(17) C(37) 3.59(2) 1_555 2_465 ? S(19) O(1) 3.40(1) 1_555 2_455 ? S(21) F(3) 3.43(2) 1_555 2_565 ? S(22) C(35) 3.41(2) 1_555 2_566 ? S(24) O(1) 3.16(2) 1_555 1_555 ? S(24) C(34) 3.40(2) 1_555 2_555 ? S(25) C(21) 3.37(2) 1_555 2_555 ? S(25) O(1) 3.37(2) 1_555 1_555 ? S(25) C(20) 3.45(2) 1_555 2_555 ? S(25) C(34) 3.60(2) 1_555 2_565 ? S(26) C(22) 3.46(2) 1_555 2_555 ? S(26) C(31) 3.59(2) 1_555 2_565 ? S(27) C(31) 3.58(2) 1_555 2_555 ? F(1) C(39) 3.05(2) 1_555 1_555 ? F(1) C(14) 3.12(2) 1_555 1_556 ? F(1) C(38) 3.13(2) 1_555 1_555 ? F(1) C(13) 3.38(2) 1_555 1_556 ? F(1) C(47) 3.49(2) 1_555 2_565 ? F(2) C(40) 3.04(3) 1_555 1_556 ? F(2) C(19) 3.11(2) 1_555 2_456 ? F(2) C(18) 3.55(3) 1_555 2_456 ? F(3) C(40) 3.34(3) 1_555 1_556 ? F(3) C(42) 3.35(2) 1_555 2_565 ? F(3) C(47) 3.49(3) 1_555 2_565 ? F(4) C(55) 3.38(3) 1_555 1_555 ? F(4) C(44) 3.49(3) 1_555 1_555 ? F(4) C(18) 3.56(3) 1_555 2_456 ? O(1) C(42) 3.36(2) 1_555 2_565 ? N(11) C(39) 3.53(3) 1_555 2_454 ? N(21) C(35) 3.54(3) 1_555 2_566 ? C(3) C(29) 3.42(2) 1_555 2_555 ? C(7) C(20) 3.50(2) 1_555 2_565 ? C(7) C(21) 3.55(2) 1_555 2_565 ? C(10) C(22) 3.35(3) 1_555 2_565 ? C(11) C(29) 3.53(2) 1_555 2_555 ? C(12) C(51) 3.60(3) 1_555 1_555 ? C(15) C(39) 3.48(3) 1_555 1_554 ? C(27) C(32) 3.31(2) 1_555 2_455 ? C(42) C(48) 3.44(3) 1_555 2_465 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2BF4(THF),300K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:08:07 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1396.77 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H36 B F4 N4 O S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.78(1) _cell_length_b 7.826(1) _cell_length_c 13.346(3) _cell_angle_alpha 90 _cell_angle_beta 101.99(2) _cell_angle_gamma 90 _cell_volume 2838.3601 _cell_formula_units_Z 2 _cell_measurement_temperature 300.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.634 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1426.00 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 300.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 3954 _reflns_number_total 3954 _reflns_number_observed 2354 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.162 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B 0 2 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 8 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.3841(2) 0.1769(7) 0.2247(4) 0.068(2) Uani d . 1.00 . S2 0.2546(2) 0.3438(5) 0.3171(3) 0.057(1) Uani d . 1.00 . S3 0.1664(2) 0.4170(5) 0.1654(3) 0.055(1) Uani d . 1.00 . S4 0.2215(2) 0.4979(8) 0.4914(4) 0.087(2) Uani d . 1.00 . S5 0.1120(2) 0.5795(6) 0.3073(4) 0.068(2) Uani d . 1.00 . S6 0.4065(2) 0.3724(5) -0.0592(3) 0.055(1) Uani d . 1.00 . S7 0.3234(2) 0.4443(5) -0.2249(4) 0.053(1) Uani d . 1.00 . S8 0.4812(2) 0.5168(7) -0.1605(4) 0.075(2) Uani d . 1.00 . S9 0.3802(2) 0.5983(6) -0.3641(4) 0.070(2) Uani d . 1.00 . F1 0.5459 0.0494 0.5232 0.0729 Uani d . 0.50 . F2 0.4920 0.0322 0.5965 0.0729 Uani d . 0.50 . F3 0.4702 0.0738 0.4396 0.0729 Uani d . 0.50 . F4 0.4975 -0.1631 0.4813 0.3694 Uani d . 0.50 . O1 0.541(1) 0.034(4) 0.100(3) 0.10(1) Uani d . 0.50 . N1 0.3279(5) 0.204(2) 0.234(1) 0.057(5) Uani d . 1.00 . N2 0.3792(6) 0.217(2) 0.101(1) 0.066(5) Uani d . 1.00 . C1 0.3017(6) 0.242(2) 0.140(1) 0.051(6) Uani d . 1.00 . C2 0.2509(6) 0.281(2) 0.115(1) 0.042(5) Uani d . 1.00 . C3 0.2258(5) 0.339(2) 0.187(1) 0.046(5) Uani d . 1.00 . C4 0.2282(6) 0.269(2) 0.003(1) 0.041(5) Uani d . 1.00 . C5 0.1787(6) 0.237(2) -0.030(1) 0.049(5) Uani d . 1.00 . C6 0.1561(6) 0.216(2) -0.135(1) 0.050(5) Uani d . 1.00 . C7 0.1059(7) 0.193(2) -0.168(1) 0.061(6) Uani d . 1.00 . C8 0.0853(7) 0.177(3) -0.271(2) 0.081(7) Uani d . 1.00 . C9 0.1145(8) 0.181(3) -0.342(2) 0.098(9) Uani d . 1.00 . C10 0.1636(8) 0.201(3) -0.314(2) 0.081(7) Uani d . 1.00 . C11 0.1869(6) 0.227(2) -0.210(1) 0.050(5) Uani d . 1.00 . C12 0.2368(6) 0.253(2) -0.175(1) 0.053(6) Uani d . 1.00 . C13 0.2597(6) 0.278(2) -0.072(1) 0.041(5) Uani d . 1.00 . C14 0.3125(6) 0.300(2) -0.041(1) 0.048(5) Uani d . 1.00 . C15 0.3440(6) 0.358(2) -0.102(1) 0.047(5) Uani d . 1.00 . C16 0.3313(6) 0.252(2) 0.063(1) 0.040(5) Uani d . 1.00 . C17 0.2081(7) 0.446(2) 0.359(1) 0.062(6) Uani d . 1.00 . C18 0.1671(7) 0.494(2) 0.291(1) 0.060(6) Uani d . 1.00 . C19 0.163(1) 0.557(5) 0.507(2) 0.17(1) Uani d . 1.00 . C20 0.131(1) 0.639(4) 0.442(2) 0.15(1) Uani d . 1.00 . C21 0.4190(6) 0.481(2) -0.166(1) 0.049(5) Uani d . 1.00 . C22 0.3803(6) 0.508(2) -0.244(1) 0.052(5) Uani d . 1.00 . C23 0.4774(9) 0.661(3) -0.271(2) 0.107(9) Uani d . 1.00 . C24 0.4465(10) 0.580(3) -0.360(2) 0.11(1) Uani d . 1.00 . C25 0.536(1) 0.078(4) 0.006(3) 0.13(1) Uani d . 1.00 . C26 0.495(1) -0.018(4) 0.089(2) 0.12(1) Uani d . 1.00 . B1 0.5000 0.0000 0.5000 0.3078 Uani d . 0.50 . H1 0.1585 0.2274 0.0195 0.0575 Uiso calc . 1.00 . H2 0.0845 0.1888 -0.1201 0.0709 Uiso calc . 1.00 . H3 0.0492 0.1650 -0.2946 0.0954 Uiso calc . 1.00 . H4 0.0999 0.1621 -0.4128 0.1211 Uiso calc . 1.00 . H5 0.1823 0.1977 -0.3655 0.0944 Uiso calc . 1.00 . H6 0.2570 0.2555 -0.2252 0.0595 Uiso calc . 1.00 . H7 0.1464 0.4513 0.5173 0.1892 Uiso calc . 1.00 . H8 0.1673 0.6207 0.5691 0.1892 Uiso calc . 1.00 . H9 0.1419 0.7557 0.4420 0.1919 Uiso calc . 1.00 . H10 0.1002 0.6423 0.4673 0.1919 Uiso calc . 1.00 . H11 0.4635 0.7670 -0.2575 0.1221 Uiso calc . 1.00 . H12 0.5098 0.6808 -0.2830 0.1221 Uiso calc . 1.00 . H13 0.4561 0.4634 -0.3573 0.1295 Uiso calc . 1.00 . H14 0.4547 0.6329 -0.4181 0.1295 Uiso calc . 1.00 . H15 0.4960 -0.1094 0.1412 0.1471 Uiso calc . 1.00 . H16 0.4764 0.0741 0.1143 0.1471 Uiso calc . 1.00 . H17 0.5264 0.1983 0.0051 0.1386 Uiso calc . 1.00 . H18 0.5684 0.0736 -0.0057 0.1386 Uiso calc . 1.00 . 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 S(1) 0.058(3) 0.108(4) 0.039(3) 0.009(3) 0.008(3) 0.013(3) S(2) 0.062(3) 0.079(3) 0.032(3) 0.001(2) 0.015(2) -0.001(2) S(3) 0.056(3) 0.076(3) 0.036(3) 0.007(2) 0.019(2) 0.007(2) S(4) 0.088(4) 0.140(5) 0.036(3) 0.000(3) 0.021(3) -0.017(3) S(5) 0.077(3) 0.081(3) 0.052(3) 0.010(2) 0.030(3) 0.004(2) S(6) 0.051(3) 0.078(3) 0.037(3) 0.003(2) 0.015(2) 0.005(2) S(7) 0.051(3) 0.068(3) 0.043(3) 0.002(2) 0.014(2) 0.009(2) S(8) 0.056(3) 0.111(4) 0.060(4) -0.009(3) 0.018(3) 0.013(3) S(9) 0.075(3) 0.085(3) 0.055(3) -0.001(3) 0.021(3) 0.025(3) F(1) 0.0729 0.0729 0.0729 0.0000 0.0151 0.0000 F(2) 0.0729 0.0729 0.0729 0.0000 0.0151 0.0000 F(3) 0.0729 0.0729 0.0729 0.0000 0.0151 0.0000 F(4) 0.3694 0.3694 0.3694 0.0000 0.0768 0.0000 O(1) 0.13(3) 0.11(2) 0.07(2) 0.00(2) 0.03(2) 0.00(2) N(1) 0.056(10) 0.080(9) 0.035(9) 0.013(7) 0.005(8) 0.019(7) N(2) 0.07(1) 0.10(1) 0.025(8) 0.012(9) 0.016(9) 0.009(8) C(1) 0.05(1) 0.061(10) 0.04(1) -0.002(8) 0.01(1) 0.000(8) C(2) 0.041(10) 0.055(9) 0.033(10) -0.011(7) 0.014(8) -0.010(7) C(3) 0.042(10) 0.056(9) 0.04(1) -0.005(7) 0.010(9) 0.009(8) C(4) 0.05(1) 0.051(9) 0.027(9) -0.004(7) 0.019(9) -0.003(7) C(5) 0.04(1) 0.07(1) 0.04(1) -0.007(7) 0.014(9) -0.013(8) C(6) 0.06(1) 0.07(1) 0.022(9) -0.001(8) 0.009(9) 0.004(8) C(7) 0.06(1) 0.08(1) 0.05(1) -0.008(9) 0.02(1) 0.006(10) C(8) 0.05(1) 0.13(2) 0.05(1) -0.01(1) 0.00(1) 0.01(1) C(9) 0.07(2) 0.16(2) 0.06(2) -0.05(1) 0.01(1) -0.03(1) C(10) 0.07(1) 0.13(2) 0.05(1) -0.02(1) 0.02(1) -0.02(1) C(11) 0.05(1) 0.07(1) 0.03(1) -0.008(8) 0.008(10) -0.004(8) C(12) 0.05(1) 0.08(1) 0.03(1) -0.003(8) 0.020(10) 0.000(9) C(13) 0.06(1) 0.044(8) 0.030(9) 0.005(7) 0.022(9) -0.001(7) C(14) 0.07(1) 0.039(8) 0.04(1) 0.015(7) 0.02(1) -0.006(7) C(15) 0.06(1) 0.041(8) 0.04(1) 0.006(7) 0.021(9) 0.001(7) C(16) 0.04(1) 0.055(9) 0.026(9) 0.000(7) 0.010(9) 0.001(7) C(17) 0.06(1) 0.09(1) 0.03(1) -0.02(1) 0.02(1) -0.003(9) C(18) 0.07(1) 0.07(1) 0.04(1) -0.008(9) 0.03(1) 0.013(9) C(19) 0.12(3) 0.37(5) 0.03(1) 0.09(3) 0.00(2) -0.02(2) C(20) 0.19(3) 0.23(3) 0.05(2) 0.09(3) 0.03(2) -0.02(2) C(21) 0.05(1) 0.07(1) 0.028(9) 0.004(8) 0.015(9) 0.003(8) C(22) 0.07(1) 0.048(9) 0.05(1) -0.004(8) 0.03(1) 0.000(8) C(23) 0.11(2) 0.14(2) 0.06(2) -0.08(2) 0.01(1) 0.03(1) C(24) 0.13(2) 0.13(2) 0.09(2) 0.01(2) 0.08(2) 0.03(2) C(25) 0.13(3) 0.13(2) 0.12(3) 0.03(2) 0.04(3) 0.00(2) C(26) 0.08(2) 0.16(2) 0.13(3) -0.03(2) 0.02(2) -0.05(2) B(1) 0.3078 0.3078 0.3078 0.0000 0.0640 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0105(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2354 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 7325369.0000 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 7654360.0000 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 194189.000 _refine_ls_shift/esd_max 20.4510 _refine_ls_shift/esd_mean 0.5200 _refine_diff_density_min -119186.00 _refine_diff_density_max 109013.20 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.60(1) 1_555 1_555 yes S(1) N(2) 1.66(1) 1_555 1_555 yes S(2) C(3) 1.76(2) 1_555 1_555 yes S(2) C(17) 1.71(2) 1_555 1_555 yes S(3) C(3) 1.73(2) 1_555 1_555 yes S(3) C(18) 1.78(2) 1_555 1_555 yes S(4) C(17) 1.77(2) 1_555 1_555 yes S(4) C(19) 1.75(3) 1_555 1_555 yes S(5) C(18) 1.73(2) 1_555 1_555 yes S(5) C(20) 1.82(3) 1_555 1_555 yes S(6) C(15) 1.72(2) 1_555 1_555 yes S(6) C(21) 1.76(1) 1_555 1_555 yes S(7) C(15) 1.75(2) 1_555 1_555 yes S(7) C(22) 1.73(2) 1_555 1_555 yes S(8) C(21) 1.74(2) 1_555 1_555 yes S(8) C(23) 1.84(2) 1_555 1_555 yes S(9) C(22) 1.75(2) 1_555 1_555 yes S(9) C(24) 1.84(2) 1_555 1_555 yes F(1) F(3) 1.2121(1) 1_555 3_656 yes F(1) F(4) 1.4900(4) 1_555 3_656 yes F(1) B(1) 1.3076(5) 1_555 1_555 yes F(2) F(3) 1.4948(4) 1_555 3_656 yes F(2) F(4) 1.530 1_555 3_656 yes F(2) B(1) 1.375 1_555 1_555 yes F(3) F(4) 1.4206(2) 1_555 3_656 yes F(3) B(1) 1.1802(2) 1_555 1_555 yes F(4) B(1) 1.300 1_555 1_555 yes O(1) C(25) 1.28(4) 1_555 1_555 yes O(1) C(26) 1.33(4) 1_555 1_555 yes N(1) C(1) 1.34(2) 1_555 1_555 yes N(2) C(16) 1.35(2) 1_555 1_555 yes C(1) C(2) 1.42(2) 1_555 1_555 yes C(1) C(16) 1.44(2) 1_555 1_555 yes C(2) C(3) 1.38(2) 1_555 1_555 yes C(2) C(4) 1.50(2) 1_555 1_555 yes C(4) C(5) 1.37(2) 1_555 1_555 yes C(4) C(13) 1.46(2) 1_555 1_555 yes C(5) C(6) 1.43(2) 1_555 1_555 yes C(6) C(7) 1.38(2) 1_555 1_555 yes C(6) C(11) 1.45(2) 1_555 1_555 yes C(7) C(8) 1.39(3) 1_555 1_555 yes C(8) C(9) 1.36(2) 1_555 1_555 yes C(9) C(10) 1.34(3) 1_555 1_555 yes C(10) C(11) 1.41(3) 1_555 1_555 yes C(11) C(12) 1.38(2) 1_555 1_555 yes C(12) C(13) 1.41(2) 1_555 1_555 yes C(13) C(14) 1.45(2) 1_555 1_555 yes C(14) C(15) 1.39(2) 1_555 1_555 yes C(14) C(16) 1.43(2) 1_555 1_555 yes C(17) C(18) 1.35(3) 1_555 1_555 yes C(19) C(20) 1.29(4) 1_555 1_555 yes C(21) C(22) 1.35(2) 1_555 1_555 yes C(23) C(24) 1.46(3) 1_555 1_555 yes C(25) C(26) 1.45(4) 1_555 3_655 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 N(1) S(1) N(2) 99.9(8) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.6(8) 1_555 1_555 1_555 yes C(3) S(3) C(18) 98.1(9) 1_555 1_555 1_555 yes C(17) S(4) C(19) 99(1) 1_555 1_555 1_555 yes C(18) S(5) C(20) 98(1) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.6(8) 1_555 1_555 1_555 yes C(15) S(7) C(22) 96.9(8) 1_555 1_555 1_555 yes C(21) S(8) C(23) 100.0(10) 1_555 1_555 1_555 yes C(22) S(9) C(24) 97(1) 1_555 1_555 1_555 yes F(3) F(1) F(4) 97.29(2) 3_656 1_555 3_656 yes F(3) F(1) B(1) 55.704(6) 3_656 1_555 1_555 yes F(4) F(1) B(1) 54.91(2) 3_656 1_555 1_555 yes F(3) F(2) F(4) 84.649(8) 3_656 1_555 3_656 yes F(3) F(2) B(1) 48.3481(8) 3_656 1_555 1_555 yes F(4) F(2) B(1) 52.854(2) 3_656 1_555 1_555 yes F(1) F(3) F(2) 92.00(1) 3_656 1_555 3_656 yes F(1) F(3) F(4) 108.489(9) 3_656 1_555 3_656 yes F(1) F(3) B(1) 66.25(2) 3_656 1_555 1_555 yes F(2) F(3) F(4) 97.68(2) 3_656 1_555 3_656 yes F(2) F(3) B(1) 60.50(1) 3_656 1_555 1_555 yes F(4) F(3) B(1) 59.120(10) 3_656 1_555 1_555 yes F(1) F(4) F(2) 80.80(1) 3_656 1_555 3_656 yes F(1) F(4) F(3) 96.76(2) 3_656 1_555 3_656 yes F(1) F(4) B(1) 55.39(1) 3_656 1_555 1_555 yes F(2) F(4) F(3) 89.648(8) 3_656 1_555 3_656 yes F(2) F(4) B(1) 57.4496(4) 3_656 1_555 1_555 yes F(3) F(4) B(1) 51.184(5) 3_656 1_555 1_555 yes C(25) O(1) C(26) 94(3) 1_555 1_555 1_555 yes S(1) N(1) C(1) 107(1) 1_555 1_555 1_555 yes S(1) N(2) C(16) 106.2(10) 1_555 1_555 1_555 yes N(1) C(1) C(2) 126(1) 1_555 1_555 1_555 yes N(1) C(1) C(16) 113(1) 1_555 1_555 1_555 yes C(2) C(1) C(16) 120(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 121(1) 1_555 1_555 1_555 yes C(1) C(2) C(4) 114(1) 1_555 1_555 1_555 yes C(3) C(2) C(4) 123(1) 1_555 1_555 1_555 yes S(2) C(3) S(3) 112.4(8) 1_555 1_555 1_555 yes S(2) C(3) C(2) 120(1) 1_555 1_555 1_555 yes S(3) C(3) C(2) 127(1) 1_555 1_555 1_555 yes C(2) C(4) C(5) 120(1) 1_555 1_555 1_555 yes C(2) C(4) C(13) 119(1) 1_555 1_555 1_555 yes C(5) C(4) C(13) 119(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 122(1) 1_555 1_555 1_555 yes C(4) C(5) H(1) 119(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 117(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 122(1) 1_555 1_555 1_555 yes C(5) C(6) C(11) 118(1) 1_555 1_555 1_555 yes C(7) C(6) C(11) 119(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 120(1) 1_555 1_555 1_555 yes C(6) C(7) H(2) 121(1) 1_555 1_555 1_555 no C(8) C(7) H(2) 118(2) 1_555 1_555 1_555 no C(7) C(8) C(9) 120(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 120(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 119(2) 1_555 1_555 1_555 no C(8) C(9) C(10) 121(2) 1_555 1_555 1_555 yes C(8) C(9) H(4) 118(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 119(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 121(1) 1_555 1_555 1_555 yes C(9) C(10) H(5) 118(2) 1_555 1_555 1_555 no C(11) C(10) H(5) 120(2) 1_555 1_555 1_555 no C(6) C(11) C(10) 116(1) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 124(1) 1_555 1_555 1_555 yes C(11) C(12) C(13) 124(1) 1_555 1_555 1_555 yes C(11) C(12) H(6) 117(1) 1_555 1_555 1_555 no C(13) C(12) H(6) 117(1) 1_555 1_555 1_555 no C(4) C(13) C(12) 116(1) 1_555 1_555 1_555 yes C(4) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 126(1) 1_555 1_555 1_555 yes C(13) C(14) C(16) 112(1) 1_555 1_555 1_555 yes C(15) C(14) C(16) 120(1) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.6(8) 1_555 1_555 1_555 yes S(6) C(15) C(14) 122(1) 1_555 1_555 1_555 yes S(7) C(15) C(14) 123(1) 1_555 1_555 1_555 yes N(2) C(16) C(1) 112(1) 1_555 1_555 1_555 yes N(2) C(16) C(14) 123(1) 1_555 1_555 1_555 yes C(1) C(16) C(14) 124(1) 1_555 1_555 1_555 yes S(2) C(17) S(4) 114(1) 1_555 1_555 1_555 yes S(2) C(17) C(18) 119(1) 1_555 1_555 1_555 yes S(4) C(17) C(18) 125(1) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114(1) 1_555 1_555 1_555 yes S(3) C(18) C(17) 112(1) 1_555 1_555 1_555 yes S(5) C(18) C(17) 131(1) 1_555 1_555 1_555 yes S(4) C(19) C(20) 125(2) 1_555 1_555 1_555 yes S(4) C(19) H(7) 105(2) 1_555 1_555 1_555 no S(4) C(19) H(8) 106(2) 1_555 1_555 1_555 no C(20) C(19) H(7) 103(3) 1_555 1_555 1_555 no C(20) C(19) H(8) 106(3) 1_555 1_555 1_555 no H(7) C(19) H(8) 108(2) 1_555 1_555 1_555 no S(5) C(20) C(19) 124(2) 1_555 1_555 1_555 yes S(5) C(20) H(9) 105(2) 1_555 1_555 1_555 no S(5) C(20) H(10) 105(2) 1_555 1_555 1_555 no C(19) C(20) H(9) 106(4) 1_555 1_555 1_555 no C(19) C(20) H(10) 107(2) 1_555 1_555 1_555 no H(9) C(20) H(10) 106(2) 1_555 1_555 1_555 no S(6) C(21) S(8) 114.0(10) 1_555 1_555 1_555 yes S(6) C(21) C(22) 116(1) 1_555 1_555 1_555 yes S(8) C(21) C(22) 129(1) 1_555 1_555 1_555 yes S(7) C(22) S(9) 115(1) 1_555 1_555 1_555 yes S(7) C(22) C(21) 116(1) 1_555 1_555 1_555 yes S(9) C(22) C(21) 128(1) 1_555 1_555 1_555 yes S(8) C(23) C(24) 108(1) 1_555 1_555 1_555 yes S(8) C(23) H(11) 109(1) 1_555 1_555 1_555 no S(8) C(23) H(12) 109(1) 1_555 1_555 1_555 no C(24) C(23) H(11) 109(2) 1_555 1_555 1_555 no C(24) C(23) H(12) 110(2) 1_555 1_555 1_555 no H(11) C(23) H(12) 108(1) 1_555 1_555 1_555 no S(9) C(24) C(23) 113(1) 1_555 1_555 1_555 yes S(9) C(24) H(13) 110(1) 1_555 1_555 1_555 no S(9) C(24) H(14) 110(2) 1_555 1_555 1_555 no C(23) C(24) H(13) 105(2) 1_555 1_555 1_555 no C(23) C(24) H(14) 106(2) 1_555 1_555 1_555 no H(13) C(24) H(14) 109(2) 1_555 1_555 1_555 no O(1) C(25) C(26) 133(3) 1_555 1_555 3_655 yes O(1) C(25) H(17) 104(3) 1_555 1_555 1_555 no O(1) C(25) H(18) 103(4) 1_555 1_555 1_555 no C(26) C(25) H(17) 101(3) 3_655 1_555 1_555 no C(26) C(25) H(18) 104(3) 3_655 1_555 1_555 no H(17) C(25) H(18) 107(2) 1_555 1_555 1_555 no O(1) C(26) C(25) 124(2) 1_555 1_555 3_655 yes O(1) C(26) H(15) 104(3) 1_555 1_555 1_555 no O(1) C(26) H(16) 107(2) 1_555 1_555 1_555 no C(25) C(26) H(15) 107(2) 3_655 1_555 1_555 no C(25) C(26) H(16) 106(3) 3_655 1_555 1_555 no H(15) C(26) H(16) 103(2) 1_555 1_555 1_555 no F(1) B(1) F(1) 180.0 1_555 1_555 3_656 yes F(1) B(1) F(2) 93.68(1) 1_555 1_555 1_555 yes F(1) B(1) F(2) 86.32(1) 1_555 1_555 3_656 yes F(1) B(1) F(3) 121.95(2) 1_555 1_555 1_555 yes F(1) B(1) F(3) 58.05(2) 1_555 1_555 3_656 yes F(1) B(1) F(4) 110.304(7) 1_555 1_555 1_555 yes F(1) B(1) F(4) 69.696(7) 1_555 1_555 3_656 yes F(1) B(1) F(2) 86.32(1) 3_656 1_555 1_555 yes F(1) B(1) F(2) 93.68(1) 3_656 1_555 3_656 yes F(1) B(1) F(3) 58.05(2) 3_656 1_555 1_555 yes F(1) B(1) F(3) 121.95(2) 3_656 1_555 3_656 yes F(1) B(1) F(4) 69.696(7) 3_656 1_555 1_555 yes F(1) B(1) F(4) 110.304(7) 3_656 1_555 3_656 yes F(2) B(1) F(2) 180.0 1_555 1_555 3_656 yes F(2) B(1) F(3) 108.85(1) 1_555 1_555 1_555 yes F(2) B(1) F(3) 71.15(1) 1_555 1_555 3_656 yes F(2) B(1) F(4) 110.304(1) 1_555 1_555 1_555 yes F(2) B(1) F(4) 69.696(1) 1_555 1_555 3_656 yes F(2) B(1) F(3) 71.15(1) 3_656 1_555 1_555 yes F(2) B(1) F(3) 108.85(1) 3_656 1_555 3_656 yes F(2) B(1) F(4) 69.696(1) 3_656 1_555 1_555 yes F(2) B(1) F(4) 110.304(1) 3_656 1_555 3_656 yes F(3) B(1) F(3) 180.0 1_555 1_555 3_656 yes F(3) B(1) F(4) 110.304(5) 1_555 1_555 1_555 yes F(3) B(1) F(4) 69.696(5) 1_555 1_555 3_656 yes F(3) B(1) F(4) 69.696(5) 3_656 1_555 1_555 yes F(3) B(1) F(4) 110.304(5) 3_656 1_555 3_656 yes F(4) B(1) F(4) 180.0 1_555 1_555 3_656 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 S(1) F(3) 3.427(5) 1_555 1_555 ? S(3) O(1) 3.44(4) 1_555 4_455 ? S(3) C(14) 3.53(1) 1_555 2_555 ? S(3) C(15) 3.55(1) 1_555 2_555 ? S(5) O(1) 3.18(4) 1_555 4_455 ? S(5) F(2) 3.417(4) 1_555 2_556 ? S(5) C(22) 3.47(2) 1_555 2_555 ? S(6) O(1) 3.59(3) 1_555 3_655 ? S(7) C(3) 3.46(1) 1_555 2_555 ? S(9) C(18) 3.58(2) 1_555 2_555 ? F(1) C(9) 3.15(3) 1_555 4_556 ? F(1) C(20) 3.16(3) 1_555 4_555 ? F(1) C(19) 3.40(3) 1_555 4_555 ? F(1) C(8) 3.47(2) 1_555 4_556 ? F(2) C(20) 3.44(4) 1_555 2_546 ? F(2) C(23) 3.47(2) 1_555 1_546 ? F(3) C(20) 3.53(3) 1_555 2_546 ? F(3) C(23) 3.59(2) 1_555 3_665 ? F(4) C(24) 3.43(2) 1_555 1_546 ? F(4) C(8) 3.47(2) 1_555 2_545 ? F(4) C(9) 3.50(2) 1_555 2_545 ? O(1) C(23) 3.42(4) 1_555 3_665 ? N(1) C(19) 3.60(3) 1_555 2_546 ? C(3) C(12) 3.42(2) 1_555 2_555 ? C(5) C(14) 3.55(2) 1_555 2_545 ? C(5) C(15) 3.57(2) 1_555 2_545 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(DHF),87K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:14:28 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1452.91 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H34 F6 N4 O P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.640(2) _cell_length_b 7.834(2) _cell_length_c 13.265(1) _cell_angle_alpha 90 _cell_angle_beta 104.225(7) _cell_angle_gamma 89 _cell_volume 2784.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 87.0 _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 a ' _symmetry_Int_Tables_number 7 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x, -y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.733 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1478.00 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 87.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4886 _reflns_number_total 4886 _reflns_number_observed 4294 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.068 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 68 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 -0.1982(6) -0.0954(4) -0.252(1) 0.0178(7) Uani d . 1.00 . S2 -0.0669(6) 0.0640(4) -0.341(1) 0.0151(7) Uani d . 1.00 . S3 0.0225(6) 0.1519(3) -0.180(1) 0.0149(7) Uani d . 1.00 . S4 -0.0353(6) 0.2144(4) -0.517(1) 0.0208(7) Uani d . 1.00 . S5 0.0758(6) 0.3154(3) -0.323(1) 0.0148(7) Uani d . 1.00 . S6 -0.2175(6) 0.1090(3) 0.032(1) 0.0181(7) Uani d . 1.00 . S7 -0.1305(6) 0.1768(3) 0.205(1) 0.0142(7) Uani d . 1.00 . S8 -0.2908(6) 0.2763(4) 0.128(1) 0.0192(7) Uani d . 1.00 . S9 -0.1862(6) 0.3453(3) 0.341(1) 0.0176(7) Uani d . 1.00 . S10 0.5781(6) 0.6104(4) 0.217(1) 0.0192(7) Uani d . 1.00 . S11 0.4480(6) 0.4353(3) 0.304(1) 0.0149(7) Uani d . 1.00 . S12 0.3571(6) 0.3467(3) 0.147(1) 0.0160(7) Uani d . 1.00 . S13 0.4159(6) 0.2865(4) 0.481(1) 0.0216(7) Uani d . 1.00 . S14 0.3050(6) 0.1776(4) 0.290(1) 0.0222(8) Uani d . 1.00 . S15 0.5976(6) 0.3995(3) -0.070(1) 0.0127(6) Uani d . 1.00 . S16 0.5108(6) 0.3332(3) -0.241(1) 0.0141(7) Uani d . 1.00 . S17 0.6713(6) 0.2318(4) -0.164(1) 0.0201(7) Uani d . 1.00 . S18 0.5659(6) 0.1578(3) -0.376(1) 0.0159(7) Uani d . 1.00 . P1 0.1907(6) 0.2420(5) 0.481(1) 0.0200(4) Uani d . 1.00 . F1 0.1326(6) 0.190(1) 0.443(1) 0.039(2) Uani d . 1.00 . F2 0.1947(7) 0.2434(10) 0.362(1) 0.041(2) Uani d . 1.00 . F3 0.1860(6) 0.2449(9) 0.599(1) 0.034(2) Uani d . 1.00 . F4 0.2479(6) 0.302(1) 0.519(1) 0.030(2) Uani d . 1.00 . F5 0.2057(6) 0.0473(9) 0.496(1) 0.050(2) Uani d . 1.00 . F6 0.1723(6) 0.4437(8) 0.474(1) 0.034(2) Uani d . 1.00 . O1 0.2378(6) 0.3048(7) 0.072(1) 0.029(1) Uani d . 1.00 . N1 -0.1417(7) -0.073(1) -0.258(1) 0.023(2) Uani d . 1.00 . N2 -0.1909(7) -0.048(1) -0.131(1) 0.017(2) Uani d . 1.00 . N3 0.5183(7) 0.578(1) 0.221(1) 0.013(2) Uani d . 1.00 . N4 0.5735(7) 0.569(1) 0.091(1) 0.012(2) Uani d . 1.00 . C1 -0.1138(7) -0.031(1) -0.166(1) 0.012(2) Uani d . 1.00 . C2 -0.0614(7) 0.016(1) -0.130(2) 0.016(2) Uani d . 1.00 . C3 -0.0367(7) 0.058(1) -0.209(1) 0.011(2) Uani d . 1.00 . C4 -0.0387(7) -0.004(1) -0.022(2) 0.022(2) Uani d . 1.00 . C5 0.0111(7) -0.037(1) 0.016(2) 0.017(2) Uani d . 1.00 . C6 0.0366(7) -0.067(1) 0.123(2) 0.015(2) Uani d . 1.00 . C7 0.0916(7) -0.099(2) 0.160(2) 0.033(3) Uani d . 1.00 . C8 0.1077(7) -0.133(2) 0.262(2) 0.031(2) Uani d . 1.00 . C9 0.0786(7) -0.140(2) 0.331(2) 0.029(3) Uani d . 1.00 . C10 0.0301(7) -0.095(1) 0.302(2) 0.025(2) Uani d . 1.00 . C11 0.0079(7) -0.060(1) 0.195(2) 0.018(2) Uani d . 1.00 . C12 -0.0458(7) -0.027(1) 0.159(2) 0.019(2) Uani d . 1.00 . C13 -0.0687(7) 0.001(1) 0.057(2) 0.013(2) Uani d . 1.00 . C14 -0.1230(7) 0.022(1) 0.022(1) 0.016(2) Uani d . 1.00 . C15 -0.1524(7) 0.085(1) 0.082(1) 0.016(2) Uani d . 1.00 . C16 -0.1440(7) -0.023(1) -0.086(2) 0.011(2) Uani d . 1.00 . C17 -0.0217(7) 0.178(1) -0.380(2) 0.014(2) Uani d . 1.00 . C18 0.0204(7) 0.219(1) -0.308(1) 0.017(2) Uani d . 1.00 . C19 0.0269(7) 0.251(1) -0.533(2) 0.019(3) Uani d . 1.00 . C20 0.0561(7) 0.388(1) -0.458(2) 0.020(2) Uani d . 1.00 . C21 -0.2296(7) 0.220(1) 0.142(1) 0.017(2) Uani d . 1.00 . C22 -0.1861(7) 0.252(1) 0.221(2) 0.017(2) Uani d . 1.00 . C23 -0.2843(7) 0.420(1) 0.236(2) 0.022(3) Uani d . 1.00 . C24 -0.2536(7) 0.348(2) 0.344(2) 0.025(3) Uani d . 1.00 . C25 0.4939(7) 0.535(1) 0.122(1) 0.014(2) Uani d . 1.00 . C26 0.4413(7) 0.492(1) 0.099(2) 0.012(2) Uani d . 1.00 . C27 0.4178(7) 0.427(1) 0.170(1) 0.013(2) Uani d . 1.00 . C28 0.4171(7) 0.505(1) -0.017(1) 0.005(2) Uani d . 1.00 . C29 0.3654(7) 0.532(1) -0.052(2) 0.014(2) Uani d . 1.00 . C30 0.3437(7) 0.553(1) -0.157(2) 0.020(2) Uani d . 1.00 . C31 0.2929(7) 0.585(1) -0.190(2) 0.025(2) Uani d . 1.00 . C32 0.2660(8) 0.619(2) -0.298(2) 0.039(3) Uani d . 1.00 . C33 0.2989(8) 0.622(2) -0.370(2) 0.031(3) Uani d . 1.00 . C34 0.3502(7) 0.600(1) -0.338(2) 0.019(2) Uani d . 1.00 . C35 0.3739(7) 0.556(1) -0.231(1) 0.015(2) Uani d . 1.00 . C36 0.4238(7) 0.531(1) -0.194(1) 0.009(2) Uani d . 1.00 . C37 0.4467(7) 0.501(1) -0.088(1) 0.009(2) Uani d . 1.00 . C38 0.5017(7) 0.478(1) -0.054(2) 0.009(2) Uani d . 1.00 . C39 0.5332(7) 0.410(1) -0.114(1) 0.011(2) Uani d . 1.00 . C40 0.5234(7) 0.528(1) 0.054(2) 0.015(2) Uani d . 1.00 . C41 0.4012(7) 0.322(1) 0.349(2) 0.019(2) Uani d . 1.00 . C42 0.3598(7) 0.279(1) 0.275(2) 0.017(2) Uani d . 1.00 . C43 0.3539(7) 0.239(1) 0.496(1) 0.016(2) Uani d . 1.00 . C44 0.3287(7) 0.101(1) 0.423(2) 0.017(2) Uani d . 1.00 . C45 0.6071(7) 0.282(1) -0.173(1) 0.014(2) Uani d . 1.00 . C46 0.5699(7) 0.254(1) -0.254(2) 0.015(2) Uani d . 1.00 . C47 0.6645(7) 0.082(1) -0.273(2) 0.017(3) Uani d . 1.00 . C48 0.6310(7) 0.154(1) -0.370(2) 0.014(2) Uani d . 1.00 . C49 0.1860(7) 0.204(2) 0.065(2) 0.033(3) Uani d . 1.00 . C50 0.1667(7) 0.212(1) -0.053(1) 0.032(2) Uani d . 1.00 . C51 0.1892(7) 0.283(2) -0.101(2) 0.026(2) Uani d . 1.00 . C52 0.2392(6) 0.368(1) -0.030(1) 0.025(2) Uani d . 1.00 . H1 0.0363 -0.0328 -0.0239 0.0046 Uiso calc . 1.00 . H2 0.1089 -0.1421 0.1195 0.0258 Uiso calc . 1.00 . H3 0.1488 -0.0954 0.2791 0.0054 Uiso calc . 1.00 . H4 0.0900 -0.1785 0.4098 0.0307 Uiso calc . 1.00 . H5 0.0138 -0.0807 0.3477 0.0041 Uiso calc . 1.00 . H6 -0.0638 -0.0244 0.2166 0.0191 Uiso calc . 1.00 . H7 0.0479 0.1524 -0.5277 0.0223 Uiso calc . 1.00 . H8 0.0258 0.2990 -0.6038 0.0223 Uiso calc . 1.00 . H9 0.0363 0.4841 -0.4565 0.0027 Uiso calc . 1.00 . H10 0.0865 0.4239 -0.4769 0.0027 Uiso calc . 1.00 . H11 -0.2687 0.5142 0.2264 0.0178 Uiso calc . 1.00 . H12 -0.3168 0.4335 0.2459 0.0178 Uiso calc . 1.00 . H13 -0.2646 0.2332 0.3574 0.0454 Uiso calc . 1.00 . H14 -0.2590 0.4189 0.3994 0.0454 Uiso calc . 1.00 . H15 0.3499 0.5421 0.0077 0.0142 Uiso calc . 1.00 . H16 0.2682 0.5581 -0.1412 0.0201 Uiso calc . 1.00 . H17 0.2408 0.7102 -0.3288 0.0356 Uiso calc . 1.00 . H18 0.2819 0.6245 -0.4374 0.0209 Uiso calc . 1.00 . H19 0.3745 0.6118 -0.3941 0.0246 Uiso calc . 1.00 . H20 0.4458 0.5379 -0.2372 -0.0002 Uiso calc . 1.00 . H21 0.3565 0.2201 0.5664 0.0047 Uiso calc . 1.00 . H22 0.3356 0.3440 0.4749 0.0047 Uiso calc . 1.00 . H23 0.3066 0.0495 0.4550 0.0306 Uiso calc . 1.00 . H24 0.3575 0.0130 0.4297 0.0306 Uiso calc . 1.00 . H25 0.6970 0.0405 -0.2803 0.0154 Uiso calc . 1.00 . H26 0.6493 -0.0281 -0.2521 0.0154 Uiso calc . 1.00 . H27 0.6367 0.0882 -0.4293 -0.0023 Uiso calc . 1.00 . H28 0.6433 0.2663 -0.3766 -0.0023 Uiso calc . 1.00 . H29 0.1901 0.0826 0.0955 0.0486 Uiso calc . 1.00 . H30 0.1634 0.2533 0.1062 0.0486 Uiso calc . 1.00 . H31 0.2361 0.4949 -0.0318 0.0296 Uiso calc . 1.00 . H32 0.2686 0.3421 -0.0500 0.0296 Uiso calc . 1.00 . H33 0.1377 0.1611 -0.0870 0.0395 Uiso calc . 1.00 . H34 0.1824 0.2884 -0.1730 0.0107 Uiso calc . 1.00 . 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 S(1) 0.012(1) 0.031(2) 0.010(1) -0.003(1) 0.003(1) -0.004(1) S(2) 0.013(1) 0.020(1) 0.013(1) -0.002(1) 0.005(1) -0.001(1) S(3) 0.013(1) 0.016(1) 0.018(1) -0.004(1) 0.009(1) -0.005(1) S(4) 0.013(1) 0.032(2) 0.018(2) -0.001(1) 0.004(1) 0.001(1) S(5) 0.016(1) 0.011(1) 0.017(1) -0.0024(10) 0.004(1) -0.0024(10) S(6) 0.014(1) 0.017(1) 0.022(1) 0.0005(10) 0.003(1) -0.003(1) S(7) 0.012(1) 0.019(1) 0.012(1) -0.0003(9) 0.002(1) -0.0039(10) S(8) 0.013(1) 0.025(2) 0.020(1) -0.001(1) 0.005(1) -0.009(1) S(9) 0.020(1) 0.017(1) 0.014(1) 0.002(1) 0.000(1) -0.004(1) S(10) 0.016(1) 0.022(1) 0.019(1) -0.002(1) 0.004(1) -0.005(1) S(11) 0.016(1) 0.016(1) 0.013(1) -0.001(1) 0.004(1) 0.001(1) S(12) 0.016(1) 0.018(1) 0.014(1) -0.003(1) 0.004(1) -0.001(1) S(13) 0.025(1) 0.025(1) 0.016(1) -0.002(1) 0.009(1) 0.005(1) S(14) 0.022(1) 0.024(2) 0.024(2) -0.006(1) 0.012(1) -0.001(1) S(15) 0.010(1) 0.022(1) 0.007(1) -0.0019(9) 0.004(1) -0.0013(10) S(16) 0.016(1) 0.012(1) 0.014(1) 0.0001(10) 0.004(1) -0.0009(10) S(17) 0.015(1) 0.025(2) 0.020(1) 0.003(1) 0.004(1) -0.003(1) S(18) 0.016(1) 0.018(1) 0.016(1) -0.002(1) 0.007(1) -0.002(1) P(1) 0.0162(7) 0.0207(8) 0.0245(7) -0.0034(6) 0.0074(6) 0.0019(6) F(1) 0.016(2) 0.040(4) 0.064(5) -0.010(3) 0.015(3) -0.011(4) F(2) 0.045(4) 0.056(5) 0.021(2) -0.016(4) 0.007(3) -0.002(3) F(3) 0.034(3) 0.047(4) 0.030(2) 0.001(3) 0.025(3) 0.004(3) F(4) 0.014(2) 0.055(4) 0.021(4) -0.008(3) 0.004(3) 0.006(3) F(5) 0.033(4) 0.024(2) 0.097(6) 0.002(3) 0.026(4) 0.026(4) F(6) 0.046(4) 0.021(2) 0.041(4) 0.005(3) 0.023(4) -0.001(3) O(1) 0.021(3) 0.042(3) 0.022(2) -0.004(2) 0.004(2) -0.003(2) N(1) 0.009(3) 0.026(5) 0.028(5) -0.004(4) -0.004(3) -0.002(4) N(2) 0.017(3) 0.024(4) 0.014(3) -0.016(3) 0.011(3) -0.010(3) N(3) 0.018(3) 0.017(4) 0.006(4) 0.000(3) 0.007(3) -0.002(3) N(4) 0.012(3) 0.009(4) 0.016(2) 0.001(3) 0.004(3) 0.007(3) C(1) 0.008(3) 0.018(6) 0.017(4) 0.008(4) 0.018(3) -0.005(4) C(2) 0.009(3) 0.022(5) 0.025(4) -0.007(4) 0.018(3) -0.008(4) C(3) 0.013(3) 0.011(5) 0.014(2) -0.004(3) 0.009(2) -0.004(3) C(4) 0.027(4) 0.015(6) 0.024(4) -0.003(5) 0.007(4) -0.002(5) C(5) 0.026(4) 0.015(5) 0.013(4) -0.004(4) 0.009(4) -0.009(4) C(6) 0.014(4) 0.009(4) 0.017(4) 0.010(4) -0.004(3) -0.007(4) C(7) 0.013(4) 0.049(8) 0.035(5) 0.024(5) 0.002(5) -0.005(5) C(8) 0.001(3) 0.043(6) 0.035(4) 0.027(4) -0.020(3) -0.013(5) C(9) 0.027(5) 0.024(6) 0.029(7) 0.019(5) -0.004(4) -0.002(5) C(10) 0.021(4) 0.018(6) 0.030(5) 0.000(4) -0.002(5) 0.002(4) C(11) 0.022(4) 0.008(5) 0.024(4) 0.006(4) 0.007(4) -0.013(4) C(12) 0.021(4) 0.009(5) 0.028(4) 0.003(4) 0.007(4) 0.000(4) C(13) 0.013(4) 0.002(4) 0.025(4) 0.002(3) 0.005(3) -0.010(4) C(14) 0.013(4) 0.019(6) 0.014(4) 0.006(4) 0.000(3) 0.005(4) C(15) 0.014(2) 0.022(5) 0.010(3) -0.004(4) 0.000(3) 0.000(3) C(16) 0.013(3) 0.013(5) 0.013(4) -0.001(4) 0.018(3) -0.002(4) C(17) 0.025(5) 0.001(5) 0.017(2) -0.003(3) 0.009(3) 0.001(3) C(18) 0.019(4) 0.014(5) 0.022(3) -0.002(3) 0.015(4) -0.006(3) C(19) 0.016(4) 0.028(6) 0.018(6) 0.006(4) 0.009(4) 0.002(4) C(20) 0.023(5) 0.015(4) 0.022(3) 0.013(3) 0.007(4) 0.012(3) C(21) 0.012(2) 0.022(6) 0.016(4) -0.002(4) -0.002(3) 0.000(3) C(22) 0.011(3) 0.011(5) 0.025(4) -0.008(3) -0.002(3) -0.011(3) C(23) 0.035(6) 0.014(6) 0.018(4) 0.004(4) 0.007(5) 0.001(3) C(24) 0.021(3) 0.030(7) 0.022(5) 0.014(5) 0.003(4) 0.002(5) C(25) 0.024(4) 0.005(5) 0.009(4) -0.005(4) -0.006(3) 0.006(3) C(26) 0.018(4) 0.007(4) 0.008(4) 0.008(3) -0.004(3) 0.001(4) C(27) 0.013(3) 0.006(4) 0.016(3) 0.009(3) -0.003(3) -0.004(3) C(28) -0.002(3) 0.004(4) 0.011(4) 0.001(3) -0.001(3) 0.001(4) C(29) -0.003(3) 0.019(5) 0.028(4) 0.002(3) 0.007(3) 0.009(4) C(30) 0.020(4) 0.019(5) 0.025(4) -0.008(4) 0.009(3) -0.002(4) C(31) 0.021(4) 0.028(6) 0.024(4) 0.001(4) 0.001(4) -0.019(4) C(32) 0.044(7) 0.056(8) 0.019(4) -0.005(6) 0.010(4) -0.017(5) C(33) 0.028(5) 0.045(7) 0.011(5) 0.001(5) -0.013(4) -0.014(5) C(34) 0.029(5) 0.023(6) 0.004(4) 0.006(5) 0.002(5) -0.012(4) C(35) 0.013(4) 0.011(5) 0.014(4) 0.000(4) -0.008(3) 0.006(4) C(36) 0.010(4) 0.015(5) 0.005(4) -0.005(4) 0.004(3) -0.003(4) C(37) 0.011(4) 0.014(5) 0.006(3) -0.001(3) 0.010(3) 0.003(3) C(38) 0.010(4) 0.007(5) 0.015(4) -0.006(3) 0.010(3) 0.003(4) C(39) 0.012(2) 0.009(5) 0.013(3) -0.002(4) 0.007(3) 0.004(4) C(40) 0.013(3) 0.007(5) 0.020(4) 0.001(4) -0.005(3) 0.001(4) C(41) 0.015(4) 0.029(7) 0.016(3) 0.004(3) 0.008(3) 0.005(4) C(42) 0.018(4) 0.014(5) 0.021(3) 0.001(4) 0.007(3) 0.005(4) C(43) 0.024(4) 0.011(5) 0.016(5) -0.003(4) 0.009(5) 0.004(3) C(44) 0.021(5) 0.012(5) 0.023(3) -0.009(3) 0.018(4) -0.002(3) C(45) 0.016(2) 0.019(5) 0.012(4) 0.000(4) 0.017(3) 0.002(3) C(46) 0.025(3) 0.014(5) 0.012(3) 0.011(4) 0.015(3) 0.010(3) C(47) 0.007(5) 0.025(6) 0.022(4) 0.004(4) 0.009(4) 0.000(3) C(48) 0.019(3) 0.022(5) 0.007(4) -0.007(4) 0.016(4) -0.007(3) C(49) 0.023(5) 0.034(7) 0.044(4) -0.005(4) 0.013(5) -0.012(6) C(50) 0.019(4) 0.029(5) 0.046(4) -0.002(3) 0.007(4) 0.001(4) C(51) 0.028(5) 0.026(6) 0.019(4) 0.007(4) -0.004(3) -0.006(4) C(52) 0.021(4) 0.035(5) 0.020(3) 0.002(3) 0.006(3) -0.005(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0157(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4294 _refine_ls_number_parameters 740 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0767 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.152 _refine_ls_shift/esd_max 4.7730 _refine_ls_shift/esd_mean 0.5500 _refine_diff_density_min -0.71 _refine_diff_density_max 0.81 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.59(1) 1_555 1_555 yes S(1) N(2) 1.62(1) 1_555 1_555 yes S(2) C(3) 1.75(1) 1_555 1_555 yes S(2) C(17) 1.71(1) 1_555 1_555 yes S(3) C(3) 1.75(1) 1_555 1_555 yes S(3) C(18) 1.76(2) 1_555 1_555 yes S(4) C(17) 1.79(2) 1_555 1_555 yes S(4) C(19) 1.81(2) 1_555 1_555 yes S(5) C(18) 1.76(1) 1_555 1_555 yes S(5) C(20) 1.83(1) 1_555 1_555 yes S(6) C(15) 1.77(1) 1_555 1_555 yes S(6) C(21) 1.79(2) 1_555 1_555 yes S(7) C(15) 1.76(2) 1_555 1_555 yes S(7) C(22) 1.71(1) 1_555 1_555 yes S(8) C(21) 1.71(1) 1_555 1_555 yes S(8) C(23) 1.80(2) 1_555 1_555 yes S(9) C(22) 1.75(2) 1_555 1_555 yes S(9) C(24) 1.87(2) 1_555 1_555 yes S(10) N(3) 1.69(1) 1_555 1_555 yes S(10) N(4) 1.67(1) 1_555 1_555 yes S(11) C(27) 1.77(1) 1_555 1_555 yes S(11) C(41) 1.79(1) 1_555 1_555 yes S(12) C(27) 1.75(2) 1_555 1_555 yes S(12) C(42) 1.76(2) 1_555 1_555 yes S(13) C(41) 1.73(2) 1_555 1_555 yes S(13) C(43) 1.81(1) 1_555 1_555 yes S(14) C(42) 1.77(1) 1_555 1_555 yes S(14) C(44) 1.82(2) 1_555 1_555 yes S(15) C(39) 1.73(2) 1_555 1_555 yes S(15) C(45) 1.73(1) 1_555 1_555 yes S(16) C(39) 1.75(2) 1_555 1_555 yes S(16) C(46) 1.79(1) 1_555 1_555 yes S(17) C(45) 1.79(1) 1_555 1_555 yes S(17) C(47) 1.84(2) 1_555 1_555 yes S(18) C(46) 1.76(2) 1_555 1_555 yes S(18) C(48) 1.78(1) 1_555 1_555 yes P(1) F(1) 1.61(1) 1_555 1_555 yes P(1) F(2) 1.61(1) 1_555 1_555 yes P(1) F(3) 1.60(1) 1_555 1_555 yes P(1) F(4) 1.607(10) 1_555 1_555 yes P(1) F(5) 1.58(1) 1_555 1_555 yes P(1) F(6) 1.66(1) 1_555 1_555 yes O(1) C(49) 1.62(2) 1_555 1_555 yes O(1) C(52) 1.45(1) 1_555 1_555 yes N(1) C(1) 1.31(2) 1_555 1_555 yes N(2) C(16) 1.30(2) 1_555 1_555 yes N(3) C(25) 1.36(2) 1_555 1_555 yes N(4) C(40) 1.39(2) 1_555 1_555 yes C(1) C(2) 1.46(2) 1_555 1_555 yes C(1) C(16) 1.51(2) 1_555 1_555 yes C(2) C(3) 1.42(2) 1_555 1_555 yes C(2) C(4) 1.43(2) 1_555 1_555 yes C(4) C(5) 1.37(2) 1_555 1_555 yes C(4) C(13) 1.49(2) 1_555 1_555 yes C(5) C(6) 1.44(2) 1_555 1_555 yes C(6) C(7) 1.50(2) 1_555 1_555 yes C(6) C(11) 1.39(2) 1_555 1_555 yes C(7) C(8) 1.34(3) 1_555 1_555 yes C(8) C(9) 1.37(3) 1_555 1_555 yes C(9) C(10) 1.35(2) 1_555 1_555 yes C(10) C(11) 1.43(2) 1_555 1_555 yes C(11) C(12) 1.47(2) 1_555 1_555 yes C(12) C(13) 1.37(2) 1_555 1_555 yes C(13) C(14) 1.47(2) 1_555 1_555 yes C(14) C(15) 1.36(2) 1_555 1_555 yes C(14) C(16) 1.44(2) 1_555 1_555 yes C(17) C(18) 1.35(2) 1_555 1_555 yes C(19) C(20) 1.55(2) 1_555 1_555 yes C(21) C(22) 1.41(2) 1_555 1_555 yes C(23) C(24) 1.58(2) 1_555 1_555 yes C(25) C(26) 1.45(2) 1_555 1_555 yes C(25) C(40) 1.36(2) 1_555 1_555 yes C(26) C(27) 1.37(2) 1_555 1_555 yes C(26) C(28) 1.52(2) 1_555 1_555 yes C(28) C(29) 1.41(2) 1_555 1_555 yes C(28) C(37) 1.40(2) 1_555 1_555 yes C(29) C(30) 1.39(2) 1_555 1_555 yes C(30) C(31) 1.39(2) 1_555 1_555 yes C(30) C(35) 1.43(2) 1_555 1_555 yes C(31) C(32) 1.46(3) 1_555 1_555 yes C(32) C(33) 1.48(3) 1_555 1_555 yes C(33) C(34) 1.39(2) 1_555 1_555 yes C(34) C(35) 1.46(2) 1_555 1_555 yes C(35) C(36) 1.36(2) 1_555 1_555 yes C(36) C(37) 1.41(2) 1_555 1_555 yes C(37) C(38) 1.49(2) 1_555 1_555 yes C(38) C(39) 1.42(2) 1_555 1_555 yes C(38) C(40) 1.46(2) 1_555 1_555 yes C(41) C(42) 1.35(2) 1_555 1_555 yes C(43) C(44) 1.50(2) 1_555 1_555 yes C(45) C(46) 1.31(2) 1_555 1_555 yes C(47) C(48) 1.50(2) 1_555 1_555 yes C(49) C(50) 1.52(2) 1_555 1_555 yes C(50) C(51) 1.14(2) 1_555 1_555 yes C(51) C(52) 1.61(2) 1_555 1_555 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 N(1) S(1) N(2) 98.1(7) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.2(7) 1_555 1_555 1_555 yes C(3) S(3) C(18) 96.2(7) 1_555 1_555 1_555 yes C(17) S(4) C(19) 100.2(8) 1_555 1_555 1_555 yes C(18) S(5) C(20) 100.6(7) 1_555 1_555 1_555 yes C(15) S(6) C(21) 97.3(7) 1_555 1_555 1_555 yes C(15) S(7) C(22) 98.2(7) 1_555 1_555 1_555 yes C(21) S(8) C(23) 100.0(7) 1_555 1_555 1_555 yes C(22) S(9) C(24) 104.2(7) 1_555 1_555 1_555 yes N(3) S(10) N(4) 99.8(6) 1_555 1_555 1_555 yes C(27) S(11) C(41) 96.6(7) 1_555 1_555 1_555 yes C(27) S(12) C(42) 97.3(7) 1_555 1_555 1_555 yes C(41) S(13) C(43) 98.6(7) 1_555 1_555 1_555 yes C(42) S(14) C(44) 98.3(7) 1_555 1_555 1_555 yes C(39) S(15) C(45) 95.7(8) 1_555 1_555 1_555 yes C(39) S(16) C(46) 95.4(7) 1_555 1_555 1_555 yes C(45) S(17) C(47) 100.1(7) 1_555 1_555 1_555 yes C(46) S(18) C(48) 97.4(7) 1_555 1_555 1_555 yes F(1) P(1) F(2) 90.1(6) 1_555 1_555 1_555 yes F(1) P(1) F(3) 89.6(7) 1_555 1_555 1_555 yes F(1) P(1) F(4) 177.5(9) 1_555 1_555 1_555 yes F(1) P(1) F(5) 90.3(7) 1_555 1_555 1_555 yes F(1) P(1) F(6) 87.4(6) 1_555 1_555 1_555 yes F(2) P(1) F(3) 178.6(9) 1_555 1_555 1_555 yes F(2) P(1) F(4) 90.3(6) 1_555 1_555 1_555 yes F(2) P(1) F(5) 92.8(7) 1_555 1_555 1_555 yes F(2) P(1) F(6) 92.0(6) 1_555 1_555 1_555 yes F(3) P(1) F(4) 90.0(6) 1_555 1_555 1_555 yes F(3) P(1) F(5) 88.5(7) 1_555 1_555 1_555 yes F(3) P(1) F(6) 86.7(6) 1_555 1_555 1_555 yes F(4) P(1) F(5) 92.1(7) 1_555 1_555 1_555 yes F(4) P(1) F(6) 90.1(6) 1_555 1_555 1_555 yes F(5) P(1) F(6) 174.7(8) 1_555 1_555 1_555 yes C(49) O(1) C(52) 109.7(10) 1_555 1_555 1_555 yes S(1) N(1) C(1) 109(1) 1_555 1_555 1_555 yes S(1) N(2) C(16) 111.1(10) 1_555 1_555 1_555 yes S(10) N(3) C(25) 105.1(10) 1_555 1_555 1_555 yes S(10) N(4) C(40) 102(1) 1_555 1_555 1_555 yes N(1) C(1) C(2) 132(1) 1_555 1_555 1_555 yes N(1) C(1) C(16) 111(1) 1_555 1_555 1_555 yes C(2) C(1) C(16) 115(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 115(1) 1_555 1_555 1_555 yes C(1) C(2) C(4) 117(1) 1_555 1_555 1_555 yes C(3) C(2) C(4) 126(1) 1_555 1_555 1_555 yes S(2) C(3) S(3) 113.6(7) 1_555 1_555 1_555 yes S(2) C(3) C(2) 123(1) 1_555 1_555 1_555 yes S(3) C(3) C(2) 121(1) 1_555 1_555 1_555 yes C(2) C(4) C(5) 122(1) 1_555 1_555 1_555 yes C(2) C(4) C(13) 121(1) 1_555 1_555 1_555 yes C(5) C(4) C(13) 115(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 126(1) 1_555 1_555 1_555 yes C(4) C(5) H(1) 125(2) 1_555 1_555 1_555 no C(6) C(5) H(1) 107(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 124(1) 1_555 1_555 1_555 yes C(5) C(6) C(11) 116(1) 1_555 1_555 1_555 yes C(7) C(6) C(11) 118(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 115(1) 1_555 1_555 1_555 yes C(6) C(7) H(2) 121(2) 1_555 1_555 1_555 no C(8) C(7) H(2) 116(2) 1_555 1_555 1_555 no C(7) C(8) C(9) 125(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 102(2) 1_555 1_555 1_555 no C(9) C(8) H(3) 126(2) 1_555 1_555 1_555 no C(8) C(9) C(10) 120(1) 1_555 1_555 1_555 yes C(8) C(9) H(4) 126(2) 1_555 1_555 1_555 no C(10) C(9) H(4) 113(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 119(1) 1_555 1_555 1_555 yes C(9) C(10) H(5) 120(2) 1_555 1_555 1_555 no C(11) C(10) H(5) 120(2) 1_555 1_555 1_555 no C(6) C(11) C(10) 120(1) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 120(1) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122(1) 1_555 1_555 1_555 yes C(11) C(12) H(6) 113(2) 1_555 1_555 1_555 no C(13) C(12) H(6) 123(1) 1_555 1_555 1_555 no C(4) C(13) C(12) 119(1) 1_555 1_555 1_555 yes C(4) C(13) C(14) 118(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 124(1) 1_555 1_555 1_555 yes C(13) C(14) C(16) 114(1) 1_555 1_555 1_555 yes C(15) C(14) C(16) 120(1) 1_555 1_555 1_555 yes S(6) C(15) S(7) 112.8(9) 1_555 1_555 1_555 yes S(6) C(15) C(14) 121(1) 1_555 1_555 1_555 yes S(7) C(15) C(14) 125(1) 1_555 1_555 1_555 yes N(2) C(16) C(1) 109(1) 1_555 1_555 1_555 yes N(2) C(16) C(14) 127(1) 1_555 1_555 1_555 yes C(1) C(16) C(14) 123(1) 1_555 1_555 1_555 yes S(2) C(17) S(4) 113.6(9) 1_555 1_555 1_555 yes S(2) C(17) C(18) 118(1) 1_555 1_555 1_555 yes S(4) C(17) C(18) 127(1) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.3(8) 1_555 1_555 1_555 yes S(3) C(18) C(17) 115(1) 1_555 1_555 1_555 yes S(5) C(18) C(17) 130(1) 1_555 1_555 1_555 yes S(4) C(19) C(20) 113(1) 1_555 1_555 1_555 yes S(4) C(19) H(7) 115(1) 1_555 1_555 1_555 no S(4) C(19) H(8) 111(1) 1_555 1_555 1_555 no C(20) C(19) H(7) 107(1) 1_555 1_555 1_555 no C(20) C(19) H(8) 103(1) 1_555 1_555 1_555 no H(7) C(19) H(8) 104(2) 1_555 1_555 1_555 no S(5) C(20) C(19) 113.5(10) 1_555 1_555 1_555 yes S(5) C(20) H(9) 105(1) 1_555 1_555 1_555 no S(5) C(20) H(10) 106(1) 1_555 1_555 1_555 no C(19) C(20) H(9) 110(1) 1_555 1_555 1_555 no C(19) C(20) H(10) 112(1) 1_555 1_555 1_555 no H(9) C(20) H(10) 108(1) 1_555 1_555 1_555 no S(6) C(21) S(8) 114.4(8) 1_555 1_555 1_555 yes S(6) C(21) C(22) 113(1) 1_555 1_555 1_555 yes S(8) C(21) C(22) 132(1) 1_555 1_555 1_555 yes S(7) C(22) S(9) 117.4(8) 1_555 1_555 1_555 yes S(7) C(22) C(21) 118(1) 1_555 1_555 1_555 yes S(9) C(22) C(21) 124(1) 1_555 1_555 1_555 yes S(8) C(23) C(24) 115(1) 1_555 1_555 1_555 yes S(8) C(23) H(11) 111(2) 1_555 1_555 1_555 no S(8) C(23) H(12) 105(1) 1_555 1_555 1_555 no C(24) C(23) H(11) 104(2) 1_555 1_555 1_555 no C(24) C(23) H(12) 103(2) 1_555 1_555 1_555 no H(11) C(23) H(12) 116(2) 1_555 1_555 1_555 no S(9) C(24) C(23) 107(1) 1_555 1_555 1_555 yes S(9) C(24) H(13) 110(1) 1_555 1_555 1_555 no S(9) C(24) H(14) 111(1) 1_555 1_555 1_555 no C(23) C(24) H(13) 111(2) 1_555 1_555 1_555 no C(23) C(24) H(14) 109(1) 1_555 1_555 1_555 no H(13) C(24) H(14) 106(2) 1_555 1_555 1_555 no N(3) C(25) C(26) 119(1) 1_555 1_555 1_555 yes N(3) C(25) C(40) 114(1) 1_555 1_555 1_555 yes C(26) C(25) C(40) 125(1) 1_555 1_555 1_555 yes C(25) C(26) C(27) 124(1) 1_555 1_555 1_555 yes C(25) C(26) C(28) 111(1) 1_555 1_555 1_555 yes C(27) C(26) C(28) 123(1) 1_555 1_555 1_555 yes S(11) C(27) S(12) 112.7(9) 1_555 1_555 1_555 yes S(11) C(27) C(26) 119(1) 1_555 1_555 1_555 yes S(12) C(27) C(26) 127(1) 1_555 1_555 1_555 yes C(26) C(28) C(29) 120(1) 1_555 1_555 1_555 yes C(26) C(28) C(37) 119(1) 1_555 1_555 1_555 yes C(29) C(28) C(37) 119(1) 1_555 1_555 1_555 yes C(28) C(29) C(30) 120(1) 1_555 1_555 1_555 yes C(28) C(29) H(15) 110(1) 1_555 1_555 1_555 no C(30) C(29) H(15) 129(1) 1_555 1_555 1_555 no C(29) C(30) C(31) 119(1) 1_555 1_555 1_555 yes C(29) C(30) C(35) 120(1) 1_555 1_555 1_555 yes C(31) C(30) C(35) 119(1) 1_555 1_555 1_555 yes C(30) C(31) C(32) 125(1) 1_555 1_555 1_555 yes C(30) C(31) H(16) 121(2) 1_555 1_555 1_555 no C(32) C(31) H(16) 112(1) 1_555 1_555 1_555 no C(31) C(32) C(33) 113(1) 1_555 1_555 1_555 yes C(31) C(32) H(17) 131(2) 1_555 1_555 1_555 no C(33) C(32) H(17) 101(2) 1_555 1_555 1_555 no C(32) C(33) C(34) 122(1) 1_555 1_555 1_555 yes C(32) C(33) H(18) 112(2) 1_555 1_555 1_555 no C(34) C(33) H(18) 123(2) 1_555 1_555 1_555 no C(33) C(34) C(35) 120(1) 1_555 1_555 1_555 yes C(33) C(34) H(19) 121(1) 1_555 1_555 1_555 no C(35) C(34) H(19) 117(1) 1_555 1_555 1_555 no C(30) C(35) C(34) 118(1) 1_555 1_555 1_555 yes C(30) C(35) C(36) 117(1) 1_555 1_555 1_555 yes C(34) C(35) C(36) 123(1) 1_555 1_555 1_555 yes C(35) C(36) C(37) 123(1) 1_555 1_555 1_555 yes C(35) C(36) H(20) 122(2) 1_555 1_555 1_555 no C(37) C(36) H(20) 114(1) 1_555 1_555 1_555 no C(28) C(37) C(36) 118(1) 1_555 1_555 1_555 yes C(28) C(37) C(38) 121(1) 1_555 1_555 1_555 yes C(36) C(37) C(38) 120(1) 1_555 1_555 1_555 yes C(37) C(38) C(39) 126(1) 1_555 1_555 1_555 yes C(37) C(38) C(40) 114(1) 1_555 1_555 1_555 yes C(39) C(38) C(40) 119(1) 1_555 1_555 1_555 yes S(15) C(39) S(16) 113.6(9) 1_555 1_555 1_555 yes S(15) C(39) C(38) 123(1) 1_555 1_555 1_555 yes S(16) C(39) C(38) 123(1) 1_555 1_555 1_555 yes N(4) C(40) C(25) 117(1) 1_555 1_555 1_555 yes N(4) C(40) C(38) 123(1) 1_555 1_555 1_555 yes C(25) C(40) C(38) 119(1) 1_555 1_555 1_555 yes S(11) C(41) S(13) 114.2(8) 1_555 1_555 1_555 yes S(11) C(41) C(42) 115(1) 1_555 1_555 1_555 yes S(13) C(41) C(42) 129(1) 1_555 1_555 1_555 yes S(12) C(42) S(14) 114.3(8) 1_555 1_555 1_555 yes S(12) C(42) C(41) 116(1) 1_555 1_555 1_555 yes S(14) C(42) C(41) 128(1) 1_555 1_555 1_555 yes S(13) C(43) C(44) 112(1) 1_555 1_555 1_555 yes S(13) C(43) H(21) 107(1) 1_555 1_555 1_555 no S(13) C(43) H(22) 103(1) 1_555 1_555 1_555 no C(44) C(43) H(21) 116(1) 1_555 1_555 1_555 no C(44) C(43) H(22) 107(1) 1_555 1_555 1_555 no H(21) C(43) H(22) 109(2) 1_555 1_555 1_555 no S(14) C(44) C(43) 112(1) 1_555 1_555 1_555 yes S(14) C(44) H(23) 117(1) 1_555 1_555 1_555 no S(14) C(44) H(24) 112(1) 1_555 1_555 1_555 no C(43) C(44) H(23) 105(1) 1_555 1_555 1_555 no C(43) C(44) H(24) 101(1) 1_555 1_555 1_555 no H(23) C(44) H(24) 104(1) 1_555 1_555 1_555 no S(15) C(45) S(17) 113.6(8) 1_555 1_555 1_555 yes S(15) C(45) C(46) 119(1) 1_555 1_555 1_555 yes S(17) C(45) C(46) 126(1) 1_555 1_555 1_555 yes S(16) C(46) S(18) 112.4(8) 1_555 1_555 1_555 yes S(16) C(46) C(45) 114(1) 1_555 1_555 1_555 yes S(18) C(46) C(45) 132(1) 1_555 1_555 1_555 yes S(17) C(47) C(48) 111(1) 1_555 1_555 1_555 yes S(17) C(47) H(25) 111(1) 1_555 1_555 1_555 no S(17) C(47) H(26) 107(1) 1_555 1_555 1_555 no C(48) C(47) H(25) 115(2) 1_555 1_555 1_555 no C(48) C(47) H(26) 109(1) 1_555 1_555 1_555 no H(25) C(47) H(26) 100(1) 1_555 1_555 1_555 no S(18) C(48) C(47) 116(1) 1_555 1_555 1_555 yes S(18) C(48) H(27) 109(1) 1_555 1_555 1_555 no S(18) C(48) H(28) 111(1) 1_555 1_555 1_555 no C(47) C(48) H(27) 107(1) 1_555 1_555 1_555 no C(47) C(48) H(28) 105(2) 1_555 1_555 1_555 no H(27) C(48) H(28) 105(2) 1_555 1_555 1_555 no O(1) C(49) C(50) 97(1) 1_555 1_555 1_555 yes O(1) C(49) H(29) 114(2) 1_555 1_555 1_555 no O(1) C(49) H(30) 115(1) 1_555 1_555 1_555 no C(50) C(49) H(29) 115(2) 1_555 1_555 1_555 no C(50) C(49) H(30) 115(2) 1_555 1_555 1_555 no H(29) C(49) H(30) 99(2) 1_555 1_555 1_555 no C(49) C(50) C(51) 119(1) 1_555 1_555 1_555 yes C(49) C(50) H(33) 122(1) 1_555 1_555 1_555 no C(51) C(50) H(33) 118(2) 1_555 1_555 1_555 no C(50) C(51) C(52) 112(1) 1_555 1_555 1_555 yes C(50) C(51) H(34) 126(2) 1_555 1_555 1_555 no C(52) C(51) H(34) 120(2) 1_555 1_555 1_555 no O(1) C(52) C(51) 100.8(10) 1_555 1_555 1_555 yes O(1) C(52) H(31) 110(1) 1_555 1_555 1_555 no O(1) C(52) H(32) 114(1) 1_555 1_555 1_555 no C(51) C(52) H(31) 109(1) 1_555 1_555 1_555 no C(51) C(52) H(32) 114(1) 1_555 1_555 1_555 no H(31) C(52) H(32) 106(2) 1_555 1_555 1_555 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 S(1) F(4) 3.44(1) 1_555 2_454 ? S(1) F(3) 3.52(1) 1_555 2_454 ? S(2) C(34) 3.50(2) 1_555 2_465 ? S(2) S(13) 3.572(6) 1_555 2_454 ? S(2) C(43) 3.57(2) 1_555 2_454 ? S(3) C(38) 3.47(1) 1_555 2_465 ? S(3) C(39) 3.54(2) 1_555 2_465 ? S(4) S(11) 3.587(6) 1_555 2_464 ? S(5) F(3) 3.50(1) 1_555 1_554 ? S(5) C(46) 3.51(1) 1_555 2_465 ? S(5) S(16) 3.595(6) 1_555 2_465 ? S(6) O(1) 3.555(9) 1_555 2_455 ? S(7) C(27) 3.46(1) 1_555 2_465 ? S(8) O(1) 3.497(9) 1_555 2_465 ? S(9) C(42) 3.41(2) 1_555 2_465 ? S(9) C(41) 3.54(2) 1_555 2_465 ? S(10) F(1) 3.39(1) 1_555 2_565 ? S(10) F(2) 3.51(1) 1_555 2_565 ? S(11) C(10) 3.50(2) 1_555 2_555 ? S(12) O(1) 3.218(9) 1_555 1_555 ? S(12) C(14) 3.44(2) 1_555 2_555 ? S(12) C(15) 3.49(2) 1_555 2_555 ? S(12) C(52) 3.52(1) 1_555 1_555 ? S(12) C(22) 3.59(1) 1_555 2_565 ? S(14) O(1) 3.191(10) 1_555 1_555 ? S(14) F(2) 3.44(1) 1_555 1_555 ? S(14) C(22) 3.51(1) 1_555 2_555 ? S(15) C(50) 3.57(1) 1_555 2_565 ? S(16) C(3) 3.40(1) 1_555 2_555 ? S(18) C(18) 3.42(1) 1_555 2_555 ? S(18) C(17) 3.57(1) 1_555 2_555 ? F(1) C(19) 3.05(2) 1_555 1_556 ? F(1) C(20) 3.16(2) 1_555 1_556 ? F(1) C(9) 3.16(2) 1_555 1_555 ? F(1) C(8) 3.44(2) 1_555 1_555 ? F(2) C(23) 3.25(2) 1_555 2_565 ? F(2) C(24) 3.54(2) 1_555 2_565 ? F(3) C(47) 3.21(2) 1_555 2_456 ? F(3) C(48) 3.55(2) 1_555 2_456 ? F(4) C(43) 3.06(2) 1_555 1_555 ? F(4) C(33) 3.07(2) 1_555 1_556 ? F(4) C(44) 3.24(2) 1_555 1_555 ? F(4) C(32) 3.43(2) 1_555 1_556 ? F(4) C(24) 3.58(2) 1_555 2_565 ? F(5) C(48) 3.43(2) 1_555 2_456 ? F(6) C(24) 3.40(2) 1_555 2_565 ? F(6) C(20) 3.57(2) 1_555 1_556 ? O(1) C(23) 3.23(2) 1_555 2_565 ? N(1) C(43) 3.49(2) 1_555 2_454 ? N(3) C(19) 3.48(2) 1_555 2_566 ? C(3) C(36) 3.43(2) 1_555 2_465 ? C(5) C(39) 3.52(2) 1_555 2_455 ? C(5) C(38) 3.57(2) 1_555 2_455 ? C(10) C(19) 3.50(2) 1_555 1_556 ? C(12) C(27) 3.30(2) 1_555 2_455 ? C(15) C(29) 3.58(2) 1_555 2_465 ? C(31) C(52) 3.34(2) 1_555 1_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(DHF),297K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:22:53 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1452.91 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H34 F6 N4 O P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.866(1) _cell_length_b 7.926(1) _cell_length_c 13.3035(6) _cell_angle_alpha 90 _cell_angle_beta 103.590(4) _cell_angle_gamma 90 _cell_volume 2855.9700 _cell_formula_units_Z 2 _cell_measurement_temperature 297.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.689 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1478.00 _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 297.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4597 _reflns_number_total 4597 _reflns_number_observed 3439 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 68 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.38618(8) 0.1552(4) 0.2327(2) 0.0545(7) Uani d . 1.00 . S2 0.40668(7) 0.3574(3) -0.0508(1) 0.0407(6) Uani d . 1.00 . S3 0.32123(7) 0.4270(3) -0.2207(1) 0.0397(6) Uani d . 1.00 . S4 0.47996(8) 0.5185(4) -0.1477(2) 0.0568(7) Uani d . 1.00 . S5 0.37709(8) 0.5918(3) -0.3570(2) 0.0494(7) Uani d . 1.00 . S6 0.25650(7) 0.3199(3) 0.3210(1) 0.0419(6) Uani d . 1.00 . S7 0.16786(7) 0.4056(3) 0.1644(1) 0.0405(6) Uani d . 1.00 . S8 0.22456(9) 0.4692(4) 0.4959(2) 0.0615(8) Uani d . 1.00 . S9 0.11563(8) 0.5711(3) 0.3065(2) 0.0506(7) Uani d . 1.00 . P1 0.0000 0.5000 0.5000 0.064(1) Uani d . 0.50 S F1 0.0031(3) 0.505(1) 0.3829(5) 0.129(3) Uani d . 1.00 . F2 0.0557(2) 0.445(1) 0.5295(5) 0.109(3) Uani d . 1.00 . F3 0.0163(3) 0.690(1) 0.5136(8) 0.135(4) Uani d . 1.00 . O1 0.0413(7) 0.452(2) 0.085(2) 0.111(8) Uani d . 0.50 . N1 0.3808(2) 0.198(1) 0.1110(5) 0.047(2) Uani d . 1.00 . N2 0.3287(2) 0.1811(10) 0.2390(5) 0.046(2) Uani d . 1.00 . C1 0.3327(2) 0.232(1) 0.0711(5) 0.034(2) Uani d . 1.00 . C2 0.3120(3) 0.277(1) -0.0386(5) 0.033(2) Uani d . 1.00 . C3 0.3431(3) 0.342(1) -0.0971(5) 0.033(2) Uani d . 1.00 . C4 0.2580(3) 0.258(1) -0.0706(5) 0.032(2) Uani d . 1.00 . C5 0.2358(3) 0.231(1) -0.1765(6) 0.037(2) Uani d . 1.00 . C6 0.1843(3) 0.199(1) -0.2096(6) 0.038(2) Uani d . 1.00 . C7 0.1627(3) 0.164(1) -0.3165(6) 0.052(3) Uani d . 1.00 . C8 0.1130(3) 0.135(2) -0.3447(7) 0.069(3) Uani d . 1.00 . C9 0.0840(3) 0.136(2) -0.2777(6) 0.070(3) Uani d . 1.00 . C10 0.1034(3) 0.164(1) -0.1700(7) 0.055(3) Uani d . 1.00 . C11 0.1553(3) 0.197(1) -0.1371(6) 0.038(2) Uani d . 1.00 . C12 0.1783(3) 0.221(1) -0.0338(6) 0.039(2) Uani d . 1.00 . C13 0.2286(3) 0.251(1) 0.0032(6) 0.036(2) Uani d . 1.00 . C14 0.2515(3) 0.265(1) 0.1114(5) 0.033(2) Uani d . 1.00 . C15 0.2276(3) 0.321(1) 0.1919(6) 0.037(2) Uani d . 1.00 . C16 0.3031(3) 0.222(1) 0.1420(5) 0.035(2) Uani d . 1.00 . C17 0.4176(3) 0.468(1) -0.1574(5) 0.039(2) Uani d . 1.00 . C18 0.3780(3) 0.499(1) -0.2346(6) 0.041(2) Uani d . 1.00 . C19 0.4741(3) 0.658(1) -0.2565(9) 0.067(3) Uani d . 1.00 . C20 0.4433(4) 0.591(2) -0.3552(7) 0.068(3) Uani d . 1.00 . C21 0.2121(3) 0.433(1) 0.3632(6) 0.043(2) Uani d . 1.00 . C22 0.1701(3) 0.472(1) 0.2873(6) 0.045(3) Uani d . 1.00 . C23 0.1641(3) 0.513(1) 0.5153(6) 0.055(3) Uani d . 1.00 . C24 0.1364(4) 0.644(1) 0.4391(8) 0.062(3) Uani d . 1.00 . C25 -0.0017(5) 0.534(2) 0.080(1) 0.087(4) Uani d . 1.00 . C26 0.0449(7) 0.412(3) 0.004(1) 0.153(8) Uani d . 1.00 . H1 0.2557 0.2341 -0.2257 0.0441 Uiso calc . 1.00 . H2 0.1822 0.1619 -0.3663 0.0635 Uiso calc . 1.00 . H3 0.0984 0.1143 -0.4154 0.0829 Uiso calc . 1.00 . H4 0.0496 0.1163 -0.3025 0.0829 Uiso calc . 1.00 . H5 0.0827 0.1618 -0.1218 0.0663 Uiso calc . 1.00 . H6 0.1584 0.2166 0.0153 0.0474 Uiso calc . 1.00 . H7 0.5062 0.6807 -0.2657 0.0810 Uiso calc . 1.00 . H8 0.4597 0.7609 -0.2400 0.0810 Uiso calc . 1.00 . H9 0.4482 0.6596 -0.4103 0.0814 Uiso calc . 1.00 . H10 0.4530 0.4790 -0.3640 0.0814 Uiso calc . 1.00 . H11 0.1673 0.5548 0.5832 0.0658 Uiso calc . 1.00 . H12 0.1455 0.4118 0.5063 0.0658 Uiso calc . 1.00 . H13 0.1085 0.6797 0.4620 0.0746 Uiso calc . 1.00 . H14 0.1580 0.7375 0.4389 0.0746 Uiso calc . 1.00 . H15 -0.0168 0.4657 0.1251 0.1019 Uiso calc . 1.00 . H16 0.0096 0.6367 0.1198 0.1019 Uiso calc . 1.00 . H17 0.0768 0.4460 -0.0098 0.1744 Uiso calc . 1.00 . H18 0.0483 0.2822 0.0031 0.1744 Uiso calc . 1.00 . 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 S(1) 0.041(1) 0.083(2) 0.040(1) 0.012(1) 0.0107(9) 0.016(1) S(2) 0.0324(9) 0.057(2) 0.0342(10) 0.0012(10) 0.0100(8) 0.0076(9) S(3) 0.037(1) 0.048(2) 0.0349(10) 0.0029(9) 0.0101(8) 0.0069(9) S(4) 0.040(1) 0.074(2) 0.058(1) -0.005(1) 0.0140(10) 0.017(1) S(5) 0.054(1) 0.053(2) 0.043(1) 0.001(1) 0.0139(10) 0.013(1) S(6) 0.041(1) 0.052(2) 0.0342(10) 0.0027(10) 0.0115(8) 0.0002(9) S(7) 0.037(1) 0.048(2) 0.038(1) 0.0041(9) 0.0121(8) 0.0061(9) S(8) 0.057(1) 0.089(2) 0.041(1) 0.002(1) 0.015(1) -0.015(1) S(9) 0.050(1) 0.054(2) 0.055(1) 0.011(1) 0.026(1) 0.002(1) P(1) 0.051(2) 0.080(3) 0.063(2) 0.020(2) 0.017(2) -0.008(2) F(1) 0.128(6) 0.20(1) 0.070(4) 0.038(6) 0.045(4) 0.004(5) F(2) 0.062(4) 0.160(8) 0.114(5) 0.038(4) 0.038(4) 0.025(5) F(3) 0.130(7) 0.083(7) 0.201(9) -0.017(5) 0.053(7) -0.017(6) O(1) 0.11(2) 0.04(1) 0.21(2) -0.01(1) 0.11(2) -0.02(1) N(1) 0.040(4) 0.070(6) 0.029(3) 0.007(4) 0.007(3) 0.008(3) N(2) 0.045(4) 0.056(6) 0.039(4) 0.012(4) 0.014(3) 0.002(3) C(1) 0.030(4) 0.044(5) 0.032(4) 0.009(3) 0.013(3) -0.001(3) C(2) 0.029(4) 0.040(5) 0.029(4) -0.001(3) 0.009(3) -0.001(3) C(3) 0.034(4) 0.035(5) 0.030(3) 0.006(3) 0.010(3) -0.005(3) C(4) 0.036(4) 0.036(5) 0.024(3) 0.003(3) 0.009(3) 0.001(3) C(5) 0.032(4) 0.040(6) 0.040(4) 0.001(3) 0.014(3) 0.003(4) C(6) 0.043(4) 0.030(5) 0.041(4) 0.001(4) 0.007(4) 0.006(4) C(7) 0.050(5) 0.069(7) 0.031(4) -0.001(5) -0.002(4) 0.002(4) C(8) 0.052(6) 0.086(9) 0.056(6) -0.011(6) -0.018(5) 0.019(6) C(9) 0.038(5) 0.13(1) 0.039(5) -0.026(6) -0.004(4) 0.013(5) C(10) 0.041(5) 0.071(8) 0.050(5) -0.007(5) 0.006(4) 0.004(5) C(11) 0.034(4) 0.045(6) 0.034(4) -0.003(4) 0.005(3) 0.007(4) C(12) 0.029(4) 0.048(6) 0.042(4) 0.000(4) 0.012(3) 0.003(4) C(13) 0.033(4) 0.028(5) 0.048(4) 0.002(3) 0.009(4) -0.001(4) C(14) 0.033(4) 0.037(5) 0.029(4) 0.000(3) 0.009(3) 0.001(3) C(15) 0.037(4) 0.034(5) 0.043(4) 0.002(4) 0.017(3) 0.002(4) C(16) 0.037(4) 0.031(5) 0.033(4) 0.000(3) 0.002(3) 0.001(3) C(17) 0.038(4) 0.053(6) 0.030(4) 0.001(4) 0.016(3) 0.003(4) C(18) 0.050(5) 0.040(6) 0.039(4) 0.000(4) 0.020(4) 0.001(4) C(19) 0.046(5) 0.051(7) 0.102(8) -0.010(5) 0.014(5) 0.015(6) C(20) 0.070(6) 0.100(10) 0.041(5) -0.020(6) 0.023(5) 0.009(5) C(21) 0.044(4) 0.045(6) 0.040(4) 0.001(4) 0.009(4) -0.009(4) C(22) 0.053(5) 0.035(6) 0.057(5) 0.003(4) 0.032(4) 0.002(4) C(23) 0.067(6) 0.065(8) 0.041(4) -0.004(5) 0.026(4) -0.011(5) C(24) 0.072(6) 0.046(7) 0.073(6) 0.007(5) 0.025(5) -0.013(5) C(25) 0.070(7) 0.067(9) 0.116(10) -0.012(7) 0.008(8) 0.008(8) C(26) 0.18(2) 0.19(2) 0.10(1) -0.05(2) 0.05(1) 0.02(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.012(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3439 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0773 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1034 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.455 _refine_ls_shift/esd_max 0.9890 _refine_ls_shift/esd_mean 0.0540 _refine_diff_density_min -0.62 _refine_diff_density_max 0.63 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.627(6) 1_555 1_555 yes S(1) N(2) 1.638(7) 1_555 1_555 yes S(2) C(3) 1.739(7) 1_555 1_555 yes S(2) C(17) 1.754(7) 1_555 1_555 yes S(3) C(3) 1.748(7) 1_555 1_555 yes S(3) C(18) 1.733(8) 1_555 1_555 yes S(4) C(17) 1.758(8) 1_555 1_555 yes S(4) C(19) 1.80(1) 1_555 1_555 yes S(5) C(18) 1.781(7) 1_555 1_555 yes S(5) C(20) 1.839(10) 1_555 1_555 yes S(6) C(15) 1.718(8) 1_555 1_555 yes S(6) C(21) 1.727(8) 1_555 1_555 yes S(7) C(15) 1.751(8) 1_555 1_555 yes S(7) C(22) 1.704(8) 1_555 1_555 yes S(8) C(21) 1.740(8) 1_555 1_555 yes S(8) C(23) 1.797(9) 1_555 1_555 yes S(9) C(22) 1.781(8) 1_555 1_555 yes S(9) C(24) 1.818(10) 1_555 1_555 yes P(1) F(1) 1.581(6) 1_555 1_555 yes P(1) F(1) 1.581(6) 1_555 3_566 yes P(1) F(2) 1.570(6) 1_555 1_555 yes P(1) F(2) 1.570(6) 1_555 3_566 yes P(1) F(3) 1.573(9) 1_555 1_555 yes P(1) F(3) 1.573(9) 1_555 3_566 yes O(1) C(25) 1.35(2) 1_555 1_555 yes O(1) C(26) 1.14(2) 1_555 1_555 yes N(1) C(1) 1.347(9) 1_555 1_555 yes N(2) C(16) 1.358(9) 1_555 1_555 yes C(1) C(2) 1.482(9) 1_555 1_555 yes C(1) C(16) 1.393(10) 1_555 1_555 yes C(2) C(3) 1.392(9) 1_555 1_555 yes C(2) C(4) 1.472(9) 1_555 1_555 yes C(4) C(5) 1.416(10) 1_555 1_555 yes C(4) C(13) 1.421(10) 1_555 1_555 yes C(5) C(6) 1.42(1) 1_555 1_555 yes C(6) C(7) 1.43(1) 1_555 1_555 yes C(6) C(11) 1.40(1) 1_555 1_555 yes C(7) C(8) 1.37(1) 1_555 1_555 yes C(8) C(9) 1.34(1) 1_555 1_555 yes C(9) C(10) 1.42(1) 1_555 1_555 yes C(10) C(11) 1.43(1) 1_555 1_555 yes C(11) C(12) 1.39(1) 1_555 1_555 yes C(12) C(13) 1.392(10) 1_555 1_555 yes C(13) C(14) 1.43(1) 1_555 1_555 yes C(14) C(15) 1.457(9) 1_555 1_555 yes C(14) C(16) 1.441(10) 1_555 1_555 yes C(17) C(18) 1.34(1) 1_555 1_555 yes C(19) C(20) 1.49(1) 1_555 1_555 yes C(21) C(22) 1.39(1) 1_555 1_555 yes C(23) C(24) 1.53(1) 1_555 1_555 yes C(25) C(26) 1.50(2) 1_555 3_565 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 N(1) S(1) N(2) 99.3(3) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.0(4) 1_555 1_555 1_555 yes C(3) S(3) C(18) 95.9(4) 1_555 1_555 1_555 yes C(17) S(4) C(19) 100.4(4) 1_555 1_555 1_555 yes C(18) S(5) C(20) 100.8(4) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.8(4) 1_555 1_555 1_555 yes C(15) S(7) C(22) 95.7(4) 1_555 1_555 1_555 yes C(21) S(8) C(23) 102.0(4) 1_555 1_555 1_555 yes C(22) S(9) C(24) 101.2(4) 1_555 1_555 1_555 yes F(1) P(1) F(1) 180.0 1_555 1_555 3_566 yes F(1) P(1) F(2) 88.4(4) 1_555 1_555 1_555 yes F(1) P(1) F(2) 91.6(4) 1_555 1_555 3_566 yes F(1) P(1) F(3) 90.6(5) 1_555 1_555 1_555 yes F(1) P(1) F(3) 89.4(5) 1_555 1_555 3_566 yes F(1) P(1) F(2) 91.6(4) 3_566 1_555 1_555 yes F(1) P(1) F(2) 88.4(4) 3_566 1_555 3_566 yes F(1) P(1) F(3) 89.4(5) 3_566 1_555 1_555 yes F(1) P(1) F(3) 90.6(5) 3_566 1_555 3_566 yes F(2) P(1) F(2) 180.0 1_555 1_555 3_566 yes F(2) P(1) F(3) 89.8(4) 1_555 1_555 1_555 yes F(2) P(1) F(3) 90.2(4) 1_555 1_555 3_566 yes F(2) P(1) F(3) 90.2(4) 3_566 1_555 1_555 yes F(2) P(1) F(3) 89.8(4) 3_566 1_555 3_566 yes F(3) P(1) F(3) 180.0 1_555 1_555 3_566 yes C(25) O(1) C(26) 111(2) 1_555 1_555 1_555 yes S(1) N(1) C(1) 106.5(5) 1_555 1_555 1_555 yes S(1) N(2) C(16) 106.4(5) 1_555 1_555 1_555 yes N(1) C(1) C(2) 123.8(6) 1_555 1_555 1_555 yes N(1) C(1) C(16) 114.5(6) 1_555 1_555 1_555 yes C(2) C(1) C(16) 121.7(6) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.4(6) 1_555 1_555 1_555 yes C(1) C(2) C(4) 113.2(6) 1_555 1_555 1_555 yes C(3) C(2) C(4) 127.2(7) 1_555 1_555 1_555 yes S(2) C(3) S(3) 114.0(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 123.0(6) 1_555 1_555 1_555 yes S(3) C(3) C(2) 122.9(6) 1_555 1_555 1_555 yes C(2) C(4) C(5) 118.8(6) 1_555 1_555 1_555 yes C(2) C(4) C(13) 121.4(7) 1_555 1_555 1_555 yes C(5) C(4) C(13) 119.5(7) 1_555 1_555 1_555 yes C(4) C(5) C(6) 120.6(6) 1_555 1_555 1_555 yes C(4) C(5) H(1) 119.4(7) 1_555 1_555 1_555 no C(6) C(5) H(1) 120.0(7) 1_555 1_555 1_555 no C(5) C(6) C(7) 120.0(7) 1_555 1_555 1_555 yes C(5) C(6) C(11) 119.6(7) 1_555 1_555 1_555 yes C(7) C(6) C(11) 120.3(7) 1_555 1_555 1_555 yes C(6) C(7) C(8) 117.9(8) 1_555 1_555 1_555 yes C(6) C(7) H(2) 121.2(8) 1_555 1_555 1_555 no C(8) C(7) H(2) 121.0(8) 1_555 1_555 1_555 no C(7) C(8) C(9) 123.3(9) 1_555 1_555 1_555 yes C(7) C(8) H(3) 118.3(10) 1_555 1_555 1_555 no C(9) C(8) H(3) 118.4(9) 1_555 1_555 1_555 no C(8) C(9) C(10) 121.7(8) 1_555 1_555 1_555 yes C(8) C(9) H(4) 119.1(9) 1_555 1_555 1_555 no C(10) C(9) H(4) 119.1(8) 1_555 1_555 1_555 no C(9) C(10) C(11) 116.9(7) 1_555 1_555 1_555 yes C(9) C(10) H(5) 121.7(8) 1_555 1_555 1_555 no C(11) C(10) H(5) 121.4(8) 1_555 1_555 1_555 no C(6) C(11) C(10) 119.9(7) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118.3(7) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.7(7) 1_555 1_555 1_555 yes C(11) C(12) C(13) 124.6(7) 1_555 1_555 1_555 yes C(11) C(12) H(6) 117.9(7) 1_555 1_555 1_555 no C(13) C(12) H(6) 117.5(8) 1_555 1_555 1_555 no C(4) C(13) C(12) 117.3(7) 1_555 1_555 1_555 yes C(4) C(13) C(14) 119.8(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 122.8(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 126.0(6) 1_555 1_555 1_555 yes C(13) C(14) C(16) 116.4(6) 1_555 1_555 1_555 yes C(15) C(14) C(16) 117.6(6) 1_555 1_555 1_555 yes S(6) C(15) S(7) 114.2(4) 1_555 1_555 1_555 yes S(6) C(15) C(14) 123.1(6) 1_555 1_555 1_555 yes S(7) C(15) C(14) 122.7(6) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113.3(6) 1_555 1_555 1_555 yes N(2) C(16) C(14) 126.2(7) 1_555 1_555 1_555 yes C(1) C(16) C(14) 120.4(6) 1_555 1_555 1_555 yes S(2) C(17) S(4) 114.2(4) 1_555 1_555 1_555 yes S(2) C(17) C(18) 116.3(6) 1_555 1_555 1_555 yes S(4) C(17) C(18) 129.4(6) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.6(5) 1_555 1_555 1_555 yes S(3) C(18) C(17) 117.7(6) 1_555 1_555 1_555 yes S(5) C(18) C(17) 127.5(6) 1_555 1_555 1_555 yes S(4) C(19) C(20) 114.2(7) 1_555 1_555 1_555 yes S(4) C(19) H(7) 108.0(8) 1_555 1_555 1_555 no S(4) C(19) H(8) 107.6(8) 1_555 1_555 1_555 no C(20) C(19) H(7) 108(1) 1_555 1_555 1_555 no C(20) C(19) H(8) 108.9(10) 1_555 1_555 1_555 no H(7) C(19) H(8) 109(1) 1_555 1_555 1_555 no S(5) C(20) C(19) 112.2(7) 1_555 1_555 1_555 yes S(5) C(20) H(9) 108.2(8) 1_555 1_555 1_555 no S(5) C(20) H(10) 108.7(8) 1_555 1_555 1_555 no C(19) C(20) H(9) 108.3(10) 1_555 1_555 1_555 no C(19) C(20) H(10) 109.0(10) 1_555 1_555 1_555 no H(9) C(20) H(10) 110.5(9) 1_555 1_555 1_555 no S(6) C(21) S(8) 115.3(5) 1_555 1_555 1_555 yes S(6) C(21) C(22) 115.1(6) 1_555 1_555 1_555 yes S(8) C(21) C(22) 129.5(6) 1_555 1_555 1_555 yes S(7) C(22) S(9) 115.7(5) 1_555 1_555 1_555 yes S(7) C(22) C(21) 117.7(6) 1_555 1_555 1_555 yes S(9) C(22) C(21) 126.4(6) 1_555 1_555 1_555 yes S(8) C(23) C(24) 112.4(6) 1_555 1_555 1_555 yes S(8) C(23) H(11) 108.9(7) 1_555 1_555 1_555 no S(8) C(23) H(12) 108.7(7) 1_555 1_555 1_555 no C(24) C(23) H(11) 108.3(9) 1_555 1_555 1_555 no C(24) C(23) H(12) 108.4(8) 1_555 1_555 1_555 no H(11) C(23) H(12) 110.1(8) 1_555 1_555 1_555 no S(9) C(24) C(23) 114.9(7) 1_555 1_555 1_555 yes S(9) C(24) H(13) 108.1(8) 1_555 1_555 1_555 no S(9) C(24) H(14) 107.5(7) 1_555 1_555 1_555 no C(23) C(24) H(13) 108.4(9) 1_555 1_555 1_555 no C(23) C(24) H(14) 107.9(9) 1_555 1_555 1_555 no H(13) C(24) H(14) 110.0(10) 1_555 1_555 1_555 no O(1) C(25) C(26) 135(1) 1_555 1_555 3_565 yes O(1) C(25) H(15) 102(1) 1_555 1_555 1_555 no O(1) C(25) H(16) 101(1) 1_555 1_555 1_555 no C(26) C(25) H(15) 103(1) 3_565 1_555 1_555 no C(26) C(25) H(16) 105(1) 3_565 1_555 1_555 no H(15) C(25) H(16) 104(1) 1_555 1_555 1_555 no O(1) C(26) C(25) 112(2) 1_555 1_555 3_565 yes O(1) C(26) H(17) 112(2) 1_555 1_555 1_555 no O(1) C(26) H(18) 108(1) 1_555 1_555 1_555 no C(25) C(26) H(17) 112(1) 3_565 1_555 1_555 no C(25) C(26) H(18) 109(1) 3_565 1_555 1_555 no H(17) C(26) H(18) 100(1) 1_555 1_555 1_555 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 S(2) O(1) 3.60(2) 1_555 2_545 ? S(3) C(15) 3.462(8) 1_555 2_555 ? S(5) C(22) 3.498(9) 1_555 2_555 ? S(6) C(7) 3.55(1) 1_555 2_555 ? S(7) O(1) 3.46(2) 1_555 1_555 ? S(7) C(2) 3.498(8) 1_555 2_555 ? S(7) C(3) 3.571(8) 1_555 2_555 ? S(7) C(26) 3.59(2) 1_555 1_555 ? S(9) O(1) 3.32(3) 1_555 1_555 ? S(9) C(18) 3.540(9) 1_555 2_555 ? S(9) F(1) 3.554(8) 1_555 1_555 ? F(1) C(19) 3.36(1) 1_555 2_545 ? F(2) C(23) 3.12(1) 1_555 1_555 ? F(2) C(8) 3.18(1) 1_555 1_556 ? F(2) C(24) 3.20(1) 1_555 1_555 ? F(2) C(9) 3.50(1) 1_555 1_556 ? F(3) C(20) 3.45(1) 1_555 4_466 ? O(1) C(19) 3.36(2) 1_555 2_545 ? N(2) C(23) 3.49(1) 1_555 2_546 ? C(3) C(12) 3.59(1) 1_555 2_555 ? C(5) C(15) 3.43(1) 1_555 2_545 ? C(7) C(23) 3.56(1) 1_555 1_554 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(DO),86K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:18:32 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1456.90 _chemical_formula_analytical ? _chemical_formula_sum 'C51 H34 F6 N4 O2 P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.627(4) _cell_length_b 7.686(2) _cell_length_c 13.304(2) _cell_angle_alpha 90 _cell_angle_beta 103.89(1) _cell_angle_gamma 89 _cell_volume 2742.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 86.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.764 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1482.00 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 86.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4231 _reflns_number_total 4231 _reflns_number_observed 2804 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.160 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 102 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 68 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.1121(1) 0.6490(4) 0.2660(2) 0.0366(9) Uani d . 1.00 . S2 0.0931(1) 0.8545(4) 0.5527(2) 0.0307(8) Uani d . 1.00 . S3 0.1802(1) 0.9204(4) 0.7222(2) 0.0316(8) Uani d . 1.00 . S4 0.0199(1) 1.0178(4) 0.6497(2) 0.0351(9) Uani d . 1.00 . S5 0.1254(1) 1.0916(4) 0.8599(2) 0.0343(9) Uani d . 1.00 . S6 0.2425(1) 0.8175(4) 0.1777(2) 0.0323(8) Uani d . 1.00 . S7 0.3329(1) 0.9034(4) 0.3348(2) 0.0311(9) Uani d . 1.00 . S8 0.2742(1) 0.9654(4) 0.0012(2) 0.0409(10) Uani d . 1.00 . S9 0.3856(1) 1.0692(4) 0.1918(2) 0.0358(9) Uani d . 1.00 . P1 0.5000 1.0000 1.0000 0.039(1) Uani d . 0.50 S F1 0.5047(3) 0.996(1) 0.8829(5) 0.060(3) Uani d . 1.00 . F2 0.4840(3) 1.1989(10) 0.9893(7) 0.060(3) Uani d . 1.00 . F3 0.4421(3) 0.944(1) 0.9632(6) 0.054(2) Uani d . 1.00 . O1 0.4551 0.9730 0.4050 0.060(7) Uani d . 0.50 S O2 0.5341 1.0877 0.4908 0.049(7) Uani d . 0.50 S N1 0.1187(3) 0.689(1) 0.3910(7) 0.037(3) Uani d . 1.00 . N2 0.1700(3) 0.674(1) 0.2600(7) 0.033(3) Uani d . 1.00 . C1 0.1677(4) 0.723(1) 0.4314(8) 0.025(3) Uani d . 1.00 . C2 0.1882(4) 0.771(1) 0.5374(9) 0.029(3) Uani d . 1.00 . C3 0.1581(4) 0.837(1) 0.5990(8) 0.025(3) Uani d . 1.00 . C4 0.2427(4) 0.751(1) 0.5730(9) 0.028(3) Uani d . 1.00 . C5 0.2659(4) 0.721(1) 0.6766(8) 0.030(3) Uani d . 1.00 . C6 0.3175(4) 0.693(1) 0.7109(9) 0.031(3) Uani d . 1.00 . C7 0.3416(4) 0.654(1) 0.8178(9) 0.034(4) Uani d . 1.00 . C8 0.3919(5) 0.625(2) 0.848(1) 0.045(4) Uani d . 1.00 . C9 0.4201(5) 0.629(2) 0.7730(9) 0.040(4) Uani d . 1.00 . C10 0.4000(4) 0.661(2) 0.6720(9) 0.036(4) Uani d . 1.00 . C11 0.3475(4) 0.691(1) 0.6388(9) 0.031(3) Uani d . 1.00 . C12 0.3236(4) 0.716(1) 0.5313(9) 0.030(3) Uani d . 1.00 . C13 0.2726(4) 0.746(1) 0.4947(8) 0.030(3) Uani d . 1.00 . C14 0.2495(4) 0.758(1) 0.3853(9) 0.030(3) Uani d . 1.00 . C15 0.2739(4) 0.816(1) 0.3106(8) 0.027(3) Uani d . 1.00 . C16 0.1970(4) 0.715(1) 0.3546(9) 0.030(3) Uani d . 1.00 . C17 0.0831(4) 0.966(1) 0.6583(9) 0.032(3) Uani d . 1.00 . C18 0.1228(4) 0.998(2) 0.7384(8) 0.031(3) Uani d . 1.00 . C19 0.0265(4) 1.166(2) 0.7579(9) 0.039(4) Uani d . 1.00 . C20 0.0595(5) 1.093(2) 0.8587(10) 0.045(4) Uani d . 1.00 . C21 0.2879(4) 0.931(1) 0.1351(8) 0.031(3) Uani d . 1.00 . C22 0.3304(4) 0.970(1) 0.2088(10) 0.034(4) Uani d . 1.00 . C23 0.3363(5) 1.003(2) -0.0152(9) 0.039(4) Uani d . 1.00 . C24 0.3645(5) 1.142(2) 0.059(1) 0.043(4) Uani d . 1.00 . C25 0.5017 1.0306 0.4036 0.08(1) Uani d . 0.50 S C26 0.5092 1.0336 0.5733 0.12(1) Uani d . 0.50 S C27 0.4688 1.0035 0.5222 0.26(2) Uani d . 0.50 S H1 0.2462 0.7201 0.7262 0.0365 Uiso calc . 1.00 . H2 0.3225 0.6503 0.8691 0.0409 Uiso calc . 1.00 . H3 0.4070 0.6015 0.9185 0.0543 Uiso calc . 1.00 . H4 0.4549 0.6078 0.7952 0.0483 Uiso calc . 1.00 . H5 0.4203 0.6626 0.6237 0.0456 Uiso calc . 1.00 . H6 0.3433 0.7102 0.4821 0.0356 Uiso calc . 1.00 . H7 -0.0060 1.1892 0.7678 0.0454 Uiso calc . 1.00 . H8 0.0406 1.2710 0.7407 0.0454 Uiso calc . 1.00 . H9 0.0550 1.1614 0.9154 0.0521 Uiso calc . 1.00 . H10 0.0495 0.9760 0.8680 0.0521 Uiso calc . 1.00 . H11 0.3346 1.0391 -0.0840 0.0457 Uiso calc . 1.00 . H12 0.3549 0.8968 -0.0020 0.0457 Uiso calc . 1.00 . H13 0.3928 1.1776 0.0357 0.0520 Uiso calc . 1.00 . H14 0.3428 1.2383 0.0577 0.0520 Uiso calc . 1.00 . H15 0.5177 0.9370 0.3781 0.0761 Uiso calc . 0.50 . H16 0.4971 1.1244 0.3557 0.0761 Uiso calc . 0.50 . H17 0.5244 0.9332 0.6092 0.1300 Uiso calc . 0.50 . H18 0.5089 1.1246 0.6215 0.1300 Uiso calc . 0.50 . H19 0.4489 1.0990 0.5331 0.9246 Uiso calc . 0.50 . H20 0.4584 0.9013 0.5513 0.9246 Uiso calc . 0.50 . 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 S(1) 0.037(2) 0.040(2) 0.035(2) -0.004(1) 0.014(1) -0.006(2) S(2) 0.033(2) 0.029(2) 0.033(2) -0.001(1) 0.012(1) -0.001(1) S(3) 0.036(2) 0.026(2) 0.034(2) 0.000(1) 0.010(1) -0.001(1) S(4) 0.038(2) 0.033(2) 0.037(2) 0.003(1) 0.014(1) -0.003(1) S(5) 0.041(2) 0.027(2) 0.034(2) 0.002(1) 0.008(1) -0.004(1) S(6) 0.038(2) 0.030(2) 0.030(2) -0.001(1) 0.010(1) -0.001(1) S(7) 0.035(2) 0.024(2) 0.035(2) 0.000(1) 0.010(1) 0.000(1) S(8) 0.043(2) 0.045(2) 0.037(2) -0.002(2) 0.014(2) 0.007(2) S(9) 0.042(2) 0.025(2) 0.043(2) -0.003(1) 0.016(2) -0.001(1) P(1) 0.038(3) 0.040(3) 0.043(3) -0.008(2) 0.015(2) 0.004(2) F(1) 0.060(5) 0.082(7) 0.044(4) -0.013(4) 0.023(4) -0.005(4) F(2) 0.059(5) 0.043(5) 0.082(6) 0.001(4) 0.028(5) 0.002(4) F(3) 0.041(4) 0.065(6) 0.058(5) -0.018(4) 0.020(4) -0.008(4) O(1) 0.09(1) 0.06(1) 0.05(1) 0.01(1) 0.04(1) -0.01(1) O(2) 0.07(2) 0.07(1) 0.016(10) 0.00(1) 0.02(1) -0.001(9) N(1) 0.031(6) 0.049(7) 0.034(6) -0.003(5) 0.011(5) -0.011(5) N(2) 0.034(6) 0.032(6) 0.030(6) 0.000(5) 0.005(5) -0.005(5) C(1) 0.032(6) 0.025(6) 0.015(5) -0.007(5) 0.004(5) 0.004(5) C(2) 0.038(7) 0.024(7) 0.029(6) 0.001(5) 0.013(6) 0.003(5) C(3) 0.029(6) 0.019(6) 0.024(6) -0.010(5) -0.001(5) 0.000(5) C(4) 0.033(6) 0.020(6) 0.033(7) 0.001(5) 0.012(5) 0.005(5) C(5) 0.040(7) 0.023(6) 0.029(7) 0.003(5) 0.011(6) -0.004(5) C(6) 0.037(7) 0.016(6) 0.036(7) 0.002(5) 0.001(6) -0.001(5) C(7) 0.042(7) 0.018(6) 0.047(8) 0.004(5) 0.021(6) 0.008(6) C(8) 0.048(8) 0.024(7) 0.062(9) 0.006(6) 0.011(7) -0.009(6) C(9) 0.042(7) 0.046(9) 0.030(7) 0.001(6) 0.003(6) -0.012(6) C(10) 0.047(8) 0.031(7) 0.029(7) 0.013(6) 0.006(6) 0.000(6) C(11) 0.042(7) 0.022(7) 0.028(6) 0.003(5) 0.008(6) 0.000(5) C(12) 0.025(6) 0.032(7) 0.037(7) 0.004(5) 0.017(6) -0.001(6) C(13) 0.041(7) 0.026(7) 0.021(6) -0.001(5) 0.001(5) -0.005(5) C(14) 0.037(7) 0.020(6) 0.034(7) 0.008(5) 0.014(6) 0.003(5) C(15) 0.036(7) 0.023(7) 0.017(6) -0.008(5) 0.000(5) -0.005(5) C(16) 0.031(7) 0.021(6) 0.040(8) -0.001(5) 0.012(6) 0.003(5) C(17) 0.044(7) 0.018(6) 0.039(7) 0.002(5) 0.018(6) 0.000(5) C(18) 0.043(7) 0.030(7) 0.024(6) 0.002(5) 0.015(6) -0.002(5) C(19) 0.042(7) 0.029(7) 0.048(8) 0.002(5) 0.016(6) 0.000(6) C(20) 0.058(8) 0.036(8) 0.046(8) 0.006(6) 0.021(7) -0.005(6) C(21) 0.033(6) 0.032(7) 0.028(6) -0.005(5) 0.009(5) 0.002(5) C(22) 0.044(7) 0.017(6) 0.050(8) 0.004(5) 0.028(7) 0.001(6) C(23) 0.053(8) 0.032(7) 0.033(7) -0.006(6) 0.013(6) 0.003(6) C(24) 0.064(9) 0.019(6) 0.054(8) -0.007(6) 0.028(7) 0.008(6) C(25) 0.03(1) 0.14(5) 0.06(2) 0.00(2) -0.01(1) -0.04(2) C(26) 0.04(1) 0.09(3) 0.18(4) 0.03(2) -0.07(2) -0.12(3) C(27) 0.31(4) 0.33(4) 0.21(4) 0.15(3) 0.21(3) 0.08(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0014(10) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2804 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0882 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1071 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.090 _refine_ls_shift/esd_max 5.0350 _refine_ls_shift/esd_mean 0.2120 _refine_diff_density_min -0.93 _refine_diff_density_max 0.83 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.657(9) 1_555 1_555 yes S(1) N(2) 1.631(9) 1_555 1_555 yes S(2) C(3) 1.76(1) 1_555 1_555 yes S(2) C(17) 1.72(1) 1_555 1_555 yes S(3) C(3) 1.73(1) 1_555 1_555 yes S(3) C(18) 1.75(1) 1_555 1_555 yes S(4) C(17) 1.77(1) 1_555 1_555 yes S(4) C(19) 1.81(1) 1_555 1_555 yes S(5) C(18) 1.76(1) 1_555 1_555 yes S(5) C(20) 1.82(1) 1_555 1_555 yes S(6) C(15) 1.77(1) 1_555 1_555 yes S(6) C(21) 1.73(1) 1_555 1_555 yes S(7) C(15) 1.72(1) 1_555 1_555 yes S(7) C(22) 1.74(1) 1_555 1_555 yes S(8) C(21) 1.75(1) 1_555 1_555 yes S(8) C(23) 1.80(1) 1_555 1_555 yes S(9) C(22) 1.77(1) 1_555 1_555 yes S(9) C(24) 1.81(1) 1_555 1_555 yes P(1) F(1) 1.595(7) 1_555 1_555 yes P(1) F(1) 1.595(7) 1_555 3_677 yes P(1) F(2) 1.588(8) 1_555 1_555 yes P(1) F(2) 1.588(8) 1_555 3_677 yes P(1) F(3) 1.615(7) 1_555 1_555 yes P(1) F(3) 1.615(7) 1_555 3_677 yes O(1) O(2) 1.425 1_555 3_676 yes O(1) C(25) 1.3657(2) 1_555 1_555 yes O(1) C(26) 0.9591(1) 1_555 3_676 yes O(1) C(27) 1.531 1_555 1_555 yes O(2) C(25) 1.3569(1) 1_555 1_555 yes O(2) C(26) 1.4883(1) 1_555 1_555 yes O(2) C(26) 1.5941(1) 1_555 3_676 yes O(2) C(27) 0.722 1_555 3_676 yes N(1) C(1) 1.36(1) 1_555 1_555 yes N(2) C(16) 1.34(1) 1_555 1_555 yes C(1) C(2) 1.44(1) 1_555 1_555 yes C(1) C(16) 1.45(1) 1_555 1_555 yes C(2) C(3) 1.40(1) 1_555 1_555 yes C(2) C(4) 1.47(2) 1_555 1_555 yes C(4) C(5) 1.39(2) 1_555 1_555 yes C(4) C(13) 1.48(1) 1_555 1_555 yes C(5) C(6) 1.40(2) 1_555 1_555 yes C(6) C(7) 1.45(2) 1_555 1_555 yes C(6) C(11) 1.41(1) 1_555 1_555 yes C(7) C(8) 1.37(2) 1_555 1_555 yes C(8) C(9) 1.40(2) 1_555 1_555 yes C(9) C(10) 1.35(2) 1_555 1_555 yes C(10) C(11) 1.43(2) 1_555 1_555 yes C(11) C(12) 1.44(2) 1_555 1_555 yes C(12) C(13) 1.40(2) 1_555 1_555 yes C(13) C(14) 1.44(2) 1_555 1_555 yes C(14) C(15) 1.40(1) 1_555 1_555 yes C(14) C(16) 1.45(2) 1_555 1_555 yes C(17) C(18) 1.36(2) 1_555 1_555 yes C(19) C(20) 1.53(2) 1_555 1_555 yes C(21) C(22) 1.37(2) 1_555 1_555 yes C(23) C(24) 1.54(2) 1_555 1_555 yes C(25) C(26) 0.688 1_555 3_676 yes C(25) C(27) 1.1487(1) 1_555 3_676 yes C(26) C(27) 1.1820(1) 1_555 1_555 yes C(26) C(27) 1.5597(1) 1_555 3_676 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 N(1) S(1) N(2) 98.9(5) 1_555 1_555 1_555 yes C(3) S(2) C(17) 95.9(6) 1_555 1_555 1_555 yes C(3) S(3) C(18) 96.7(5) 1_555 1_555 1_555 yes C(17) S(4) C(19) 100.3(6) 1_555 1_555 1_555 yes C(18) S(5) C(20) 100.1(6) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.3(5) 1_555 1_555 1_555 yes C(15) S(7) C(22) 96.8(5) 1_555 1_555 1_555 yes C(21) S(8) C(23) 99.6(5) 1_555 1_555 1_555 yes C(22) S(9) C(24) 100.0(6) 1_555 1_555 1_555 yes F(1) P(1) F(1) 180.0 1_555 1_555 3_677 yes F(1) P(1) F(2) 91.1(4) 1_555 1_555 1_555 yes F(1) P(1) F(2) 88.9(4) 1_555 1_555 3_677 yes F(1) P(1) F(3) 90.4(3) 1_555 1_555 1_555 yes F(1) P(1) F(3) 89.6(3) 1_555 1_555 3_677 yes F(1) P(1) F(2) 88.9(4) 3_677 1_555 1_555 yes F(1) P(1) F(2) 91.1(4) 3_677 1_555 3_677 yes F(1) P(1) F(3) 89.6(3) 3_677 1_555 1_555 yes F(1) P(1) F(3) 90.4(3) 3_677 1_555 3_677 yes F(2) P(1) F(2) 180.0 1_555 1_555 3_677 yes F(2) P(1) F(3) 89.6(4) 1_555 1_555 1_555 yes F(2) P(1) F(3) 90.4(4) 1_555 1_555 3_677 yes F(2) P(1) F(3) 90.4(4) 3_677 1_555 1_555 yes F(2) P(1) F(3) 89.6(4) 3_677 1_555 3_677 yes F(3) P(1) F(3) 180.0 1_555 1_555 3_677 yes O(2) O(1) C(25) 98.183(3) 3_676 1_555 1_555 yes O(2) O(1) C(26) 74.4105(8) 3_676 1_555 3_676 yes O(2) O(1) C(27) 28.0 3_676 1_555 1_555 yes O(2) O(1) H(17) 116.196(3) 3_676 1_555 3_676 no C(25) O(1) C(26) 28.055(4) 1_555 1_555 3_676 yes C(25) O(1) C(27) 87.721(2) 1_555 1_555 1_555 yes C(25) O(1) H(17) 32.219(1) 1_555 1_555 3_676 no C(26) O(1) C(27) 73.5432(4) 3_676 1_555 1_555 yes C(26) O(1) H(17) 59.228(6) 3_676 1_555 3_676 no C(27) O(1) H(17) 94.136(2) 1_555 1_555 3_676 no O(1) O(2) C(25) 131.780(1) 3_676 1_555 1_555 yes O(1) O(2) C(26) 38.367(5) 3_676 1_555 1_555 yes O(1) O(2) C(26) 106.4683(2) 3_676 1_555 3_676 yes O(1) O(2) C(27) 84.2501(1) 3_676 1_555 3_676 yes O(1) O(2) H(20) 148.215(4) 3_676 1_555 3_676 no C(25) O(2) C(26) 102.279(7) 1_555 1_555 1_555 yes C(25) O(2) C(26) 25.361(1) 1_555 1_555 3_676 yes C(25) O(2) C(27) 57.8428(8) 1_555 1_555 3_676 yes C(25) O(2) H(20) 65.399(7) 1_555 1_555 3_676 no C(26) O(2) C(26) 79.048(6) 1_555 1_555 3_676 yes C(26) O(2) C(27) 81.8736(5) 1_555 1_555 3_676 yes C(26) O(2) H(20) 167.0523(2) 1_555 1_555 3_676 no C(26) O(2) C(27) 43.657(3) 3_676 1_555 3_676 yes C(26) O(2) H(20) 88.100(6) 3_676 1_555 3_676 no C(27) O(2) H(20) 87.7640(8) 3_676 1_555 3_676 no S(1) N(1) C(1) 107.0(7) 1_555 1_555 1_555 yes S(1) N(2) C(16) 108.4(7) 1_555 1_555 1_555 yes N(1) C(1) C(2) 124.1(9) 1_555 1_555 1_555 yes N(1) C(1) C(16) 112.6(10) 1_555 1_555 1_555 yes C(2) C(1) C(16) 123(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 121(1) 1_555 1_555 1_555 yes C(1) C(2) C(4) 114.8(9) 1_555 1_555 1_555 yes C(3) C(2) C(4) 123(1) 1_555 1_555 1_555 yes S(2) C(3) S(3) 113.8(6) 1_555 1_555 1_555 yes S(2) C(3) C(2) 121.7(9) 1_555 1_555 1_555 yes S(3) C(3) C(2) 124.4(9) 1_555 1_555 1_555 yes C(2) C(4) C(5) 121.9(9) 1_555 1_555 1_555 yes C(2) C(4) C(13) 118(1) 1_555 1_555 1_555 yes C(5) C(4) C(13) 119(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 122.5(10) 1_555 1_555 1_555 yes C(4) C(5) H(1) 118(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 118(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 122(1) 1_555 1_555 1_555 yes C(5) C(6) C(11) 119(1) 1_555 1_555 1_555 yes C(7) C(6) C(11) 117(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 121(1) 1_555 1_555 1_555 yes C(6) C(7) H(2) 120(1) 1_555 1_555 1_555 no C(8) C(7) H(2) 118(1) 1_555 1_555 1_555 no C(7) C(8) C(9) 119(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 119(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 121(1) 1_555 1_555 1_555 no C(8) C(9) C(10) 122(1) 1_555 1_555 1_555 yes C(8) C(9) H(4) 117(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 119(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 118(1) 1_555 1_555 1_555 yes C(9) C(10) H(5) 120(1) 1_555 1_555 1_555 no C(11) C(10) H(5) 120(1) 1_555 1_555 1_555 no C(6) C(11) C(10) 120(1) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.1(10) 1_555 1_555 1_555 yes C(11) C(12) C(13) 123.5(10) 1_555 1_555 1_555 yes C(11) C(12) H(6) 118(1) 1_555 1_555 1_555 no C(13) C(12) H(6) 117(1) 1_555 1_555 1_555 no C(4) C(13) C(12) 116(1) 1_555 1_555 1_555 yes C(4) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 124(1) 1_555 1_555 1_555 yes C(13) C(14) C(16) 116.1(10) 1_555 1_555 1_555 yes C(15) C(14) C(16) 119(1) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.5(6) 1_555 1_555 1_555 yes S(6) C(15) C(14) 120.4(9) 1_555 1_555 1_555 yes S(7) C(15) C(14) 126.0(9) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113.2(10) 1_555 1_555 1_555 yes N(2) C(16) C(14) 128.0(10) 1_555 1_555 1_555 yes C(1) C(16) C(14) 118(1) 1_555 1_555 1_555 yes S(2) C(17) S(4) 114.2(7) 1_555 1_555 1_555 yes S(2) C(17) C(18) 118.1(8) 1_555 1_555 1_555 yes S(4) C(17) C(18) 127.7(9) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.4(7) 1_555 1_555 1_555 yes S(3) C(18) C(17) 115.4(8) 1_555 1_555 1_555 yes S(5) C(18) C(17) 130.1(9) 1_555 1_555 1_555 yes S(4) C(19) C(20) 113.1(8) 1_555 1_555 1_555 yes S(4) C(19) H(7) 108.1(10) 1_555 1_555 1_555 no S(4) C(19) H(8) 108.3(9) 1_555 1_555 1_555 no C(20) C(19) H(7) 109(1) 1_555 1_555 1_555 no C(20) C(19) H(8) 109(1) 1_555 1_555 1_555 no H(7) C(19) H(8) 108(1) 1_555 1_555 1_555 no S(5) C(20) C(19) 113.1(8) 1_555 1_555 1_555 yes S(5) C(20) H(9) 108(1) 1_555 1_555 1_555 no S(5) C(20) H(10) 108.2(10) 1_555 1_555 1_555 no C(19) C(20) H(9) 109(1) 1_555 1_555 1_555 no C(19) C(20) H(10) 109(1) 1_555 1_555 1_555 no H(9) C(20) H(10) 108(1) 1_555 1_555 1_555 no S(6) C(21) S(8) 114.4(7) 1_555 1_555 1_555 yes S(6) C(21) C(22) 116.2(8) 1_555 1_555 1_555 yes S(8) C(21) C(22) 129.3(8) 1_555 1_555 1_555 yes S(7) C(22) S(9) 114.5(7) 1_555 1_555 1_555 yes S(7) C(22) C(21) 117.0(8) 1_555 1_555 1_555 yes S(9) C(22) C(21) 128.4(9) 1_555 1_555 1_555 yes S(8) C(23) C(24) 112.6(8) 1_555 1_555 1_555 yes S(8) C(23) H(11) 109.6(10) 1_555 1_555 1_555 no S(8) C(23) H(12) 109.0(9) 1_555 1_555 1_555 no C(24) C(23) H(11) 108(1) 1_555 1_555 1_555 no C(24) C(23) H(12) 108(1) 1_555 1_555 1_555 no H(11) C(23) H(12) 109(1) 1_555 1_555 1_555 no S(9) C(24) C(23) 113.9(8) 1_555 1_555 1_555 yes S(9) C(24) H(13) 108(1) 1_555 1_555 1_555 no S(9) C(24) H(14) 108.3(9) 1_555 1_555 1_555 no C(23) C(24) H(13) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(14) 108(1) 1_555 1_555 1_555 no H(13) C(24) H(14) 109(1) 1_555 1_555 1_555 no O(1) C(25) O(2) 121.635(5) 1_555 1_555 1_555 yes O(1) C(25) C(26) 40.975(1) 1_555 1_555 3_676 yes O(1) C(25) C(27) 112.955(7) 1_555 1_555 3_676 yes O(1) C(25) H(15) 106.353(6) 1_555 1_555 1_555 no O(1) C(25) H(16) 106.353(3) 1_555 1_555 1_555 no O(1) C(25) H(17) 43.007(6) 1_555 1_555 3_676 no O(1) C(25) H(18) 62.2253(5) 1_555 1_555 3_676 no O(1) C(25) H(20) 149.683(4) 1_555 1_555 3_676 no O(2) C(25) C(26) 96.982(4) 1_555 1_555 3_676 yes O(2) C(25) C(27) 32.145(2) 1_555 1_555 3_676 yes O(2) C(25) H(15) 106.353(7) 1_555 1_555 1_555 no O(2) C(25) H(16) 106.3532(4) 1_555 1_555 1_555 no O(2) C(25) H(17) 118.328(5) 1_555 1_555 3_676 no O(2) C(25) H(18) 126.8206(2) 1_555 1_555 3_676 no O(2) C(25) H(20) 28.3789(9) 1_555 1_555 3_676 no C(26) C(25) C(27) 75.505(7) 3_676 1_555 3_676 yes C(26) C(25) H(15) 84.769(5) 3_676 1_555 1_555 no C(26) C(25) H(16) 147.277(4) 3_676 1_555 1_555 no C(26) C(25) H(17) 82.358(7) 3_676 1_555 3_676 no C(26) C(25) H(18) 48.4598(2) 3_676 1_555 3_676 no C(26) C(25) H(20) 121.500(4) 3_676 1_555 3_676 no C(27) C(25) H(15) 80.743(5) 3_676 1_555 1_555 no C(27) C(25) H(16) 134.564(3) 3_676 1_555 1_555 no C(27) C(25) H(17) 136.191(3) 3_676 1_555 3_676 no C(27) C(25) H(18) 94.810(2) 3_676 1_555 3_676 no C(27) C(25) H(20) 46.766(4) 3_676 1_555 3_676 no H(15) C(25) H(16) 109.4597(2) 1_555 1_555 1_555 no H(15) C(25) H(17) 134.591(2) 1_555 1_555 3_676 no H(15) C(25) H(18) 44.264(6) 1_555 1_555 3_676 no H(15) C(25) H(20) 93.221(8) 1_555 1_555 3_676 no H(16) C(25) H(17) 66.548(3) 1_555 1_555 3_676 no H(16) C(25) H(18) 123.9345(4) 1_555 1_555 3_676 no H(16) C(25) H(20) 87.9058(9) 1_555 1_555 3_676 no H(17) C(25) H(18) 98.074(5) 3_676 1_555 3_676 no H(17) C(25) H(20) 130.286(7) 3_676 1_555 3_676 no H(18) C(25) H(20) 130.970(2) 3_676 1_555 3_676 no O(1) C(26) O(2) 67.223(6) 3_676 1_555 1_555 yes O(1) C(26) O(2) 135.721(4) 3_676 1_555 3_676 yes O(1) C(26) C(25) 110.969(5) 3_676 1_555 3_676 yes O(1) C(26) C(27) 157.290(3) 3_676 1_555 1_555 yes O(1) C(26) C(27) 70.319(6) 3_676 1_555 3_676 yes O(1) C(26) H(15) 127.938(6) 3_676 1_555 3_676 no O(1) C(26) H(17) 60.612(2) 3_676 1_555 1_555 no O(1) C(26) H(18) 90.626(2) 3_676 1_555 1_555 no O(2) C(26) O(2) 100.952(6) 1_555 1_555 3_676 yes O(2) C(26) C(25) 149.292(1) 1_555 1_555 3_676 yes O(2) C(26) C(27) 99.782(7) 1_555 1_555 1_555 yes O(2) C(26) C(27) 27.273(1) 1_555 1_555 3_676 yes O(2) C(26) H(15) 149.129(2) 1_555 1_555 3_676 no O(2) C(26) H(17) 111.839(6) 1_555 1_555 1_555 no O(2) C(26) H(18) 111.8403(3) 1_555 1_555 1_555 no O(2) C(26) C(25) 57.657(3) 3_676 1_555 3_676 yes O(2) C(26) C(27) 24.938(2) 3_676 1_555 1_555 yes O(2) C(26) C(27) 81.165(7) 3_676 1_555 3_676 yes O(2) C(26) H(15) 84.729(9) 3_676 1_555 3_676 no O(2) C(26) H(17) 88.755(5) 3_676 1_555 1_555 no O(2) C(26) H(18) 131.618(5) 3_676 1_555 1_555 no C(25) C(26) C(27) 70.201(5) 3_676 1_555 1_555 yes C(25) C(26) C(27) 122.029(2) 3_676 1_555 3_676 yes C(25) C(26) H(15) 57.561(3) 3_676 1_555 3_676 no C(25) C(26) H(17) 51.780(7) 3_676 1_555 1_555 no C(25) C(26) H(18) 98.722(1) 3_676 1_555 1_555 no C(27) C(26) C(27) 89.610(8) 1_555 1_555 3_676 yes C(27) C(26) H(15) 72.819(9) 1_555 1_555 3_676 no C(27) C(26) H(17) 111.839(3) 1_555 1_555 1_555 no C(27) C(26) H(18) 111.839(4) 1_555 1_555 1_555 no C(27) C(26) H(15) 161.6300(6) 3_676 1_555 3_676 no C(27) C(26) H(17) 92.914(4) 3_676 1_555 1_555 no C(27) C(26) H(18) 138.756(1) 3_676 1_555 1_555 no H(15) C(26) H(17) 98.506(4) 3_676 1_555 1_555 no H(15) C(26) H(18) 49.272(3) 3_676 1_555 1_555 no H(17) C(26) H(18) 109.4602(3) 1_555 1_555 1_555 no O(1) C(27) O(2) 67.7749(1) 1_555 1_555 3_676 yes O(1) C(27) C(25) 142.270(2) 1_555 1_555 3_676 yes O(1) C(27) C(26) 125.782(3) 1_555 1_555 1_555 yes O(1) C(27) C(26) 36.138(5) 1_555 1_555 3_676 yes O(1) C(27) H(19) 105.256(2) 1_555 1_555 1_555 no O(1) C(27) H(20) 105.255(1) 1_555 1_555 1_555 no O(2) C(27) C(25) 90.0124(9) 3_676 1_555 3_676 yes O(2) C(27) C(26) 111.405(1) 3_676 1_555 1_555 yes O(2) C(27) C(26) 70.853(2) 3_676 1_555 3_676 yes O(2) C(27) H(19) 138.610(5) 3_676 1_555 1_555 no O(2) C(27) H(20) 42.8294(4) 3_676 1_555 1_555 no C(25) C(27) C(26) 34.294(2) 3_676 1_555 1_555 yes C(25) C(27) C(26) 108.941(8) 3_676 1_555 3_676 yes C(25) C(27) H(19) 111.246(5) 3_676 1_555 1_555 no C(25) C(27) H(20) 71.477(6) 3_676 1_555 1_555 no C(26) C(27) C(26) 90.390(8) 1_555 1_555 3_676 yes C(26) C(27) H(19) 105.255(7) 1_555 1_555 1_555 no C(26) C(27) H(20) 105.256(4) 1_555 1_555 1_555 no C(26) C(27) H(19) 128.241(3) 3_676 1_555 1_555 no C(26) C(27) H(20) 113.313(2) 3_676 1_555 1_555 no H(19) C(27) H(20) 109.460(6) 1_555 1_555 1_555 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 S(1) F(3) 3.438(9) 1_555 2_546 ? S(1) F(1) 3.557(9) 1_555 2_546 ? S(2) C(27) 3.222(3) 1_555 2_546 ? S(2) O(1) 3.324(3) 1_555 2_546 ? S(3) C(15) 3.37(1) 1_555 2_556 ? S(3) S(9) 3.591(4) 1_555 2_546 ? S(4) C(26) 3.587(3) 1_555 4_475 ? S(5) C(22) 3.37(1) 1_555 2_556 ? S(5) C(21) 3.53(1) 1_555 2_556 ? S(6) C(7) 3.49(1) 1_555 2_556 ? S(6) S(8) 3.560(4) 1_555 2_545 ? S(7) O(1) 3.322(3) 1_555 1_555 ? S(7) C(2) 3.42(1) 1_555 2_556 ? S(7) C(3) 3.44(1) 1_555 2_556 ? S(7) C(18) 3.57(1) 1_555 2_546 ? S(9) O(1) 3.109(3) 1_555 1_555 ? S(9) C(18) 3.44(1) 1_555 2_556 ? S(9) F(1) 3.445(7) 1_555 3_676 ? F(1) C(19) 3.22(1) 1_555 4_575 ? F(1) C(20) 3.55(1) 1_555 4_575 ? F(2) C(20) 3.41(1) 1_555 4_575 ? F(3) C(23) 3.04(1) 1_555 1_556 ? F(3) C(8) 3.05(1) 1_555 1_555 ? F(3) C(24) 3.14(1) 1_555 1_556 ? F(3) C(9) 3.45(1) 1_555 1_555 ? O(1) C(19) 3.33(1) 1_555 2_546 ? N(1) C(27) 3.249(9) 1_555 2_546 ? N(2) C(23) 3.48(1) 1_555 2_545 ? C(2) C(12) 3.53(2) 1_555 2_556 ? C(3) C(12) 3.48(1) 1_555 2_556 ? C(5) C(15) 3.31(2) 1_555 2_546 ? C(7) C(23) 3.51(2) 1_555 1_556 ? C(19) C(26) 3.32(1) 1_555 4_475 ? C(19) C(25) 3.51(1) 1_555 2_556 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(DO),296K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:20:54 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1456.90 _chemical_formula_analytical ? _chemical_formula_sum 'C51 H34 F6 N4 O2 P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.879(5) _cell_length_b 7.954(6) _cell_length_c 13.337(2) _cell_angle_alpha 90 _cell_angle_beta 103.61(1) _cell_angle_gamma 90 _cell_volume 2874.3701 _cell_formula_units_Z 2 _cell_measurement_temperature 296.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _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_density_diffrn 1.683 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1482.00 _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 3755 _reflns_number_total 3755 _reflns_number_observed 2030 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.185 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 102 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 68 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.3851(2) 0.1589(8) 0.2321(4) 0.073(2) Uani d . 1.00 . S2 0.4058(2) 0.3591(6) -0.0522(3) 0.058(1) Uani d . 1.00 . S3 0.3206(2) 0.4295(6) -0.2201(3) 0.058(2) Uani d . 1.00 . S4 0.4789(2) 0.5156(7) -0.1494(4) 0.074(2) Uani d . 1.00 . S5 0.3758(2) 0.5935(6) -0.3567(4) 0.067(2) Uani d . 1.00 . S6 0.2565(2) 0.3252(6) 0.3198(3) 0.059(2) Uani d . 1.00 . S7 0.1679(2) 0.4089(6) 0.1639(3) 0.055(1) Uani d . 1.00 . S8 0.2242(2) 0.4744(8) 0.4949(4) 0.084(2) Uani d . 1.00 . S9 0.1153(2) 0.5733(7) 0.3063(4) 0.071(2) Uani d . 1.00 . P1 0.0000 0.5000 0.5000 0.088(3) Uani d . 0.50 S F1 -0.0154(6) 0.313(2) 0.486(1) 0.169(8) Uani d . 1.00 . F2 -0.0055(5) 0.489(3) 0.613(1) 0.175(8) Uani d . 1.00 . F3 0.0555(5) 0.445(2) 0.531(1) 0.138(6) Uani d . 1.00 . O1 0.036(1) 0.469(4) 0.080(3) 0.11(2) Uani d . 0.50 . N1 0.3811(5) 0.196(2) 0.108(1) 0.068(6) Uani d . 1.00 . N2 0.3287(5) 0.184(2) 0.2388(10) 0.064(5) Uani d . 1.00 . C1 0.3306(6) 0.231(2) 0.071(1) 0.054(6) Uani d . 1.00 . C2 0.3118(6) 0.281(2) -0.041(1) 0.051(6) Uani d . 1.00 . C3 0.3414(5) 0.342(2) -0.097(1) 0.044(5) Uani d . 1.00 . C4 0.2581(6) 0.256(2) -0.073(1) 0.052(6) Uani d . 1.00 . C5 0.2353(6) 0.232(2) -0.175(1) 0.051(6) Uani d . 1.00 . C6 0.1835(7) 0.203(2) -0.209(1) 0.062(6) Uani d . 1.00 . C7 0.1613(7) 0.167(3) -0.312(1) 0.074(7) Uani d . 1.00 . C8 0.1148(8) 0.142(3) -0.346(2) 0.100(10) Uani d . 1.00 . C9 0.0846(7) 0.141(3) -0.277(1) 0.090(8) Uani d . 1.00 . C10 0.1021(6) 0.167(3) -0.173(1) 0.068(7) Uani d . 1.00 . C11 0.1565(6) 0.200(2) -0.139(1) 0.054(6) Uani d . 1.00 . C12 0.1794(7) 0.226(2) -0.031(1) 0.056(6) Uani d . 1.00 . C13 0.2295(6) 0.253(2) 0.004(1) 0.048(5) Uani d . 1.00 . C14 0.2518(6) 0.268(2) 0.115(1) 0.050(6) Uani d . 1.00 . C15 0.2263(6) 0.324(2) 0.189(1) 0.048(5) Uani d . 1.00 . C16 0.3028(6) 0.224(2) 0.144(1) 0.043(5) Uani d . 1.00 . C17 0.4179(7) 0.471(2) -0.155(1) 0.065(7) Uani d . 1.00 . C18 0.3765(6) 0.500(2) -0.239(1) 0.049(5) Uani d . 1.00 . C19 0.4737(8) 0.662(3) -0.258(2) 0.100(9) Uani d . 1.00 . C20 0.4410(10) 0.587(4) -0.354(2) 0.12(1) Uani d . 1.00 . C21 0.2120(7) 0.438(2) 0.359(1) 0.065(7) Uani d . 1.00 . C22 0.1693(7) 0.479(2) 0.291(1) 0.060(6) Uani d . 1.00 . C23 0.1659(7) 0.516(3) 0.513(1) 0.078(8) Uani d . 1.00 . C24 0.1373(9) 0.639(3) 0.439(1) 0.096(9) Uani d . 1.00 . C25 0.029(2) 0.426(5) -0.012(4) 0.06(1) Uani d . 0.50 . C26 0.000(2) 0.491(6) 0.081(3) 0.08(1) Uani d . 0.50 . H1 0.2550 0.2329 -0.2247 0.0602 Uiso calc . 1.00 . H2 0.1821 0.1588 -0.3593 0.0886 Uiso calc . 1.00 . H3 0.1024 0.1246 -0.4179 0.1234 Uiso calc . 1.00 . H4 0.0507 0.1221 -0.3046 0.1082 Uiso calc . 1.00 . H5 0.0812 0.1639 -0.1268 0.0795 Uiso calc . 1.00 . H6 0.1595 0.2218 0.0172 0.0666 Uiso calc . 1.00 . H7 0.5058 0.6822 -0.2701 0.1194 Uiso calc . 1.00 . H8 0.4605 0.7667 -0.2419 0.1194 Uiso calc . 1.00 . H9 0.4447 0.6505 -0.4136 0.1382 Uiso calc . 1.00 . H10 0.4494 0.4748 -0.3616 0.1382 Uiso calc . 1.00 . H11 0.1691 0.5606 0.5805 0.0921 Uiso calc . 1.00 . H12 0.1476 0.4147 0.5063 0.0921 Uiso calc . 1.00 . H13 0.1089 0.6707 0.4633 0.1138 Uiso calc . 1.00 . H14 0.1574 0.7353 0.4388 0.1138 Uiso calc . 1.00 . H15 0.0618 0.4173 -0.0273 0.0705 Uiso calc . 1.00 . H16 0.0170 0.3063 -0.0198 0.0705 Uiso calc . 1.00 . H17 -0.0193 0.3974 0.0936 0.0818 Uiso calc . 1.00 . H18 0.0019 0.5630 0.1479 0.0818 Uiso calc . 1.00 . 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 S(1) 0.066(3) 0.093(5) 0.061(3) 0.018(3) 0.014(3) 0.022(3) S(2) 0.059(3) 0.061(3) 0.059(3) 0.000(2) 0.021(2) 0.006(2) S(3) 0.062(3) 0.051(3) 0.061(3) 0.004(2) 0.014(2) 0.010(2) S(4) 0.062(3) 0.088(4) 0.074(3) -0.009(3) 0.020(3) 0.018(3) S(5) 0.081(3) 0.058(4) 0.065(3) 0.001(3) 0.024(3) 0.016(3) S(6) 0.059(3) 0.067(4) 0.055(3) 0.000(2) 0.019(2) -0.001(3) S(7) 0.057(3) 0.056(3) 0.056(3) 0.004(2) 0.019(2) 0.005(2) S(8) 0.088(4) 0.105(5) 0.064(3) 0.007(3) 0.029(3) -0.018(3) S(9) 0.078(3) 0.060(4) 0.081(4) 0.014(3) 0.033(3) -0.001(3) P(1) 0.084(6) 0.100(9) 0.083(6) 0.027(6) 0.028(5) -0.010(6) F(1) 0.17(2) 0.09(1) 0.25(2) 0.00(1) 0.06(1) -0.02(1) F(2) 0.14(1) 0.28(2) 0.11(1) 0.06(1) 0.06(1) 0.00(1) F(3) 0.089(9) 0.17(2) 0.16(1) 0.062(10) 0.041(9) 0.03(1) O(1) 0.12(3) 0.06(2) 0.16(4) -0.03(2) 0.07(3) 0.02(2) N(1) 0.08(1) 0.06(1) 0.06(1) 0.017(9) 0.023(9) 0.017(8) N(2) 0.062(9) 0.09(1) 0.042(9) 0.003(9) 0.011(8) 0.011(9) C(1) 0.06(1) 0.04(1) 0.06(1) 0.008(9) 0.009(10) -0.010(9) C(2) 0.05(1) 0.05(1) 0.05(1) 0.007(9) 0.018(9) -0.009(9) C(3) 0.046(9) 0.05(1) 0.040(9) 0.005(8) 0.017(8) 0.007(8) C(4) 0.05(1) 0.03(1) 0.07(1) -0.003(8) 0.01(1) -0.005(9) C(5) 0.05(1) 0.05(1) 0.05(1) 0.002(9) 0.009(9) 0.004(9) C(6) 0.08(1) 0.05(1) 0.05(1) 0.00(1) 0.00(1) 0.010(10) C(7) 0.06(1) 0.09(2) 0.07(1) -0.02(1) 0.01(1) -0.01(1) C(8) 0.09(2) 0.15(3) 0.07(1) -0.02(2) 0.04(1) 0.01(1) C(9) 0.09(1) 0.10(2) 0.06(1) -0.02(1) -0.05(1) 0.01(1) C(10) 0.06(1) 0.07(2) 0.07(1) 0.00(1) 0.002(10) 0.02(1) C(11) 0.05(1) 0.04(1) 0.07(1) -0.008(9) 0.01(1) -0.006(10) C(12) 0.08(1) 0.04(1) 0.05(1) -0.009(9) 0.02(1) 0.004(9) C(13) 0.044(10) 0.06(1) 0.045(10) -0.003(8) 0.011(9) 0.008(9) C(14) 0.05(1) 0.04(1) 0.05(1) 0.001(8) 0.002(9) 0.002(9) C(15) 0.07(1) 0.05(1) 0.032(9) -0.003(9) 0.028(9) -0.001(8) C(16) 0.06(1) 0.04(1) 0.04(1) 0.001(8) 0.027(9) 0.006(8) C(17) 0.08(1) 0.06(1) 0.08(1) 0.00(1) 0.04(1) 0.01(1) C(18) 0.07(1) 0.04(1) 0.05(1) 0.003(9) 0.020(9) 0.006(9) C(19) 0.11(2) 0.08(2) 0.11(2) -0.04(1) 0.03(2) 0.02(1) C(20) 0.15(2) 0.13(3) 0.08(2) -0.03(2) 0.03(2) 0.01(2) C(21) 0.08(1) 0.06(1) 0.06(1) 0.01(1) 0.02(1) -0.02(1) C(22) 0.07(1) 0.05(1) 0.06(1) 0.00(1) 0.03(1) -0.004(10) C(23) 0.08(1) 0.08(2) 0.08(1) 0.00(1) 0.03(1) -0.01(1) C(24) 0.15(2) 0.08(2) 0.07(1) 0.04(2) 0.06(2) 0.01(1) C(25) 0.08(3) 0.07(3) 0.06(2) -0.02(2) 0.05(3) -0.02(3) C(26) 0.03(2) 0.13(3) 0.05(2) -0.06(2) -0.02(2) 0.05(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2030 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0952 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1175 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.344 _refine_ls_shift/esd_max 1.0830 _refine_ls_shift/esd_mean 0.0660 _refine_diff_density_min -0.53 _refine_diff_density_max 0.69 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.65(1) 1_555 1_555 yes S(1) N(2) 1.61(1) 1_555 1_555 yes S(2) C(3) 1.76(1) 1_555 1_555 yes S(2) C(17) 1.73(2) 1_555 1_555 yes S(3) C(3) 1.75(1) 1_555 1_555 yes S(3) C(18) 1.73(1) 1_555 1_555 yes S(4) C(17) 1.72(2) 1_555 1_555 yes S(4) C(19) 1.84(2) 1_555 1_555 yes S(5) C(18) 1.73(2) 1_555 1_555 yes S(5) C(20) 1.81(2) 1_555 1_555 yes S(6) C(15) 1.75(1) 1_555 1_555 yes S(6) C(21) 1.71(2) 1_555 1_555 yes S(7) C(15) 1.72(2) 1_555 1_555 yes S(7) C(22) 1.77(2) 1_555 1_555 yes S(8) C(21) 1.78(2) 1_555 1_555 yes S(8) C(23) 1.73(2) 1_555 1_555 yes S(9) C(22) 1.74(2) 1_555 1_555 yes S(9) C(24) 1.81(2) 1_555 1_555 yes P(1) F(1) 1.54(2) 1_555 1_555 yes P(1) F(1) 1.54(2) 1_555 3_566 yes P(1) F(2) 1.55(1) 1_555 1_555 yes P(1) F(2) 1.55(1) 1_555 3_566 yes P(1) F(3) 1.57(1) 1_555 1_555 yes P(1) F(3) 1.57(1) 1_555 3_566 yes O(1) C(25) 1.25(5) 1_555 1_555 yes O(1) C(26) 1.03(4) 1_555 1_555 yes N(1) C(1) 1.40(2) 1_555 1_555 yes N(2) C(16) 1.34(2) 1_555 1_555 yes C(1) C(2) 1.51(2) 1_555 1_555 yes C(1) C(16) 1.38(2) 1_555 1_555 yes C(2) C(3) 1.33(2) 1_555 1_555 yes C(2) C(4) 1.47(2) 1_555 1_555 yes C(4) C(5) 1.37(2) 1_555 1_555 yes C(4) C(13) 1.44(2) 1_555 1_555 yes C(5) C(6) 1.43(2) 1_555 1_555 yes C(6) C(7) 1.40(2) 1_555 1_555 yes C(6) C(11) 1.33(2) 1_555 1_555 yes C(7) C(8) 1.28(3) 1_555 1_555 yes C(8) C(9) 1.38(2) 1_555 1_555 yes C(9) C(10) 1.38(2) 1_555 1_555 yes C(10) C(11) 1.50(2) 1_555 1_555 yes C(11) C(12) 1.45(2) 1_555 1_555 yes C(12) C(13) 1.38(2) 1_555 1_555 yes C(13) C(14) 1.48(2) 1_555 1_555 yes C(14) C(15) 1.41(2) 1_555 1_555 yes C(14) C(16) 1.43(2) 1_555 1_555 yes C(17) C(18) 1.42(2) 1_555 1_555 yes C(19) C(20) 1.51(3) 1_555 1_555 yes C(21) C(22) 1.36(2) 1_555 1_555 yes C(23) C(24) 1.48(3) 1_555 1_555 yes C(25) C(26) 1.73(5) 1_555 1_555 yes C(25) C(26) 1.26(5) 1_555 3_565 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 N(1) S(1) N(2) 101.3(7) 1_555 1_555 1_555 yes C(3) S(2) C(17) 98.4(8) 1_555 1_555 1_555 yes C(3) S(3) C(18) 98.9(7) 1_555 1_555 1_555 yes C(17) S(4) C(19) 101.7(10) 1_555 1_555 1_555 yes C(18) S(5) C(20) 100.1(9) 1_555 1_555 1_555 yes C(15) S(6) C(21) 95.6(8) 1_555 1_555 1_555 yes C(15) S(7) C(22) 97.6(8) 1_555 1_555 1_555 yes C(21) S(8) C(23) 102.1(9) 1_555 1_555 1_555 yes C(22) S(9) C(24) 97.9(9) 1_555 1_555 1_555 yes F(1) P(1) F(1) 180.0000(1) 1_555 1_555 3_566 yes F(1) P(1) F(2) 88.5(9) 1_555 1_555 1_555 yes F(1) P(1) F(2) 91.5(9) 1_555 1_555 3_566 yes F(1) P(1) F(3) 89.5(8) 1_555 1_555 1_555 yes F(1) P(1) F(3) 90.5(8) 1_555 1_555 3_566 yes F(1) P(1) F(2) 91.5(9) 3_566 1_555 1_555 yes F(1) P(1) F(2) 88.5(9) 3_566 1_555 3_566 yes F(1) P(1) F(3) 90.5(8) 3_566 1_555 1_555 yes F(1) P(1) F(3) 89.5(8) 3_566 1_555 3_566 yes F(2) P(1) F(2) 180.0 1_555 1_555 3_566 yes F(2) P(1) F(3) 92.6(7) 1_555 1_555 1_555 yes F(2) P(1) F(3) 87.4(7) 1_555 1_555 3_566 yes F(2) P(1) F(3) 87.4(7) 3_566 1_555 1_555 yes F(2) P(1) F(3) 92.6(7) 3_566 1_555 3_566 yes F(3) P(1) F(3) 180.0 1_555 1_555 3_566 yes C(25) O(1) C(26) 98(5) 1_555 1_555 1_555 yes S(1) N(1) C(1) 102(1) 1_555 1_555 1_555 yes S(1) N(2) C(16) 107.1(10) 1_555 1_555 1_555 yes N(1) C(1) C(2) 119(1) 1_555 1_555 1_555 yes N(1) C(1) C(16) 114(1) 1_555 1_555 1_555 yes C(2) C(1) C(16) 125(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 122(1) 1_555 1_555 1_555 yes C(1) C(2) C(4) 110(1) 1_555 1_555 1_555 yes C(3) C(2) C(4) 127(1) 1_555 1_555 1_555 yes S(2) C(3) S(3) 111.8(7) 1_555 1_555 1_555 yes S(2) C(3) C(2) 124(1) 1_555 1_555 1_555 yes S(3) C(3) C(2) 124(1) 1_555 1_555 1_555 yes C(2) C(4) C(5) 120(1) 1_555 1_555 1_555 yes C(2) C(4) C(13) 119(1) 1_555 1_555 1_555 yes C(5) C(4) C(13) 119(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 122(1) 1_555 1_555 1_555 yes C(4) C(5) H(1) 118(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 118(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 121(1) 1_555 1_555 1_555 yes C(5) C(6) C(11) 118(1) 1_555 1_555 1_555 yes C(7) C(6) C(11) 119(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 123(1) 1_555 1_555 1_555 yes C(6) C(7) H(2) 117(1) 1_555 1_555 1_555 no C(8) C(7) H(2) 118(2) 1_555 1_555 1_555 no C(7) C(8) C(9) 119(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 118(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 122(2) 1_555 1_555 1_555 no C(8) C(9) C(10) 122(1) 1_555 1_555 1_555 yes C(8) C(9) H(4) 117(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 119(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 114(1) 1_555 1_555 1_555 yes C(9) C(10) H(5) 121(1) 1_555 1_555 1_555 no C(11) C(10) H(5) 123(1) 1_555 1_555 1_555 no C(6) C(11) C(10) 119(1) 1_555 1_555 1_555 yes C(6) C(11) C(12) 120(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 119(1) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122(1) 1_555 1_555 1_555 yes C(11) C(12) H(6) 118(1) 1_555 1_555 1_555 no C(13) C(12) H(6) 119(1) 1_555 1_555 1_555 no C(4) C(13) C(12) 116(1) 1_555 1_555 1_555 yes C(4) C(13) C(14) 122(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 124(1) 1_555 1_555 1_555 yes C(13) C(14) C(16) 113(1) 1_555 1_555 1_555 yes C(15) C(14) C(16) 121(1) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.5(7) 1_555 1_555 1_555 yes S(6) C(15) C(14) 119(1) 1_555 1_555 1_555 yes S(7) C(15) C(14) 126(1) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113(1) 1_555 1_555 1_555 yes N(2) C(16) C(14) 126(1) 1_555 1_555 1_555 yes C(1) C(16) C(14) 119(1) 1_555 1_555 1_555 yes S(2) C(17) S(4) 116(1) 1_555 1_555 1_555 yes S(2) C(17) C(18) 115(1) 1_555 1_555 1_555 yes S(4) C(17) C(18) 127(1) 1_555 1_555 1_555 yes S(3) C(18) S(5) 116.9(10) 1_555 1_555 1_555 yes S(3) C(18) C(17) 115(1) 1_555 1_555 1_555 yes S(5) C(18) C(17) 127(1) 1_555 1_555 1_555 yes S(4) C(19) C(20) 109(1) 1_555 1_555 1_555 yes S(4) C(19) H(7) 109(1) 1_555 1_555 1_555 no S(4) C(19) H(8) 109(1) 1_555 1_555 1_555 no C(20) C(19) H(7) 109(2) 1_555 1_555 1_555 no C(20) C(19) H(8) 110(2) 1_555 1_555 1_555 no H(7) C(19) H(8) 108(2) 1_555 1_555 1_555 no S(5) C(20) C(19) 113(1) 1_555 1_555 1_555 yes S(5) C(20) H(9) 105(1) 1_555 1_555 1_555 no S(5) C(20) H(10) 107(2) 1_555 1_555 1_555 no C(19) C(20) H(9) 109(2) 1_555 1_555 1_555 no C(19) C(20) H(10) 110(2) 1_555 1_555 1_555 no H(9) C(20) H(10) 109(2) 1_555 1_555 1_555 no S(6) C(21) S(8) 114(1) 1_555 1_555 1_555 yes S(6) C(21) C(22) 119(1) 1_555 1_555 1_555 yes S(8) C(21) C(22) 124(1) 1_555 1_555 1_555 yes S(7) C(22) S(9) 115(1) 1_555 1_555 1_555 yes S(7) C(22) C(21) 112(1) 1_555 1_555 1_555 yes S(9) C(22) C(21) 131(1) 1_555 1_555 1_555 yes S(8) C(23) C(24) 114(1) 1_555 1_555 1_555 yes S(8) C(23) H(11) 108(1) 1_555 1_555 1_555 no S(8) C(23) H(12) 109(1) 1_555 1_555 1_555 no C(24) C(23) H(11) 107(1) 1_555 1_555 1_555 no C(24) C(23) H(12) 107(1) 1_555 1_555 1_555 no H(11) C(23) H(12) 109(1) 1_555 1_555 1_555 no S(9) C(24) C(23) 117(1) 1_555 1_555 1_555 yes S(9) C(24) H(13) 106(1) 1_555 1_555 1_555 no S(9) C(24) H(14) 107(1) 1_555 1_555 1_555 no C(23) C(24) H(13) 107(1) 1_555 1_555 1_555 no C(23) C(24) H(14) 107(2) 1_555 1_555 1_555 no H(13) C(24) H(14) 108(2) 1_555 1_555 1_555 no O(1) C(25) C(26) 36(2) 1_555 1_555 1_555 yes O(1) C(25) C(26) 119(4) 1_555 1_555 3_565 yes O(1) C(25) H(15) 106(5) 1_555 1_555 1_555 no O(1) C(25) H(16) 108(3) 1_555 1_555 1_555 no C(26) C(25) C(26) 92(2) 1_555 1_555 3_565 yes C(26) C(25) H(15) 142(4) 1_555 1_555 1_555 no C(26) C(25) H(16) 98(2) 1_555 1_555 1_555 no C(26) C(25) H(15) 110(4) 3_565 1_555 1_555 no C(26) C(25) H(16) 106(4) 3_565 1_555 1_555 no H(15) C(25) H(16) 102(3) 1_555 1_555 1_555 no O(1) C(26) C(25) 45(3) 1_555 1_555 1_555 yes O(1) C(26) C(25) 122(3) 1_555 1_555 3_565 yes O(1) C(26) H(17) 117(6) 1_555 1_555 1_555 no O(1) C(26) H(18) 104(4) 1_555 1_555 1_555 no C(25) C(26) C(25) 87(2) 1_555 1_555 3_565 yes C(25) C(26) H(17) 105(4) 1_555 1_555 1_555 no C(25) C(26) H(18) 146(3) 1_555 1_555 1_555 no C(25) C(26) H(17) 104(3) 3_565 1_555 1_555 no C(25) C(26) H(18) 103(5) 3_565 1_555 1_555 no H(17) C(26) H(18) 102(3) 1_555 1_555 1_555 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 S(2) O(1) 3.56(3) 1_555 2_545 ? S(3) C(15) 3.46(2) 1_555 2_555 ? S(5) C(22) 3.50(2) 1_555 2_555 ? S(6) C(7) 3.57(2) 1_555 2_555 ? S(7) C(2) 3.49(2) 1_555 2_555 ? S(7) C(3) 3.56(2) 1_555 2_555 ? S(9) O(1) 3.39(4) 1_555 1_555 ? S(9) F(2) 3.51(1) 1_555 3_566 ? S(9) C(18) 3.53(2) 1_555 2_555 ? F(1) C(20) 3.51(3) 1_555 2_545 ? F(2) C(19) 3.39(3) 1_555 4_466 ? F(3) C(8) 3.16(3) 1_555 1_556 ? F(3) C(23) 3.19(2) 1_555 1_555 ? F(3) C(24) 3.23(2) 1_555 1_555 ? F(3) C(9) 3.47(2) 1_555 1_556 ? O(1) C(19) 3.46(4) 1_555 2_545 ? N(2) C(23) 3.54(2) 1_555 2_546 ? C(5) C(15) 3.44(2) 1_555 2_545 ? C(19) C(26) 3.48(5) 1_555 2_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(THF),100K #------------------------------------------------------------------------------ _audit_creation_date 'Mon Dec 7 16:41:30 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1454.93 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H36 F6 N4 O P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.665(2) _cell_length_b 7.781(2) _cell_length_c 13.3065(7) _cell_angle_alpha 90 _cell_angle_beta 103.709(5) _cell_angle_gamma 90 _cell_volume 2782.9299 _cell_formula_units_Z 2 _cell_measurement_temperature 100.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1482.00 _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 100.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4667 _reflns_number_total 4667 _reflns_number_observed 3738 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.085 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.11221(7) 0.3544(3) -0.2307(1) 0.0285(5) Uani d . 1.00 . S2 0.24243(6) 0.1906(3) -0.3223(1) 0.0247(5) Uani d . 1.00 . S3 0.33230(7) 0.1034(2) -0.1672(1) 0.0240(5) Uani d . 1.00 . S4 0.27424(7) 0.0445(3) -0.4996(1) 0.0308(6) Uani d . 1.00 . S5 0.38480(7) -0.0611(3) -0.3119(1) 0.0270(5) Uani d . 1.00 . S6 0.09313(6) 0.1490(2) 0.0554(1) 0.0235(5) Uani d . 1.00 . S7 0.17977(7) 0.0848(2) 0.2241(1) 0.0239(5) Uani d . 1.00 . S8 0.02012(7) -0.0102(3) 0.1555(1) 0.0266(5) Uani d . 1.00 . S9 0.12511(7) -0.0831(3) 0.3631(1) 0.0261(5) Uani d . 1.00 . P1 0.0000 0.5000 0.5000 0.0312(8) Uani d . 0.50 S F1 0.0566(2) 0.5604(6) 0.5372(4) 0.047(2) Uani d . 1.00 . F2 0.0052(2) 0.4967(7) 0.3836(3) 0.055(2) Uani d . 1.00 . F3 0.0175(2) 0.3030(6) 0.5129(4) 0.056(2) Uani d . 1.00 . O1 0.0468(3) 0.537(1) 0.0990(5) 0.106(3) Uani d . 1.00 . N1 0.1701(2) 0.3285(8) -0.2381(4) 0.024(2) Uani d . 1.00 . N2 0.1183(2) 0.3127(8) -0.1080(5) 0.028(2) Uani d . 1.00 . C1 0.1963(2) 0.2875(9) -0.1427(5) 0.021(2) Uani d . 1.00 . C2 0.2486(2) 0.2433(9) -0.1159(5) 0.020(2) Uani d . 1.00 . C3 0.2721(2) 0.1885(9) -0.1916(5) 0.023(2) Uani d . 1.00 . C4 0.2724(3) 0.2582(10) -0.0048(5) 0.025(2) Uani d . 1.00 . C5 0.3231(3) 0.2861(9) 0.0308(5) 0.025(2) Uani d . 1.00 . C6 0.3464(3) 0.3117(9) 0.1355(5) 0.021(2) Uani d . 1.00 . C7 0.3988(3) 0.340(1) 0.1695(6) 0.030(2) Uani d . 1.00 . C8 0.4195(3) 0.370(1) 0.2728(6) 0.035(2) Uani d . 1.00 . C9 0.3894(3) 0.375(1) 0.3440(6) 0.032(2) Uani d . 1.00 . C10 0.3392(3) 0.3461(10) 0.3159(5) 0.026(2) Uani d . 1.00 . C11 0.3167(3) 0.3119(9) 0.2088(5) 0.024(2) Uani d . 1.00 . C12 0.2651(3) 0.2843(9) 0.1745(5) 0.023(2) Uani d . 1.00 . C13 0.2420(3) 0.2555(9) 0.0716(5) 0.022(2) Uani d . 1.00 . C14 0.1876(3) 0.2335(9) 0.0390(5) 0.024(2) Uani d . 1.00 . C15 0.1575(3) 0.1669(9) 0.0999(5) 0.024(2) Uani d . 1.00 . C16 0.1665(3) 0.2791(9) -0.0679(5) 0.023(2) Uani d . 1.00 . C17 0.2881(3) 0.0807(10) -0.3655(6) 0.026(2) Uani d . 1.00 . C18 0.3302(3) 0.0361(10) -0.2949(5) 0.025(2) Uani d . 1.00 . C19 0.3355(3) 0.0020(10) -0.5171(5) 0.028(2) Uani d . 1.00 . C20 0.3630(3) -0.1350(10) -0.4437(6) 0.030(2) Uani d . 1.00 . C21 0.0829(2) 0.0390(9) 0.1646(5) 0.021(2) Uani d . 1.00 . C22 0.1225(3) 0.0112(9) 0.2414(5) 0.023(2) Uani d . 1.00 . C23 0.0271(3) -0.159(1) 0.2633(5) 0.030(2) Uani d . 1.00 . C24 0.0595(3) -0.087(1) 0.3618(6) 0.032(2) Uani d . 1.00 . C25 0.0355(4) 0.593(1) -0.0018(6) 0.064(3) Uani d . 1.00 . C26 -0.0038(3) 0.496(1) 0.0892(7) 0.046(3) Uani d . 1.00 . H1 0.3439 0.2916 -0.0186 0.0221 Uiso calc . 1.00 . H2 0.4207 0.3368 0.1222 0.0327 Uiso calc . 1.00 . H3 0.4554 0.3878 0.2987 0.0320 Uiso calc . 1.00 . H4 0.4045 0.4046 0.4163 0.0336 Uiso calc . 1.00 . H5 0.3207 0.3457 0.3696 0.0238 Uiso calc . 1.00 . H6 0.2448 0.2850 0.2250 0.0194 Uiso calc . 1.00 . H7 0.3340 -0.0259 -0.5879 0.0244 Uiso calc . 1.00 . H8 0.3556 0.1079 -0.5027 0.0244 Uiso calc . 1.00 . H9 0.3897 -0.1788 -0.4719 0.0307 Uiso calc . 1.00 . H10 0.3393 -0.2297 -0.4484 0.0307 Uiso calc . 1.00 . H11 -0.0058 -0.1892 0.2732 0.0298 Uiso calc . 1.00 . H12 0.0414 -0.2658 0.2465 0.0298 Uiso calc . 1.00 . H13 0.0540 -0.1525 0.4193 0.0343 Uiso calc . 1.00 . H14 0.0478 0.0283 0.3688 0.0343 Uiso calc . 1.00 . H15 0.0671 0.6126 -0.0156 0.0677 Uiso calc . 1.00 . H16 0.0201 0.7038 0.0029 0.0677 Uiso calc . 1.00 . H17 -0.0047 0.4303 0.1514 0.0506 Uiso calc . 1.00 . H18 -0.0196 0.6051 0.0969 0.0506 Uiso calc . 1.00 . 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 S(1) 0.0199(9) 0.044(1) 0.0240(9) 0.0038(9) 0.0096(8) 0.0041(9) S(2) 0.0212(9) 0.034(1) 0.0224(9) 0.0030(8) 0.0117(8) 0.0011(8) S(3) 0.0196(9) 0.031(1) 0.0252(9) 0.0015(8) 0.0123(8) 0.0017(8) S(4) 0.0251(10) 0.046(1) 0.0245(10) 0.0014(9) 0.0117(9) -0.0051(9) S(5) 0.0234(10) 0.030(1) 0.032(1) 0.0017(8) 0.0159(9) 0.0003(9) S(6) 0.0174(9) 0.033(1) 0.0223(9) -0.0008(8) 0.0098(8) 0.0003(8) S(7) 0.0196(9) 0.031(1) 0.0237(9) -0.0008(8) 0.0109(8) 0.0015(8) S(8) 0.0191(9) 0.036(1) 0.0284(10) -0.0005(8) 0.0124(8) 0.0041(9) S(9) 0.0239(10) 0.030(1) 0.0268(10) -0.0006(8) 0.0118(9) 0.0034(8) P(1) 0.026(1) 0.037(2) 0.035(2) -0.005(1) 0.017(1) 0.001(1) F(1) 0.023(2) 0.060(3) 0.059(3) -0.010(2) 0.015(2) -0.006(3) F(2) 0.048(3) 0.088(4) 0.033(3) -0.008(3) 0.021(2) 0.002(3) F(3) 0.050(3) 0.038(3) 0.090(4) 0.005(2) 0.034(3) 0.013(3) O(1) 0.081(4) 0.130(6) 0.111(5) -0.001(4) 0.029(4) -0.006(4) N(1) 0.022(3) 0.035(4) 0.018(3) 0.007(3) 0.009(3) 0.007(3) N(2) 0.020(3) 0.035(4) 0.032(3) 0.006(3) 0.012(3) 0.003(3) C(1) 0.017(4) 0.022(4) 0.026(4) 0.003(3) 0.009(3) 0.001(3) C(2) 0.018(4) 0.025(4) 0.019(3) -0.005(3) 0.008(3) 0.000(3) C(3) 0.019(4) 0.028(4) 0.025(4) -0.008(3) 0.010(3) -0.004(3) C(4) 0.029(4) 0.020(4) 0.033(4) -0.002(3) 0.025(4) 0.001(3) C(5) 0.025(4) 0.027(4) 0.030(4) -0.001(3) 0.018(3) -0.001(3) C(6) 0.020(4) 0.025(4) 0.020(4) 0.000(3) 0.006(3) 0.006(3) C(7) 0.024(4) 0.034(5) 0.035(4) -0.003(4) 0.015(4) 0.006(4) C(8) 0.027(4) 0.047(6) 0.031(4) -0.010(4) 0.008(4) -0.002(4) C(9) 0.027(4) 0.048(5) 0.023(4) -0.005(4) 0.007(3) 0.000(4) C(10) 0.026(4) 0.032(5) 0.020(4) 0.002(3) 0.006(3) 0.001(3) C(11) 0.021(4) 0.027(4) 0.029(4) 0.001(3) 0.015(3) 0.004(3) C(12) 0.024(4) 0.024(4) 0.024(4) -0.002(3) 0.011(3) 0.002(3) C(13) 0.022(4) 0.024(4) 0.027(4) 0.000(3) 0.017(3) 0.004(3) C(14) 0.023(4) 0.021(4) 0.033(4) 0.002(3) 0.015(3) -0.002(3) C(15) 0.022(4) 0.026(4) 0.029(4) 0.003(3) 0.017(3) 0.002(3) C(16) 0.026(4) 0.026(4) 0.022(4) -0.001(3) 0.017(3) 0.001(3) C(17) 0.026(4) 0.026(4) 0.032(4) -0.004(3) 0.019(4) -0.003(3) C(18) 0.024(4) 0.025(4) 0.030(4) -0.002(3) 0.015(3) 0.001(3) C(19) 0.028(4) 0.033(5) 0.029(4) 0.005(4) 0.015(3) 0.000(4) C(20) 0.032(4) 0.029(5) 0.034(4) -0.001(4) 0.019(4) -0.002(4) C(21) 0.021(4) 0.024(4) 0.021(4) 0.002(3) 0.009(3) 0.000(3) C(22) 0.024(4) 0.028(4) 0.020(3) 0.002(3) 0.010(3) -0.001(3) C(23) 0.028(4) 0.041(5) 0.022(4) -0.009(4) 0.008(3) -0.001(4) C(24) 0.039(5) 0.032(5) 0.034(4) -0.004(4) 0.027(4) 0.000(4) C(25) 0.116(10) 0.052(7) 0.027(4) 0.020(6) 0.022(5) -0.004(4) C(26) 0.020(4) 0.044(6) 0.077(6) -0.011(4) 0.019(4) -0.015(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00014|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.023(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3738 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0752 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0929 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.812 _refine_ls_shift/esd_max 7.8558 _refine_ls_shift/esd_mean 0.2766 _refine_diff_density_min -0.96 _refine_diff_density_max 0.63 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.640(6) 1_555 1_555 yes S(1) N(2) 1.633(6) 1_555 1_555 yes S(2) C(3) 1.738(7) 1_555 1_555 yes S(2) C(17) 1.734(7) 1_555 1_555 yes S(3) C(3) 1.750(7) 1_555 1_555 yes S(3) C(18) 1.766(7) 1_555 1_555 yes S(4) C(17) 1.756(7) 1_555 1_555 yes S(4) C(19) 1.796(7) 1_555 1_555 yes S(5) C(18) 1.751(7) 1_555 1_555 yes S(5) C(20) 1.808(7) 1_555 1_555 yes S(6) C(15) 1.744(7) 1_555 1_555 yes S(6) C(21) 1.766(7) 1_555 1_555 yes S(7) C(15) 1.743(7) 1_555 1_555 yes S(7) C(22) 1.750(7) 1_555 1_555 yes S(8) C(21) 1.756(7) 1_555 1_555 yes S(8) C(23) 1.815(7) 1_555 1_555 yes S(9) C(22) 1.764(7) 1_555 1_555 yes S(9) C(24) 1.810(8) 1_555 1_555 yes P(1) F(1) 1.598(4) 1_555 1_555 yes P(1) F(1) 1.598(4) 1_555 3_566 yes P(1) F(2) 1.589(4) 1_555 1_555 yes P(1) F(2) 1.589(4) 1_555 3_566 yes P(1) F(3) 1.604(5) 1_555 1_555 yes P(1) F(3) 1.604(5) 1_555 3_566 yes O(1) C(25) 1.375(10) 1_555 1_555 yes O(1) C(26) 1.410(9) 1_555 1_555 yes N(1) C(1) 1.342(8) 1_555 1_555 yes N(2) C(16) 1.340(8) 1_555 1_555 yes C(1) C(2) 1.449(9) 1_555 1_555 yes C(1) C(16) 1.435(9) 1_555 1_555 yes C(2) C(3) 1.389(9) 1_555 1_555 yes C(2) C(4) 1.473(9) 1_555 1_555 yes C(4) C(5) 1.387(9) 1_555 1_555 yes C(4) C(13) 1.467(9) 1_555 1_555 yes C(5) C(6) 1.404(9) 1_555 1_555 yes C(6) C(7) 1.430(9) 1_555 1_555 yes C(6) C(11) 1.415(9) 1_555 1_555 yes C(7) C(8) 1.378(10) 1_555 1_555 yes C(8) C(9) 1.402(10) 1_555 1_555 yes C(9) C(10) 1.370(10) 1_555 1_555 yes C(10) C(11) 1.438(9) 1_555 1_555 yes C(11) C(12) 1.410(9) 1_555 1_555 yes C(12) C(13) 1.386(9) 1_555 1_555 yes C(13) C(14) 1.473(9) 1_555 1_555 yes C(14) C(15) 1.393(9) 1_555 1_555 yes C(14) C(16) 1.447(9) 1_555 1_555 yes C(17) C(18) 1.356(10) 1_555 1_555 yes C(19) C(20) 1.52(1) 1_555 1_555 yes C(21) C(22) 1.326(9) 1_555 1_555 yes C(23) C(24) 1.51(1) 1_555 1_555 yes C(25) C(26) 1.46(1) 1_555 3_565 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 N(1) S(1) N(2) 99.5(3) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.8(3) 1_555 1_555 1_555 yes C(3) S(3) C(18) 97.0(3) 1_555 1_555 1_555 yes C(17) S(4) C(19) 100.1(3) 1_555 1_555 1_555 yes C(18) S(5) C(20) 99.4(3) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.2(3) 1_555 1_555 1_555 yes C(15) S(7) C(22) 96.7(3) 1_555 1_555 1_555 yes C(21) S(8) C(23) 99.5(3) 1_555 1_555 1_555 yes C(22) S(9) C(24) 100.2(3) 1_555 1_555 1_555 yes F(1) P(1) F(1) 180.0 1_555 1_555 3_566 yes F(1) P(1) F(2) 89.9(2) 1_555 1_555 1_555 yes F(1) P(1) F(2) 90.1(2) 1_555 1_555 3_566 yes F(1) P(1) F(3) 90.0(3) 1_555 1_555 1_555 yes F(1) P(1) F(3) 90.0(3) 1_555 1_555 3_566 yes F(1) P(1) F(2) 90.1(2) 3_566 1_555 1_555 yes F(1) P(1) F(2) 89.9(2) 3_566 1_555 3_566 yes F(1) P(1) F(3) 90.0(3) 3_566 1_555 1_555 yes F(1) P(1) F(3) 90.0(3) 3_566 1_555 3_566 yes F(2) P(1) F(2) 180.0 1_555 1_555 3_566 yes F(2) P(1) F(3) 89.7(3) 1_555 1_555 1_555 yes F(2) P(1) F(3) 90.3(3) 1_555 1_555 3_566 yes F(2) P(1) F(3) 90.3(3) 3_566 1_555 1_555 yes F(2) P(1) F(3) 89.7(3) 3_566 1_555 3_566 yes F(3) P(1) F(3) 180.0 1_555 1_555 3_566 yes C(25) O(1) C(26) 89.4(7) 1_555 1_555 1_555 yes S(1) N(1) C(1) 106.7(4) 1_555 1_555 1_555 yes S(1) N(2) C(16) 107.1(4) 1_555 1_555 1_555 yes N(1) C(1) C(2) 125.0(6) 1_555 1_555 1_555 yes N(1) C(1) C(16) 113.4(6) 1_555 1_555 1_555 yes C(2) C(1) C(16) 121.5(6) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.4(6) 1_555 1_555 1_555 yes C(1) C(2) C(4) 114.3(6) 1_555 1_555 1_555 yes C(3) C(2) C(4) 125.2(6) 1_555 1_555 1_555 yes S(2) C(3) S(3) 113.1(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 122.1(5) 1_555 1_555 1_555 yes S(3) C(3) C(2) 124.8(5) 1_555 1_555 1_555 yes C(2) C(4) C(5) 122.1(6) 1_555 1_555 1_555 yes C(2) C(4) C(13) 120.0(6) 1_555 1_555 1_555 yes C(5) C(4) C(13) 117.8(6) 1_555 1_555 1_555 yes C(4) C(5) C(6) 123.4(6) 1_555 1_555 1_555 yes C(4) C(5) H(1) 119.3(7) 1_555 1_555 1_555 no C(6) C(5) H(1) 117.3(7) 1_555 1_555 1_555 no C(5) C(6) C(7) 121.9(6) 1_555 1_555 1_555 yes C(5) C(6) C(11) 118.7(6) 1_555 1_555 1_555 yes C(7) C(6) C(11) 119.5(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.4(6) 1_555 1_555 1_555 yes C(6) C(7) H(2) 122.2(7) 1_555 1_555 1_555 no C(8) C(7) H(2) 118.4(7) 1_555 1_555 1_555 no C(7) C(8) C(9) 120.5(7) 1_555 1_555 1_555 yes C(7) C(8) H(3) 121.3(7) 1_555 1_555 1_555 no C(9) C(8) H(3) 118.2(7) 1_555 1_555 1_555 no C(8) C(9) C(10) 122.4(7) 1_555 1_555 1_555 yes C(8) C(9) H(4) 119.1(7) 1_555 1_555 1_555 no C(10) C(9) H(4) 118.4(7) 1_555 1_555 1_555 no C(9) C(10) C(11) 118.2(6) 1_555 1_555 1_555 yes C(9) C(10) H(5) 118.4(6) 1_555 1_555 1_555 no C(11) C(10) H(5) 123.4(7) 1_555 1_555 1_555 no C(6) C(11) C(10) 119.9(6) 1_555 1_555 1_555 yes C(6) C(11) C(12) 119.1(6) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.0(6) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122.6(6) 1_555 1_555 1_555 yes C(11) C(12) H(6) 118.9(6) 1_555 1_555 1_555 no C(13) C(12) H(6) 118.5(6) 1_555 1_555 1_555 no C(4) C(13) C(12) 118.5(6) 1_555 1_555 1_555 yes C(4) C(13) C(14) 120.8(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120.6(6) 1_555 1_555 1_555 yes C(13) C(14) C(15) 125.6(6) 1_555 1_555 1_555 yes C(13) C(14) C(16) 114.0(6) 1_555 1_555 1_555 yes C(15) C(14) C(16) 120.4(6) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.3(4) 1_555 1_555 1_555 yes S(6) C(15) C(14) 122.4(5) 1_555 1_555 1_555 yes S(7) C(15) C(14) 124.2(5) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113.2(6) 1_555 1_555 1_555 yes N(2) C(16) C(14) 124.8(6) 1_555 1_555 1_555 yes C(1) C(16) C(14) 121.9(6) 1_555 1_555 1_555 yes S(2) C(17) S(4) 114.5(4) 1_555 1_555 1_555 yes S(2) C(17) C(18) 118.0(5) 1_555 1_555 1_555 yes S(4) C(17) C(18) 127.4(6) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.8(4) 1_555 1_555 1_555 yes S(3) C(18) C(17) 114.7(5) 1_555 1_555 1_555 yes S(5) C(18) C(17) 130.3(6) 1_555 1_555 1_555 yes S(4) C(19) C(20) 112.9(5) 1_555 1_555 1_555 yes S(4) C(19) H(7) 110.3(5) 1_555 1_555 1_555 no S(4) C(19) H(8) 109.0(5) 1_555 1_555 1_555 no C(20) C(19) H(7) 111.8(7) 1_555 1_555 1_555 no C(20) C(19) H(8) 106.7(6) 1_555 1_555 1_555 no H(7) C(19) H(8) 105.8(7) 1_555 1_555 1_555 no S(5) C(20) C(19) 113.7(5) 1_555 1_555 1_555 yes S(5) C(20) H(9) 112.3(6) 1_555 1_555 1_555 no S(5) C(20) H(10) 111.4(5) 1_555 1_555 1_555 no C(19) C(20) H(9) 108.0(6) 1_555 1_555 1_555 no C(19) C(20) H(10) 105.2(6) 1_555 1_555 1_555 no H(9) C(20) H(10) 105.7(7) 1_555 1_555 1_555 no S(6) C(21) S(8) 113.4(4) 1_555 1_555 1_555 yes S(6) C(21) C(22) 116.7(5) 1_555 1_555 1_555 yes S(8) C(21) C(22) 129.8(5) 1_555 1_555 1_555 yes S(7) C(22) S(9) 114.6(4) 1_555 1_555 1_555 yes S(7) C(22) C(21) 116.9(5) 1_555 1_555 1_555 yes S(9) C(22) C(21) 128.4(6) 1_555 1_555 1_555 yes S(8) C(23) C(24) 112.6(5) 1_555 1_555 1_555 yes S(8) C(23) H(11) 109.4(6) 1_555 1_555 1_555 no S(8) C(23) H(12) 109.7(5) 1_555 1_555 1_555 no C(24) C(23) H(11) 110.6(6) 1_555 1_555 1_555 no C(24) C(23) H(12) 109.0(7) 1_555 1_555 1_555 no H(11) C(23) H(12) 105.3(7) 1_555 1_555 1_555 no S(9) C(24) C(23) 113.7(5) 1_555 1_555 1_555 yes S(9) C(24) H(13) 110.5(6) 1_555 1_555 1_555 no S(9) C(24) H(14) 109.9(6) 1_555 1_555 1_555 no C(23) C(24) H(13) 108.9(7) 1_555 1_555 1_555 no C(23) C(24) H(14) 106.3(7) 1_555 1_555 1_555 no H(13) C(24) H(14) 107.2(7) 1_555 1_555 1_555 no O(1) C(25) C(26) 125.5(9) 1_555 1_555 3_565 yes O(1) C(25) H(15) 103.5(9) 1_555 1_555 1_555 no O(1) C(25) H(16) 102.8(7) 1_555 1_555 1_555 no C(26) C(25) H(15) 109.2(8) 3_565 1_555 1_555 no C(26) C(25) H(16) 106.7(9) 3_565 1_555 1_555 no H(15) C(25) H(16) 108(1) 1_555 1_555 1_555 no O(1) C(26) C(25) 125.2(9) 1_555 1_555 3_565 yes O(1) C(26) H(17) 105.2(8) 1_555 1_555 1_555 no O(1) C(26) H(18) 105.0(7) 1_555 1_555 1_555 no C(25) C(26) H(17) 107.0(8) 3_565 1_555 1_555 no C(25) C(26) H(18) 107.5(8) 3_565 1_555 1_555 no H(17) C(26) H(18) 105.5(8) 1_555 1_555 1_555 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 S(5) O(1) 3.106(7) 1_555 2_545 ? F(1) C(19) 3.092(8) 1_555 2_555 ? F(1) C(9) 3.101(9) 1_555 2_556 ? F(1) C(20) 3.181(8) 1_555 2_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2PF6(THF),297K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 15:26:48 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1452.91 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H34 F6 N4 O P S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.972(3) _cell_length_b 7.934(2) _cell_length_c 13.366(1) _cell_angle_alpha 90 _cell_angle_beta 102.931(8) _cell_angle_gamma 90 _cell_volume 2891.1299 _cell_formula_units_Z 2 _cell_measurement_temperature 297.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1478.00 _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 297.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4194 _reflns_number_total 4194 _reflns_number_observed 2612 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.141 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 68 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags S1 0.1145(1) 0.1593(5) 0.2709(2) 0.060(1) Uani d . 1.00 . S2 0.2429(1) 0.3221(4) 0.1801(2) 0.0469(9) Uani d . 1.00 . S3 0.3316(1) 0.4066(4) 0.3338(2) 0.0441(9) Uani d . 1.00 . S4 0.2749(1) 0.4710(6) 0.0051(2) 0.069(1) Uani d . 1.00 . S5 0.3839(1) 0.5698(5) 0.1907(2) 0.057(1) Uani d . 1.00 . S6 0.0941(1) 0.3605(5) 0.5553(2) 0.0463(9) Uani d . 1.00 . S7 0.1791(1) 0.4278(4) 0.7225(2) 0.0442(9) Uani d . 1.00 . S8 0.0214(1) 0.5125(5) 0.6557(2) 0.060(1) Uani d . 1.00 . S9 0.1240(1) 0.5890(5) 0.8607(2) 0.055(1) Uani d . 1.00 . P1 0.0000 0.0000 0.0000 0.070(2) Uani d . 0.50 S F1 0.0171(5) 0.190(2) 0.015(1) 0.175(6) Uani d . 1.00 . F2 0.0559(3) -0.055(2) 0.0331(8) 0.128(4) Uani d . 1.00 . F3 -0.0046(4) -0.006(2) 0.1141(7) 0.149(5) Uani d . 1.00 . O1 0.0473(8) -0.035(3) 0.597(2) 0.100(9) Uani d . 0.50 . N1 0.1711(3) 0.183(1) 0.2650(6) 0.054(3) Uani d . 1.00 . N2 0.1196(3) 0.200(1) 0.3928(6) 0.046(3) Uani d . 1.00 . C1 0.1973(4) 0.226(1) 0.3593(7) 0.036(3) Uani d . 1.00 . C2 0.2485(4) 0.265(1) 0.3861(8) 0.037(3) Uani d . 1.00 . C3 0.2723(3) 0.324(2) 0.3106(7) 0.037(3) Uani d . 1.00 . C4 0.2709(3) 0.253(1) 0.4956(7) 0.035(3) Uani d . 1.00 . C5 0.3226(4) 0.224(1) 0.5302(8) 0.042(4) Uani d . 1.00 . C6 0.3442(4) 0.199(2) 0.6363(8) 0.044(4) Uani d . 1.00 . C7 0.3970(4) 0.174(2) 0.6670(8) 0.051(4) Uani d . 1.00 . C8 0.4169(5) 0.144(2) 0.771(1) 0.081(5) Uani d . 1.00 . C9 0.3863(4) 0.139(2) 0.8448(9) 0.072(5) Uani d . 1.00 . C10 0.3381(5) 0.168(2) 0.8148(9) 0.060(4) Uani d . 1.00 . C11 0.3157(4) 0.202(2) 0.7086(8) 0.042(4) Uani d . 1.00 . C12 0.2638(4) 0.231(2) 0.6744(8) 0.041(3) Uani d . 1.00 . C13 0.2415(4) 0.258(1) 0.5713(8) 0.039(3) Uani d . 1.00 . C14 0.1876(4) 0.282(1) 0.5393(7) 0.038(3) Uani d . 1.00 . C15 0.1585(4) 0.342(1) 0.5977(7) 0.034(3) Uani d . 1.00 . C16 0.1667(4) 0.234(1) 0.4330(8) 0.040(3) Uani d . 1.00 . C17 0.2893(4) 0.432(2) 0.1356(9) 0.050(4) Uani d . 1.00 . C18 0.3301(4) 0.473(2) 0.2083(8) 0.048(4) Uani d . 1.00 . C19 0.3361(4) 0.515(2) -0.0153(9) 0.066(5) Uani d . 1.00 . C20 0.3645(5) 0.646(2) 0.0580(9) 0.067(5) Uani d . 1.00 . C21 0.0842(4) 0.467(2) 0.6604(8) 0.044(4) Uani d . 1.00 . C22 0.1240(4) 0.498(2) 0.7390(8) 0.041(3) Uani d . 1.00 . C23 0.0288(5) 0.655(2) 0.761(1) 0.073(5) Uani d . 1.00 . C24 0.0617(5) 0.589(2) 0.857(1) 0.080(6) Uani d . 1.00 . C25 -0.0046(5) 0.010(3) 0.590(1) 0.096(7) Uani d . 1.00 . C26 0.0380(7) -0.082(2) 0.499(1) 0.098(7) Uani d . 1.00 . H1 0.3427 0.2214 0.4816 0.0511 Uiso calc . 1.00 . H2 0.4174 0.1792 0.6193 0.0615 Uiso calc . 1.00 . H3 0.4512 0.1241 0.7939 0.0956 Uiso calc . 1.00 . H4 0.4007 0.1188 0.9154 0.0902 Uiso calc . 1.00 . H5 0.3182 0.1664 0.8640 0.0730 Uiso calc . 1.00 . H6 0.2440 0.2315 0.7239 0.0478 Uiso calc . 1.00 . H7 0.3541 0.4118 -0.0078 0.0768 Uiso calc . 1.00 . H8 0.3326 0.5544 -0.0841 0.0768 Uiso calc . 1.00 . H9 0.3444 0.7408 0.0570 0.0790 Uiso calc . 1.00 . H10 0.3931 0.6745 0.0343 0.0790 Uiso calc . 1.00 . H11 0.0419 0.7556 0.7418 0.0898 Uiso calc . 1.00 . H12 -0.0028 0.6743 0.7738 0.0898 Uiso calc . 1.00 . H13 0.0520 0.4772 0.8677 0.0933 Uiso calc . 1.00 . H14 0.0564 0.6586 0.9122 0.0933 Uiso calc . 1.00 . H15 -0.0208 -0.0932 0.6037 0.1022 Uiso calc . 1.00 . H16 -0.0043 0.0834 0.6482 0.1022 Uiso calc . 1.00 . H17 0.0705 -0.0915 0.4814 0.1167 Uiso calc . 1.00 . H18 0.0278 -0.2030 0.4997 0.1167 Uiso calc . 1.00 . 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 S(1) 0.045(2) 0.087(3) 0.049(2) -0.013(2) 0.008(1) -0.016(2) S(2) 0.044(2) 0.059(2) 0.040(2) -0.004(2) 0.015(1) -0.002(1) S(3) 0.043(2) 0.049(2) 0.043(2) -0.003(2) 0.016(1) -0.003(1) S(4) 0.065(2) 0.093(4) 0.051(2) -0.005(2) 0.018(2) 0.016(2) S(5) 0.059(2) 0.053(3) 0.065(2) -0.011(2) 0.030(2) -0.002(2) S(6) 0.037(1) 0.060(3) 0.045(2) -0.002(2) 0.015(1) -0.006(2) S(7) 0.041(2) 0.047(2) 0.044(2) -0.004(1) 0.007(1) -0.008(1) S(8) 0.041(2) 0.080(3) 0.063(2) 0.003(2) 0.020(2) -0.015(2) S(9) 0.062(2) 0.054(3) 0.051(2) 0.002(2) 0.016(2) -0.012(2) P(1) 0.058(3) 0.087(5) 0.070(3) 0.023(3) 0.024(3) -0.002(3) F(1) 0.17(1) 0.078(10) 0.29(2) -0.008(9) 0.09(1) -0.03(1) F(2) 0.070(6) 0.16(1) 0.168(9) 0.043(7) 0.055(6) 0.046(8) F(3) 0.128(8) 0.26(2) 0.080(6) 0.055(9) 0.066(6) 0.021(8) O(1) 0.11(2) 0.08(2) 0.09(2) -0.01(2) -0.01(1) 0.00(1) N(1) 0.048(6) 0.085(10) 0.033(5) -0.010(6) 0.015(5) -0.009(5) N(2) 0.032(5) 0.065(9) 0.042(5) -0.007(5) 0.012(4) -0.012(5) C(1) 0.032(6) 0.050(9) 0.033(6) -0.002(5) 0.019(5) -0.001(5) C(2) 0.054(7) 0.021(7) 0.037(5) 0.002(5) 0.009(5) 0.001(5) C(3) 0.035(6) 0.048(8) 0.037(6) 0.004(6) 0.025(5) -0.003(5) C(4) 0.027(5) 0.041(8) 0.040(6) -0.001(5) 0.015(5) -0.001(5) C(5) 0.054(7) 0.035(8) 0.040(6) -0.001(6) 0.014(6) 0.004(6) C(6) 0.038(6) 0.038(9) 0.049(7) 0.013(6) -0.003(5) -0.006(6) C(7) 0.038(6) 0.07(1) 0.049(7) 0.000(6) 0.011(6) -0.009(7) C(8) 0.076(10) 0.08(1) 0.066(9) 0.017(9) -0.032(8) -0.006(9) C(9) 0.047(7) 0.13(2) 0.039(7) 0.011(9) 0.014(6) -0.015(8) C(10) 0.059(8) 0.07(1) 0.041(7) -0.007(8) -0.003(6) -0.002(7) C(11) 0.036(6) 0.053(10) 0.038(6) -0.003(6) 0.012(5) 0.000(6) C(12) 0.050(7) 0.036(8) 0.034(6) -0.004(6) 0.004(5) 0.001(5) C(13) 0.047(6) 0.025(7) 0.044(6) 0.001(5) 0.010(6) -0.001(5) C(14) 0.039(6) 0.046(9) 0.038(6) -0.008(5) 0.025(5) 0.005(5) C(15) 0.042(6) 0.031(7) 0.029(5) -0.007(5) 0.006(5) 0.000(5) C(16) 0.054(7) 0.025(8) 0.039(6) -0.008(6) 0.006(6) 0.007(5) C(17) 0.046(7) 0.060(10) 0.055(7) -0.001(7) 0.037(6) 0.002(6) C(18) 0.053(7) 0.056(10) 0.050(7) -0.010(7) 0.042(6) -0.007(6) C(19) 0.055(7) 0.09(1) 0.063(8) 0.014(8) 0.040(7) 0.025(8) C(20) 0.10(1) 0.06(1) 0.058(8) -0.009(9) 0.057(8) -0.002(7) C(21) 0.051(7) 0.034(9) 0.050(6) 0.006(6) 0.019(6) 0.008(6) C(22) 0.045(6) 0.041(9) 0.041(6) -0.001(6) 0.017(5) -0.004(6) C(23) 0.057(8) 0.09(1) 0.077(9) 0.018(8) 0.016(7) -0.023(9) C(24) 0.071(9) 0.10(1) 0.076(10) 0.028(9) 0.020(8) -0.018(9) C(25) 0.054(9) 0.15(2) 0.09(1) 0.01(1) 0.011(9) 0.02(1) C(26) 0.11(1) 0.09(2) 0.10(1) -0.02(1) 0.03(1) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0007(9) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2612 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0783 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1031 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.132 _refine_ls_shift/esd_max 0.0300 _refine_ls_shift/esd_mean 0.0030 _refine_diff_density_min -0.49 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _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 S(1) N(1) 1.613(9) 1_555 1_555 yes S(1) N(2) 1.636(9) 1_555 1_555 yes S(2) C(3) 1.75(1) 1_555 1_555 yes S(2) C(17) 1.77(1) 1_555 1_555 yes S(3) C(3) 1.74(1) 1_555 1_555 yes S(3) C(18) 1.75(1) 1_555 1_555 yes S(4) C(17) 1.73(1) 1_555 1_555 yes S(4) C(19) 1.83(1) 1_555 1_555 yes S(5) C(18) 1.75(1) 1_555 1_555 yes S(5) C(20) 1.84(1) 1_555 1_555 yes S(6) C(15) 1.77(1) 1_555 1_555 yes S(6) C(21) 1.71(1) 1_555 1_555 yes S(7) C(15) 1.773(10) 1_555 1_555 yes S(7) C(22) 1.70(1) 1_555 1_555 yes S(8) C(21) 1.78(1) 1_555 1_555 yes S(8) C(23) 1.78(1) 1_555 1_555 yes S(9) C(22) 1.78(1) 1_555 1_555 yes S(9) C(24) 1.73(1) 1_555 1_555 yes P(1) F(1) 1.58(1) 1_555 1_555 yes P(1) F(1) 1.58(1) 1_555 3_555 yes P(1) F(2) 1.588(8) 1_555 1_555 yes P(1) F(2) 1.588(8) 1_555 3_555 yes P(1) F(3) 1.560(8) 1_555 1_555 yes P(1) F(3) 1.560(8) 1_555 3_555 yes O(1) C(25) 1.48(2) 1_555 1_555 yes O(1) C(26) 1.33(2) 1_555 1_555 yes N(1) C(1) 1.35(1) 1_555 1_555 yes N(2) C(16) 1.33(1) 1_555 1_555 yes C(1) C(2) 1.43(1) 1_555 1_555 yes C(1) C(16) 1.44(1) 1_555 1_555 yes C(2) C(3) 1.41(1) 1_555 1_555 yes C(2) C(4) 1.46(1) 1_555 1_555 yes C(4) C(5) 1.43(1) 1_555 1_555 yes C(4) C(13) 1.44(1) 1_555 1_555 yes C(5) C(6) 1.42(1) 1_555 1_555 yes C(6) C(7) 1.45(1) 1_555 1_555 yes C(6) C(11) 1.38(1) 1_555 1_555 yes C(7) C(8) 1.40(2) 1_555 1_555 yes C(8) C(9) 1.45(2) 1_555 1_555 yes C(9) C(10) 1.34(2) 1_555 1_555 yes C(10) C(11) 1.44(1) 1_555 1_555 yes C(11) C(12) 1.44(1) 1_555 1_555 yes C(12) C(13) 1.40(1) 1_555 1_555 yes C(13) C(14) 1.48(1) 1_555 1_555 yes C(14) C(15) 1.34(1) 1_555 1_555 yes C(14) C(16) 1.46(1) 1_555 1_555 yes C(17) C(18) 1.36(2) 1_555 1_555 yes C(19) C(20) 1.53(2) 1_555 1_555 yes C(21) C(22) 1.37(1) 1_555 1_555 yes C(23) C(24) 1.50(2) 1_555 1_555 yes C(25) C(26) 1.45(2) 1_555 3_556 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 N(1) S(1) N(2) 99.1(4) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.5(5) 1_555 1_555 1_555 yes C(3) S(3) C(18) 97.2(5) 1_555 1_555 1_555 yes C(17) S(4) C(19) 99.8(6) 1_555 1_555 1_555 yes C(18) S(5) C(20) 101.4(6) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.7(5) 1_555 1_555 1_555 yes C(15) S(7) C(22) 97.8(5) 1_555 1_555 1_555 yes C(21) S(8) C(23) 99.4(6) 1_555 1_555 1_555 yes C(22) S(9) C(24) 100.4(6) 1_555 1_555 1_555 yes F(1) P(1) F(1) 180.0 1_555 1_555 3_555 yes F(1) P(1) F(2) 88.6(6) 1_555 1_555 1_555 yes F(1) P(1) F(2) 91.4(6) 1_555 1_555 3_555 yes F(1) P(1) F(3) 89.7(7) 1_555 1_555 1_555 yes F(1) P(1) F(3) 90.3(7) 1_555 1_555 3_555 yes F(1) P(1) F(2) 91.4(6) 3_555 1_555 1_555 yes F(1) P(1) F(2) 88.6(6) 3_555 1_555 3_555 yes F(1) P(1) F(3) 90.3(7) 3_555 1_555 1_555 yes F(1) P(1) F(3) 89.7(7) 3_555 1_555 3_555 yes F(2) P(1) F(2) 180.0 1_555 1_555 3_555 yes F(2) P(1) F(3) 90.6(5) 1_555 1_555 1_555 yes F(2) P(1) F(3) 89.4(5) 1_555 1_555 3_555 yes F(2) P(1) F(3) 89.4(5) 3_555 1_555 1_555 yes F(2) P(1) F(3) 90.6(5) 3_555 1_555 3_555 yes F(3) P(1) F(3) 180.0 1_555 1_555 3_555 yes C(25) O(1) C(26) 91(1) 1_555 1_555 1_555 yes S(1) N(1) C(1) 108.4(6) 1_555 1_555 1_555 yes S(1) N(2) C(16) 107.4(7) 1_555 1_555 1_555 yes N(1) C(1) C(2) 126.2(9) 1_555 1_555 1_555 yes N(1) C(1) C(16) 111.6(9) 1_555 1_555 1_555 yes C(2) C(1) C(16) 122.2(10) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.1(9) 1_555 1_555 1_555 yes C(1) C(2) C(4) 114.7(9) 1_555 1_555 1_555 yes C(3) C(2) C(4) 125.0(10) 1_555 1_555 1_555 yes S(2) C(3) S(3) 113.3(5) 1_555 1_555 1_555 yes S(2) C(3) C(2) 121.2(8) 1_555 1_555 1_555 yes S(3) C(3) C(2) 125.5(8) 1_555 1_555 1_555 yes C(2) C(4) C(5) 120.7(9) 1_555 1_555 1_555 yes C(2) C(4) C(13) 121.2(9) 1_555 1_555 1_555 yes C(5) C(4) C(13) 118.0(9) 1_555 1_555 1_555 yes C(4) C(5) C(6) 121.1(9) 1_555 1_555 1_555 yes C(4) C(5) H(1) 119(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 119(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 118.5(10) 1_555 1_555 1_555 yes C(5) C(6) C(11) 120.6(10) 1_555 1_555 1_555 yes C(7) C(6) C(11) 120(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 117(1) 1_555 1_555 1_555 yes C(6) C(7) H(2) 122(1) 1_555 1_555 1_555 no C(8) C(7) H(2) 120(1) 1_555 1_555 1_555 no C(7) C(8) C(9) 121(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 120(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 118(1) 1_555 1_555 1_555 no C(8) C(9) C(10) 120(1) 1_555 1_555 1_555 yes C(8) C(9) H(4) 119(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 120(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 120(1) 1_555 1_555 1_555 yes C(9) C(10) H(5) 119(1) 1_555 1_555 1_555 no C(11) C(10) H(5) 119(1) 1_555 1_555 1_555 no C(6) C(11) C(10) 119(1) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118.6(10) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.8(10) 1_555 1_555 1_555 yes C(11) C(12) C(13) 122.2(9) 1_555 1_555 1_555 yes C(11) C(12) H(6) 118.8(10) 1_555 1_555 1_555 no C(13) C(12) H(6) 118(1) 1_555 1_555 1_555 no C(4) C(13) C(12) 119.4(10) 1_555 1_555 1_555 yes C(4) C(13) C(14) 120.2(9) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120.3(9) 1_555 1_555 1_555 yes C(13) C(14) C(15) 126.1(10) 1_555 1_555 1_555 yes C(13) C(14) C(16) 114.0(9) 1_555 1_555 1_555 yes C(15) C(14) C(16) 119.9(10) 1_555 1_555 1_555 yes S(6) C(15) S(7) 111.3(5) 1_555 1_555 1_555 yes S(6) C(15) C(14) 123.5(8) 1_555 1_555 1_555 yes S(7) C(15) C(14) 125.1(8) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113.5(9) 1_555 1_555 1_555 yes N(2) C(16) C(14) 126.0(10) 1_555 1_555 1_555 yes C(1) C(16) C(14) 120.4(10) 1_555 1_555 1_555 yes S(2) C(17) S(4) 113.8(7) 1_555 1_555 1_555 yes S(2) C(17) C(18) 116.0(8) 1_555 1_555 1_555 yes S(4) C(17) C(18) 130.1(8) 1_555 1_555 1_555 yes S(3) C(18) S(5) 115.1(7) 1_555 1_555 1_555 yes S(3) C(18) C(17) 116.5(8) 1_555 1_555 1_555 yes S(5) C(18) C(17) 128.1(8) 1_555 1_555 1_555 yes S(4) C(19) C(20) 113.9(8) 1_555 1_555 1_555 yes S(4) C(19) H(7) 108(1) 1_555 1_555 1_555 no S(4) C(19) H(8) 108.0(10) 1_555 1_555 1_555 no C(20) C(19) H(7) 109(1) 1_555 1_555 1_555 no C(20) C(19) H(8) 108(1) 1_555 1_555 1_555 no H(7) C(19) H(8) 108(1) 1_555 1_555 1_555 no S(5) C(20) C(19) 113.2(10) 1_555 1_555 1_555 yes S(5) C(20) H(9) 109.0(9) 1_555 1_555 1_555 no S(5) C(20) H(10) 108(1) 1_555 1_555 1_555 no C(19) C(20) H(9) 108(1) 1_555 1_555 1_555 no C(19) C(20) H(10) 107(1) 1_555 1_555 1_555 no H(9) C(20) H(10) 110(1) 1_555 1_555 1_555 no S(6) C(21) S(8) 114.2(7) 1_555 1_555 1_555 yes S(6) C(21) C(22) 117.8(8) 1_555 1_555 1_555 yes S(8) C(21) C(22) 127.9(8) 1_555 1_555 1_555 yes S(7) C(22) S(9) 115.9(6) 1_555 1_555 1_555 yes S(7) C(22) C(21) 116.4(8) 1_555 1_555 1_555 yes S(9) C(22) C(21) 127.5(8) 1_555 1_555 1_555 yes S(8) C(23) C(24) 113(1) 1_555 1_555 1_555 yes S(8) C(23) H(11) 108(1) 1_555 1_555 1_555 no S(8) C(23) H(12) 107(1) 1_555 1_555 1_555 no C(24) C(23) H(11) 108(1) 1_555 1_555 1_555 no C(24) C(23) H(12) 108(1) 1_555 1_555 1_555 no H(11) C(23) H(12) 110(1) 1_555 1_555 1_555 no S(9) C(24) C(23) 116(1) 1_555 1_555 1_555 yes S(9) C(24) H(13) 108(1) 1_555 1_555 1_555 no S(9) C(24) H(14) 107(1) 1_555 1_555 1_555 no C(23) C(24) H(13) 108(1) 1_555 1_555 1_555 no C(23) C(24) H(14) 106(1) 1_555 1_555 1_555 no H(13) C(24) H(14) 109(1) 1_555 1_555 1_555 no O(1) C(25) C(26) 126(1) 1_555 1_555 3_556 yes O(1) C(25) H(15) 105(1) 1_555 1_555 1_555 no O(1) C(25) H(16) 105(1) 1_555 1_555 1_555 no C(26) C(25) H(15) 104(1) 3_556 1_555 1_555 no C(26) C(25) H(16) 108(1) 3_556 1_555 1_555 no H(15) C(25) H(16) 105(1) 1_555 1_555 1_555 no O(1) C(26) C(25) 129(2) 1_555 1_555 3_556 yes O(1) C(26) H(17) 105(1) 1_555 1_555 1_555 no O(1) C(26) H(18) 104(1) 1_555 1_555 1_555 no C(25) C(26) H(17) 106(1) 3_556 1_555 1_555 no C(25) C(26) H(18) 104(1) 3_556 1_555 1_555 no H(17) C(26) H(18) 102(1) 1_555 1_555 1_555 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 S(2) C(10) 3.57(1) 1_555 2_556 ? S(3) O(1) 3.34(2) 1_555 2_556 ? S(3) C(14) 3.53(1) 1_555 2_556 ? S(3) C(15) 3.57(1) 1_555 2_556 ? S(5) O(1) 3.16(2) 1_555 2_556 ? S(5) F(3) 3.530(10) 1_555 4_555 ? S(5) C(22) 3.55(1) 1_555 2_556 ? S(6) O(1) 3.49(2) 1_555 1_555 ? S(7) C(3) 3.49(1) 1_555 2_556 ? S(9) C(18) 3.51(1) 1_555 2_556 ? F(1) C(24) 3.54(2) 1_555 3_566 ? F(2) C(19) 3.13(1) 1_555 2_545 ? F(2) C(9) 3.16(2) 1_555 2_546 ? F(2) C(20) 3.19(2) 1_555 2_545 ? F(2) C(8) 3.50(2) 1_555 2_546 ? F(3) C(23) 3.39(2) 1_555 3_566 ? O(1) C(23) 3.41(3) 1_555 1_545 ? N(1) C(19) 3.56(1) 1_555 2_545 ? C(3) C(12) 3.41(2) 1_555 2_556 ? C(5) C(15) 3.57(2) 1_555 2_546 ? C(10) C(19) 3.58(2) 1_555 1_556 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(BEDT-ATD)2AsF6(THF),75K #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 23 14:58:06 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1498.87 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H36 As F6 N4 O S18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 27.712(2) _cell_length_b 7.787(2) _cell_length_c 13.3297(9) _cell_angle_alpha 90 _cell_angle_beta 103.888(6) _cell_angle_gamma 90 _cell_volume 2792.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 75.0 _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/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1518.00 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 75.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _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 4616 _reflns_number_total 4616 _reflns_number_observed 3611 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.103 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 0 104 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 36 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; As 0 2 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags As1 0.0000 0.5000 0.0000 0.0257(4) Uani d . 0.50 S S1 0.11195(8) 0.6420(3) 0.2687(2) 0.0250(6) Uani d . 1.00 . S2 0.24173(7) 0.8058(3) 0.1776(2) 0.0225(6) Uani d . 1.00 . S3 0.33165(7) 0.8943(3) 0.3328(2) 0.0217(6) Uani d . 1.00 . S4 0.27296(8) 0.9506(3) -0.0003(2) 0.0277(6) Uani d . 1.00 . S5 0.38372(8) 1.0589(3) 0.1885(2) 0.0242(6) Uani d . 1.00 . S6 0.09379(7) 0.8481(3) 0.5547(2) 0.0207(5) Uani d . 1.00 . S7 0.18061(7) 0.9116(3) 0.7240(2) 0.0208(5) Uani d . 1.00 . S8 0.02116(7) 1.0082(3) 0.6548(2) 0.0230(6) Uani d . 1.00 . S9 0.12640(8) 1.0795(3) 0.8629(2) 0.0234(6) Uani d . 1.00 . F1 -0.0066(2) 0.4951(8) 0.1241(4) 0.043(2) Uani d . 1.00 . F2 0.0614(2) 0.4356(8) 0.0406(4) 0.042(2) Uani d . 1.00 . F3 0.0192(2) 0.7114(8) 0.0148(5) 0.052(2) Uani d . 1.00 . O1 0.0468(4) 0.464(2) 0.6013(8) 0.028(3) Uani d . 0.50 . N1 0.1697(2) 0.6666(10) 0.2626(5) 0.022(2) Uani d . 1.00 . N2 0.1178(2) 0.6846(9) 0.3923(5) 0.023(2) Uani d . 1.00 . C1 0.1962(3) 0.709(1) 0.3569(6) 0.017(2) Uani d . 1.00 . C2 0.2478(3) 0.753(1) 0.3851(6) 0.019(2) Uani d . 1.00 . C3 0.2723(3) 0.809(1) 0.3079(6) 0.019(2) Uani d . 1.00 . C4 0.2717(3) 0.739(1) 0.4968(6) 0.017(2) Uani d . 1.00 . C5 0.3226(3) 0.711(1) 0.5311(6) 0.021(2) Uani d . 1.00 . C6 0.3464(3) 0.685(1) 0.6372(6) 0.020(2) Uani d . 1.00 . C7 0.3995(3) 0.657(1) 0.6681(7) 0.028(2) Uani d . 1.00 . C8 0.4198(3) 0.624(1) 0.7735(7) 0.032(3) Uani d . 1.00 . C9 0.3894(3) 0.612(1) 0.8444(7) 0.032(3) Uani d . 1.00 . C10 0.3410(3) 0.646(1) 0.8139(7) 0.028(2) Uani d . 1.00 . C11 0.3176(3) 0.684(1) 0.7089(6) 0.023(2) Uani d . 1.00 . C12 0.2661(3) 0.711(1) 0.6736(6) 0.021(2) Uani d . 1.00 . C13 0.2422(3) 0.742(1) 0.5712(6) 0.019(2) Uani d . 1.00 . C14 0.1875(3) 0.765(1) 0.5389(6) 0.019(2) Uani d . 1.00 . C15 0.1583(3) 0.829(1) 0.6008(6) 0.018(2) Uani d . 1.00 . C16 0.1666(3) 0.719(1) 0.4317(5) 0.016(2) Uani d . 1.00 . C17 0.2871(3) 0.918(1) 0.1339(6) 0.023(2) Uani d . 1.00 . C18 0.3296(3) 0.960(1) 0.2052(7) 0.023(2) Uani d . 1.00 . C19 0.3330(3) 0.993(1) -0.0166(6) 0.028(2) Uani d . 1.00 . C20 0.3601(3) 1.132(1) 0.0569(7) 0.029(3) Uani d . 1.00 . C21 0.0828(3) 0.957(1) 0.6629(6) 0.022(2) Uani d . 1.00 . C22 0.1234(3) 0.986(1) 0.7416(6) 0.020(2) Uani d . 1.00 . C23 0.0286(3) 1.156(1) 0.7638(6) 0.025(2) Uani d . 1.00 . C24 0.0604(3) 1.087(1) 0.8635(7) 0.030(3) Uani d . 1.00 . C25 -0.0029(4) 0.504(1) 0.5886(8) 0.038(3) Uani d . 1.00 . C26 0.0347(5) 0.409(2) 0.5011(8) 0.063(4) Uani d . 1.00 . H1 0.3422 0.7080 0.4818 0.0257 Uiso calc . 1.00 . H2 0.4196 0.6611 0.6198 0.0334 Uiso calc . 1.00 . H3 0.4546 0.6086 0.7976 0.0382 Uiso calc . 1.00 . H4 0.4037 0.5803 0.9141 0.0379 Uiso calc . 1.00 . H5 0.3215 0.6446 0.8640 0.0335 Uiso calc . 1.00 . H6 0.2465 0.7093 0.7235 0.0252 Uiso calc . 1.00 . H7 0.3521 0.8904 -0.0048 0.0339 Uiso calc . 1.00 . H8 0.3303 1.0302 -0.0860 0.0339 Uiso calc . 1.00 . H9 0.3377 1.2239 0.0570 0.0349 Uiso calc . 1.00 . H10 0.3874 1.1720 0.0314 0.0349 Uiso calc . 1.00 . H11 0.0436 1.2585 0.7471 0.0303 Uiso calc . 1.00 . H12 -0.0033 1.1813 0.7743 0.0303 Uiso calc . 1.00 . H13 0.0496 0.9741 0.8740 0.0360 Uiso calc . 1.00 . H14 0.0565 1.1588 0.9187 0.0360 Uiso calc . 1.00 . H15 -0.0193 0.3964 0.5940 0.0460 Uiso calc . 1.00 . H16 -0.0046 0.5712 0.6486 0.0460 Uiso calc . 1.00 . H17 0.0670 0.3923 0.4836 0.0764 Uiso calc . 1.00 . H18 0.0209 0.2959 0.5020 0.0764 Uiso calc . 1.00 . 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) 0.0231(7) 0.0249(8) 0.0308(7) 0.0051(5) 0.0101(6) -0.0009(6) S(1) 0.021(1) 0.029(1) 0.025(1) -0.0026(9) 0.0053(9) -0.0035(10) S(2) 0.022(1) 0.022(1) 0.024(1) -0.0014(9) 0.0074(9) 0.0016(9) S(3) 0.0204(10) 0.020(1) 0.026(1) -0.0013(9) 0.0087(9) -0.0022(9) S(4) 0.026(1) 0.032(1) 0.026(1) -0.0006(10) 0.0079(10) 0.004(1) S(5) 0.023(1) 0.019(1) 0.032(1) -0.0019(9) 0.0097(10) -0.0004(9) S(6) 0.020(1) 0.020(1) 0.023(1) -0.0012(8) 0.0057(9) -0.0026(9) S(7) 0.022(1) 0.018(1) 0.023(1) 0.0005(9) 0.0054(9) -0.0022(9) S(8) 0.0201(10) 0.023(1) 0.026(1) 0.0004(9) 0.0062(9) -0.0034(9) S(9) 0.026(1) 0.021(1) 0.023(1) 0.0005(9) 0.0055(9) -0.0031(9) F(1) 0.038(3) 0.062(4) 0.034(3) 0.011(3) 0.019(3) 0.002(3) F(2) 0.030(3) 0.053(4) 0.048(3) 0.013(3) 0.022(3) 0.009(3) F(3) 0.056(4) 0.025(4) 0.080(5) -0.003(3) 0.026(4) -0.010(3) O(1) 0.030(6) 0.030(8) 0.020(6) -0.005(6) -0.001(5) 0.010(5) N(1) 0.015(3) 0.028(5) 0.024(4) 0.000(3) 0.007(3) 0.000(3) N(2) 0.025(4) 0.021(4) 0.023(4) -0.003(3) 0.005(3) -0.003(3) C(1) 0.010(4) 0.023(5) 0.020(4) -0.001(3) 0.005(3) -0.003(3) C(2) 0.021(4) 0.013(5) 0.019(4) -0.001(3) 0.000(3) -0.001(3) C(3) 0.024(4) 0.017(5) 0.021(4) 0.002(3) 0.014(4) -0.002(3) C(4) 0.020(4) 0.012(4) 0.023(4) -0.003(3) 0.010(3) 0.000(3) C(5) 0.029(4) 0.013(4) 0.020(4) 0.000(4) 0.002(4) 0.001(3) C(6) 0.025(4) 0.011(4) 0.021(4) -0.002(4) 0.002(4) -0.005(3) C(7) 0.029(5) 0.023(5) 0.031(5) 0.000(4) 0.007(4) -0.003(4) C(8) 0.023(5) 0.033(6) 0.033(5) 0.002(4) -0.006(4) -0.010(4) C(9) 0.032(5) 0.036(6) 0.028(5) 0.004(4) 0.009(4) -0.005(4) C(10) 0.026(5) 0.024(5) 0.031(5) 0.002(4) 0.004(4) 0.000(4) C(11) 0.020(4) 0.021(5) 0.031(5) 0.001(4) 0.011(4) -0.004(4) C(12) 0.025(4) 0.014(5) 0.021(4) 0.001(4) -0.001(4) 0.001(4) C(13) 0.021(4) 0.011(4) 0.025(4) 0.000(3) 0.004(4) -0.001(3) C(14) 0.025(4) 0.010(4) 0.019(4) -0.004(3) -0.002(3) 0.003(3) C(15) 0.021(4) 0.018(5) 0.016(4) -0.004(3) 0.009(3) 0.002(3) C(16) 0.021(4) 0.013(4) 0.013(4) -0.005(3) 0.000(3) 0.001(3) C(17) 0.019(4) 0.022(5) 0.031(4) 0.001(4) 0.011(4) -0.001(4) C(18) 0.027(4) 0.010(5) 0.032(5) 0.005(3) 0.008(4) 0.004(4) C(19) 0.033(5) 0.027(5) 0.024(4) 0.000(4) 0.008(4) 0.000(4) C(20) 0.040(5) 0.021(5) 0.033(5) -0.008(4) 0.020(4) 0.000(4) C(21) 0.033(5) 0.017(5) 0.017(4) -0.004(4) 0.010(4) 0.002(3) C(22) 0.025(4) 0.012(4) 0.025(4) -0.002(3) 0.009(4) 0.002(3) C(23) 0.029(5) 0.023(5) 0.020(4) 0.007(4) 0.000(4) 0.001(4) C(24) 0.033(5) 0.024(5) 0.033(5) 0.007(4) 0.006(4) 0.001(4) C(25) 0.035(5) 0.029(6) 0.051(6) 0.008(4) 0.011(5) 0.005(5) C(26) 0.11(1) 0.040(8) 0.024(5) -0.028(7) -0.004(6) 0.008(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0067(10) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3611 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0702 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0925 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.283 _refine_ls_shift/esd_max 0.1740 _refine_ls_shift/esd_mean 0.0210 _refine_diff_density_min -1.06 _refine_diff_density_max 0.83 #------------------------------------------------------------------------------ _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) 1.709(5) 1_555 1_555 yes As(1) F(1) 1.709(5) 1_555 3_565 yes As(1) F(2) 1.733(5) 1_555 1_555 yes As(1) F(2) 1.733(5) 1_555 3_565 yes As(1) F(3) 1.726(6) 1_555 1_555 yes As(1) F(3) 1.726(6) 1_555 3_565 yes S(1) N(1) 1.632(6) 1_555 1_555 yes S(1) N(2) 1.650(7) 1_555 1_555 yes S(2) C(3) 1.740(8) 1_555 1_555 yes S(2) C(17) 1.742(8) 1_555 1_555 yes S(3) C(3) 1.732(8) 1_555 1_555 yes S(3) C(18) 1.763(8) 1_555 1_555 yes S(4) C(17) 1.755(8) 1_555 1_555 yes S(4) C(19) 1.760(9) 1_555 1_555 yes S(5) C(18) 1.749(8) 1_555 1_555 yes S(5) C(20) 1.811(9) 1_555 1_555 yes S(6) C(15) 1.751(8) 1_555 1_555 yes S(6) C(21) 1.763(8) 1_555 1_555 yes S(7) C(15) 1.733(8) 1_555 1_555 yes S(7) C(22) 1.757(8) 1_555 1_555 yes S(8) C(21) 1.732(8) 1_555 1_555 yes S(8) C(23) 1.826(9) 1_555 1_555 yes S(9) C(22) 1.756(8) 1_555 1_555 yes S(9) C(24) 1.831(9) 1_555 1_555 yes O(1) C(25) 1.38(1) 1_555 1_555 yes O(1) C(26) 1.37(1) 1_555 1_555 yes N(1) C(1) 1.337(10) 1_555 1_555 yes N(2) C(16) 1.356(10) 1_555 1_555 yes C(1) C(2) 1.43(1) 1_555 1_555 yes C(1) C(16) 1.436(10) 1_555 1_555 yes C(2) C(3) 1.43(1) 1_555 1_555 yes C(2) C(4) 1.48(1) 1_555 1_555 yes C(4) C(5) 1.39(1) 1_555 1_555 yes C(4) C(13) 1.429(10) 1_555 1_555 yes C(5) C(6) 1.42(1) 1_555 1_555 yes C(6) C(7) 1.45(1) 1_555 1_555 yes C(6) C(11) 1.38(1) 1_555 1_555 yes C(7) C(8) 1.41(1) 1_555 1_555 yes C(8) C(9) 1.41(1) 1_555 1_555 yes C(9) C(10) 1.33(1) 1_555 1_555 yes C(10) C(11) 1.43(1) 1_555 1_555 yes C(11) C(12) 1.41(1) 1_555 1_555 yes C(12) C(13) 1.39(1) 1_555 1_555 yes C(13) C(14) 1.48(1) 1_555 1_555 yes C(14) C(15) 1.38(1) 1_555 1_555 yes C(14) C(16) 1.45(1) 1_555 1_555 yes C(17) C(18) 1.36(1) 1_555 1_555 yes C(19) C(20) 1.53(1) 1_555 1_555 yes C(21) C(22) 1.36(1) 1_555 1_555 yes C(23) C(24) 1.51(1) 1_555 1_555 yes C(25) C(26) 1.47(1) 1_555 3_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 F(1) As(1) F(1) 180.0 1_555 1_555 3_565 yes F(1) As(1) F(2) 91.0(2) 1_555 1_555 1_555 yes F(1) As(1) F(2) 89.0(2) 1_555 1_555 3_565 yes F(1) As(1) F(3) 90.7(3) 1_555 1_555 1_555 yes F(1) As(1) F(3) 89.3(3) 1_555 1_555 3_565 yes F(1) As(1) F(2) 89.0(2) 3_565 1_555 1_555 yes F(1) As(1) F(2) 91.0(2) 3_565 1_555 3_565 yes F(1) As(1) F(3) 89.3(3) 3_565 1_555 1_555 yes F(1) As(1) F(3) 90.7(3) 3_565 1_555 3_565 yes F(2) As(1) F(2) 180.0 1_555 1_555 3_565 yes F(2) As(1) F(3) 89.3(3) 1_555 1_555 1_555 yes F(2) As(1) F(3) 90.7(3) 1_555 1_555 3_565 yes F(2) As(1) F(3) 90.7(3) 3_565 1_555 1_555 yes F(2) As(1) F(3) 89.3(3) 3_565 1_555 3_565 yes F(3) As(1) F(3) 180.0 1_555 1_555 3_565 yes N(1) S(1) N(2) 99.4(3) 1_555 1_555 1_555 yes C(3) S(2) C(17) 96.3(4) 1_555 1_555 1_555 yes C(3) S(3) C(18) 96.7(4) 1_555 1_555 1_555 yes C(17) S(4) C(19) 99.6(4) 1_555 1_555 1_555 yes C(18) S(5) C(20) 98.1(4) 1_555 1_555 1_555 yes C(15) S(6) C(21) 96.6(4) 1_555 1_555 1_555 yes C(15) S(7) C(22) 96.9(4) 1_555 1_555 1_555 yes C(21) S(8) C(23) 100.0(4) 1_555 1_555 1_555 yes C(22) S(9) C(24) 100.9(4) 1_555 1_555 1_555 yes C(25) O(1) C(26) 87.0(9) 1_555 1_555 1_555 yes S(1) N(1) C(1) 107.9(5) 1_555 1_555 1_555 yes S(1) N(2) C(16) 105.9(5) 1_555 1_555 1_555 yes N(1) C(1) C(2) 126.6(7) 1_555 1_555 1_555 yes N(1) C(1) C(16) 112.8(6) 1_555 1_555 1_555 yes C(2) C(1) C(16) 120.5(7) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.0(7) 1_555 1_555 1_555 yes C(1) C(2) C(4) 115.2(7) 1_555 1_555 1_555 yes C(3) C(2) C(4) 124.8(7) 1_555 1_555 1_555 yes S(2) C(3) S(3) 114.1(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 120.9(6) 1_555 1_555 1_555 yes S(3) C(3) C(2) 124.9(6) 1_555 1_555 1_555 yes C(2) C(4) C(5) 121.0(7) 1_555 1_555 1_555 yes C(2) C(4) C(13) 120.2(7) 1_555 1_555 1_555 yes C(5) C(4) C(13) 118.6(7) 1_555 1_555 1_555 yes C(4) C(5) C(6) 122.7(7) 1_555 1_555 1_555 yes C(4) C(5) H(1) 118.7(8) 1_555 1_555 1_555 no C(6) C(5) H(1) 118.6(8) 1_555 1_555 1_555 no C(5) C(6) C(7) 120.1(7) 1_555 1_555 1_555 yes C(5) C(6) C(11) 118.7(7) 1_555 1_555 1_555 yes C(7) C(6) C(11) 121.2(7) 1_555 1_555 1_555 yes C(6) C(7) C(8) 116.6(7) 1_555 1_555 1_555 yes C(6) C(7) H(2) 121.7(8) 1_555 1_555 1_555 no C(8) C(7) H(2) 121.7(9) 1_555 1_555 1_555 no C(7) C(8) C(9) 121.3(8) 1_555 1_555 1_555 yes C(7) C(8) H(3) 119.5(9) 1_555 1_555 1_555 no C(9) C(8) H(3) 119.1(9) 1_555 1_555 1_555 no C(8) C(9) C(10) 120.2(8) 1_555 1_555 1_555 yes C(8) C(9) H(4) 119.7(8) 1_555 1_555 1_555 no C(10) C(9) H(4) 120.1(8) 1_555 1_555 1_555 no C(9) C(10) C(11) 121.9(8) 1_555 1_555 1_555 yes C(9) C(10) H(5) 118.9(9) 1_555 1_555 1_555 no C(11) C(10) H(5) 119.2(8) 1_555 1_555 1_555 no C(6) C(11) C(10) 118.5(7) 1_555 1_555 1_555 yes C(6) C(11) C(12) 118.3(8) 1_555 1_555 1_555 yes C(10) C(11) C(12) 123.1(7) 1_555 1_555 1_555 yes C(11) C(12) C(13) 124.2(8) 1_555 1_555 1_555 yes C(11) C(12) H(6) 117.8(8) 1_555 1_555 1_555 no C(13) C(12) H(6) 118.0(8) 1_555 1_555 1_555 no C(4) C(13) C(12) 117.4(7) 1_555 1_555 1_555 yes C(4) C(13) C(14) 121.1(7) 1_555 1_555 1_555 yes C(12) C(13) C(14) 121.4(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 125.1(7) 1_555 1_555 1_555 yes C(13) C(14) C(16) 113.2(7) 1_555 1_555 1_555 yes C(15) C(14) C(16) 121.7(7) 1_555 1_555 1_555 yes S(6) C(15) S(7) 113.8(4) 1_555 1_555 1_555 yes S(6) C(15) C(14) 121.1(6) 1_555 1_555 1_555 yes S(7) C(15) C(14) 125.0(6) 1_555 1_555 1_555 yes N(2) C(16) C(1) 113.9(7) 1_555 1_555 1_555 yes N(2) C(16) C(14) 123.6(7) 1_555 1_555 1_555 yes C(1) C(16) C(14) 122.5(7) 1_555 1_555 1_555 yes S(2) C(17) S(4) 114.3(5) 1_555 1_555 1_555 yes S(2) C(17) C(18) 117.2(6) 1_555 1_555 1_555 yes S(4) C(17) C(18) 128.4(6) 1_555 1_555 1_555 yes S(3) C(18) S(5) 114.8(5) 1_555 1_555 1_555 yes S(3) C(18) C(17) 115.3(6) 1_555 1_555 1_555 yes S(5) C(18) C(17) 129.8(7) 1_555 1_555 1_555 yes S(4) C(19) C(20) 112.9(6) 1_555 1_555 1_555 yes S(4) C(19) H(7) 109.0(7) 1_555 1_555 1_555 no S(4) C(19) H(8) 108.8(7) 1_555 1_555 1_555 no C(20) C(19) H(7) 108.7(8) 1_555 1_555 1_555 no C(20) C(19) H(8) 108.6(8) 1_555 1_555 1_555 no H(7) C(19) H(8) 108.9(8) 1_555 1_555 1_555 no S(5) C(20) C(19) 114.0(6) 1_555 1_555 1_555 yes S(5) C(20) H(9) 108.6(6) 1_555 1_555 1_555 no S(5) C(20) H(10) 108.3(7) 1_555 1_555 1_555 no C(19) C(20) H(9) 108.3(8) 1_555 1_555 1_555 no C(19) C(20) H(10) 108.3(7) 1_555 1_555 1_555 no H(9) C(20) H(10) 109.3(9) 1_555 1_555 1_555 no S(6) C(21) S(8) 114.9(5) 1_555 1_555 1_555 yes S(6) C(21) C(22) 116.0(6) 1_555 1_555 1_555 yes S(8) C(21) C(22) 129.1(6) 1_555 1_555 1_555 yes S(7) C(22) S(9) 114.5(5) 1_555 1_555 1_555 yes S(7) C(22) C(21) 116.6(6) 1_555 1_555 1_555 yes S(9) C(22) C(21) 128.8(6) 1_555 1_555 1_555 yes S(8) C(23) C(24) 114.1(6) 1_555 1_555 1_555 yes S(8) C(23) H(11) 108.4(6) 1_555 1_555 1_555 no S(8) C(23) H(12) 108.4(7) 1_555 1_555 1_555 no C(24) C(23) H(11) 108.1(8) 1_555 1_555 1_555 no C(24) C(23) H(12) 108.2(7) 1_555 1_555 1_555 no H(11) C(23) H(12) 109.5(9) 1_555 1_555 1_555 no S(9) C(24) C(23) 112.4(6) 1_555 1_555 1_555 yes S(9) C(24) H(13) 108.8(7) 1_555 1_555 1_555 no S(9) C(24) H(14) 108.8(7) 1_555 1_555 1_555 no C(23) C(24) H(13) 108.7(8) 1_555 1_555 1_555 no C(23) C(24) H(14) 108.8(8) 1_555 1_555 1_555 no H(13) C(24) H(14) 109.2(9) 1_555 1_555 1_555 no O(1) C(25) C(26) 126.0(10) 1_555 1_555 3_566 yes O(1) C(25) H(15) 105.4(9) 1_555 1_555 1_555 no O(1) C(25) H(16) 105.4(10) 1_555 1_555 1_555 no C(26) C(25) H(15) 105.1(9) 3_566 1_555 1_555 no C(26) C(25) H(16) 106.8(9) 3_566 1_555 1_555 no H(15) C(25) H(16) 106.9(9) 1_555 1_555 1_555 no O(1) C(26) C(25) 127(1) 1_555 1_555 3_566 yes O(1) C(26) H(17) 104(1) 1_555 1_555 1_555 no O(1) C(26) H(18) 106.3(9) 1_555 1_555 1_555 no C(25) C(26) H(17) 105.6(9) 3_566 1_555 1_555 no C(25) C(26) H(18) 105(1) 3_566 1_555 1_555 no H(17) C(26) H(18) 105(1) 1_555 1_555 1_555 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 S(1) F(2) 3.427(6) 1_555 1_555 ? S(1) F(1) 3.575(6) 1_555 1_555 ? S(2) C(10) 3.523(9) 1_555 2_556 ? S(2) C(19) 3.561(9) 1_555 2_545 ? S(2) S(4) 3.598(3) 1_555 2_545 ? S(3) O(1) 3.32(1) 1_555 2_556 ? S(3) C(14) 3.459(8) 1_555 2_556 ? S(3) C(15) 3.496(8) 1_555 2_556 ? S(5) O(1) 3.09(1) 1_555 2_556 ? S(5) F(1) 3.376(5) 1_555 4_565 ? S(5) C(22) 3.473(8) 1_555 2_556 ? S(6) O(1) 3.38(1) 1_555 1_555 ? S(7) C(3) 3.422(8) 1_555 2_556 ? S(9) C(18) 3.406(8) 1_555 2_556 ? S(9) C(17) 3.558(9) 1_555 2_556 ? F(1) C(23) 3.23(1) 1_555 3_576 ? F(1) C(24) 3.60(1) 1_555 3_576 ? F(2) C(19) 3.052(10) 1_555 2_545 ? F(2) C(9) 3.09(1) 1_555 2_546 ? F(2) C(20) 3.180(10) 1_555 2_545 ? F(2) C(8) 3.42(1) 1_555 2_546 ? F(2) C(24) 3.59(1) 1_555 1_544 ? F(3) C(24) 3.42(1) 1_555 3_576 ? O(1) C(23) 3.35(1) 1_555 1_545 ? N(1) C(19) 3.53(1) 1_555 2_545 ? N(2) C(25) 3.57(1) 1_555 3_566 ? C(3) C(12) 3.34(1) 1_555 2_556 ? C(5) C(15) 3.56(1) 1_555 2_546 ? C(5) C(14) 3.59(1) 1_555 2_546 ? C(10) C(19) 3.57(1) 1_555 1_556 ? C(23) C(25) 3.55(1) 1_555 1_565 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _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. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;