# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 1145/266 data_General _audit_creation_date 'Thu Oct 24 20:43:56 2030' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_2EMETH #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C27 H12 Cl0.50 F6 N4 O2 P S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 843.59 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.60(1) _cell_length_b 16.323(10) _cell_length_c 6.96(1) _cell_angle_alpha 103.94(8) _cell_angle_beta 103.98(8) _cell_angle_gamma 95.77(6) _cell_volume 1645(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 288.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 5185 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.05 _diffrn_measured_fraction_theta_max 0.5382 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.5382 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 4.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5185 _reflns_number_gt 2385 _reflns_threshold_expression F^2^>4.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.0792 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2385 _refine_ls_number_parameters 436 _refine_ls_goodness_of_fit_ref 0.296 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.1826 _refine_diff_density_max 0.47 _refine_diff_density_min -0.46 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl 0.0033 1.1162 0.8379 0.167(6) Uani 0.50 d P . . S(1) S 0.2277(2) 0.0642(2) 0.7314(6) 0.051(1) Uani 1.00 d . . . S(2) S 0.4225(3) 0.0738(2) 0.8559(6) 0.050(1) Uani 1.00 d . . . S(3) S 0.1171(3) 0.3551(2) 0.8436(6) 0.055(1) Uani 1.00 d . . . S(4) S 0.2584(3) 0.5050(2) 1.0359(7) 0.061(1) Uani 1.00 d . . . S(5) S 0.2108(3) -0.0189(2) 0.1740(6) 0.056(1) Uani 1.00 d . . . S(6) S 0.4061(3) -0.0065(2) 0.2910(6) 0.055(1) Uani 1.00 d . . . S(7) S 0.0981(3) 0.2694(3) 0.2895(7) 0.071(2) Uani 1.00 d . . . S(8) S 0.2357(3) 0.4231(2) 0.4650(6) 0.067(1) Uani 1.00 d . . . P P 0.1853(3) 0.7045(2) 0.5472(8) 0.068(1) Uani 1.00 d . . . F(1) F 0.0969(7) 0.6449(7) 0.421(2) 0.162(5) Uani 1.00 d . . . F(2) F 0.186(1) 0.672(1) 0.734(3) 0.189(9) Uani 1.00 d . . . F(3) F 0.2751(7) 0.7648(6) 0.676(2) 0.144(5) Uani 1.00 d . . . F(4) F 0.189(1) 0.741(1) 0.371(3) 0.23(1) Uani 1.00 d . . . F(5) F 0.1318(7) 0.7724(7) 0.638(3) 0.159(6) Uani 1.00 d . . . F(6) F 0.2402(7) 0.6336(7) 0.470(2) 0.158(5) Uani 1.00 d . . . O(1) O 0.2665(6) 0.2532(5) 0.878(1) 0.045(3) Uani 1.00 d . . . O(2) O 0.2473(6) 0.1715(5) 0.317(2) 0.051(3) Uani 1.00 d . . . N(1) N 0.5056(8) 0.2734(8) 1.038(2) 0.055(4) Uani 1.00 d . . . N(2) N 0.4440(9) 0.4352(6) 1.118(2) 0.056(4) Uani 1.00 d . . . N(3) N 0.4873(8) 0.1896(8) 0.465(2) 0.063(4) Uani 1.00 d . . . N(4) N 0.425(1) 0.3534(8) 0.540(2) 0.072(5) Uani 1.00 d . . . C(1) C 0.269(1) -0.0306(9) 0.695(2) 0.059(5) Uani 1.00 d . . . C(2) C 0.355(1) -0.0262(8) 0.750(2) 0.056(5) Uani 1.00 d . . . C(3) C 0.3327(9) 0.1290(9) 0.838(2) 0.046(4) Uani 1.00 d . . . C(4) C 0.3423(9) 0.2152(8) 0.899(2) 0.043(4) Uani 1.00 d . . . C(5) C 0.420(1) 0.2806(9) 0.992(2) 0.045(5) Uani 1.00 d . . . C(6) C 0.560(1) 0.349(1) 1.123(3) 0.072(6) Uani 1.00 d . . . C(7) C 0.530(1) 0.4284(9) 1.168(3) 0.067(5) Uani 1.00 d . . . C(8) C 0.3901(9) 0.3596(8) 1.027(2) 0.046(4) Uani 1.00 d . . . C(9) C 0.294(1) 0.3430(8) 0.952(2) 0.048(4) Uani 1.00 d . . . C(10) C 0.2314(10) 0.3936(8) 0.946(2) 0.047(4) Uani 1.00 d . . . C(11) C 0.084(1) 0.453(1) 0.884(3) 0.065(6) Uani 1.00 d . . . C(12) C 0.148(1) 0.5220(9) 0.968(2) 0.059(5) Uani 1.00 d . . . C(13) C 0.254(1) -0.1143(9) 0.134(3) 0.077(6) Uani 1.00 d . . . C(14) C 0.342(1) -0.107(1) 0.181(3) 0.070(6) Uani 1.00 d . . . C(15) C 0.3134(8) 0.0450(7) 0.272(2) 0.037(4) Uani 1.00 d . . . C(16) C 0.3241(10) 0.1332(9) 0.335(2) 0.050(5) Uani 1.00 d . . . C(17) C 0.402(1) 0.1985(9) 0.423(2) 0.049(5) Uani 1.00 d . . . C(18) C 0.542(1) 0.268(1) 0.550(3) 0.071(6) Uani 1.00 d . . . C(19) C 0.513(1) 0.345(1) 0.583(3) 0.077(6) Uani 1.00 d . . . C(20) C 0.369(1) 0.2783(10) 0.458(2) 0.055(5) Uani 1.00 d . . . C(21) C 0.275(1) 0.2608(9) 0.391(2) 0.051(5) Uani 1.00 d . . . C(22) C 0.2120(10) 0.3112(8) 0.381(2) 0.049(5) Uani 1.00 d . . . C(23) C 0.064(1) 0.371(1) 0.326(3) 0.087(8) Uani 1.00 d . . . C(24) C 0.127(1) 0.438(1) 0.403(3) 0.085(7) Uani 1.00 d . . . C(25) C -0.003(2) 1.047(2) 0.667(7) 0.17(2) Uani 1.00 d . . . C(26) C 0.007(1) 0.965(2) 0.641(6) 0.14(1) Uani 1.00 d . . . C(27) C -0.0050 1.0988 0.5211 0.26(2) Uani 1.00 d . . . H(1) H 0.2319 -0.1011 0.5566 0.0396 Uiso 1.00 calc . . . H(2) H 0.3915 -0.0839 0.7528 0.0396 Uiso 1.00 calc . . . H(3) H 0.6375 0.3458 1.1269 0.0396 Uiso 1.00 calc . . . H(4) H 0.5776 0.4804 1.2084 0.0396 Uiso 1.00 calc . . . H(5) H 0.0175 0.4599 0.8611 0.0396 Uiso 1.00 calc . . . H(6) H 0.1278 0.5855 0.9859 0.0396 Uiso 1.00 calc . . . H(7) H 0.2161 -0.1686 0.0804 0.0892 Uiso 1.00 calc . . . H(8) H 0.3693 -0.1564 0.1541 0.0838 Uiso 1.00 calc . . . H(9) H 0.6049 0.2684 0.5879 0.0847 Uiso 1.00 calc . . . H(10) H 0.5573 0.3956 0.6405 0.0922 Uiso 1.00 calc . . . H(11) H 0.0022 0.3768 0.2920 0.1029 Uiso 1.00 calc . . . H(12) H 0.1134 0.4940 0.4244 0.1018 Uiso 1.00 calc . . . H(13) H 0.0163 0.9458 0.7720 0.1802 Uiso 1.00 calc . . . H(14) H -0.0051 1.1584 0.5408 0.1802 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl 0.14(1) 0.13(1) 0.18(1) -0.062(10) 0.05(1) -0.03(1) S(1) 0.050(2) 0.043(2) 0.054(3) 0.005(2) 0.014(2) 0.006(2) S(2) 0.053(2) 0.044(2) 0.057(3) 0.014(2) 0.021(2) 0.014(2) S(3) 0.060(3) 0.049(2) 0.055(3) 0.011(2) 0.018(2) 0.008(2) S(4) 0.074(3) 0.036(2) 0.071(3) 0.013(2) 0.016(2) 0.010(2) S(5) 0.050(2) 0.051(2) 0.061(3) -0.001(2) 0.010(2) 0.011(2) S(6) 0.052(2) 0.053(2) 0.057(3) 0.017(2) 0.012(2) 0.013(2) S(7) 0.082(3) 0.056(3) 0.079(3) 0.024(2) 0.024(3) 0.020(2) S(8) 0.112(4) 0.039(2) 0.054(3) 0.014(2) 0.030(3) 0.010(2) P 0.066(3) 0.033(2) 0.092(4) 0.005(2) 0.015(3) 0.000(2) F(1) 0.058(7) 0.104(9) 0.24(2) -0.001(6) -0.006(9) -0.054(10) F(2) 0.26(2) 0.20(2) 0.17(2) 0.08(1) 0.10(1) 0.11(1) F(3) 0.090(8) 0.064(7) 0.23(2) 0.010(6) 0.030(9) -0.027(8) F(4) 0.29(2) 0.27(2) 0.15(2) 0.01(2) 0.05(2) 0.12(2) F(5) 0.085(8) 0.096(9) 0.25(2) 0.039(7) 0.012(10) -0.021(10) F(6) 0.093(8) 0.080(7) 0.23(2) 0.011(6) 0.031(9) -0.068(9) O(1) 0.041(6) 0.042(5) 0.051(6) 0.004(4) 0.012(5) 0.010(4) O(2) 0.054(6) 0.028(5) 0.068(7) 0.007(4) 0.018(6) 0.004(5) N(1) 0.050(8) 0.058(8) 0.055(9) 0.010(7) 0.009(7) 0.016(7) N(2) 0.078(10) 0.024(6) 0.053(8) -0.002(6) 0.003(8) 0.005(5) N(3) 0.052(8) 0.060(9) 0.074(10) -0.010(7) 0.019(8) 0.021(7) N(4) 0.09(1) 0.058(9) 0.062(10) -0.011(8) 0.012(9) 0.011(7) C(1) 0.08(1) 0.040(9) 0.05(1) 0.014(8) 0.024(10) 0.010(7) C(2) 0.08(1) 0.031(8) 0.06(1) 0.012(8) 0.015(9) 0.008(7) C(3) 0.035(8) 0.048(9) 0.050(9) 0.005(6) 0.015(7) 0.005(7) C(4) 0.038(8) 0.030(7) 0.06(1) 0.004(6) 0.013(8) 0.006(7) C(5) 0.06(1) 0.043(8) 0.032(9) 0.010(8) 0.006(8) 0.018(6) C(6) 0.05(1) 0.08(1) 0.08(1) -0.001(9) 0.003(10) 0.021(10) C(7) 0.05(1) 0.036(8) 0.09(1) -0.009(8) -0.01(1) 0.011(8) C(8) 0.057(10) 0.031(7) 0.054(10) 0.005(7) 0.017(8) 0.019(7) C(9) 0.07(1) 0.023(7) 0.049(9) 0.012(7) 0.008(8) 0.005(6) C(10) 0.07(1) 0.036(7) 0.029(8) 0.009(7) 0.015(8) 0.000(6) C(11) 0.06(1) 0.07(1) 0.07(1) 0.043(9) 0.025(9) 0.014(9) C(12) 0.07(1) 0.044(9) 0.07(1) 0.034(8) 0.028(10) 0.015(8) C(13) 0.10(1) 0.043(10) 0.08(1) 0.003(9) 0.02(1) 0.008(9) C(14) 0.07(1) 0.06(1) 0.07(1) 0.025(9) 0.02(1) 0.008(9) C(15) 0.048(8) 0.027(7) 0.040(8) 0.011(6) 0.017(7) 0.007(6) C(16) 0.058(10) 0.048(9) 0.046(9) 0.018(8) 0.018(8) 0.014(7) C(17) 0.055(10) 0.048(9) 0.05(1) -0.014(8) 0.028(9) 0.020(7) C(18) 0.06(1) 0.06(1) 0.08(1) -0.010(9) 0.016(10) 0.023(9) C(19) 0.08(1) 0.06(1) 0.08(1) -0.024(10) 0.01(1) 0.010(9) C(20) 0.09(1) 0.046(9) 0.034(9) -0.002(9) 0.029(9) 0.005(7) C(21) 0.06(1) 0.037(8) 0.051(10) 0.003(8) 0.022(8) 0.008(7) C(22) 0.07(1) 0.038(8) 0.049(10) 0.010(7) 0.029(8) 0.012(7) C(23) 0.12(2) 0.08(1) 0.09(1) 0.05(1) 0.05(1) 0.04(1) C(24) 0.12(2) 0.06(1) 0.08(1) 0.03(1) 0.02(1) 0.01(1) C(25) 0.06(1) 0.12(2) 0.33(5) -0.02(1) 0.08(2) 0.05(3) C(26) 0.05(1) 0.11(2) 0.27(4) -0.01(1) -0.02(2) 0.14(2) C(27) 0.06(2) 0.12(3) 0.64(9) 0.02(2) 0.08(3) 0.18(4) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl C(25) 1.40(3) . . yes S(1) C(1) 1.72(1) . . yes S(1) C(3) 1.74(1) . . yes S(2) C(2) 1.74(1) . . yes S(2) C(3) 1.74(1) . . yes S(3) C(10) 1.74(2) . . yes S(3) C(11) 1.71(1) . . yes S(4) C(10) 1.75(1) . . yes S(4) C(12) 1.74(2) . . yes S(5) C(13) 1.75(2) . . yes S(5) C(15) 1.71(1) . . yes S(6) C(14) 1.72(2) . . yes S(6) C(15) 1.74(1) . . yes S(7) C(22) 1.74(2) . . yes S(7) C(23) 1.77(2) . . yes S(8) C(22) 1.75(1) . . yes S(8) C(24) 1.70(2) . . yes P F(1) 1.53(1) . . yes P F(2) 1.51(1) . . yes P F(3) 1.56(1) . . yes P F(4) 1.50(2) . . yes P F(5) 1.56(1) . . yes P F(6) 1.58(1) . . yes O(1) C(4) 1.38(1) . . yes O(1) C(9) 1.41(1) . . yes O(2) C(16) 1.40(2) . . yes O(2) C(21) 1.41(2) . . yes N(1) C(5) 1.32(2) . . yes N(1) C(6) 1.34(2) . . yes N(2) C(7) 1.32(2) . . yes N(2) C(8) 1.34(2) . . yes N(3) C(17) 1.33(2) . . yes N(3) C(18) 1.37(2) . . yes N(4) C(19) 1.37(2) . . yes N(4) C(20) 1.34(2) . . yes C(1) C(2) 1.30(2) . . yes C(3) C(4) 1.35(2) . . yes C(4) C(5) 1.43(2) . . yes C(5) C(8) 1.40(2) . . yes C(6) C(7) 1.42(2) . . yes C(8) C(9) 1.44(2) . . yes C(9) C(10) 1.34(2) . . yes C(11) C(12) 1.34(2) . . yes C(13) C(14) 1.31(2) . . yes C(15) C(16) 1.38(2) . . yes C(16) C(17) 1.43(2) . . yes C(17) C(20) 1.43(2) . . yes C(18) C(19) 1.36(2) . . yes C(20) C(21) 1.40(2) . . yes C(21) C(22) 1.35(2) . . yes C(23) C(24) 1.31(2) . . yes C(25) C(26) 1.33(3) . . yes C(25) C(27) 1.47(4) . . yes C(26) C(27) 1.34(4) . 2_576 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(3) 95.1(7) . 1_555 1_555 yes C(2) S(2) C(3) 94.1(7) . 1_555 1_555 yes C(10) S(3) C(11) 96.2(7) . 1_555 1_555 yes C(10) S(4) C(12) 94.9(7) . 1_555 1_555 yes C(13) S(5) C(15) 94.4(7) . 1_555 1_555 yes C(14) S(6) C(15) 93.3(7) . 1_555 1_555 yes C(22) S(7) C(23) 94.6(9) . 1_555 1_555 yes C(22) S(8) C(24) 95.7(8) . 1_555 1_555 yes F(1) P F(2) 92.3(10) . 1_555 1_555 yes F(1) P F(3) 179.8(9) . 1_555 1_555 yes F(1) P F(4) 91(1) . 1_555 1_555 yes F(1) P F(5) 89.9(6) . 1_555 1_555 yes F(1) P F(6) 90.7(6) . 1_555 1_555 yes F(2) P F(3) 87.6(10) . 1_555 1_555 yes F(2) P F(4) 176(1) . 1_555 1_555 yes F(2) P F(5) 85.7(9) . 1_555 1_555 yes F(2) P F(6) 90.1(9) . 1_555 1_555 yes F(3) P F(4) 88.9(10) . 1_555 1_555 yes F(3) P F(5) 90.2(6) . 1_555 1_555 yes F(3) P F(6) 89.2(6) . 1_555 1_555 yes F(4) P F(5) 93(1) . 1_555 1_555 yes F(4) P F(6) 90(1) . 1_555 1_555 yes F(5) P F(6) 175(1) . 1_555 1_555 yes C(4) O(1) C(9) 108.4(10) . 1_555 1_555 yes C(16) O(2) C(21) 107(1) . 1_555 1_555 yes C(5) N(1) C(6) 113(1) . 1_555 1_555 yes C(7) N(2) C(8) 112(1) . 1_555 1_555 yes C(17) N(3) C(18) 110(1) . 1_555 1_555 yes C(19) N(4) C(20) 113(1) . 1_555 1_555 yes S(1) C(1) C(2) 117(1) . 1_555 1_555 yes S(2) C(2) C(1) 118(1) . 1_555 1_555 yes S(1) C(3) S(2) 114.6(8) . 1_555 1_555 yes S(1) C(3) C(4) 122(1) . 1_555 1_555 yes S(2) C(3) C(4) 123(1) . 1_555 1_555 yes O(1) C(4) C(3) 118(1) . 1_555 1_555 yes O(1) C(4) C(5) 108(1) . 1_555 1_555 yes C(3) C(4) C(5) 132(1) . 1_555 1_555 yes N(1) C(5) C(4) 129(1) . 1_555 1_555 yes N(1) C(5) C(8) 123(1) . 1_555 1_555 yes C(4) C(5) C(8) 107(1) . 1_555 1_555 yes N(1) C(6) C(7) 123(1) . 1_555 1_555 yes N(2) C(7) C(6) 122(1) . 1_555 1_555 yes N(2) C(8) C(5) 124(1) . 1_555 1_555 yes N(2) C(8) C(9) 127(1) . 1_555 1_555 yes C(5) C(8) C(9) 107(1) . 1_555 1_555 yes O(1) C(9) C(8) 107(1) . 1_555 1_555 yes O(1) C(9) C(10) 119(1) . 1_555 1_555 yes C(8) C(9) C(10) 133(1) . 1_555 1_555 yes S(3) C(10) S(4) 114.1(8) . 1_555 1_555 yes S(3) C(10) C(9) 123(1) . 1_555 1_555 yes S(4) C(10) C(9) 122(1) . 1_555 1_555 yes S(3) C(11) C(12) 117(1) . 1_555 1_555 yes S(4) C(12) C(11) 117(1) . 1_555 1_555 yes S(5) C(13) C(14) 116(1) . 1_555 1_555 yes S(6) C(14) C(13) 119(1) . 1_555 1_555 yes S(5) C(15) S(6) 116.6(7) . 1_555 1_555 yes S(5) C(15) C(16) 122(1) . 1_555 1_555 yes S(6) C(15) C(16) 120(1) . 1_555 1_555 yes O(2) C(16) C(15) 118(1) . 1_555 1_555 yes O(2) C(16) C(17) 108(1) . 1_555 1_555 yes C(15) C(16) C(17) 132(1) . 1_555 1_555 yes N(3) C(17) C(16) 128(1) . 1_555 1_555 yes N(3) C(17) C(20) 125(1) . 1_555 1_555 yes C(16) C(17) C(20) 106(1) . 1_555 1_555 yes N(3) C(18) C(19) 125(1) . 1_555 1_555 yes N(4) C(19) C(18) 123(1) . 1_555 1_555 yes N(4) C(20) C(17) 121(1) . 1_555 1_555 yes N(4) C(20) C(21) 130(1) . 1_555 1_555 yes C(17) C(20) C(21) 108(1) . 1_555 1_555 yes O(2) C(21) C(20) 108(1) . 1_555 1_555 yes O(2) C(21) C(22) 118(1) . 1_555 1_555 yes C(20) C(21) C(22) 132(1) . 1_555 1_555 yes S(7) C(22) S(8) 114.0(8) . 1_555 1_555 yes S(7) C(22) C(21) 122(1) . 1_555 1_555 yes S(8) C(22) C(21) 123(1) . 1_555 1_555 yes S(7) C(23) C(24) 116(1) . 1_555 1_555 yes S(8) C(24) C(23) 119(1) . 1_555 1_555 yes Cl C(25) C(26) 134(4) . 1_555 1_555 yes Cl C(25) C(27) 95(1) . 1_555 1_555 yes C(26) C(25) C(27) 128(3) . 1_555 1_555 yes C(25) C(26) C(27) 134(3) . 1_555 2_576 yes C(25) C(27) C(26) 96(1) . 1_555 2_576 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl S(7) 3.398(5) . 1_566 ? Cl S(5) 3.525(5) . 2_566 ? S(1) C(25) 3.49(2) . 1_545 ? S(1) C(26) 3.49(2) . 1_545 ? S(2) S(6) 3.282(5) . 2_656 ? S(3) F(1) 3.40(1) . 2_566 ? S(3) C(23) 3.57(2) . . ? S(4) F(6) 3.33(1) . 1_556 ? S(5) C(1) 3.58(2) . . ? S(6) S(6) 3.543(8) . 2_656 ? S(6) C(2) 3.55(2) . . ? S(6) C(2) 3.58(2) . 1_554 ? S(8) F(6) 3.42(1) . . ? S(8) C(10) 3.51(1) . 1_554 ? S(8) C(10) 3.51(1) . . ? F(1) C(11) 3.10(2) . 2_566 ? F(1) C(23) 3.41(2) . 2_566 ? F(1) C(24) 3.44(2) . . ? F(2) C(12) 3.34(2) . . ? F(3) C(1) 3.32(2) . 1_565 ? F(3) C(2) 3.38(2) . 1_565 ? F(3) C(13) 3.43(2) . 1_566 ? F(3) C(14) 3.47(2) . 1_566 ? F(3) C(6) 3.53(2) . 2_667 ? F(4) C(13) 3.40(2) . 1_565 ? F(5) C(27) 3.24(1) . 2_576 ? F(5) C(13) 3.46(2) . 1_566 ? F(5) C(1) 3.56(2) . 1_565 ? F(6) C(24) 3.36(2) . . ? F(6) C(12) 3.40(2) . 1_554 ? F(6) C(6) 3.60(2) . 2_667 ? O(1) C(21) 3.46(2) . . ? O(1) C(21) 3.51(2) . 1_556 ? N(1) C(18) 3.49(2) . 1_556 ? N(1) C(18) 3.56(2) . . ? N(2) C(7) 3.38(2) . 2_667 ? N(2) N(2) 3.54(2) . 2_667 ? N(2) N(4) 3.57(2) . 1_556 ? N(2) C(19) 3.59(2) . 2_667 ? N(4) C(8) 3.51(2) . 1_554 ? N(4) C(8) 3.54(2) . . ? N(4) C(7) 3.55(2) . 2_667 ? C(2) C(14) 3.60(3) . 1_556 ? C(3) C(16) 3.48(2) . 1_556 ? C(3) C(16) 3.49(2) . . ? C(4) C(20) 3.57(2) . . ? C(5) C(20) 3.53(2) . 1_556 ? C(6) C(19) 3.47(3) . 1_556 ? C(6) C(18) 3.59(3) . 1_556 ? C(7) C(19) 3.53(3) . 1_556 ? C(11) C(24) 3.52(3) . . ? C(11) C(24) 3.59(3) . 1_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_RU3B #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C27 H12 As Cl F6 N4 O2 S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 905.26 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 15.66(2) _cell_length_b 16.531(10) _cell_length_c 6.980(3) _cell_angle_alpha 104.21(2) _cell_angle_beta 102.92(3) _cell_angle_gamma 96.42(5) _cell_volume 1680(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 288.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.657 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 4577 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.11 _diffrn_measured_fraction_theta_max 0.4629 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.4629 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.9 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 4.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4577 _reflns_number_gt 1749 _reflns_threshold_expression F^2^>4.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.0884 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1749 _refine_ls_number_parameters 402 _refine_ls_goodness_of_fit_ref 0.241 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.3952 _refine_diff_density_max 1.72 _refine_diff_density_min -2.02 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As As 0.1857(2) 0.7053(2) 0.5563(5) 0.0605(8) Uiso 1.00 d . . . Cl Cl 0.000(2) 1.118(2) 0.833(5) 0.19(1) Uani 0.50 d P . . S1 S 0.2274(4) 0.0674(3) 0.7350(10) 0.050(2) Uani 1.00 d . . . S2 S 0.4214(4) 0.0786(3) 0.8584(9) 0.045(2) Uani 1.00 d . . . S3 S 0.1166(4) 0.3547(4) 0.8374(9) 0.052(2) Uani 1.00 d . . . S4 S 0.2569(5) 0.5043(3) 1.0327(10) 0.058(2) Uani 1.00 d . . . S5 S 0.2141(4) -0.0164(4) 0.179(1) 0.055(2) Uani 1.00 d . . . S6 S 0.4072(4) -0.0058(4) 0.2920(9) 0.054(2) Uani 1.00 d . . . S7 S 0.1051(5) 0.2694(4) 0.286(1) 0.067(2) Uani 1.00 d . . . S8 S 0.2428(6) 0.4218(4) 0.4652(10) 0.065(2) Uani 1.00 d . . . F1 F 0.092(1) 0.638(1) 0.434(5) 0.26(1) Uani 1.00 d . . . F2 F 0.195(2) 0.678(2) 0.754(4) 0.21(1) Uani 1.00 d . . . F3 F 0.280(1) 0.774(1) 0.680(4) 0.183(10) Uani 1.00 d . . . F4 F 0.185(2) 0.736(2) 0.368(4) 0.26(2) Uani 1.00 d . . . F5 F 0.125(1) 0.776(1) 0.658(4) 0.165(9) Uani 1.00 d . . . F6 F 0.246(1) 0.6315(10) 0.473(4) 0.172(9) Uani 1.00 d . . . O1 O 0.264(1) 0.2538(8) 0.876(2) 0.043(5) Uani 1.00 d . . . O2 O 0.253(1) 0.1725(8) 0.317(2) 0.042(5) Uani 1.00 d . . . N1 N 0.501(1) 0.277(1) 1.036(3) 0.059(7) Uani 1.00 d . . . N2 N 0.440(1) 0.435(1) 1.112(3) 0.056(7) Uani 1.00 d . . . N3 N 0.492(1) 0.189(1) 0.469(3) 0.048(2) Uiso 1.00 d . . . N4 N 0.429(2) 0.352(1) 0.544(3) 0.071(8) Uani 1.00 d . . . C1 C 0.269(2) -0.027(1) 0.696(4) 0.055(1) Uiso 1.00 d . . . C2 C 0.355(2) -0.023(1) 0.747(3) 0.055(8) Uani 1.00 d . . . C3 C 0.332(1) 0.132(1) 0.840(3) 0.040(7) Uani 1.00 d . . . C4 C 0.340(1) 0.216(1) 0.900(3) 0.035(2) Uiso 1.00 d . . . C5 C 0.414(1) 0.285(1) 0.992(3) 0.045(8) Uani 1.00 d . . . C6 C 0.556(2) 0.350(2) 1.122(4) 0.08(1) Uani 1.00 d . . . C7 C 0.523(2) 0.429(1) 1.162(4) 0.068(9) Uani 1.00 d . . . C8 C 0.383(2) 0.361(1) 1.022(3) 0.058(8) Uani 1.00 d . . . C9 C 0.289(2) 0.341(1) 0.952(3) 0.041(7) Uani 1.00 d . . . C10 C 0.229(1) 0.394(1) 0.940(3) 0.028(2) Uiso 1.00 d . . . C11 C 0.084(2) 0.454(1) 0.877(4) 0.060(8) Uani 1.00 d . . . C12 C 0.148(2) 0.520(1) 0.966(4) 0.058(8) Uani 1.00 d . . . C13 C 0.255(2) -0.108(1) 0.137(4) 0.058(8) Uani 1.00 d . . . C14 C 0.341(2) -0.102(1) 0.191(4) 0.064(9) Uani 1.00 d . . . C15 C 0.319(1) 0.047(1) 0.276(3) 0.036(6) Uani 1.00 d . . . C16 C 0.327(2) 0.130(1) 0.334(3) 0.046(7) Uani 1.00 d . . . C17 C 0.409(2) 0.199(1) 0.429(3) 0.042(7) Uani 1.00 d . . . C18 C 0.545(2) 0.266(2) 0.550(4) 0.072(10) Uani 1.00 d . . . C19 C 0.515(2) 0.341(2) 0.584(4) 0.074(1) Uiso 1.00 d . . . C20 C 0.374(1) 0.277(1) 0.462(3) 0.038(1) Uiso 1.00 d . . . C21 C 0.285(2) 0.260(1) 0.391(3) 0.043(1) Uiso 1.00 d . . . C22 C 0.216(2) 0.309(1) 0.380(3) 0.058(8) Uani 1.00 d . . . C23 C 0.067(2) 0.369(2) 0.327(4) 0.08(1) Uani 1.00 d . . . C24 C 0.133(2) 0.436(2) 0.402(4) 0.08(1) Uani 1.00 d . . . C25 C -0.003(3) 1.057(4) 0.67(1) 0.20(3) Uani 1.00 d . . . C26 C 0.005(4) 0.977(5) 0.694(8) 0.20(2) Uani 1.00 d . . . C27 C -0.002(3) 1.077(3) 0.489(10) 0.22(2) Uani 1.00 d . . . H1 H 0.2300 -0.0823 0.6376 0.0632 Uiso 1.00 calc . . . H2 H 0.3828 -0.0734 0.7248 0.0621 Uiso 1.00 calc . . . H3 H 0.6219 0.3508 1.1592 0.0909 Uiso 1.00 calc . . . H4 H 0.5680 0.4804 1.2300 0.0813 Uiso 1.00 calc . . . H5 H 0.0204 0.4595 0.8343 0.0705 Uiso 1.00 calc . . . H6 H 0.1346 0.5771 0.9939 0.0662 Uiso 1.00 calc . . . H7 H 0.2165 -0.1624 0.0726 0.0681 Uiso 1.00 calc . . . H8 H 0.3677 -0.1536 0.1749 0.0748 Uiso 1.00 calc . . . H9 H 0.6084 0.2649 0.5839 0.0838 Uiso 1.00 calc . . . H10 H 0.5615 0.3928 0.6443 0.0831 Uiso 1.00 calc . . . H11 H 0.0030 0.3729 0.2961 0.0976 Uiso 1.00 calc . . . H12 H 0.1183 0.4925 0.4229 0.0963 Uiso 1.00 calc . . . H13 H 0.0043 0.9551 0.8105 0.2015 Uiso 1.00 calc . . . H15 H -0.0034 1.1379 0.5021 0.2276 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl 0.16(2) 0.13(2) 0.22(3) -0.07(2) 0.08(2) -0.05(2) S1 0.052(4) 0.028(3) 0.064(4) -0.002(3) 0.017(3) 0.005(3) S2 0.043(4) 0.038(3) 0.058(4) 0.010(3) 0.020(3) 0.011(3) S3 0.055(5) 0.047(4) 0.053(4) 0.015(3) 0.016(3) 0.007(3) S4 0.081(5) 0.027(3) 0.067(4) 0.018(3) 0.019(4) 0.009(3) S5 0.048(5) 0.046(4) 0.065(4) 0.003(3) 0.011(3) 0.012(3) S6 0.060(5) 0.046(4) 0.059(4) 0.020(3) 0.016(3) 0.015(3) S7 0.084(6) 0.044(4) 0.072(5) 0.019(4) 0.021(4) 0.012(3) S8 0.107(7) 0.032(3) 0.060(4) 0.010(4) 0.031(4) 0.014(3) F1 0.05(1) 0.11(2) 0.44(4) -0.01(1) -0.02(2) -0.13(2) F2 0.27(3) 0.19(2) 0.21(3) 0.06(2) 0.13(2) 0.07(2) F3 0.13(2) 0.05(1) 0.30(3) -0.03(1) 0.04(2) -0.06(1) F4 0.32(4) 0.32(4) 0.13(2) 0.03(3) 0.03(2) 0.08(2) F5 0.09(1) 0.07(1) 0.30(3) 0.046(10) 0.03(2) -0.02(1) F6 0.10(1) 0.06(1) 0.29(3) -0.002(10) 0.04(2) -0.07(1) O1 0.06(1) 0.026(8) 0.044(9) 0.005(7) 0.015(8) 0.003(6) O2 0.06(1) 0.023(7) 0.043(9) -0.008(7) 0.011(8) 0.007(6) N1 0.07(2) 0.05(1) 0.06(1) -0.01(1) 0.01(1) 0.018(10) N2 0.06(2) 0.03(1) 0.06(1) -0.01(1) -0.01(1) 0.015(9) N4 0.11(2) 0.04(1) 0.05(1) 0.00(1) 0.02(1) 0.001(10) C2 0.11(2) 0.009(10) 0.05(1) 0.01(1) 0.04(1) -0.001(9) C3 0.05(2) 0.04(1) 0.04(1) 0.02(1) 0.02(1) 0.009(10) C5 0.02(1) 0.08(2) 0.04(1) 0.00(1) 0.02(1) 0.02(1) C6 0.05(2) 0.09(2) 0.07(2) -0.01(2) -0.02(1) 0.03(2) C7 0.08(2) 0.02(1) 0.07(2) -0.04(1) -0.02(2) 0.01(1) C8 0.09(2) 0.02(1) 0.06(2) 0.02(1) 0.02(1) 0.00(1) C9 0.03(2) 0.07(2) 0.04(1) 0.02(1) 0.02(1) 0.02(1) C11 0.07(2) 0.03(1) 0.07(2) 0.02(1) 0.01(1) 0.02(1) C12 0.07(2) 0.03(1) 0.07(2) 0.02(1) 0.02(1) 0.01(1) C13 0.04(2) 0.04(1) 0.08(2) -0.02(1) 0.00(1) 0.02(1) C14 0.08(2) 0.05(2) 0.08(2) 0.03(1) 0.02(2) 0.04(1) C15 0.04(1) 0.018(10) 0.04(1) -0.02(1) 0.00(1) 0.003(9) C16 0.03(1) 0.04(1) 0.06(2) 0.01(1) 0.01(1) 0.01(1) C17 0.09(2) 0.012(9) 0.03(1) 0.00(1) 0.02(1) 0.016(8) C18 0.06(2) 0.08(2) 0.07(2) 0.00(2) 0.03(1) 0.02(1) C22 0.12(2) 0.03(1) 0.03(1) -0.01(1) 0.02(1) 0.010(9) C23 0.11(2) 0.09(2) 0.08(2) 0.07(2) 0.05(2) 0.04(2) C24 0.15(3) 0.07(2) 0.05(2) 0.03(2) 0.03(2) 0.05(1) C25 0.06(3) 0.22(5) 0.39(8) 0.03(3) 0.11(4) 0.16(5) C26 0.11(4) 0.37(7) 0.18(4) 0.02(4) 0.02(3) 0.20(4) C27 0.07(3) 0.24(3) 0.43(5) -0.02(3) -0.01(4) 0.31(3) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag AS F1 1.65(2) . . yes AS F2 1.53(3) . . yes AS F3 1.67(2) . . yes AS F4 1.52(3) . . yes AS F5 1.70(2) . . yes AS F6 1.70(2) . . yes CL C25 1.32(6) . . yes S1 C1 1.74(2) . . yes S1 C3 1.75(2) . . yes S2 C2 1.77(2) . . yes S2 C3 1.73(2) . . yes S3 C10 1.73(2) . . yes S3 C11 1.75(2) . . yes S4 C10 1.75(2) . . yes S4 C12 1.74(3) . . yes S5 C13 1.69(2) . . yes S5 C15 1.74(2) . . yes S6 C14 1.69(3) . . yes S6 C15 1.72(2) . . yes S7 C22 1.70(3) . . yes S7 C23 1.79(3) . . yes S8 C22 1.78(2) . . yes S8 C24 1.73(4) . . yes O1 C4 1.40(2) . . yes O1 C9 1.38(2) . . yes O2 C16 1.41(2) . . yes O2 C21 1.41(2) . . yes N1 C5 1.36(3) . . yes N1 C6 1.32(3) . . yes N2 C7 1.29(3) . . yes N2 C8 1.34(3) . . yes N3 C17 1.31(3) . . yes N3 C18 1.35(3) . . yes N4 C19 1.36(3) . . yes N4 C20 1.35(3) . . yes C1 C2 1.31(3) . . yes C3 C4 1.34(3) . . yes C4 C5 1.43(3) . . yes C5 C8 1.39(3) . . yes C6 C7 1.45(4) . . yes C8 C9 1.42(3) . . yes C9 C10 1.36(3) . . yes C11 C12 1.31(3) . . yes C13 C14 1.29(3) . . yes C15 C16 1.32(3) . . yes C16 C17 1.52(3) . . yes C17 C20 1.44(3) . . yes C18 C19 1.36(3) . . yes C20 C21 1.34(3) . . yes C21 C22 1.42(3) . . yes C23 C24 1.33(4) . . yes C25 C26 1.38(7) . . yes C25 C27 1.37(7) . . yes C26 C27 1.35(8) . 2_576 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 F1 AS F2 94(1) . 1_555 1_555 yes F1 AS F3 179(1) . 1_555 1_555 yes F1 AS F4 90(1) . 1_555 1_555 yes F1 AS F5 88.9(10) . 1_555 1_555 yes F1 AS F6 90.7(9) . 1_555 1_555 yes F2 AS F3 85(1) . 1_555 1_555 yes F2 AS F4 174(1) . 1_555 1_555 yes F2 AS F5 85(1) . 1_555 1_555 yes F2 AS F6 89(1) . 1_555 1_555 yes F3 AS F4 89(1) . 1_555 1_555 yes F3 AS F5 90.8(9) . 1_555 1_555 yes F3 AS F6 89.6(9) . 1_555 1_555 yes F4 AS F5 95(1) . 1_555 1_555 yes F4 AS F6 89(1) . 1_555 1_555 yes F5 AS F6 174(1) . 1_555 1_555 yes C1 S1 C3 94(1) . 1_555 1_555 yes C2 S2 C3 94(1) . 1_555 1_555 yes C10 S3 C11 95(1) . 1_555 1_555 yes C10 S4 C12 94.0(10) . 1_555 1_555 yes C13 S5 C15 93(1) . 1_555 1_555 yes C14 S6 C15 92(1) . 1_555 1_555 yes C22 S7 C23 97(1) . 1_555 1_555 yes C22 S8 C24 94(1) . 1_555 1_555 yes C4 O1 C9 109(1) . 1_555 1_555 yes C16 O2 C21 108(1) . 1_555 1_555 yes C5 N1 C6 113(2) . 1_555 1_555 yes C7 N2 C8 115(2) . 1_555 1_555 yes C17 N3 C18 108(1) . 1_555 1_555 yes C19 N4 C20 110(2) . 1_555 1_555 yes S1 C1 C2 118(1) . 1_555 1_555 yes S2 C2 C1 116(1) . 1_555 1_555 yes S1 C3 S2 115(1) . 1_555 1_555 yes S1 C3 C4 120(1) . 1_555 1_555 yes S2 C3 C4 124(1) . 1_555 1_555 yes O1 C4 C3 120(1) . 1_555 1_555 yes O1 C4 C5 105(1) . 1_555 1_555 yes C3 C4 C5 134(2) . 1_555 1_555 yes N1 C5 C4 125(2) . 1_555 1_555 yes N1 C5 C8 125(2) . 1_555 1_555 yes C4 C5 C8 109(2) . 1_555 1_555 yes N1 C6 C7 120(2) . 1_555 1_555 yes N2 C7 C6 124(2) . 1_555 1_555 yes N2 C8 C5 120(2) . 1_555 1_555 yes N2 C8 C9 132(2) . 1_555 1_555 yes C5 C8 C9 106(1) . 1_555 1_555 yes O1 C9 C8 109(1) . 1_555 1_555 yes O1 C9 C10 122(1) . 1_555 1_555 yes C8 C9 C10 128(2) . 1_555 1_555 yes S3 C10 S4 115(1) . 1_555 1_555 yes S3 C10 C9 120(1) . 1_555 1_555 yes S4 C10 C9 124(1) . 1_555 1_555 yes S3 C11 C12 116(2) . 1_555 1_555 yes S4 C12 C11 119(1) . 1_555 1_555 yes S5 C13 C14 117(1) . 1_555 1_555 yes S6 C14 C13 120(1) . 1_555 1_555 yes S5 C15 S6 115(1) . 1_555 1_555 yes S5 C15 C16 120(1) . 1_555 1_555 yes S6 C15 C16 123(1) . 1_555 1_555 yes O2 C16 C15 122(1) . 1_555 1_555 yes O2 C16 C17 106(1) . 1_555 1_555 yes C15 C16 C17 130(2) . 1_555 1_555 yes N3 C17 C16 127(1) . 1_555 1_555 yes N3 C17 C20 129(1) . 1_555 1_555 yes C16 C17 C20 103(2) . 1_555 1_555 yes N3 C18 C19 125(2) . 1_555 1_555 yes N4 C19 C18 126(2) . 1_555 1_555 yes N4 C20 C17 120(2) . 1_555 1_555 yes N4 C20 C21 129(2) . 1_555 1_555 yes C17 C20 C21 110(1) . 1_555 1_555 yes O2 C21 C20 111(1) . 1_555 1_555 yes O2 C21 C22 113(1) . 1_555 1_555 yes C20 C21 C22 135(2) . 1_555 1_555 yes S7 C22 S8 114(1) . 1_555 1_555 yes S7 C22 C21 125(1) . 1_555 1_555 yes S8 C22 C21 119(1) . 1_555 1_555 yes S7 C23 C24 113(2) . 1_555 1_555 yes S8 C24 C23 120(2) . 1_555 1_555 yes CL C25 C26 117(6) . 1_555 1_555 yes CL C25 C27 119(5) . 1_555 1_555 yes C26 C25 C27 122(5) . 1_555 1_555 yes C25 C26 C27 109(4) . 1_555 2_576 yes C25 C27 C26 127(4) . 1_555 2_576 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CL S7 3.44(2) . 1_566 ? CL S5 3.55(3) . 2_566 ? S1 C25 3.51(4) . 1_545 ? S1 C26 3.55(6) . 1_545 ? S2 S6 3.333(8) . 2_656 ? S3 F1 3.43(2) . 2_566 ? S3 C23 3.55(3) . . ? S4 F6 3.32(2) . 1_556 ? S5 C1 3.57(3) . . ? S6 C2 3.52(2) . . ? S6 S6 3.57(1) . 2_656 ? S8 F6 3.45(2) . . ? S8 C10 3.51(2) . . ? S8 C10 3.54(2) . 1_554 ? F1 C11 3.07(3) . 2_566 ? F1 C23 3.31(4) . 2_566 ? F1 C24 3.44(4) . . ? F2 C12 3.40(4) . . ? F3 C1 3.29(3) . 1_565 ? F3 C2 3.31(3) . 1_565 ? F3 C13 3.43(4) . 1_566 ? F3 C14 3.50(3) . 1_566 ? F3 C18 3.52(3) . 2_666 ? F4 C13 3.57(4) . 1_565 ? F5 C13 3.46(3) . 1_566 ? F5 C27 3.48(4) . 2_576 ? F6 C24 3.38(3) . . ? F6 C12 3.47(3) . 1_554 ? F6 C18 3.57(3) . 2_666 ? O1 C21 3.50(3) . . ? O1 C21 3.51(3) . 1_556 ? N1 C18 3.55(3) . 1_556 ? N1 C18 3.58(3) . . ? N2 C7 3.37(3) . 2_667 ? N2 N2 3.56(4) . 2_667 ? N4 C8 3.54(3) . . ? N4 C7 3.59(3) . 2_667 ? C3 C16 3.47(3) . 1_556 ? C3 C16 3.51(3) . . ? C4 C20 3.57(3) . . ? C5 C20 3.51(3) . 1_556 ? C5 C20 3.57(3) . . ? C6 C19 3.46(4) . 1_556 ? C9 C22 3.56(3) . 1_556 ? C11 C24 3.52(4) . . ? #------------------------------------------------------------------------------