data_global _audit_creation_date 2017-04-04 _audit_creation_method 'by CrystalStructure 4.2.2' _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_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_references ; ENTER OTHER REFERENCES Rigaku (2016). CrystalStructure. Version 4.2.2. Rigaku Corporation, Tokyo, Japan. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. and Spagna R. (2005). J. Appl. Cryst. 38, 381-388. SIR2004 Sheldrick, G.M. (2008) SHELXL Version 2014/7, Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, 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_170313 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H16 N2 Na2 O12 S2' _chemical_formula_moiety 'C26 H16 N2 Na2 O12 S2' _chemical_formula_weight 658.52 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '+X,-1/2-Y,-1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 21.0006(4) _cell_length_b 8.10823(15) _cell_length_c 7.57570(14) _cell_angle_alpha 90.0000 _cell_angle_beta 97.5156(11) _cell_angle_gamma 90.0000 _cell_volume 1278.89(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4419 _cell_measurement_theta_min 4.25 _cell_measurement_theta_max 68.19 _cell_measurement_temperature 100 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672.00 _exptl_absorpt_coefficient_mu 2.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.971 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 13855 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_theta_max 68.232 _diffrn_reflns_theta_min 4.247 _diffrn_reflns_theta_full 67.687 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 2346 _reflns_number_gt 1842 _reflns_threshold_expression F^2^>2.0\s(F^2^) _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1252 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2346 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.3411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.61 _refine_diff_density_min -0.56 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.0492 0.0322 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.3331 0.5567 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Na' 'Na' 0.1353 0.1239 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.08242(3) 0.05528(9) 0.84125(10) 0.0248(2) Uani 1 1 d . . . . . Na1 Na 0.02008(5) -0.29179(14) 0.95351(15) 0.0299(3) Uani 1 1 d . . . . . O1 O 0.08154(9) -0.0491(2) 0.9971(3) 0.0303(5) Uani 1 1 d . . . . . O2 O 0.30016(9) -0.0354(2) 0.3634(3) 0.0298(5) Uani 1 1 d . . . . . O3 O 0.39303(9) 0.1479(2) 0.9045(3) 0.0296(5) Uani 1 1 d . . . . . O4 O 0.04511(9) -0.0165(3) 0.6847(3) 0.0328(5) Uani 1 1 d . . . . . O5 O 0.06294(9) 0.2247(2) 0.8690(3) 0.0344(5) Uani 1 1 d . . . . . O6 O 0.10980(9) -0.4226(3) 0.8617(3) 0.0324(5) Uani 1 1 d . . . . . N1 N 0.34707(11) 0.0489(3) 0.6367(3) 0.0256(6) Uani 1 1 d . . . . . C3 C 0.16288(13) 0.0603(3) 0.7945(4) 0.0232(6) Uani 1 1 d . . . . . C4 C 0.34941(13) -0.0051(3) 0.4614(4) 0.0253(6) Uani 1 1 d . . . . . C5 C 0.42026(13) -0.0872(3) 0.2398(4) 0.0260(6) Uani 1 1 d . . . . . H5 H 0.3829 -0.1129 0.1597 0.031 Uiso 1 1 calc R U . . . C6 C 0.39981(13) 0.0956(3) 0.7566(4) 0.0249(6) Uani 1 1 d . . . . . C7 C 0.46396(13) 0.0741(3) 0.6979(4) 0.0237(6) Uani 1 1 d . . . . . C8 C 0.41422(13) -0.0272(3) 0.4062(4) 0.0245(6) Uani 1 1 d . . . . . C9 C 0.46906(13) 0.0115(3) 0.5262(4) 0.0243(6) Uani 1 1 d . . . . . C10 C 0.18631(12) 0.2004(4) 0.7195(4) 0.0255(6) Uani 1 1 d . . . . . H10 H 0.1606 0.2970 0.7030 0.031 Uiso 1 1 calc R U . . . C11 C 0.26088(14) -0.0824(4) 0.7715(4) 0.0307(7) Uani 1 1 d . . . . . H11 H 0.2868 -0.1785 0.7890 0.037 Uiso 1 1 calc R U . . . C12 C 0.24783(13) 0.1986(4) 0.6683(4) 0.0268(6) Uani 1 1 d . . . . . H12 H 0.2645 0.2934 0.6165 0.032 Uiso 1 1 calc R U . . . C13 C 0.28371(13) 0.0571(3) 0.6944(4) 0.0251(6) Uani 1 1 d . . . . . C14 C 0.19984(13) -0.0806(4) 0.8227(4) 0.0296(7) Uani 1 1 d . . . . . H14 H 0.1837 -0.1750 0.8764 0.036 Uiso 1 1 calc R U . . . C15 C 0.51878(13) 0.1111(4) 0.8129(4) 0.0272(7) Uani 1 1 d . . . . . H15 H 0.5152 0.1528 0.9283 0.033 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0205(4) 0.0219(4) 0.0332(5) -0.0003(3) 0.0079(3) 0.0000(3) Na1 0.0258(6) 0.0272(7) 0.0381(7) -0.0022(5) 0.0095(5) -0.0011(5) O1 0.0273(11) 0.0291(12) 0.0365(12) 0.0080(9) 0.0113(9) -0.0003(8) O2 0.0220(10) 0.0277(11) 0.0405(13) -0.0042(9) 0.0068(9) -0.0014(8) O3 0.0264(11) 0.0287(12) 0.0348(12) -0.0027(9) 0.0084(9) 0.0004(9) O4 0.0231(10) 0.0414(13) 0.0333(12) -0.0090(10) 0.0016(9) -0.0020(9) O5 0.0270(11) 0.0216(11) 0.0583(14) -0.0020(10) 0.0192(10) 0.0015(8) O6 0.0276(11) 0.0313(12) 0.0391(13) 0.0006(9) 0.0080(9) 0.0004(9) N1 0.0188(12) 0.0257(13) 0.0338(14) 0.0001(10) 0.0087(10) 0.0003(10) C3 0.0193(14) 0.0237(15) 0.0271(16) -0.0037(11) 0.0048(11) -0.0020(11) C4 0.0229(14) 0.0189(15) 0.0348(17) 0.0012(12) 0.0071(12) 0.0022(11) C5 0.0215(14) 0.0241(16) 0.0325(16) 0.0000(12) 0.0033(12) -0.0013(11) C6 0.0209(15) 0.0191(15) 0.0360(17) 0.0014(12) 0.0081(12) -0.0005(11) C7 0.0218(15) 0.0183(14) 0.0321(16) 0.0013(11) 0.0075(12) -0.0005(11) C8 0.0212(14) 0.0213(15) 0.0314(16) 0.0041(12) 0.0045(12) 0.0006(11) C9 0.0236(14) 0.0183(15) 0.0321(16) 0.0020(12) 0.0074(12) 0.0001(11) C10 0.0228(14) 0.0230(15) 0.0312(15) -0.0010(12) 0.0058(12) 0.0028(11) C11 0.0269(15) 0.0231(16) 0.0439(19) 0.0047(13) 0.0117(13) 0.0035(12) C12 0.0264(15) 0.0209(15) 0.0339(16) 0.0007(12) 0.0074(12) -0.0016(12) C13 0.0183(14) 0.0274(16) 0.0303(16) -0.0015(12) 0.0054(12) 0.0000(11) C14 0.0260(16) 0.0231(15) 0.0405(18) 0.0040(13) 0.0073(13) 0.0003(12) C15 0.0256(15) 0.0239(16) 0.0330(16) -0.0002(13) 0.0077(12) -0.0013(12) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.2.2 (Rigaku, 2016)' _computing_molecular_graphics 'CrystalStructure 4.2.2' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O4 1.454(2) . ? S1 O1 1.455(2) . ? S1 O5 1.456(2) . ? S1 C3 1.772(3) . ? S1 Na1 3.1464(13) 2_556 ? S1 Na1 3.2630(13) . ? Na1 O6 2.346(2) . ? Na1 O4 2.350(2) 4_556 ? Na1 O1 2.353(2) . ? Na1 O5 2.399(2) 3_557 ? Na1 O4 2.432(2) 2_546 ? Na1 O5 2.813(3) 2_546 ? Na1 S1 3.1464(13) 2_546 ? Na1 Na1 3.573(2) 3_547 ? Na1 Na1 3.8480(4) 4_556 ? Na1 Na1 3.8480(4) 4 ? O2 C4 1.217(3) . ? O3 C6 1.224(3) . ? O4 Na1 2.350(2) 4 ? O4 Na1 2.432(2) 2_556 ? O5 Na1 2.399(2) 3_557 ? O5 Na1 2.813(3) 2_556 ? N1 C6 1.390(4) . ? N1 C4 1.405(4) . ? N1 C13 1.456(3) . ? C3 C14 1.382(4) . ? C3 C10 1.389(4) . ? C4 C8 1.486(4) . ? C5 C8 1.373(4) . ? C5 C15 1.403(4) 3_656 ? C5 H5 0.9500 . ? C6 C7 1.483(4) . ? C7 C15 1.383(4) . ? C7 C9 1.413(4) . ? C8 C9 1.406(4) . ? C9 C9 1.420(5) 3_656 ? C10 C12 1.397(4) . ? C10 H10 0.9500 . ? C11 C13 1.387(4) . ? C11 C14 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.373(4) . ? C12 H12 0.9500 . ? C14 H14 0.9500 . ? C15 C5 1.404(4) 3_656 ? C15 H15 0.9500 . ? 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_3 _geom_angle_publ_flag O4 S1 O1 111.49(13) . . ? O4 S1 O5 111.31(13) . . ? O1 S1 O5 113.45(12) . . ? O4 S1 C3 105.81(12) . . ? O1 S1 C3 106.80(12) . . ? O5 S1 C3 107.49(12) . . ? O4 S1 Na1 48.20(9) . 2_556 ? O1 S1 Na1 136.48(8) . 2_556 ? O5 S1 Na1 63.37(9) . 2_556 ? C3 S1 Na1 115.54(10) . 2_556 ? O4 S1 Na1 71.08(9) . . ? O1 S1 Na1 40.42(9) . . ? O5 S1 Na1 130.24(8) . . ? C3 S1 Na1 119.82(9) . . ? Na1 S1 Na1 105.32(3) 2_556 . ? O6 Na1 O4 79.14(8) . 4_556 ? O6 Na1 O1 88.44(8) . . ? O4 Na1 O1 112.56(8) 4_556 . ? O6 Na1 O5 159.96(9) . 3_557 ? O4 Na1 O5 80.81(8) 4_556 3_557 ? O1 Na1 O5 99.05(8) . 3_557 ? O6 Na1 O4 87.84(8) . 2_546 ? O4 Na1 O4 83.33(8) 4_556 2_546 ? O1 Na1 O4 162.65(8) . 2_546 ? O5 Na1 O4 90.10(8) 3_557 2_546 ? O6 Na1 O5 101.23(7) . 2_546 ? O4 Na1 O5 137.03(8) 4_556 2_546 ? O1 Na1 O5 110.39(7) . 2_546 ? O5 Na1 O5 93.59(7) 3_557 2_546 ? O4 Na1 O5 53.95(6) 2_546 2_546 ? O6 Na1 S1 96.48(6) . 2_546 ? O4 Na1 S1 109.50(7) 4_556 2_546 ? O1 Na1 S1 137.82(7) . 2_546 ? O5 Na1 S1 90.41(6) 3_557 2_546 ? O4 Na1 S1 26.47(5) 2_546 2_546 ? O5 Na1 S1 27.57(4) 2_546 2_546 ? O6 Na1 S1 87.00(6) . . ? O4 Na1 S1 134.97(7) 4_556 . ? O1 Na1 S1 23.63(5) . . ? O5 Na1 S1 107.23(6) 3_557 . ? O4 Na1 S1 139.13(6) 2_546 . ? O5 Na1 S1 87.53(5) 2_546 . ? S1 Na1 S1 114.55(4) 2_546 . ? O6 Na1 Na1 81.40(6) . 3_547 ? O4 Na1 Na1 42.54(6) 4_556 3_547 ? O1 Na1 Na1 154.44(8) . 3_547 ? O5 Na1 Na1 84.04(6) 3_557 3_547 ? O4 Na1 Na1 40.79(5) 2_546 3_547 ? O5 Na1 Na1 94.63(6) 2_546 3_547 ? S1 Na1 Na1 67.06(4) 2_546 3_547 ? S1 Na1 Na1 168.40(5) . 3_547 ? O6 Na1 Na1 118.35(6) . 4_556 ? O4 Na1 Na1 53.95(6) 4_556 4_556 ? O1 Na1 Na1 77.60(6) . 4_556 ? O5 Na1 Na1 46.76(6) 3_557 4_556 ? O4 Na1 Na1 118.90(6) 2_546 4_556 ? O5 Na1 Na1 140.07(5) 2_546 4_556 ? S1 Na1 Na1 132.84(3) 2_546 4_556 ? S1 Na1 Na1 98.99(4) . 4_556 ? Na1 Na1 Na1 86.67(4) 3_547 4_556 ? O6 Na1 Na1 71.60(6) . 4 ? O4 Na1 Na1 145.24(8) 4_556 4 ? O1 Na1 Na1 85.42(6) . 4 ? O5 Na1 Na1 127.25(6) 3_557 4 ? O4 Na1 Na1 77.32(5) 2_546 4 ? O5 Na1 Na1 38.41(4) 2_546 4 ? S1 Na1 Na1 57.24(2) 2_546 4 ? S1 Na1 Na1 62.61(3) . 4 ? Na1 Na1 Na1 113.01(5) 3_547 4 ? Na1 Na1 Na1 159.71(7) 4_556 4 ? S1 O1 Na1 115.95(12) . . ? S1 O4 Na1 156.43(14) . 4 ? S1 O4 Na1 105.33(11) . 2_556 ? Na1 O4 Na1 96.67(8) 4 2_556 ? S1 O5 Na1 122.22(11) . 3_557 ? S1 O5 Na1 89.06(10) . 2_556 ? Na1 O5 Na1 94.83(7) 3_557 2_556 ? C6 N1 C4 125.4(2) . . ? C6 N1 C13 118.2(2) . . ? C4 N1 C13 116.4(2) . . ? C14 C3 C10 121.2(3) . . ? C14 C3 S1 118.8(2) . . ? C10 C3 S1 119.9(2) . . ? O2 C4 N1 120.5(2) . . ? O2 C4 C8 122.7(3) . . ? N1 C4 C8 116.7(2) . . ? C8 C5 C15 120.5(3) . 3_656 ? C8 C5 H5 119.8 . . ? C15 C5 H5 119.8 3_656 . ? O3 C6 N1 121.0(2) . . ? O3 C6 C7 122.3(3) . . ? N1 C6 C7 116.7(3) . . ? C15 C7 C9 120.0(3) . . ? C15 C7 C6 120.0(3) . . ? C9 C7 C6 120.0(3) . . ? C5 C8 C9 120.4(3) . . ? C5 C8 C4 119.9(3) . . ? C9 C8 C4 119.6(3) . . ? C8 C9 C7 121.4(2) . . ? C8 C9 C9 119.5(3) . 3_656 ? C7 C9 C9 119.1(3) . 3_656 ? C3 C10 C12 119.7(3) . . ? C3 C10 H10 120.2 . . ? C12 C10 H10 120.2 . . ? C13 C11 C14 119.5(3) . . ? C13 C11 H11 120.3 . . ? C14 C11 H11 120.3 . . ? C13 C12 C10 118.6(3) . . ? C13 C12 H12 120.7 . . ? C10 C12 H12 120.7 . . ? C12 C13 C11 121.9(3) . . ? C12 C13 N1 120.1(2) . . ? C11 C13 N1 118.0(2) . . ? C3 C14 C11 119.1(3) . . ? C3 C14 H14 120.4 . . ? C11 C14 H14 120.4 . . ? C7 C15 C5 120.4(3) . 3_656 ? C7 C15 H15 119.8 . . ? C5 C15 H15 119.8 3_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Na1 -1.40(16) . . . . ? O5 S1 O1 Na1 125.22(13) . . . . ? C3 S1 O1 Na1 -116.54(13) . . . . ? Na1 S1 O1 Na1 49.87(17) 2_556 . . . ? O1 S1 O4 Na1 -67.7(4) . . . 4 ? O5 S1 O4 Na1 164.5(3) . . . 4 ? C3 S1 O4 Na1 48.0(4) . . . 4 ? Na1 S1 O4 Na1 158.4(4) 2_556 . . 4 ? Na1 S1 O4 Na1 -68.7(3) . . . 4 ? O1 S1 O4 Na1 133.90(11) . . . 2_556 ? O5 S1 O4 Na1 6.12(14) . . . 2_556 ? C3 S1 O4 Na1 -110.36(12) . . . 2_556 ? Na1 S1 O4 Na1 132.94(9) . . . 2_556 ? O4 S1 O5 Na1 90.02(16) . . . 3_557 ? O1 S1 O5 Na1 -36.69(18) . . . 3_557 ? C3 S1 O5 Na1 -154.53(14) . . . 3_557 ? Na1 S1 O5 Na1 95.12(13) 2_556 . . 3_557 ? Na1 S1 O5 Na1 7.2(2) . . . 3_557 ? O4 S1 O5 Na1 -5.10(12) . . . 2_556 ? O1 S1 O5 Na1 -131.82(10) . . . 2_556 ? C3 S1 O5 Na1 110.34(11) . . . 2_556 ? Na1 S1 O5 Na1 -87.88(10) . . . 2_556 ? O4 S1 C3 C14 -82.9(3) . . . . ? O1 S1 C3 C14 36.0(3) . . . . ? O5 S1 C3 C14 158.1(2) . . . . ? Na1 S1 C3 C14 -133.7(2) 2_556 . . . ? Na1 S1 C3 C14 -6.0(3) . . . . ? O4 S1 C3 C10 92.7(2) . . . . ? O1 S1 C3 C10 -148.4(2) . . . . ? O5 S1 C3 C10 -26.3(3) . . . . ? Na1 S1 C3 C10 41.9(3) 2_556 . . . ? Na1 S1 C3 C10 169.65(19) . . . . ? C6 N1 C4 O2 -176.3(3) . . . . ? C13 N1 C4 O2 3.2(4) . . . . ? C6 N1 C4 C8 5.5(4) . . . . ? C13 N1 C4 C8 -175.0(2) . . . . ? C4 N1 C6 O3 176.8(3) . . . . ? C13 N1 C6 O3 -2.6(4) . . . . ? C4 N1 C6 C7 -4.9(4) . . . . ? C13 N1 C6 C7 175.7(2) . . . . ? O3 C6 C7 C15 1.1(4) . . . . ? N1 C6 C7 C15 -177.2(3) . . . . ? O3 C6 C7 C9 179.3(3) . . . . ? N1 C6 C7 C9 1.1(4) . . . . ? C15 C5 C8 C9 0.1(4) 3_656 . . . ? C15 C5 C8 C4 -179.0(3) 3_656 . . . ? O2 C4 C8 C5 -1.3(4) . . . . ? N1 C4 C8 C5 176.9(3) . . . . ? O2 C4 C8 C9 179.5(3) . . . . ? N1 C4 C8 C9 -2.3(4) . . . . ? C5 C8 C9 C7 179.7(3) . . . . ? C4 C8 C9 C7 -1.1(4) . . . . ? C5 C8 C9 C9 0.2(5) . . . 3_656 ? C4 C8 C9 C9 179.3(3) . . . 3_656 ? C15 C7 C9 C8 180.0(3) . . . . ? C6 C7 C9 C8 1.8(4) . . . . ? C15 C7 C9 C9 -0.4(5) . . . 3_656 ? C6 C7 C9 C9 -178.7(3) . . . 3_656 ? C14 C3 C10 C12 1.2(4) . . . . ? S1 C3 C10 C12 -174.3(2) . . . . ? C3 C10 C12 C13 -0.1(4) . . . . ? C10 C12 C13 C11 -0.7(4) . . . . ? C10 C12 C13 N1 177.7(3) . . . . ? C14 C11 C13 C12 0.6(5) . . . . ? C14 C11 C13 N1 -177.9(3) . . . . ? C6 N1 C13 C12 90.4(3) . . . . ? C4 N1 C13 C12 -89.1(3) . . . . ? C6 N1 C13 C11 -91.1(3) . . . . ? C4 N1 C13 C11 89.4(3) . . . . ? C10 C3 C14 C11 -1.3(4) . . . . ? S1 C3 C14 C11 174.2(2) . . . . ? C13 C11 C14 C3 0.4(5) . . . . ? C9 C7 C15 C5 0.2(4) . . . 3_656 ? C6 C7 C15 C5 178.4(2) . . . 3_656 ? #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 170313 CELL 1.54187 21.00058 8.10823 7.57570 90.00000 97.51560 90.00000 ZERR 2 0.00038 0.00015 0.00014 0.00000 0.00110 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H O N S NA UNIT 52 32 24 4 4 4 L.S. 5 FMAP 2 PLAN 52 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -173.0 ACTA SIZE 0.100 0.100 0.010 WGHT 0.073200 0.341100 FVAR 1.57308 S1 5 0.082418 0.055280 0.841250 11.00000 0.02054 0.02194 = 0.03320 -0.00028 0.00789 -0.00002 NA1 6 0.020083 -0.291789 0.953510 11.00000 0.02583 0.02720 = 0.03810 -0.00215 0.00954 -0.00107 O1 3 0.081542 -0.049075 0.997091 11.00000 0.02727 0.02908 = 0.03652 0.00799 0.01129 -0.00032 O2 3 0.300160 -0.035409 0.363355 11.00000 0.02200 0.02767 = 0.04054 -0.00416 0.00675 -0.00139 O3 3 0.393033 0.147879 0.904473 11.00000 0.02645 0.02867 = 0.03475 -0.00269 0.00843 0.00037 O4 3 0.045108 -0.016465 0.684727 11.00000 0.02310 0.04137 = 0.03333 -0.00896 0.00161 -0.00195 O5 3 0.062940 0.224692 0.869004 11.00000 0.02703 0.02157 = 0.05828 -0.00203 0.01925 0.00148 O6 3 0.109803 -0.422648 0.861722 11.00000 0.02764 0.03131 = 0.03910 0.00055 0.00805 0.00037 N1 4 0.347074 0.048887 0.636663 11.00000 0.01879 0.02568 = 0.03381 0.00009 0.00868 0.00026 C3 1 0.162877 0.060257 0.794544 11.00000 0.01928 0.02368 = 0.02714 -0.00367 0.00475 -0.00200 C4 1 0.349409 -0.005066 0.461397 11.00000 0.02295 0.01894 = 0.03479 0.00123 0.00711 0.00215 C5 1 0.420257 -0.087246 0.239811 11.00000 0.02154 0.02407 = 0.03247 0.00004 0.00330 -0.00135 AFIX 43 H5 2 0.382888 -0.112858 0.159728 11.00000 -1.20000 AFIX 0 C6 1 0.399812 0.095570 0.756587 11.00000 0.02090 0.01908 = 0.03601 0.00138 0.00808 -0.00055 C7 1 0.463956 0.074081 0.697883 11.00000 0.02179 0.01825 = 0.03211 0.00125 0.00748 -0.00053 C8 1 0.414223 -0.027222 0.406249 11.00000 0.02121 0.02127 = 0.03138 0.00408 0.00448 0.00064 C9 1 0.469060 0.011522 0.526215 11.00000 0.02363 0.01825 = 0.03212 0.00195 0.00740 0.00012 C10 1 0.186306 0.200398 0.719467 11.00000 0.02278 0.02295 = 0.03121 -0.00101 0.00575 0.00276 AFIX 43 H10 2 0.160602 0.296972 0.703005 11.00000 -1.20000 AFIX 0 C11 1 0.260877 -0.082435 0.771461 11.00000 0.02689 0.02310 = 0.04391 0.00465 0.01170 0.00350 AFIX 43 H11 2 0.286840 -0.178483 0.789017 11.00000 -1.20000 AFIX 0 C12 1 0.247826 0.198645 0.668304 11.00000 0.02644 0.02091 = 0.03387 0.00068 0.00740 -0.00155 AFIX 43 H12 2 0.264494 0.293402 0.616543 11.00000 -1.20000 AFIX 0 C13 1 0.283710 0.057096 0.694385 11.00000 0.01826 0.02740 = 0.03028 -0.00149 0.00541 -0.00002 C14 1 0.199836 -0.080640 0.822708 11.00000 0.02605 0.02310 = 0.04047 0.00398 0.00733 0.00027 AFIX 43 H14 2 0.183659 -0.174991 0.876437 11.00000 -1.20000 AFIX 0 C15 1 0.518778 0.111050 0.812915 11.00000 0.02557 0.02390 = 0.03303 -0.00022 0.00774 -0.00132 AFIX 43 H15 2 0.515151 0.152818 0.928338 11.00000 -1.20000 AFIX 0 HKLF 4 REM 170313 REM R1 = 0.0461 for 1842 Fo > 4sig(Fo) and 0.0581 for all 2346 data REM 199 parameters refined using 0 restraints END WGHT 0.0732 0.3411 REM Instructions for potential hydrogen bonds EQIV $1 x, -y-1/2, z+1/2 HTAB C11 O2_$1 HTAB C14 O6 REM Highest difference peak 0.611, deepest hole -0.564, 1-sigma level 0.078 Q1 1 0.1010 -0.5397 0.9055 11.00000 0.05 0.61 Q2 1 0.1082 -0.4400 0.7253 11.00000 0.05 0.55 Q3 1 0.0730 -0.4689 0.8154 11.00000 0.05 0.36 Q4 1 0.1316 0.0669 0.8283 11.00000 0.05 0.32 Q5 1 0.1050 0.2875 0.8745 11.00000 0.05 0.30 Q6 1 0.0327 0.1755 0.8482 11.00000 0.05 0.29 Q7 1 0.2298 -0.0814 0.8052 11.00000 0.05 0.25 Q8 1 0.1691 -0.0379 0.7801 11.00000 0.05 0.25 Q9 1 0.0814 0.1956 0.7872 11.00000 0.05 0.25 Q10 1 0.1228 -0.5511 0.7523 11.00000 0.05 0.22 Q11 1 0.0800 -0.0866 0.7291 11.00000 0.05 0.22 Q12 1 0.3239 0.0556 0.6513 11.00000 0.05 0.22 Q13 1 0.0800 -0.2875 0.9063 11.00000 0.05 0.22 Q14 1 0.2189 0.1985 0.6995 11.00000 0.05 0.22 Q15 1 0.1809 -0.4531 0.7965 11.00000 0.05 0.21 Q16 1 0.0905 0.1043 1.1344 11.00000 0.05 0.21 Q17 1 0.0568 -0.4023 0.9458 11.00000 0.05 0.21 Q18 1 0.5000 0.0000 0.5000 10.50000 0.05 0.20 Q19 1 0.0485 0.0411 0.5068 11.00000 0.05 0.20 Q20 1 0.1113 -0.4394 1.0545 11.00000 0.05 0.19 Q21 1 0.2068 0.4571 0.8817 11.00000 0.05 0.19 Q22 1 0.4379 0.0668 0.7451 11.00000 0.05 0.19 Q23 1 0.2234 0.4340 0.6236 11.00000 0.05 0.19 Q24 1 0.1270 -0.2968 0.9696 11.00000 0.05 0.19 Q25 1 -0.0090 -0.2732 0.7805 11.00000 0.05 0.19 Q26 1 0.1803 0.1449 0.8272 11.00000 0.05 0.19 Q27 1 -0.0296 0.0375 0.7676 11.00000 0.05 0.19 Q28 1 0.4823 0.0889 0.7469 11.00000 0.05 0.19 Q29 1 -0.0296 -0.3627 0.9220 11.00000 0.05 0.19 Q30 1 0.3974 -0.3310 0.3098 11.00000 0.05 0.18 Q31 1 0.0155 -0.2578 0.7748 11.00000 0.05 0.18 Q32 1 0.4311 -0.0165 0.4831 11.00000 0.05 0.18 Q33 1 0.1978 -0.1217 0.8402 11.00000 0.05 0.18 Q34 1 0.3201 0.1438 0.9029 11.00000 0.05 0.18 Q35 1 0.1318 0.3690 0.6249 11.00000 0.05 0.18 Q36 1 -0.0029 0.2836 0.8525 11.00000 0.05 0.18 Q37 1 0.3904 0.0162 0.9630 11.00000 0.05 0.18 Q38 1 0.1711 -0.5390 0.8770 11.00000 0.05 0.18 Q39 1 0.1846 -0.2928 1.0061 11.00000 0.05 0.18 Q40 1 0.3521 0.2400 0.8777 11.00000 0.05 0.17 Q41 1 0.2396 -0.0246 0.2740 11.00000 0.05 0.17 Q42 1 0.1534 0.0780 0.7474 11.00000 0.05 0.17 Q43 1 0.2856 0.2632 0.5208 11.00000 0.05 0.17 Q44 1 0.1716 0.2068 0.6913 11.00000 0.05 0.17 Q45 1 0.0818 0.0409 1.0087 11.00000 0.05 0.17 Q46 1 0.1804 0.0791 0.8651 11.00000 0.05 0.17 Q47 1 0.3055 -0.1949 0.4583 11.00000 0.05 0.17 Q48 1 0.2957 -0.0741 0.0300 11.00000 0.05 0.17 Q49 1 0.3517 -0.2339 0.0639 11.00000 0.05 0.17 Q50 1 0.2625 0.0259 0.4124 11.00000 0.05 0.17 Q51 1 0.2596 -0.0913 0.4106 11.00000 0.05 0.17 Q52 1 0.1637 0.4485 0.6322 11.00000 0.05 0.17 ; _shelx_res_checksum 6206 _shelx_hkl_file ; 0 0 1 0.53 12.60 0 0 1 2.57 5.80 0 0 1 -0.94 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