# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 207 _publ_requested_journal 'Perkin Transactions 1' loop_ _publ_author_name 'Habata, Yoichi' 'Akabori, Sadatoshi' 'Bradshaw, Jerald S.' 'Fukuda, Yoji' _publ_contact_author_name 'Prof Yoichi Habata' _publ_contact_author_address ; Department of Chemistry, Faculty of Science Toho University 2-2-1 Miyama Funabashi Chiba 274-8510 JAPAN ; _publ_contact_author_email 'HABATA@CHEM.SCI.TOHO-U.AC.JP' _publ_section_title ; Alkali metal ion selectivities in the gas phase of podands that form pseudo-cyclic structures by intramolecular hydrogen bonding ; data_haba111-Py-CH2O-Ph-OH _database_code_CSD 175380 _audit_creation_date 'Fri Feb 8 13:08:00 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C38 H34 N2 O8 ' _chemical_formula_moiety '?' _chemical_formula_weight 646.70 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 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 _cell_length_a 8.117(6) _cell_length_b 19.978(7) _cell_length_c 19.981(8) _cell_angle_alpha 90 _cell_angle_beta 92.91(5) _cell_angle_gamma 90 _cell_volume 3236(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 12.3 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360.00 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3879 _diffrn_reflns_av_R_equivalents 0.219 _diffrn_reflns_theta_max 22.50 _diffrn_measured_fraction_theta_max 0.8137 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.8137 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.60 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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). ; _reflns_number_total 3447 _reflns_number_gt 1020 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.3288 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3438 _refine_ls_number_parameters 433 _refine_ls_goodness_of_fit_ref 1.414 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0045 _refine_diff_density_max 0.78 _refine_diff_density_min -0.42 _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) ; #------------------------------------------------------------------------------ # 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 O(1) O 0.835(2) 0.1667(6) 0.5284(7) 0.069(5) Uani 1.00 d . . . O(2) O 0.887(1) 0.2489(6) 0.6389(6) 0.052(5) Uani 1.00 d . . . O(3) O 0.673(1) 0.2215(6) 0.4117(6) 0.058(5) Uani 1.00 d . . . O(4) O 0.764(2) 0.0921(6) 0.4183(6) 0.067(5) Uani 1.00 d . . . O(5) O 0.728(2) 0.4117(6) 0.0819(7) 0.089(6) Uani 1.00 d . . . O(6) O 0.641(1) 0.2808(6) 0.0838(6) 0.052(4) Uani 1.00 d . . . O(7) O 0.755(2) 0.2600(8) -0.1492(7) 0.074(6) Uani 1.00 d . . . O(8) O 0.751(1) 0.3398(7) -0.0373(6) 0.070(5) Uani 1.00 d . . . N(1) N 0.809(2) 0.2992(7) 0.5089(9) 0.055(6) Uani 1.00 d . . . N(2) N 0.721(2) 0.2060(8) -0.0263(9) 0.066(7) Uani 1.00 d . . . C(1) C 0.911(2) 0.140(1) 0.585(1) 0.049(8) Uani 1.00 d . . . C(2) C 0.953(3) 0.076(1) 0.590(1) 0.09(1) Uani 1.00 d . . . C(3) C 1.023(3) 0.050(1) 0.649(1) 0.093(10) Uani 1.00 d . . . C(4) C 1.057(3) 0.092(1) 0.702(1) 0.11(1) Uani 1.00 d . . . C(5) C 1.013(2) 0.158(1) 0.6980(10) 0.070(8) Uani 1.00 d . . . C(6) C 0.942(2) 0.185(1) 0.640(1) 0.054(8) Uani 1.00 d . . . C(7) C 0.993(2) 0.2966(10) 0.6078(10) 0.065(7) Uani 1.00 d . . . C(8) C 0.897(2) 0.336(1) 0.553(1) 0.054(8) Uani 1.00 d . . . C(9) C 0.907(3) 0.402(1) 0.547(1) 0.083(10) Uani 1.00 d . . . C(10) C 0.823(3) 0.435(1) 0.495(1) 0.083(9) Uani 1.00 d . . . C(11) C 0.724(2) 0.3982(10) 0.450(1) 0.068(8) Uani 1.00 d . . . C(12) C 0.718(2) 0.328(1) 0.4593(9) 0.053(8) Uani 1.00 d . . . C(13) C 0.610(2) 0.2890(9) 0.4108(9) 0.060(7) Uani 1.00 d . . . C(14) C 0.588(2) 0.1788(10) 0.3673(10) 0.048(8) Uani 1.00 d . . . C(15) C 0.471(3) 0.1939(10) 0.320(1) 0.067(8) Uani 1.00 d . . . C(16) C 0.390(2) 0.148(1) 0.2788(9) 0.067(8) Uani 1.00 d . . . C(17) C 0.442(2) 0.082(1) 0.284(1) 0.067(8) Uani 1.00 d . . . C(18) C 0.578(3) 0.064(1) 0.328(1) 0.072(8) Uani 1.00 d . . . C(19) C 0.629(3) 0.111(1) 0.375(1) 0.064(9) Uani 1.00 d . . . C(20) C 0.611(3) 0.391(1) 0.124(1) 0.078(9) Uani 1.00 d . . . C(21) C 0.550(3) 0.4378(10) 0.168(1) 0.073(8) Uani 1.00 d . . . C(22) C 0.436(3) 0.416(1) 0.2131(10) 0.088(10) Uani 1.00 d . . . C(23) C 0.383(3) 0.353(1) 0.2183(10) 0.075(8) Uani 1.00 d . . . C(24) C 0.452(2) 0.3056(9) 0.1697(10) 0.052(7) Uani 1.00 d . . . C(25) C 0.567(2) 0.328(1) 0.1266(9) 0.048(7) Uani 1.00 d . . . C(26) C 0.580(2) 0.2136(10) 0.0798(9) 0.055(7) Uani 1.00 d . . . C(27) C 0.679(2) 0.1746(10) 0.031(1) 0.048(7) Uani 1.00 d . . . C(28) C 0.711(2) 0.1076(9) 0.048(1) 0.062(7) Uani 1.00 d . . . C(29) C 0.803(3) 0.073(1) -0.001(1) 0.085(9) Uani 1.00 d . . . C(30) C 0.849(3) 0.102(1) -0.056(1) 0.09(1) Uani 1.00 d . . . C(31) C 0.806(2) 0.167(1) -0.068(1) 0.075(9) Uani 1.00 d . . . C(32) C 0.859(3) 0.208(1) -0.132(1) 0.11(1) Uani 1.00 d . . . C(33) C 0.847(3) 0.318(1) -0.148(1) 0.070(9) Uani 1.00 d . . . C(34) C 0.921(3) 0.346(1) -0.201(1) 0.080(9) Uani 1.00 d . . . C(35) C 0.996(3) 0.407(1) -0.202(1) 0.11(1) Uani 1.00 d . . . C(36) C 0.985(3) 0.447(1) -0.144(1) 0.086(9) Uani 1.00 d . . . C(37) C 0.910(3) 0.424(1) -0.089(1) 0.073(9) Uani 1.00 d . . . C(38) C 0.829(2) 0.364(1) -0.093(1) 0.057(8) Uani 1.00 d . . . H(1) H 0.7072 0.1709 0.5350 0.0554 Uiso 1.00 calc . . . H(2) H 0.9378 0.0473 0.5505 0.0963 Uiso 1.00 calc . . . H(3) H 1.0478 0.0021 0.6516 0.1137 Uiso 1.00 calc . . . H(4) H 1.1158 0.0718 0.7436 0.1354 Uiso 1.00 calc . . . H(5) H 1.0309 0.1868 0.7392 0.0926 Uiso 1.00 calc . . . H(6) H 1.0468 0.3280 0.6414 0.0840 Uiso 1.00 calc . . . H(7) H 1.0936 0.2738 0.5901 0.0840 Uiso 1.00 calc . . . H(8) H 0.9725 0.4275 0.5814 0.0979 Uiso 1.00 calc . . . H(9) H 0.8367 0.4840 0.4883 0.1110 Uiso 1.00 calc . . . H(10) H 0.6592 0.4200 0.4122 0.0779 Uiso 1.00 calc . . . H(11) H 0.4923 0.2908 0.4190 0.0976 Uiso 1.00 calc . . . H(12) H 0.6112 0.3079 0.3631 0.0976 Uiso 1.00 calc . . . H(13) H 0.4354 0.2412 0.3155 0.0913 Uiso 1.00 calc . . . H(14) H 0.2956 0.1606 0.2482 0.0795 Uiso 1.00 calc . . . H(15) H 0.3844 0.0486 0.2539 0.0846 Uiso 1.00 calc . . . H(16) H 0.6296 0.0184 0.3250 0.0952 Uiso 1.00 calc . . . H(17) H 0.7149 0.0924 0.4688 0.0554 Uiso 1.00 calc . . . H(18) H 0.7676 0.3724 0.0496 0.0554 Uiso 1.00 calc . . . H(19) H 0.5761 0.4853 0.1636 0.0920 Uiso 1.00 calc . . . H(20) H 0.3874 0.4490 0.2452 0.1172 Uiso 1.00 calc . . . H(21) H 0.3062 0.3366 0.2525 0.0988 Uiso 1.00 calc . . . H(22) H 0.4094 0.2596 0.1677 0.0697 Uiso 1.00 calc . . . H(23) H 0.5845 0.1916 0.1250 0.0720 Uiso 1.00 calc . . . H(24) H 0.4608 0.2118 0.0668 0.0720 Uiso 1.00 calc . . . H(25) H 0.6752 0.0838 0.0899 0.0845 Uiso 1.00 calc . . . H(26) H 0.8440 0.0263 0.0099 0.0990 Uiso 1.00 calc . . . H(27) H 0.9103 0.0759 -0.0906 0.1155 Uiso 1.00 calc . . . H(28) H 0.8674 0.1750 -0.1715 0.1527 Uiso 1.00 calc . . . H(29) H 0.9787 0.2217 -0.1266 0.1527 Uiso 1.00 calc . . . H(30) H 0.9196 0.3187 -0.2438 0.1110 Uiso 1.00 calc . . . H(31) H 1.0628 0.4238 -0.2402 0.1516 Uiso 1.00 calc . . . H(32) H 1.0304 0.4941 -0.1423 0.1144 Uiso 1.00 calc . . . H(33) H 0.9176 0.4524 -0.0457 0.1016 Uiso 1.00 calc . . . H(34) H 0.8939 0.3282 -0.0261 0.0554 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 O(1) 0.09(1) 0.06(1) 0.056(10) 0.013(7) 0.003(8) -0.005(8) O(2) 0.058(9) 0.036(9) 0.063(10) -0.002(7) -0.003(7) 0.001(7) O(3) 0.051(8) 0.048(9) 0.07(1) 0.001(7) -0.009(7) -0.004(8) O(4) 0.079(10) 0.042(9) 0.08(1) 0.020(7) -0.007(8) -0.008(7) O(5) 0.15(1) 0.013(8) 0.11(1) -0.013(8) 0.06(1) -0.010(8) O(6) 0.072(9) 0.033(8) 0.053(9) -0.008(7) 0.023(7) -0.002(7) O(7) 0.07(1) 0.07(1) 0.08(1) -0.019(9) 0.017(8) -0.010(9) O(8) 0.073(9) 0.08(1) 0.056(9) 0.006(7) 0.011(8) -0.003(8) N(1) 0.07(1) 0.04(1) 0.06(1) -0.002(10) 0.013(10) 0.00(1) N(2) 0.05(1) 0.07(1) 0.08(1) -0.004(10) -0.005(10) 0.00(1) C(1) 0.05(1) 0.04(2) 0.06(2) -0.02(1) 0.02(1) -0.01(1) C(2) 0.16(2) 0.03(2) 0.07(2) 0.02(1) -0.03(2) -0.01(1) C(3) 0.17(2) 0.03(2) 0.08(2) -0.02(1) 0.00(2) 0.00(1) C(4) 0.17(3) 0.06(2) 0.09(2) 0.00(2) -0.03(2) 0.02(2) C(5) 0.07(2) 0.10(2) 0.04(2) 0.01(1) 0.01(1) 0.01(2) C(6) 0.05(1) 0.05(2) 0.06(2) 0.00(1) 0.02(1) 0.01(1) C(7) 0.07(1) 0.05(1) 0.08(2) 0.00(1) 0.01(1) 0.00(1) C(8) 0.05(1) 0.01(1) 0.10(2) 0.01(1) 0.02(1) 0.02(1) C(9) 0.09(2) 0.07(2) 0.09(2) 0.01(1) -0.01(1) -0.02(2) C(10) 0.10(2) 0.06(2) 0.08(2) -0.03(1) 0.00(1) 0.02(2) C(11) 0.11(2) 0.01(1) 0.08(2) -0.02(1) -0.03(1) 0.01(1) C(12) 0.05(1) 0.08(2) 0.03(1) 0.02(1) 0.01(1) -0.01(1) C(13) 0.07(1) 0.03(1) 0.07(2) 0.03(1) -0.02(1) -0.01(1) C(14) 0.05(1) 0.05(2) 0.05(2) 0.00(1) 0.03(1) 0.00(1) C(15) 0.07(2) 0.06(1) 0.07(2) 0.01(1) -0.03(1) 0.00(1) C(16) 0.05(1) 0.07(2) 0.07(2) 0.00(1) -0.04(1) -0.03(1) C(17) 0.05(1) 0.05(2) 0.10(2) -0.01(1) -0.01(1) -0.05(1) C(18) 0.10(2) 0.07(2) 0.05(1) 0.02(1) 0.00(1) -0.02(1) C(19) 0.09(2) 0.04(2) 0.06(2) 0.02(1) 0.00(1) -0.01(1) C(20) 0.17(3) 0.02(2) 0.04(2) -0.01(2) -0.01(2) 0.00(1) C(21) 0.12(2) 0.04(1) 0.06(2) -0.04(1) 0.01(1) -0.03(1) C(22) 0.15(2) 0.09(2) 0.03(1) 0.03(2) 0.05(1) 0.01(1) C(23) 0.10(2) 0.08(2) 0.05(2) 0.02(1) 0.04(1) 0.01(1) C(24) 0.04(1) 0.05(1) 0.06(1) -0.004(10) 0.01(1) 0.02(1) C(25) 0.03(1) 0.05(2) 0.06(2) 0.00(1) 0.00(1) 0.01(1) C(26) 0.06(1) 0.05(1) 0.05(1) -0.01(1) 0.00(1) 0.02(1) C(27) 0.01(1) 0.06(2) 0.07(2) -0.01(1) 0.00(1) -0.02(1) C(28) 0.10(2) 0.01(1) 0.09(2) 0.00(1) 0.02(1) -0.01(1) C(29) 0.12(2) 0.03(1) 0.11(2) -0.02(1) 0.02(2) -0.01(2) C(30) 0.11(2) 0.02(2) 0.15(3) 0.00(1) 0.00(2) -0.01(2) C(31) 0.05(1) 0.07(2) 0.10(2) 0.01(1) 0.00(1) -0.02(2) C(32) 0.13(2) 0.11(2) 0.09(2) 0.02(2) 0.05(2) -0.02(2) C(33) 0.09(2) 0.07(2) 0.05(2) 0.02(1) 0.05(1) 0.00(2) C(34) 0.11(2) 0.07(2) 0.07(2) -0.01(1) 0.01(1) 0.01(1) C(35) 0.17(3) 0.07(2) 0.08(2) -0.01(2) 0.01(2) 0.02(2) C(36) 0.15(2) 0.05(2) 0.05(2) 0.01(1) -0.01(2) 0.00(1) C(37) 0.13(2) 0.06(2) 0.04(2) -0.02(1) 0.03(1) 0.01(1) C(38) 0.05(1) 0.07(2) 0.06(2) 0.00(1) -0.01(1) 0.04(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(1) 1.37(2) . . yes O(1) H(1) 1.052 . . no O(2) C(6) 1.36(2) . . yes O(2) C(7) 1.44(2) . . yes O(3) C(13) 1.44(2) . . yes O(3) C(14) 1.39(2) . . yes O(4) C(19) 1.41(2) . . yes O(4) H(17) 1.103 . . no O(5) C(20) 1.37(2) . . yes O(5) H(18) 1.074 . . no O(6) C(25) 1.42(2) . . yes O(6) C(26) 1.43(2) . . yes O(7) C(32) 1.37(3) . . yes O(7) C(33) 1.38(2) . . yes O(8) C(38) 1.39(2) . . yes O(8) H(34) 1.196 . . no N(1) C(8) 1.32(2) . . yes N(1) C(12) 1.34(2) . . yes N(2) C(27) 1.36(2) . . yes N(2) C(31) 1.35(2) . . yes C(1) C(2) 1.33(2) . . yes C(1) C(6) 1.42(2) . . yes C(2) C(3) 1.39(3) . . yes C(2) H(2) 0.983 . . no C(3) C(4) 1.37(3) . . yes C(3) H(3) 0.972 . . no C(4) C(5) 1.38(3) . . yes C(4) H(4) 1.014 . . no C(5) C(6) 1.37(2) . . yes C(5) H(5) 1.008 . . no C(7) C(8) 1.53(2) . . yes C(7) H(6) 1.004 . . no C(7) H(7) 1.017 . . no C(8) C(9) 1.34(2) . . yes C(9) C(10) 1.37(3) . . yes C(9) H(8) 0.988 . . no C(10) C(11) 1.39(3) . . yes C(10) H(9) 1.004 . . no C(11) C(12) 1.42(2) . . yes C(11) H(10) 0.998 . . no C(12) C(13) 1.49(2) . . yes C(13) H(11) 0.979 . . no C(13) H(12) 1.027 . . no C(14) C(15) 1.33(2) . . yes C(14) C(19) 1.41(2) . . yes C(15) C(16) 1.38(2) . . yes C(15) H(13) 0.992 . . no C(16) C(17) 1.39(2) . . yes C(16) H(14) 0.988 . . no C(17) C(18) 1.43(2) . . yes C(17) H(15) 1.000 . . no C(18) C(19) 1.38(2) . . yes C(18) H(16) 1.007 . . no C(20) C(21) 1.39(3) . . yes C(20) C(25) 1.31(2) . . yes C(21) C(22) 1.40(3) . . yes C(21) H(19) 0.978 . . no C(22) C(23) 1.33(3) . . yes C(22) H(20) 1.017 . . no C(23) C(24) 1.49(2) . . yes C(23) H(21) 1.003 . . no C(24) C(25) 1.38(2) . . yes C(24) H(22) 0.980 . . no C(26) C(27) 1.51(2) . . yes C(26) H(23) 1.003 . . no C(26) H(24) 0.991 . . no C(27) C(28) 1.40(2) . . yes C(28) C(29) 1.43(3) . . yes C(28) H(25) 1.026 . . no C(29) C(30) 1.32(3) . . yes C(29) H(26) 1.000 . . no C(30) C(31) 1.35(3) . . yes C(30) H(27) 1.025 . . no C(31) C(32) 1.59(3) . . yes C(32) H(28) 1.035 . . no C(32) H(29) 1.013 . . no C(33) C(34) 1.37(2) . . yes C(33) C(38) 1.43(2) . . yes C(34) C(35) 1.37(3) . . yes C(34) H(30) 1.003 . . no C(35) C(36) 1.41(3) . . yes C(35) H(31) 1.018 . . no C(36) C(37) 1.35(2) . . yes C(36) H(32) 1.015 . . no C(37) C(38) 1.38(2) . . yes C(37) H(33) 1.034 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(1) H(1) 109.3 . . 0_555 no C(6) O(2) C(7) 115(1) . . 0_555 yes C(13) O(3) C(14) 113(1) . . 0_555 yes C(19) O(4) H(17) 104.8 . . 0_555 no C(20) O(5) H(18) 112.8 . . 0_555 no C(25) O(6) C(26) 119(1) . . 0_555 yes C(32) O(7) C(33) 108(1) . . 0_555 yes C(38) O(8) H(34) 74.7 . . 0_555 no C(8) N(1) C(12) 121(1) . . 0_555 yes C(27) N(2) C(31) 113(1) . . 0_555 yes O(1) C(1) C(2) 121(1) . . 0_555 yes O(1) C(1) C(6) 117(1) . . 0_555 yes C(2) C(1) C(6) 121(2) . . 0_555 yes C(1) C(2) C(3) 121(2) . . 0_555 yes C(1) C(2) H(2) 119.8 . . 0_555 no C(3) C(2) H(2) 118.9 . . 0_555 no C(2) C(3) C(4) 118(2) . . 0_555 yes C(2) C(3) H(3) 119.6 . . 0_555 no C(4) C(3) H(3) 121.6 . . 0_555 no C(3) C(4) C(5) 119(2) . . 0_555 yes C(3) C(4) H(4) 117.5 . . 0_555 no C(5) C(4) H(4) 122.6 . . 0_555 no C(4) C(5) C(6) 121(2) . . 0_555 yes C(4) C(5) H(5) 118.0 . . 0_555 no C(6) C(5) H(5) 120.6 . . 0_555 no O(2) C(6) C(1) 122(1) . . 0_555 yes O(2) C(6) C(5) 120(2) . . 0_555 yes C(1) C(6) C(5) 117(2) . . 0_555 yes O(2) C(7) C(8) 110(1) . . 0_555 yes O(2) C(7) H(6) 112.0 . . 0_555 no O(2) C(7) H(7) 111.1 . . 0_555 no C(8) C(7) H(6) 110.7 . . 0_555 no C(8) C(7) H(7) 111.4 . . 0_555 no H(6) C(7) H(7) 100.3 . . 0_555 no N(1) C(8) C(7) 115(1) . . 0_555 yes N(1) C(8) C(9) 121(2) . . 0_555 yes C(7) C(8) C(9) 122(2) . . 0_555 yes C(8) C(9) C(10) 120(2) . . 0_555 yes C(8) C(9) H(8) 119.2 . . 0_555 no C(10) C(9) H(8) 120.6 . . 0_555 no C(9) C(10) C(11) 119(2) . . 0_555 yes C(9) C(10) H(9) 121.0 . . 0_555 no C(11) C(10) H(9) 119.4 . . 0_555 no C(10) C(11) C(12) 117(1) . . 0_555 yes C(10) C(11) H(10) 122.0 . . 0_555 no C(12) C(11) H(10) 120.8 . . 0_555 no N(1) C(12) C(11) 119(1) . . 0_555 yes N(1) C(12) C(13) 122(1) . . 0_555 yes C(11) C(12) C(13) 117(1) . . 0_555 yes O(3) C(13) C(12) 106(1) . . 0_555 yes O(3) C(13) H(11) 112.5 . . 0_555 no O(3) C(13) H(12) 109.7 . . 0_555 no C(12) C(13) H(11) 114.6 . . 0_555 no C(12) C(13) H(12) 112.3 . . 0_555 no H(11) C(13) H(12) 101.3 . . 0_555 no O(3) C(14) C(15) 128(1) . . 0_555 yes O(3) C(14) C(19) 114(1) . . 0_555 yes C(15) C(14) C(19) 117(1) . . 0_555 yes C(14) C(15) C(16) 125(1) . . 0_555 yes C(14) C(15) H(13) 118.6 . . 0_555 no C(16) C(15) H(13) 116.3 . . 0_555 no C(15) C(16) C(17) 116(1) . . 0_555 yes C(15) C(16) H(14) 122.9 . . 0_555 no C(17) C(16) H(14) 120.1 . . 0_555 no C(16) C(17) C(18) 120(1) . . 0_555 yes C(16) C(17) H(15) 118.0 . . 0_555 no C(18) C(17) H(15) 121.2 . . 0_555 no C(17) C(18) C(19) 116(1) . . 0_555 yes C(17) C(18) H(16) 120.3 . . 0_555 no C(19) C(18) H(16) 123.0 . . 0_555 no O(4) C(19) C(14) 120(1) . . 0_555 yes O(4) C(19) C(18) 115(1) . . 0_555 yes C(14) C(19) C(18) 121(2) . . 0_555 yes O(5) C(20) C(21) 117(1) . . 0_555 yes O(5) C(20) C(25) 120(2) . . 0_555 yes C(21) C(20) C(25) 121(2) . . 0_555 yes C(20) C(21) C(22) 117(1) . . 0_555 yes C(20) C(21) H(19) 120.5 . . 0_555 no C(22) C(21) H(19) 121.4 . . 0_555 no C(21) C(22) C(23) 125(2) . . 0_555 yes C(21) C(22) H(20) 119.2 . . 0_555 no C(23) C(22) H(20) 115.5 . . 0_555 no C(22) C(23) C(24) 114(1) . . 0_555 yes C(22) C(23) H(21) 125.4 . . 0_555 no C(24) C(23) H(21) 120.1 . . 0_555 no C(23) C(24) C(25) 119(1) . . 0_555 yes C(23) C(24) H(22) 118.6 . . 0_555 no C(25) C(24) H(22) 121.8 . . 0_555 no O(6) C(25) C(20) 119(1) . . 0_555 yes O(6) C(25) C(24) 118(1) . . 0_555 yes C(20) C(25) C(24) 121(2) . . 0_555 yes O(6) C(26) C(27) 109(1) . . 0_555 yes O(6) C(26) H(23) 111.4 . . 0_555 no O(6) C(26) H(24) 112.3 . . 0_555 no C(27) C(26) H(23) 111.4 . . 0_555 no C(27) C(26) H(24) 110.6 . . 0_555 no H(23) C(26) H(24) 102.1 . . 0_555 no N(2) C(27) C(26) 118(1) . . 0_555 yes N(2) C(27) C(28) 126(1) . . 0_555 yes C(26) C(27) C(28) 115(1) . . 0_555 yes C(27) C(28) C(29) 113(1) . . 0_555 yes C(27) C(28) H(25) 125.7 . . 0_555 no C(29) C(28) H(25) 120.6 . . 0_555 no C(28) C(29) C(30) 121(2) . . 0_555 yes C(28) C(29) H(26) 119.1 . . 0_555 no C(30) C(29) H(26) 119.4 . . 0_555 no C(29) C(30) C(31) 119(2) . . 0_555 yes C(29) C(30) H(27) 119.7 . . 0_555 no C(31) C(30) H(27) 120.5 . . 0_555 no N(2) C(31) C(30) 125(2) . . 0_555 yes N(2) C(31) C(32) 111(2) . . 0_555 yes C(30) C(31) C(32) 123(2) . . 0_555 yes O(7) C(32) C(31) 114(1) . . 0_555 yes O(7) C(32) H(28) 110.3 . . 0_555 no O(7) C(32) H(29) 112.7 . . 0_555 no C(31) C(32) H(28) 109.1 . . 0_555 no C(31) C(32) H(29) 110.9 . . 0_555 no H(28) C(32) H(29) 98.5 . . 0_555 no O(7) C(33) C(34) 125(2) . . 0_555 yes O(7) C(33) C(38) 118(1) . . 0_555 yes C(34) C(33) C(38) 114(2) . . 0_555 yes C(33) C(34) C(35) 125(2) . . 0_555 yes C(33) C(34) H(30) 117.4 . . 0_555 no C(35) C(34) H(30) 117.5 . . 0_555 no C(34) C(35) C(36) 116(2) . . 0_555 yes C(34) C(35) H(31) 123.5 . . 0_555 no C(36) C(35) H(31) 119.6 . . 0_555 no C(35) C(36) C(37) 121(2) . . 0_555 yes C(35) C(36) H(32) 120.5 . . 0_555 no C(37) C(36) H(32) 117.6 . . 0_555 no C(36) C(37) C(38) 118(2) . . 0_555 yes C(36) C(37) H(33) 119.4 . . 0_555 no C(38) C(37) H(33) 121.6 . . 0_555 no O(8) C(38) C(33) 117(1) . . 0_555 yes O(8) C(38) C(37) 119(2) . . 0_555 yes C(33) C(38) C(37) 121(2) . . 0_555 yes #------------------------------------------------------------------------------ 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 O(1) C(1) C(2) C(3) -176(1) 0_555 21_1 5_555 55_5 yes O(1) C(1) C(6) O(2) 5(2) 0_555 21_1 5_555 55_5 yes O(1) C(1) C(6) C(5) 177(1) 0_555 21_1 5_555 55_5 yes O(2) C(6) C(1) C(2) -174(1) 0_555 21_1 5_555 55_5 yes O(2) C(6) C(5) C(4) 174(1) 0_555 21_1 5_555 55_5 yes O(2) C(7) C(8) N(1) -49(2) 0_555 21_1 5_555 55_5 yes O(2) C(7) C(8) C(9) 133(1) 0_555 21_1 5_555 55_5 yes O(3) C(13) C(12) N(1) -21(2) 0_555 21_1 5_555 55_5 yes O(3) C(13) C(12) C(11) 156(1) 0_555 21_1 5_555 55_5 yes O(3) C(14) C(15) C(16) -178(1) 0_555 21_1 5_555 55_5 yes O(3) C(14) C(19) O(4) -8(2) 0_555 21_1 5_555 55_5 yes O(3) C(14) C(19) C(18) -168(1) 0_555 21_1 5_555 55_5 yes O(4) C(19) C(14) C(15) 172(1) 0_555 21_1 5_555 55_5 yes O(4) C(19) C(18) C(17) -179(1) 0_555 21_1 5_555 55_5 yes O(5) C(20) C(21) C(22) -177(1) 0_555 21_1 5_555 55_5 yes O(5) C(20) C(25) O(6) -1(2) 0_555 21_1 5_555 55_5 yes O(5) C(20) C(25) C(24) 178(1) 0_555 21_1 5_555 55_5 yes O(6) C(25) C(20) C(21) -176(1) 0_555 21_1 5_555 55_5 yes O(6) C(25) C(24) C(23) 175(1) 0_555 21_1 5_555 55_5 yes O(6) C(26) C(27) N(2) -39(1) 0_555 21_1 5_555 55_5 yes O(6) C(26) C(27) C(28) 142(1) 0_555 21_1 5_555 55_5 yes O(7) C(32) C(31) N(2) -27(2) 0_555 21_1 5_555 55_5 yes O(7) C(32) C(31) C(30) 154(2) 0_555 21_1 5_555 55_5 yes O(7) C(33) C(34) C(35) 172(2) 0_555 21_1 5_555 55_5 yes O(7) C(33) C(38) O(8) 13(2) 0_555 21_1 5_555 55_5 yes O(7) C(33) C(38) C(37) -176(1) 0_555 21_1 5_555 55_5 yes O(8) C(38) C(33) C(34) 178(1) 0_555 21_1 5_555 55_5 yes O(8) C(38) C(37) C(36) -179(1) 0_555 21_1 5_555 55_5 yes N(1) C(8) C(9) C(10) 0(3) 0_555 21_1 5_555 55_5 yes N(1) C(12) C(11) C(10) -2(3) 0_555 21_1 5_555 55_5 yes N(2) C(27) C(28) C(29) 2(2) 0_555 21_1 5_555 55_5 yes N(2) C(31) C(30) C(29) 1(3) 0_555 21_1 5_555 55_5 yes C(1) C(2) C(3) C(4) -4(3) 0_555 21_1 5_555 55_5 yes C(1) C(6) O(2) C(7) -85(1) 0_555 21_1 5_555 55_5 yes C(1) C(6) C(5) C(4) 2(3) 0_555 21_1 5_555 55_5 yes C(2) C(1) C(6) C(5) -1(2) 0_555 21_1 5_555 55_5 yes C(2) C(3) C(4) C(5) 4(3) 0_555 21_1 5_555 55_5 yes C(3) C(2) C(1) C(6) 2(3) 0_555 21_1 5_555 55_5 yes C(3) C(4) C(5) C(6) -3(3) 0_555 21_1 5_555 55_5 yes C(5) C(6) O(2) C(7) 102(1) 0_555 21_1 5_555 55_5 yes C(6) O(2) C(7) C(8) 125(1) 0_555 21_1 5_555 55_5 yes C(7) C(8) N(1) C(12) 178(1) 0_555 21_1 5_555 55_5 yes C(7) C(8) C(9) C(10) 177(1) 0_555 21_1 5_555 55_5 yes C(8) N(1) C(12) C(11) 5(2) 0_555 21_1 5_555 55_5 yes C(8) N(1) C(12) C(13) -176(1) 0_555 21_1 5_555 55_5 yes C(8) C(9) C(10) C(11) 2(3) 0_555 21_1 5_555 55_5 yes C(9) C(8) N(1) C(12) -4(3) 0_555 21_1 5_555 55_5 yes C(9) C(10) C(11) C(12) -1(3) 0_555 21_1 5_555 55_5 yes C(10) C(11) C(12) C(13) 179(1) 0_555 21_1 5_555 55_5 yes C(12) C(13) O(3) C(14) -178(1) 0_555 21_1 5_555 55_5 yes C(13) O(3) C(14) C(15) 7(2) 0_555 21_1 5_555 55_5 yes C(13) O(3) C(14) C(19) -169(1) 0_555 21_1 5_555 55_5 yes C(14) C(15) C(16) C(17) -3(3) 0_555 21_1 5_555 55_5 yes C(14) C(19) C(18) C(17) -19(3) 0_555 21_1 5_555 55_5 yes C(15) C(14) C(19) C(18) 13(2) 0_555 21_1 5_555 55_5 yes C(15) C(16) C(17) C(18) -2(3) 0_555 21_1 5_555 55_5 yes C(16) C(15) C(14) C(19) -1(3) 0_555 21_1 5_555 55_5 yes C(16) C(17) C(18) C(19) 13(3) 0_555 21_1 5_555 55_5 yes C(20) C(21) C(22) C(23) 1(3) 0_555 21_1 5_555 55_5 yes C(20) C(25) O(6) C(26) -172(1) 0_555 21_1 5_555 55_5 yes C(20) C(25) C(24) C(23) -4(2) 0_555 21_1 5_555 55_5 yes C(21) C(20) C(25) C(24) 3(3) 0_555 21_1 5_555 55_5 yes C(21) C(22) C(23) C(24) -1(3) 0_555 21_1 5_555 55_5 yes C(22) C(21) C(20) C(25) -2(3) 0_555 21_1 5_555 55_5 yes C(22) C(23) C(24) C(25) 3(2) 0_555 21_1 5_555 55_5 yes C(24) C(25) O(6) C(26) 7(2) 0_555 21_1 5_555 55_5 yes C(25) O(6) C(26) C(27) 179(1) 0_555 21_1 5_555 55_5 yes C(26) C(27) N(2) C(31) -179(1) 0_555 21_1 5_555 55_5 yes C(26) C(27) C(28) C(29) 179(1) 0_555 21_1 5_555 55_5 yes C(27) N(2) C(31) C(30) 0(2) 0_555 21_1 5_555 55_5 yes C(27) N(2) C(31) C(32) -177(1) 0_555 21_1 5_555 55_5 yes C(27) C(28) C(29) C(30) 0(3) 0_555 21_1 5_555 55_5 yes C(28) C(27) N(2) C(31) -2(2) 0_555 21_1 5_555 55_5 yes C(28) C(29) C(30) C(31) 0(3) 0_555 21_1 5_555 55_5 yes C(29) C(30) C(31) C(32) 178(2) 0_555 21_1 5_555 55_5 yes C(31) C(32) O(7) C(33) 121(2) 0_555 21_1 5_555 55_5 yes C(32) O(7) C(33) C(34) 92(2) 0_555 21_1 5_555 55_5 yes C(32) O(7) C(33) C(38) -104(2) 0_555 21_1 5_555 55_5 yes C(33) C(34) C(35) C(36) -4(3) 0_555 21_1 5_555 55_5 yes C(33) C(38) C(37) C(36) 11(3) 0_555 21_1 5_555 55_5 yes C(34) C(33) C(38) C(37) -12(2) 0_555 21_1 5_555 55_5 yes C(34) C(35) C(36) C(37) 2(3) 0_555 21_1 5_555 55_5 yes C(35) C(34) C(33) C(38) 9(3) 0_555 21_1 5_555 55_5 yes C(35) C(36) C(37) C(38) -5(3) 0_555 21_1 5_555 55_5 yes C(35) C(36) C(37) C(38) -5(3) 0_555 21_1 5_555 55_5 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 O(1) C(7) 3.35(2) . 4_455 ? O(1) C(13) 3.44(2) . 4_555 ? O(1) C(12) 3.47(2) . 4_555 ? O(2) C(7) 3.36(2) . 4_455 ? O(3) C(15) 3.53(2) . 4_555 ? O(3) C(13) 3.55(2) . 4_555 ? O(6) C(24) 3.44(2) . 4_555 ? O(6) C(26) 3.57(2) . 4_555 ? O(7) C(32) 3.32(3) . 4_455 ? O(7) C(34) 3.55(2) . 4_455 ? O(8) C(30) 3.46(3) . 4_455 ? C(12) C(15) 3.57(3) . 4_555 ? C(13) C(15) 3.54(3) . 4_555 ? C(20) C(28) 3.52(3) . 4_455 ? C(20) C(29) 3.52(3) . 4_455 ? C(24) C(26) 3.45(2) . 4_455 ? C(24) C(27) 3.49(2) . 4_455 ? C(24) C(28) 3.50(2) . 4_455 ? C(25) C(28) 3.47(2) . 4_455 ? C(29) C(37) 3.57(3) . 4_455 ? C(30) C(36) 3.50(3) . 4_455 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(4) H(17) O(1) . . . 1.103 2.109 2.69(1) 110.110 no O(5) H(18) O(6) . . . 1.074 2.224 2.71(1) 105.141 no O(5) H(18) O(8) . . . 1.074 1.853 2.80(1) 144.041 no #------------------------------------------------------------------------------ data_haba107_saly _database_code_CSD 175381 _audit_creation_date 'Thu Oct 25 18:51:24 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C21 H17 N O6 ' _chemical_formula_moiety 'C21 H17 N O6 ' _chemical_formula_weight 379.37 _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 8.254(9) _cell_length_b 14.99(1) _cell_length_c 8.05(1) _cell_angle_alpha 102.1(1) _cell_angle_beta 111.99(9) _cell_angle_gamma 78.40(9) _cell_volume 894(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 369.00 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3384 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.0022 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.0022 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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). ; _reflns_number_total 3147 _reflns_number_gt 1642 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1518 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3147 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.45 _refine_diff_density_min -0.41 _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) ; #------------------------------------------------------------------------------ # 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 O(1) O 0.5752(3) 0.3146(1) 0.6177(3) 0.0506(6) Uani 1.00 d . . . O(2) O 0.4367(3) 0.3169(2) 0.3237(3) 0.0758(8) Uani 1.00 d . . . O(3) O 0.2236(3) 0.4661(2) 0.2178(3) 0.0778(9) Uani 1.00 d . . . O(4) O 1.2684(3) -0.0267(1) 0.9921(3) 0.0554(7) Uani 1.00 d . . . O(5) O 1.2895(3) -0.1726(1) 0.8585(3) 0.0686(7) Uani 1.00 d . . . O(6) O 1.5471(3) -0.2918(1) 1.0332(3) 0.0690(7) Uani 1.00 d . . . N(1) N 0.9009(3) 0.1188(2) 0.7298(3) 0.0442(7) Uani 1.00 d . . . C(1) C 0.8278(4) 0.2070(2) 0.7378(4) 0.0430(9) Uani 1.00 d . . . C(2) C 0.8977(4) 0.2733(2) 0.8844(4) 0.0513(9) Uani 1.00 d . . . C(3) C 1.0481(4) 0.2469(2) 1.0219(4) 0.0560(10) Uani 1.00 d . . . C(4) C 1.1252(4) 0.1562(2) 1.0150(4) 0.0520(9) Uani 1.00 d . . . C(5) C 1.0467(4) 0.0942(2) 0.8649(4) 0.0442(9) Uani 1.00 d . . . C(6) C 0.6731(4) 0.2275(2) 0.5741(4) 0.0534(9) Uani 1.00 d . . . C(7) C 0.4571(4) 0.3528(2) 0.4785(4) 0.0481(9) Uani 1.00 d . . . C(8) C 0.3530(4) 0.4389(2) 0.5278(4) 0.0480(9) Uani 1.00 d . . . C(9) C 0.2402(4) 0.4900(2) 0.3951(5) 0.058(1) Uani 1.00 d . . . C(10) C 0.1386(4) 0.5707(2) 0.4409(6) 0.072(1) Uani 1.00 d . . . C(11) C 0.1522(5) 0.5987(2) 0.6178(7) 0.083(1) Uani 1.00 d . . . C(12) C 0.2630(5) 0.5494(3) 0.7522(5) 0.077(1) Uani 1.00 d . . . C(13) C 0.3637(4) 0.4688(2) 0.7083(4) 0.061(1) Uani 1.00 d . . . C(14) C 1.1139(4) -0.0059(2) 0.8387(4) 0.0510(9) Uani 1.00 d . . . C(15) C 1.3457(4) -0.1141(2) 0.9872(4) 0.0460(9) Uani 1.00 d . . . C(16) C 1.4996(4) -0.1303(2) 1.1473(4) 0.0445(9) Uani 1.00 d . . . C(17) C 1.5935(4) -0.2192(2) 1.1646(4) 0.0487(9) Uani 1.00 d . . . C(18) C 1.7386(4) -0.2354(2) 1.3163(4) 0.0541(10) Uani 1.00 d . . . C(19) C 1.7936(4) -0.1634(2) 1.4550(4) 0.061(1) Uani 1.00 d . . . C(20) C 1.7035(4) -0.0752(2) 1.4406(4) 0.063(1) Uani 1.00 d . . . C(21) C 1.5600(4) -0.0591(2) 1.2917(4) 0.0553(10) Uani 1.00 d . . . H(1) H 0.3199 0.4003 0.2049 0.0871 Uiso 1.00 calc . . . H(2) H 1.4410 -0.2698 0.9214 0.0871 Uiso 1.00 calc . . . H(3) H 0.8402 0.3464 0.8728 0.0871 Uiso 1.00 calc . . . H(4) H 1.0835 0.2913 1.1309 0.0871 Uiso 1.00 calc . . . H(5) H 1.2440 0.1380 1.1150 0.0871 Uiso 1.00 calc . . . H(6) H 1.1267 -0.0243 0.7170 0.0871 Uiso 1.00 calc . . . H(7) H 1.0261 -0.0517 0.8337 0.0871 Uiso 1.00 calc . . . H(8) H 1.7999 -0.3051 1.3384 0.0871 Uiso 1.00 calc . . . H(9) H 1.8896 -0.1928 1.5588 0.0871 Uiso 1.00 calc . . . H(10) H 1.7450 -0.0238 1.5445 0.0871 Uiso 1.00 calc . . . H(11) H 1.4836 0.0104 1.2539 0.0871 Uiso 1.00 calc . . . H(12) H 0.6012 0.1734 0.5337 0.0871 Uiso 1.00 calc . . . H(13) H 0.6900 0.2256 0.4339 0.0871 Uiso 1.00 calc . . . H(14) H 0.0525 0.6049 0.3312 0.0871 Uiso 1.00 calc . . . H(15) H 0.0791 0.6618 0.6360 0.0871 Uiso 1.00 calc . . . H(16) H 0.2686 0.5588 0.9026 0.0871 Uiso 1.00 calc . . . H(17) H 0.4476 0.4366 0.8056 0.0871 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 O(1) 0.046(1) 0.048(1) 0.049(1) 0.0089(10) 0.013(1) 0.0097(10) O(2) 0.072(2) 0.085(2) 0.047(1) 0.021(1) 0.011(1) 0.006(1) O(3) 0.065(2) 0.088(2) 0.074(2) 0.009(1) 0.015(1) 0.030(1) O(4) 0.049(1) 0.043(1) 0.061(1) 0.005(1) 0.007(1) 0.012(1) O(5) 0.076(2) 0.055(1) 0.052(1) 0.009(1) 0.010(1) -0.001(1) O(6) 0.086(2) 0.051(1) 0.052(1) 0.011(1) 0.016(1) 0.002(1) N(1) 0.039(1) 0.041(1) 0.052(1) -0.001(1) 0.015(1) 0.010(1) C(1) 0.041(2) 0.044(2) 0.045(2) -0.001(1) 0.017(1) 0.007(1) C(2) 0.050(2) 0.046(2) 0.053(2) 0.001(1) 0.017(2) 0.005(1) C(3) 0.055(2) 0.050(2) 0.054(2) -0.005(2) 0.013(2) -0.002(2) C(4) 0.042(2) 0.057(2) 0.052(2) -0.004(2) 0.012(1) 0.009(2) C(5) 0.038(2) 0.046(2) 0.052(2) -0.001(1) 0.017(1) 0.014(1) C(6) 0.052(2) 0.042(2) 0.053(2) 0.010(1) 0.014(2) 0.000(1) C(7) 0.041(2) 0.048(2) 0.054(2) -0.003(1) 0.013(2) 0.013(2) C(8) 0.033(2) 0.043(2) 0.066(2) -0.002(1) 0.013(2) 0.012(2) C(9) 0.043(2) 0.053(2) 0.082(3) -0.005(2) 0.019(2) 0.022(2) C(10) 0.053(2) 0.059(2) 0.109(3) 0.011(2) 0.028(2) 0.037(2) C(11) 0.076(3) 0.047(2) 0.134(4) 0.009(2) 0.052(3) 0.017(2) C(12) 0.074(3) 0.060(2) 0.094(3) 0.006(2) 0.035(2) 0.003(2) C(13) 0.050(2) 0.058(2) 0.069(2) 0.000(2) 0.019(2) 0.006(2) C(14) 0.046(2) 0.047(2) 0.051(2) 0.002(1) 0.006(2) 0.013(1) C(15) 0.046(2) 0.046(2) 0.048(2) 0.002(1) 0.021(2) 0.010(2) C(16) 0.041(2) 0.049(2) 0.046(2) 0.000(1) 0.019(1) 0.011(1) C(17) 0.052(2) 0.046(2) 0.050(2) 0.002(1) 0.023(2) 0.008(1) C(18) 0.047(2) 0.057(2) 0.055(2) 0.009(2) 0.016(2) 0.017(2) C(19) 0.049(2) 0.068(2) 0.059(2) 0.002(2) 0.010(2) 0.017(2) C(20) 0.050(2) 0.062(2) 0.064(2) -0.009(2) 0.008(2) 0.000(2) C(21) 0.047(2) 0.051(2) 0.063(2) -0.003(2) 0.016(2) 0.006(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(6) 1.441(3) . . yes O(1) C(7) 1.327(3) . . yes O(2) C(7) 1.212(3) . . yes O(3) C(9) 1.357(4) . . yes O(3) H(1) 1.149 . . no O(4) C(14) 1.439(3) . . yes O(4) C(15) 1.336(3) . . yes O(5) C(15) 1.216(3) . . yes O(6) C(17) 1.354(3) . . yes O(6) H(2) 1.051 . . no N(1) C(1) 1.338(3) . . yes N(1) C(5) 1.334(3) . . yes C(1) C(2) 1.393(4) . . yes C(1) C(6) 1.488(4) . . yes C(2) C(3) 1.371(4) . . yes C(2) H(3) 1.112 . . no C(3) C(4) 1.380(4) . . yes C(3) H(4) 0.969 . . no C(4) C(5) 1.389(4) . . yes C(4) H(5) 1.038 . . no C(5) C(14) 1.491(4) . . yes C(6) H(12) 1.026 . . no C(6) H(13) 1.182 . . no C(7) C(8) 1.469(4) . . yes C(8) C(9) 1.381(4) . . yes C(8) C(13) 1.401(4) . . yes C(9) C(10) 1.393(4) . . yes C(10) C(11) 1.365(5) . . yes C(10) H(14) 1.058 . . no C(11) C(12) 1.370(5) . . yes C(11) H(15) 1.029 . . no C(12) C(13) 1.383(4) . . yes C(12) H(16) 1.174 . . no C(13) H(17) 0.971 . . no C(14) H(6) 1.000 . . no C(14) H(7) 1.080 . . no C(15) C(16) 1.454(4) . . yes C(16) C(17) 1.407(4) . . yes C(16) C(21) 1.413(4) . . yes C(17) C(18) 1.378(4) . . yes C(18) C(19) 1.389(4) . . yes C(18) H(8) 1.085 . . no C(19) C(20) 1.385(4) . . yes C(19) H(9) 1.019 . . no C(20) C(21) 1.357(4) . . yes C(20) H(10) 1.014 . . no C(21) H(11) 1.141 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(6) O(1) C(7) 116.3(2) . . 0_555 yes C(9) O(3) H(1) 107.9 . . 0_555 no C(14) O(4) C(15) 116.6(2) . . 0_555 yes C(17) O(6) H(2) 110.0 . . 0_555 no C(1) N(1) C(5) 118.8(2) . . 0_555 yes N(1) C(1) C(2) 121.9(3) . . 0_555 yes N(1) C(1) C(6) 114.0(2) . . 0_555 yes C(2) C(1) C(6) 124.0(3) . . 0_555 yes C(1) C(2) C(3) 118.5(3) . . 0_555 yes C(1) C(2) H(3) 117.5 . . 0_555 no C(3) C(2) H(3) 123.3 . . 0_555 no C(2) C(3) C(4) 120.1(3) . . 0_555 yes C(2) C(3) H(4) 117.0 . . 0_555 no C(4) C(3) H(4) 121.9 . . 0_555 no C(3) C(4) C(5) 117.9(3) . . 0_555 yes C(3) C(4) H(5) 119.4 . . 0_555 no C(5) C(4) H(5) 122.5 . . 0_555 no N(1) C(5) C(4) 122.7(3) . . 0_555 yes N(1) C(5) C(14) 113.2(2) . . 0_555 yes C(4) C(5) C(14) 124.1(3) . . 0_555 yes O(1) C(6) C(1) 108.9(2) . . 0_555 yes O(1) C(6) H(12) 113.5 . . 0_555 no O(1) C(6) H(13) 109.0 . . 0_555 no C(1) C(6) H(12) 107.4 . . 0_555 no C(1) C(6) H(13) 121.2 . . 0_555 no H(12) C(6) H(13) 96.6 . . 0_555 no O(1) C(7) O(2) 121.4(3) . . 0_555 yes O(1) C(7) C(8) 114.9(3) . . 0_555 yes O(2) C(7) C(8) 123.7(3) . . 0_555 yes C(7) C(8) C(9) 119.9(3) . . 0_555 yes C(7) C(8) C(13) 120.6(3) . . 0_555 yes C(9) C(8) C(13) 119.5(3) . . 0_555 yes O(3) C(9) C(8) 123.0(3) . . 0_555 yes O(3) C(9) C(10) 116.9(3) . . 0_555 yes C(8) C(9) C(10) 120.1(3) . . 0_555 yes C(9) C(10) C(11) 119.3(3) . . 0_555 yes C(9) C(10) H(14) 115.6 . . 0_555 no C(11) C(10) H(14) 125.0 . . 0_555 no C(10) C(11) C(12) 121.8(3) . . 0_555 yes C(10) C(11) H(15) 112.0 . . 0_555 no C(12) C(11) H(15) 125.9 . . 0_555 no C(11) C(12) C(13) 119.4(4) . . 0_555 yes C(11) C(12) H(16) 128.0 . . 0_555 no C(13) C(12) H(16) 111.7 . . 0_555 no C(8) C(13) C(12) 119.9(3) . . 0_555 yes C(8) C(13) H(17) 121.3 . . 0_555 no C(12) C(13) H(17) 118.6 . . 0_555 no O(4) C(14) C(5) 109.5(2) . . 0_555 yes O(4) C(14) H(6) 116.4 . . 0_555 no O(4) C(14) H(7) 103.4 . . 0_555 no C(5) C(14) H(6) 109.9 . . 0_555 no C(5) C(14) H(7) 115.3 . . 0_555 no H(6) C(14) H(7) 102.3 . . 0_555 no O(4) C(15) O(5) 121.6(3) . . 0_555 yes O(4) C(15) C(16) 113.5(3) . . 0_555 yes O(5) C(15) C(16) 124.9(3) . . 0_555 yes C(15) C(16) C(17) 120.5(3) . . 0_555 yes C(15) C(16) C(21) 122.3(3) . . 0_555 yes C(17) C(16) C(21) 117.2(3) . . 0_555 yes O(6) C(17) C(16) 121.8(3) . . 0_555 yes O(6) C(17) C(18) 117.3(3) . . 0_555 yes C(16) C(17) C(18) 120.9(3) . . 0_555 yes C(17) C(18) C(19) 119.9(3) . . 0_555 yes C(17) C(18) H(8) 120.9 . . 0_555 no C(19) C(18) H(8) 118.6 . . 0_555 no C(18) C(19) C(20) 120.2(3) . . 0_555 yes C(18) C(19) H(9) 105.9 . . 0_555 no C(20) C(19) H(9) 133.3 . . 0_555 no C(19) C(20) C(21) 120.0(3) . . 0_555 yes C(19) C(20) H(10) 118.8 . . 0_555 no C(21) C(20) H(10) 121.2 . . 0_555 no C(16) C(21) C(20) 121.7(3) . . 0_555 yes C(16) C(21) H(11) 110.2 . . 0_555 no C(20) C(21) H(11) 127.6 . . 0_555 no #------------------------------------------------------------------------------ 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 O(1) C(6) C(1) N(1) 163.0(2) 0_555 27_1 5_555 55_5 yes O(1) C(6) C(1) C(2) -19.8(4) 0_555 27_1 5_555 55_5 yes O(1) C(7) C(8) C(9) 172.8(3) 0_555 27_1 5_555 55_5 yes O(1) C(7) C(8) C(13) -8.7(4) 0_555 27_1 5_555 55_5 yes O(2) C(7) O(1) C(6) -1.7(4) 0_555 27_1 5_555 55_5 yes O(2) C(7) C(8) C(9) -8.7(5) 0_555 27_1 5_555 55_5 yes O(2) C(7) C(8) C(13) 169.7(3) 0_555 27_1 5_555 55_5 yes O(3) C(9) C(8) C(7) -2.2(5) 0_555 27_1 5_555 55_5 yes O(3) C(9) C(8) C(13) 179.3(3) 0_555 27_1 5_555 55_5 yes O(3) C(9) C(10) C(11) -179.0(3) 0_555 27_1 5_555 55_5 yes O(4) C(14) C(5) N(1) -178.6(2) 0_555 27_1 5_555 55_5 yes O(4) C(14) C(5) C(4) 0.6(4) 0_555 27_1 5_555 55_5 yes O(4) C(15) C(16) C(17) 178.6(2) 0_555 27_1 5_555 55_5 yes O(4) C(15) C(16) C(21) -0.6(4) 0_555 27_1 5_555 55_5 yes O(5) C(15) O(4) C(14) 0.9(4) 0_555 27_1 5_555 55_5 yes O(5) C(15) C(16) C(17) -1.6(5) 0_555 27_1 5_555 55_5 yes O(5) C(15) C(16) C(21) 179.2(3) 0_555 27_1 5_555 55_5 yes O(6) C(17) C(16) C(15) 1.4(4) 0_555 27_1 5_555 55_5 yes O(6) C(17) C(16) C(21) -179.4(3) 0_555 27_1 5_555 55_5 yes O(6) C(17) C(18) C(19) 179.4(3) 0_555 27_1 5_555 55_5 yes N(1) C(1) C(2) C(3) 1.5(4) 0_555 27_1 5_555 55_5 yes N(1) C(5) C(4) C(3) -0.4(5) 0_555 27_1 5_555 55_5 yes C(1) N(1) C(5) C(4) 0.7(4) 0_555 27_1 5_555 55_5 yes C(1) N(1) C(5) C(14) 180.0(2) 0_555 27_1 5_555 55_5 yes C(1) C(2) C(3) C(4) -1.2(5) 0_555 27_1 5_555 55_5 yes C(1) C(6) O(1) C(7) 165.4(2) 0_555 27_1 5_555 55_5 yes C(2) C(1) N(1) C(5) -1.3(4) 0_555 27_1 5_555 55_5 yes C(2) C(3) C(4) C(5) 0.7(5) 0_555 27_1 5_555 55_5 yes C(3) C(2) C(1) C(6) -175.6(3) 0_555 27_1 5_555 55_5 yes C(3) C(4) C(5) C(14) -179.6(3) 0_555 27_1 5_555 55_5 yes C(5) N(1) C(1) C(6) 176.1(3) 0_555 27_1 5_555 55_5 yes C(5) C(14) O(4) C(15) -179.0(2) 0_555 27_1 5_555 55_5 yes C(6) O(1) C(7) C(8) 176.8(2) 0_555 27_1 5_555 55_5 yes C(7) C(8) C(9) C(10) 178.7(3) 0_555 27_1 5_555 55_5 yes C(7) C(8) C(13) C(12) -179.1(3) 0_555 27_1 5_555 55_5 yes C(8) C(9) C(10) C(11) 0.2(5) 0_555 27_1 5_555 55_5 yes C(8) C(13) C(12) C(11) 0.7(5) 0_555 27_1 5_555 55_5 yes C(9) C(8) C(13) C(12) -0.7(5) 0_555 27_1 5_555 55_5 yes C(9) C(10) C(11) C(12) -0.2(6) 0_555 27_1 5_555 55_5 yes C(10) C(9) C(8) C(13) 0.2(5) 0_555 27_1 5_555 55_5 yes C(10) C(11) C(12) C(13) -0.3(6) 0_555 27_1 5_555 55_5 yes C(14) O(4) C(15) C(16) -179.3(2) 0_555 27_1 5_555 55_5 yes C(15) C(16) C(17) C(18) -179.5(3) 0_555 27_1 5_555 55_5 yes C(15) C(16) C(21) C(20) 179.9(3) 0_555 27_1 5_555 55_5 yes C(16) C(17) C(18) C(19) 0.2(5) 0_555 27_1 5_555 55_5 yes C(16) C(21) C(20) C(19) -0.9(5) 0_555 27_1 5_555 55_5 yes C(17) C(16) C(21) C(20) 0.6(5) 0_555 27_1 5_555 55_5 yes C(17) C(18) C(19) C(20) -0.5(5) 0_555 27_1 5_555 55_5 yes C(18) C(17) C(16) C(21) -0.3(4) 0_555 27_1 5_555 55_5 yes C(18) C(19) C(20) C(21) 0.8(5) 0_555 27_1 5_555 55_5 yes C(18) C(19) C(20) C(21) 0.8(5) 0_555 27_1 5_555 55_5 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 O(1) C(17) 3.276(4) . 2_757 ? O(1) C(18) 3.306(5) . 2_757 ? O(1) C(10) 3.401(5) . 2_666 ? O(1) O(6) 3.420(3) . 2_757 ? O(1) C(9) 3.600(4) . 2_666 ? O(2) O(6) 2.868(3) . 2_756 ? O(2) O(5) 3.336(4) . 2_756 ? O(2) C(3) 3.426(5) . 1_454 ? O(3) C(13) 3.533(5) . 2_666 ? O(4) C(5) 3.592(4) . 2_757 ? O(5) C(6) 3.522(4) . 2_756 ? O(6) C(12) 3.506(5) . 1_645 ? O(6) C(13) 3.507(4) . 2_757 ? N(1) C(20) 3.570(4) . 1_454 ? N(1) C(19) 3.595(5) . 2_857 ? N(1) C(15) 3.597(4) . 2_757 ? C(4) C(17) 3.513(5) . 2_857 ? C(7) C(9) 3.506(5) . 2_666 ? C(7) C(10) 3.532(6) . 2_666 ? C(7) C(18) 3.578(4) . 2_757 ? C(8) C(8) 3.521(6) . 2_666 ? C(8) C(9) 3.521(5) . 2_666 ? C(14) C(21) 3.591(5) . 2_857 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(3) H(1) O(2) . . . 1.149 1.653 2.630(4) 139.002 no O(6) H(2) O(5) . . . 1.051 1.746 2.643(4) 140.496 no #------------------------------------------------------------------------------ data_haba101_Py(CH2OPhOH)2NaSCN _database_code_CSD 175382 _audit_creation_date 'Fri Jun 29 10:07:30 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H17 N2 Na O4 S ' _chemical_formula_moiety '?' _chemical_formula_weight 404.42 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.744(5) _cell_length_b 16.192(8) _cell_length_c 12.099(6) _cell_angle_alpha 90 _cell_angle_beta 95.72(4) _cell_angle_gamma 90 _cell_volume 1899(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.7 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.750 _exptl_crystal_size_mid 0.750 _exptl_crystal_size_min 0.500 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840.00 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4733 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.72 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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). ; _reflns_number_total 4365 _reflns_number_gt 2088 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1390 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4361 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 0.24 _refine_diff_density_min -0.33 _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) ; 'Na' 'Na' 0.036 0.025 ;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 S(1) S 0.8808(1) -0.17511(7) 0.38684(8) 0.1014(4) Uani 1.00 d . . . Na(1) Na 0.4751(1) 0.00796(7) 0.23709(9) 0.0731(4) Uani 1.00 d . . . O(1) O 0.5768(2) -0.0881(1) 0.3727(1) 0.0644(6) Uani 1.00 d . . . O(2) O 0.3266(2) -0.0314(1) 0.3758(1) 0.0608(6) Uani 1.00 d . . . O(3) O 0.4521(2) 0.1047(1) 0.0834(1) 0.0621(6) Uani 1.00 d . . . O(4) O 0.6716(2) 0.0208(1) 0.1440(1) 0.0700(6) Uani 1.00 d . . . N(1) N 0.2581(2) 0.0803(1) 0.2183(2) 0.0520(6) Uani 1.00 d . . . N(2) N 0.8799(3) -0.0864(2) 0.1919(3) 0.097(1) Uani 1.00 d . . . C(1) C 0.5059(3) -0.1135(1) 0.4591(2) 0.0524(7) Uani 1.00 d . . . C(2) C 0.5622(3) -0.1648(2) 0.5421(2) 0.0622(8) Uani 1.00 d . . . C(3) C 0.4846(4) -0.1886(2) 0.6269(2) 0.0707(10) Uani 1.00 d . . . C(4) C 0.3522(4) -0.1621(2) 0.6264(2) 0.080(1) Uani 1.00 d . . . C(5) C 0.2954(3) -0.1104(2) 0.5435(2) 0.0734(10) Uani 1.00 d . . . C(6) C 0.3717(3) -0.0849(2) 0.4601(2) 0.0550(8) Uani 1.00 d . . . C(7) C 0.1926(3) 0.0024(2) 0.3780(2) 0.0648(9) Uani 1.00 d . . . C(8) C 0.1621(3) 0.0645(2) 0.2870(2) 0.0557(8) Uani 1.00 d . . . C(9) C 0.0346(3) 0.1029(2) 0.2762(2) 0.0731(10) Uani 1.00 d . . . C(10) C 0.0048(3) 0.1584(2) 0.1927(3) 0.081(1) Uani 1.00 d . . . C(11) C 0.1028(3) 0.1747(2) 0.1208(2) 0.0682(9) Uani 1.00 d . . . C(12) C 0.2269(3) 0.1351(2) 0.1364(2) 0.0537(8) Uani 1.00 d . . . C(13) C 0.3328(3) 0.1534(2) 0.0579(2) 0.0620(8) Uani 1.00 d . . . C(14) C 0.5563(3) 0.1125(2) 0.0152(2) 0.0559(8) Uani 1.00 d . . . C(15) C 0.5517(3) 0.1594(2) -0.0799(2) 0.0690(9) Uani 1.00 d . . . C(16) C 0.6646(4) 0.1614(2) -0.1408(2) 0.080(1) Uani 1.00 d . . . C(17) C 0.7797(4) 0.1169(2) -0.1080(2) 0.076(1) Uani 1.00 d . . . C(18) C 0.7855(3) 0.0686(2) -0.0130(2) 0.0665(9) Uani 1.00 d . . . C(19) C 0.6742(3) 0.0665(2) 0.0491(2) 0.0574(8) Uani 1.00 d . . . C(20) C 0.8800(3) -0.1234(2) 0.2734(3) 0.0694(10) Uani 1.00 d . . . H(1) H 0.6571 -0.1846 0.5411 0.0767 Uiso 1.00 calc . . . H(2) H 0.5242 -0.2244 0.6869 0.0877 Uiso 1.00 calc . . . H(3) H 0.2961 -0.1790 0.6851 0.0947 Uiso 1.00 calc . . . H(4) H 0.2000 -0.0926 0.5419 0.0899 Uiso 1.00 calc . . . H(5) H 0.1256 -0.0416 0.3702 0.0796 Uiso 1.00 calc . . . H(6) H 0.1856 0.0276 0.4494 0.0796 Uiso 1.00 calc . . . H(7) H -0.0328 0.0900 0.3278 0.0878 Uiso 1.00 calc . . . H(8) H -0.0818 0.1869 0.1827 0.0955 Uiso 1.00 calc . . . H(9) H 0.0841 0.2139 0.0605 0.0814 Uiso 1.00 calc . . . H(10) H 0.3569 0.2114 0.0621 0.0756 Uiso 1.00 calc . . . H(11) H 0.2944 0.1431 -0.0175 0.0756 Uiso 1.00 calc . . . H(12) H 0.4707 0.1913 -0.1027 0.0844 Uiso 1.00 calc . . . H(13) H 0.6610 0.1940 -0.2073 0.0949 Uiso 1.00 calc . . . H(14) H 0.8578 0.1191 -0.1512 0.0919 Uiso 1.00 calc . . . H(15) H 0.8671 0.0351 0.0103 0.0802 Uiso 1.00 calc . . . H(16) H 0.7729 0.0018 0.1505 0.1113 Uiso 1.00 calc . . . H(17) H 0.6800 -0.1034 0.3797 0.1113 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 S(1) 0.0993(7) 0.1190(8) 0.0891(6) 0.0395(6) 0.0258(5) 0.0250(5) Na(1) 0.0624(7) 0.0862(8) 0.0741(7) 0.0165(6) 0.0227(5) 0.0239(6) O(1) 0.053(1) 0.077(1) 0.065(1) 0.0031(9) 0.0139(9) 0.0130(9) O(2) 0.056(1) 0.070(1) 0.059(1) 0.0082(9) 0.0176(8) 0.0107(9) O(3) 0.058(1) 0.069(1) 0.061(1) 0.0112(9) 0.0123(9) 0.0123(9) O(4) 0.063(1) 0.085(1) 0.064(1) 0.012(1) 0.0164(9) 0.014(1) N(1) 0.050(1) 0.053(1) 0.053(1) -0.0002(10) 0.0031(10) -0.005(1) N(2) 0.084(2) 0.099(2) 0.108(2) 0.023(2) 0.017(2) 0.022(2) C(1) 0.059(2) 0.049(1) 0.049(1) -0.008(1) 0.005(1) -0.003(1) C(2) 0.066(2) 0.060(2) 0.058(2) -0.006(1) -0.004(1) 0.001(1) C(3) 0.094(2) 0.062(2) 0.055(2) -0.011(2) 0.002(2) 0.004(1) C(4) 0.099(3) 0.081(2) 0.064(2) -0.006(2) 0.028(2) 0.012(2) C(5) 0.079(2) 0.077(2) 0.068(2) 0.005(2) 0.026(2) 0.015(2) C(6) 0.063(2) 0.052(2) 0.051(1) -0.003(1) 0.010(1) 0.000(1) C(7) 0.053(2) 0.074(2) 0.070(2) 0.000(1) 0.018(1) 0.001(1) C(8) 0.049(2) 0.060(2) 0.058(2) -0.001(1) 0.005(1) -0.008(1) C(9) 0.052(2) 0.087(2) 0.082(2) 0.010(2) 0.016(1) -0.002(2) C(10) 0.062(2) 0.091(2) 0.089(2) 0.027(2) 0.003(2) -0.002(2) C(11) 0.062(2) 0.071(2) 0.070(2) 0.019(1) 0.000(2) 0.004(1) C(12) 0.055(2) 0.051(1) 0.053(1) 0.001(1) -0.002(1) -0.006(1) C(13) 0.063(2) 0.063(2) 0.059(2) 0.009(1) 0.001(1) 0.006(1) C(14) 0.064(2) 0.056(2) 0.049(1) -0.005(1) 0.013(1) -0.003(1) C(15) 0.081(2) 0.070(2) 0.057(2) 0.003(2) 0.011(1) 0.008(1) C(16) 0.103(3) 0.082(2) 0.058(2) -0.013(2) 0.023(2) 0.004(2) C(17) 0.087(2) 0.079(2) 0.066(2) -0.017(2) 0.028(2) -0.009(2) C(18) 0.064(2) 0.068(2) 0.069(2) -0.004(1) 0.018(1) -0.012(1) C(19) 0.062(2) 0.059(2) 0.052(2) -0.006(1) 0.009(1) -0.006(1) C(20) 0.054(2) 0.071(2) 0.084(2) 0.012(1) 0.008(2) -0.002(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _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 S(1) C(20) 1.607(3) . . yes Na(1) O(1) 2.402(2) . . yes Na(1) O(2) 2.408(2) . . yes Na(1) O(3) 2.425(2) . . yes Na(1) O(4) 2.326(2) . . yes Na(1) N(1) 2.408(2) . . yes O(1) C(1) 1.372(3) . . yes O(1) H(17) 1.031 . . no O(2) C(6) 1.377(3) . . yes O(2) C(7) 1.418(3) . . yes O(3) C(13) 1.414(3) . . yes O(3) C(14) 1.376(3) . . yes O(4) C(19) 1.368(3) . . yes O(4) H(16) 1.030 . . no N(1) C(8) 1.336(3) . . yes N(1) C(12) 1.343(3) . . yes N(2) C(20) 1.154(4) . . yes C(1) C(2) 1.375(3) . . yes C(1) C(6) 1.388(4) . . yes C(2) C(3) 1.388(4) . . yes C(2) H(1) 0.980 . . no C(3) C(4) 1.359(4) . . yes C(3) H(2) 0.978 . . no C(4) C(5) 1.379(4) . . yes C(4) H(3) 0.978 . . no C(5) C(6) 1.375(4) . . yes C(5) H(4) 0.972 . . no C(7) C(8) 1.499(4) . . yes C(7) H(5) 0.965 . . no C(7) H(6) 0.965 . . no C(8) C(9) 1.385(4) . . yes C(9) C(10) 1.362(4) . . yes C(9) H(7) 0.972 . . no C(10) C(11) 1.379(4) . . yes C(10) H(8) 0.959 . . no C(11) C(12) 1.365(3) . . yes C(11) H(9) 0.971 . . no C(12) C(13) 1.500(4) . . yes C(13) H(10) 0.968 . . no C(13) H(11) 0.965 . . no C(14) C(15) 1.375(3) . . yes C(14) C(19) 1.396(4) . . yes C(15) C(16) 1.383(4) . . yes C(15) H(12) 0.960 . . no C(16) C(17) 1.359(4) . . yes C(16) H(13) 0.961 . . no C(17) C(18) 1.387(4) . . yes C(17) H(14) 0.966 . . no C(18) C(19) 1.380(4) . . yes C(18) H(15) 0.980 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Na(1) O(2) 65.70(6) . 1_555 1_555 yes O(1) Na(1) O(3) 160.48(7) . 1_555 1_555 yes O(1) Na(1) O(4) 94.91(7) . 1_555 1_555 yes O(1) Na(1) N(1) 132.67(8) . 1_555 1_555 yes O(2) Na(1) O(3) 133.57(7) . 1_555 1_555 yes O(2) Na(1) O(4) 160.43(8) . 1_555 1_555 yes O(2) Na(1) N(1) 67.12(7) . 1_555 1_555 yes O(3) Na(1) O(4) 65.67(6) . 1_555 1_555 yes O(3) Na(1) N(1) 66.45(7) . 1_555 1_555 yes O(4) Na(1) N(1) 131.94(8) . 1_555 1_555 yes Na(1) O(1) C(1) 120.7(1) . 1_555 1_555 yes Na(1) O(1) H(17) 123.0 . 1_555 1_555 no C(1) O(1) H(17) 115.2 . 1_555 1_555 no Na(1) O(2) C(6) 120.8(1) . 1_555 1_555 yes Na(1) O(2) C(7) 122.0(1) . 1_555 1_555 yes C(6) O(2) C(7) 117.1(2) . 1_555 1_555 yes Na(1) O(3) C(13) 122.6(1) . 1_555 1_555 yes Na(1) O(3) C(14) 120.1(2) . 1_555 1_555 yes C(13) O(3) C(14) 117.3(2) . 1_555 1_555 yes Na(1) O(4) C(19) 122.7(2) . 1_555 1_555 yes Na(1) O(4) H(16) 139.9 . 1_555 1_555 no C(19) O(4) H(16) 97.3 . 1_555 1_555 no Na(1) N(1) C(8) 120.7(2) . 1_555 1_555 yes Na(1) N(1) C(12) 121.5(2) . 1_555 1_555 yes C(8) N(1) C(12) 117.7(2) . 1_555 1_555 yes O(1) C(1) C(2) 122.9(2) . 1_555 1_555 yes O(1) C(1) C(6) 116.9(2) . 1_555 1_555 yes C(2) C(1) C(6) 120.2(2) . 1_555 1_555 yes C(1) C(2) C(3) 120.0(3) . 1_555 1_555 yes C(1) C(2) H(1) 119.8 . 1_555 1_555 no C(3) C(2) H(1) 120.2 . 1_555 1_555 no C(2) C(3) C(4) 119.7(3) . 1_555 1_555 yes C(2) C(3) H(2) 120.6 . 1_555 1_555 no C(4) C(3) H(2) 119.7 . 1_555 1_555 no C(3) C(4) C(5) 120.4(3) . 1_555 1_555 yes C(3) C(4) H(3) 120.6 . 1_555 1_555 no C(5) C(4) H(3) 119.0 . 1_555 1_555 no C(4) C(5) C(6) 120.6(3) . 1_555 1_555 yes C(4) C(5) H(4) 120.5 . 1_555 1_555 no C(6) C(5) H(4) 118.9 . 1_555 1_555 no O(2) C(6) C(1) 115.8(2) . 1_555 1_555 yes O(2) C(6) C(5) 125.2(2) . 1_555 1_555 yes C(1) C(6) C(5) 119.0(2) . 1_555 1_555 yes O(2) C(7) C(8) 111.1(2) . 1_555 1_555 yes O(2) C(7) H(5) 109.3 . 1_555 1_555 no O(2) C(7) H(6) 109.1 . 1_555 1_555 no C(8) C(7) H(5) 109.9 . 1_555 1_555 no C(8) C(7) H(6) 110.3 . 1_555 1_555 no H(5) C(7) H(6) 107.0 . 1_555 1_555 no N(1) C(8) C(7) 119.1(2) . 1_555 1_555 yes N(1) C(8) C(9) 122.2(3) . 1_555 1_555 yes C(7) C(8) C(9) 118.7(2) . 1_555 1_555 yes C(8) C(9) C(10) 119.3(3) . 1_555 1_555 yes C(8) C(9) H(7) 120.0 . 1_555 1_555 no C(10) C(9) H(7) 120.7 . 1_555 1_555 no C(9) C(10) C(11) 119.0(3) . 1_555 1_555 yes C(9) C(10) H(8) 122.0 . 1_555 1_555 no C(11) C(10) H(8) 119.0 . 1_555 1_555 no C(10) C(11) C(12) 118.8(3) . 1_555 1_555 yes C(10) C(11) H(9) 120.6 . 1_555 1_555 no C(12) C(11) H(9) 120.5 . 1_555 1_555 no N(1) C(12) C(11) 123.0(2) . 1_555 1_555 yes N(1) C(12) C(13) 118.6(2) . 1_555 1_555 yes C(11) C(12) C(13) 118.4(2) . 1_555 1_555 yes O(3) C(13) C(12) 110.8(2) . 1_555 1_555 yes O(3) C(13) H(10) 109.9 . 1_555 1_555 no O(3) C(13) H(11) 110.0 . 1_555 1_555 no C(12) C(13) H(10) 109.7 . 1_555 1_555 no C(12) C(13) H(11) 109.7 . 1_555 1_555 no H(10) C(13) H(11) 106.7 . 1_555 1_555 no O(3) C(14) C(15) 126.0(2) . 1_555 1_555 yes O(3) C(14) C(19) 114.2(2) . 1_555 1_555 yes C(15) C(14) C(19) 119.8(2) . 1_555 1_555 yes C(14) C(15) C(16) 119.8(3) . 1_555 1_555 yes C(14) C(15) H(12) 119.6 . 1_555 1_555 no C(16) C(15) H(12) 120.6 . 1_555 1_555 no C(15) C(16) C(17) 120.6(3) . 1_555 1_555 yes C(15) C(16) H(13) 119.6 . 1_555 1_555 no C(17) C(16) H(13) 119.7 . 1_555 1_555 no C(16) C(17) C(18) 120.4(3) . 1_555 1_555 yes C(16) C(17) H(14) 119.6 . 1_555 1_555 no C(18) C(17) H(14) 120.0 . 1_555 1_555 no C(17) C(18) C(19) 119.7(3) . 1_555 1_555 yes C(17) C(18) H(15) 121.0 . 1_555 1_555 no C(19) C(18) H(15) 119.3 . 1_555 1_555 no O(4) C(19) C(14) 116.8(2) . 1_555 1_555 yes O(4) C(19) C(18) 123.5(2) . 1_555 1_555 yes C(14) C(19) C(18) 119.7(2) . 1_555 1_555 yes S(1) C(20) N(2) 179.7(3) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Na(1) O(1) C(1) C(2) -176.4(2) 1_555 1_555 1_555 1_555 yes Na(1) O(1) C(1) C(6) 3.5(3) 1_555 1_555 1_555 1_555 yes Na(1) O(2) C(6) C(1) 0.1(3) 1_555 1_555 1_555 1_555 yes Na(1) O(2) C(6) C(5) 179.4(2) 1_555 1_555 1_555 1_555 yes Na(1) O(2) C(7) C(8) -1.4(3) 1_555 1_555 1_555 1_555 yes Na(1) O(3) C(13) C(12) -1.0(3) 1_555 1_555 1_555 1_555 yes Na(1) O(3) C(14) C(15) 174.0(2) 1_555 1_555 1_555 1_555 yes Na(1) O(3) C(14) C(19) -5.2(3) 1_555 1_555 1_555 1_555 yes Na(1) O(4) C(19) C(14) 6.1(3) 1_555 1_555 1_555 1_555 yes Na(1) O(4) C(19) C(18) -173.7(2) 1_555 1_555 1_555 1_555 yes Na(1) N(1) C(8) C(7) 1.5(3) 1_555 1_555 1_555 1_555 yes Na(1) N(1) C(8) C(9) -177.8(2) 1_555 1_555 1_555 1_555 yes Na(1) N(1) C(12) C(11) 177.3(2) 1_555 1_555 1_555 1_555 yes Na(1) N(1) C(12) C(13) -2.3(3) 1_555 1_555 1_555 1_555 yes O(1) Na(1) O(2) C(6) 1.2(2) 1_555 1_555 1_555 1_555 yes O(1) Na(1) O(2) C(7) 177.9(2) 1_555 1_555 1_555 1_555 yes O(1) Na(1) O(3) C(13) -169.6(2) 1_555 1_555 1_555 1_555 yes O(1) Na(1) O(3) C(14) 11.9(3) 1_555 1_555 1_555 1_555 yes O(1) Na(1) O(4) C(19) 175.8(2) 1_555 1_555 1_555 1_555 yes O(1) Na(1) N(1) C(8) -6.2(2) 1_555 1_555 1_555 1_555 yes O(1) Na(1) N(1) C(12) 176.6(2) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(3) -179.7(2) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(6) O(2) -2.3(3) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(6) C(5) 178.3(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) O(1) C(1) -2.4(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) O(3) C(13) 0.0(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) O(3) C(14) -178.5(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) O(4) C(19) -176.7(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) N(1) C(8) -1.6(2) 1_555 1_555 1_555 1_555 yes O(2) Na(1) N(1) C(12) -178.8(2) 1_555 1_555 1_555 1_555 yes O(2) C(6) C(1) C(2) 177.7(2) 1_555 1_555 1_555 1_555 yes O(2) C(6) C(5) C(4) -177.8(3) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) N(1) 0.0(3) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 179.3(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) O(1) C(1) 169.3(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) O(2) C(6) -175.0(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) O(2) C(7) 1.7(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) O(4) C(19) -6.2(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) N(1) C(8) 178.5(2) 1_555 1_555 1_555 1_555 yes O(3) Na(1) N(1) C(12) 1.3(2) 1_555 1_555 1_555 1_555 yes O(3) C(13) C(12) N(1) 2.1(3) 1_555 1_555 1_555 1_555 yes O(3) C(13) C(12) C(11) -177.6(2) 1_555 1_555 1_555 1_555 yes O(3) C(14) C(15) C(16) -179.8(3) 1_555 1_555 1_555 1_555 yes O(3) C(14) C(19) O(4) -0.3(3) 1_555 1_555 1_555 1_555 yes O(3) C(14) C(19) C(18) 179.4(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) O(1) C(1) 174.8(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) O(2) C(6) -7.0(3) 1_555 1_555 1_555 1_555 yes O(4) Na(1) O(2) C(7) 169.6(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) O(3) C(13) -175.7(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) O(3) C(14) 5.9(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) N(1) C(8) -176.2(2) 1_555 1_555 1_555 1_555 yes O(4) Na(1) N(1) C(12) 6.6(2) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(14) C(15) -179.6(2) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(18) C(17) -179.8(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(1) C(1) 2.3(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(2) C(6) -175.1(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(2) C(7) 1.6(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(3) C(13) 0.0(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(3) C(14) -178.4(2) 1_555 1_555 1_555 1_555 yes N(1) Na(1) O(4) C(19) -11.5(2) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(9) C(10) 0.4(4) 1_555 1_555 1_555 1_555 yes N(1) C(12) C(11) C(10) 0.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 1.2(4) 1_555 1_555 1_555 1_555 yes C(1) C(6) O(2) C(7) -176.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 1.5(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) -1.7(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -1.5(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 0.4(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 0.1(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) O(2) C(7) 2.6(4) 1_555 1_555 1_555 1_555 yes C(6) O(2) C(7) C(8) 175.3(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(12) 178.8(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -178.9(3) 1_555 1_555 1_555 1_555 yes C(8) N(1) C(12) C(11) 0.1(4) 1_555 1_555 1_555 1_555 yes C(8) N(1) C(12) C(13) -179.6(2) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 0.1(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) N(1) C(12) -0.5(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) -0.5(5) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) -179.9(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) O(3) C(14) 177.4(2) 1_555 1_555 1_555 1_555 yes C(13) O(3) C(14) C(15) -4.5(4) 1_555 1_555 1_555 1_555 yes C(13) O(3) C(14) C(19) 176.3(2) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 0.4(5) 1_555 1_555 1_555 1_555 yes C(14) C(19) C(18) C(17) 0.5(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(19) C(18) 0.2(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) 0.3(5) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(14) C(19) -0.7(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) -0.8(4) 1_555 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(1) O(1) 3.270(2) . . ? S(1) C(15) 3.572(3) . 2_645 ? Na(1) C(16) 3.226(3) . 3_655 ? Na(1) C(19) 3.274(3) . . ? Na(1) C(8) 3.297(3) . . ? Na(1) C(15) 3.306(3) . 3_655 ? Na(1) C(12) 3.315(3) . . ? Na(1) C(1) 3.318(3) . . ? Na(1) C(6) 3.331(3) . . ? Na(1) C(14) 3.336(3) . . ? Na(1) C(4) 3.352(4) . 3_656 ? Na(1) C(3) 3.359(3) . 3_656 ? Na(1) C(7) 3.380(3) . . ? Na(1) C(13) 3.402(3) . . ? Na(1) C(17) 3.452(3) . 3_655 ? O(1) C(20) 3.348(4) . . ? O(1) C(6) 3.461(3) . 3_656 ? O(1) C(5) 3.558(4) . 3_656 ? O(2) C(1) 3.392(3) . 3_656 ? O(2) C(2) 3.470(3) . 3_656 ? O(2) C(16) 3.546(4) . 3_655 ? O(2) C(17) 3.581(3) . 3_655 ? O(3) C(19) 3.373(3) . 3_655 ? O(3) O(4) 3.534(3) . 3_655 ? O(4) N(2) 2.690(3) . . ? O(4) C(20) 3.376(4) . . ? O(4) C(14) 3.528(3) . 3_655 ? N(1) C(3) 3.454(4) . 3_656 ? N(1) C(18) 3.458(3) . 3_655 ? N(1) C(17) 3.467(4) . 3_655 ? N(1) C(2) 3.512(3) . 3_656 ? N(2) C(9) 3.522(4) . 1_655 ? N(2) C(19) 3.527(4) . . ? N(2) C(18) 3.582(4) . . ? N(2) C(17) 3.599(5) . 3_755 ? C(1) C(6) 3.530(3) . 3_656 ? C(2) C(11) 3.547(4) . 2_545 ? C(10) C(18) 3.438(4) . 1_455 ?