# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/210 data_paper # TITLE ################################################ _publ_section_title ;On the Role of Hydronium Ions in the Protonated Micellar Aggregates of Bile Salts. ; # AUTHOR LIST ############################################ loop_ _publ_author_name _publ_author_address 'Candeloro De Sanctis, Sofia' ;Dipartimento di Chimica, Universita' di Roma La Sapienza ; 'DArchivio, Angelo A.' ;Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita' di L'Aquila ; 'Galantini, Luciano' ;Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita' di L'Aquila ; 'Gavuzzo, Enrico' ;Istituto di Strutturistica Chimica "Giordano Giacomello" CNR ; 'Giglio, Edoardo' ;Dipartimento di Chimica, Universita' di Roma La Sapienza 'To whom correspondence should be addressed' ; #MATERIAL RELEVANT TO HGDC# data_HGDC _chemical_formula_sum 'H49C29N1O6' _chemical_formula_weight 507.7 _computing_structure_solution 'SIR92(Altomare al.,J.Appl.Cryst.,1994,27,435)' _computing_structure_refinement 'SIR-CAOS(Camalli al.,User Guide,1986)' _cell_length_a 18.275(2) _cell_length_b 18.275(2) _cell_length_c 7.383(1) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_volume 2135.4(4) _cell_formula_units_Z 3 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'p 31' _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-y,+x-y,1/3+z' '-x+y,-x,2/3+z' _exptl_crystal_density_diffrn 1.18 _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 0.661 _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'X-ray tube,12kW rotating anode' _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 61.97 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 147 'Hydrogen ' 0.0000 0.0000 ' Int. Tab.IV,1974' 'c ' 87 'Carbon ' 0.0170 0.0090 ' Int. Tab.IV,1974' 'n ' 3 'Nitrogen ' 0.0290 0.0180 ' Int. Tab.IV,1974' 'o ' 18 'Oxygen ' 0.0470 0.0320 ' Int. Tab.IV,1974' _reflns_number_total 2238 _reflns_number_observed 1936 _reflns_observed_criterion ' F >4.0 sigma(F) ' _reflns_limit_h_max 20 _reflns_limit_h_min 0 _reflns_limit_k_max 0 _reflns_limit_k_min -17 _reflns_limit_l_max 8 _reflns_limit_l_min -8 _reflns_d_resolution_high 0.873 _reflns_d_resolution_low 15.827 _refine_ls_structure_factor_coef F _refine_ls_extinction_method 'none' _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ' H atoms rigid to parent C atom ' _refine_ls_weighting_scheme 'W=(Sin(Theta)/Lambda)^P(2)' _refine_ls_number_reflns 1936 _refine_ls_number_parameters 324 _refine_ls_R_factor_obs 0.044 _refine_ls_wR_factor_obs 0.056 _refine_diff_density_max 0.202 _refine_diff_density_min -0.145 _refine_diff_density_rms 0.038 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type c(1) 0.1723(3) 0.4048(3) 0.9253(8) 1.000 0.055(2) uani c(2) 0.1239(3) 0.3128(3) 0.8697(9) 1.000 0.057(2) uani c(3) 0.1627(3) 0.2974(3) 0.7042(9) 1.000 0.062(2) uani c(4) 0.1719(3) 0.3560(3) 0.5492(9) 1.000 0.060(2) uani c(5) 0.2190(3) 0.4500(3) 0.6054(8) 1.000 0.051(2) uani c(6) 0.2259(3) 0.5072(3) 0.4468(8) 1.000 0.056(2) uani c(7) 0.1412(3) 0.5012(3) 0.3998(8) 1.000 0.052(2) uani c(8) 0.0983(2) 0.5146(3) 0.5649(7) 1.000 0.043(2) uani c(9) 0.0911(2) 0.4543(3) 0.7198(7) 1.000 0.041(2) uani c(10) 0.1785(3) 0.4667(3) 0.7754(8) 1.000 0.048(2) uani c(11) 0.0386(3) 0.4571(3) 0.8792(7) 1.000 0.045(2) uani c(12) -0.0482(3) 0.4425(3) 0.8228(7) 1.000 0.045(2) uani c(13) -0.0387(2) 0.5075(2) 0.6792(7) 1.000 0.040(2) uani c(14) 0.0109(2) 0.4994(2) 0.5181(7) 1.000 0.041(2) uani c(15) 0.0009(3) 0.5513(3) 0.3693(8) 1.000 0.051(2) uani c(16) -0.0877(3) 0.5381(3) 0.3984(8) 1.000 0.052(2) uani c(17) -0.1215(3) 0.4901(3) 0.5804(7) 1.000 0.043(2) uani c(18) 0.0059(3) 0.5967(3) 0.7617(8) 1.000 0.053(2) uani c(19) 0.2372(3) 0.5558(3) 0.8481(9) 1.000 0.061(2) uani c(20) -0.1824(3) 0.5124(3) 0.6756(8) 1.000 0.048(2) uani c(21) -0.2091(4) 0.4741(4) 0.8656(9) 1.000 0.070(3) uani c(22) -0.2615(3) 0.4839(3) 0.5598(9) 1.000 0.059(2) uani c(23) -0.3070(3) 0.5337(3) 0.5995(9) 1.000 0.057(2) uani c(24) -0.2615(3) 0.6196(3) 0.5181(8) 1.000 0.054(2) uani o(25) 0.1134(3) 0.2099(2) 0.6459(8) 1.000 0.076(2) uani o(26) -0.0986(2) 0.3600(2) 0.7485 1.000 0.055(1) uani o(27) -0.2461(2) 0.6307(3) 0.3534(7) 1.000 0.073(2) uani n(28) -0.2365(3) 0.6862(3) 0.6265(8) 1.000 0.061(2) uani c(29) -0.1842(4) 0.7703(4) 0.555(1) 1.000 0.069(3) uani c(30) -0.0936(4) 0.7895(3) 0.5208(9) 1.000 0.062(2) uani o(31) -0.0652(3) 0.7484(3) 0.5723(8) 1.000 0.078(2) uani o(32) -0.0520(3) 0.8597(3) 0.4270(8) 1.000 0.084(2) uani c(33) -0.0933(4) 0.7924(4) 0.991(1) 1.000 0.073(3) uani c(34) -0.0787(5) 0.7226(5) 1.043(1) 1.000 0.093(4) uani c(35) -0.0183(5) 0.8768(5) 0.954(1) 1.000 0.103(4) uani o(36) -0.1638(3) 0.7808(3) 0.9776(9) 1.000 0.087(2) uani h(11) 0.2356(3) 0.4201(3) 0.9625(8) 1.000 0.056 uiso h(12) 0.1412(3) 0.4131(3) 1.0412(8) 1.000 0.056 uiso h(21) 0.1249(3) 0.2744(3) 0.9798(9) 1.000 0.058 uiso h(22) 0.0594(3) 0.2957(3) 0.8401(9) 1.000 0.058 uiso h(31) 0.2252(3) 0.3103(3) 0.7422(9) 1.000 0.063 uiso h(41) 0.2069(3) 0.3475(3) 0.4415(9) 1.000 0.059 uiso h(42) 0.1096(3) 0.3394(3) 0.5010(9) 1.000 0.059 uiso h(51) 0.2824(3) 0.4660(3) 0.6427(8) 1.000 0.051 uiso h(61) 0.2703(3) 0.5719(3) 0.4829(8) 1.000 0.059 uiso h(62) 0.2489(3) 0.4895(3) 0.3295(8) 1.000 0.059 uiso h(71) 0.1518(3) 0.5480(3) 0.2982(8) 1.000 0.052 uiso h(72) 0.0995(3) 0.4389(3) 0.3464(8) 1.000 0.052 uiso h(81) 0.1367(2) 0.5796(3) 0.6071(7) 1.000 0.044 uiso h(91) 0.0565(2) 0.3907(3) 0.6669(7) 1.000 0.041 uiso h(111) 0.0300(3) 0.4091(3) 0.9758(7) 1.000 0.046 uiso h(112) 0.0733(3) 0.5186(3) 0.9421(7) 1.000 0.046 uiso h(121) -0.0781(3) 0.4492(3) 0.9427(7) 1.000 0.047 uiso h(141) -0.0137(2) 0.4352(2) 0.4719(7) 1.000 0.041 uiso h(151) 0.0482(3) 0.6173(3) 0.3812(8) 1.000 0.052 uiso h(152) 0.0056(3) 0.5282(3) 0.2376(8) 1.000 0.052 uiso h(161) -0.0848(3) 0.5985(3) 0.4053(8) 1.000 0.052 uiso h(162) -0.1288(3) 0.5014(3) 0.2886(8) 1.000 0.052 uiso h(171) -0.1636(3) 0.4227(3) 0.5729(7) 1.000 0.044 uiso h(181) 0.0126(3) 0.6421(3) 0.6600(8) 1.000 0.054 uiso h(182) -0.0312(3) 0.5989(3) 0.8731(8) 1.000 0.054 uiso h(183) 0.0676(3) 0.6116(3) 0.8102(8) 1.000 0.054 uiso h(191) 0.2970(3) 0.5619(3) 0.8862(9) 1.000 0.061 uiso h(192) 0.2473(3) 0.6018(3) 0.7447(9) 1.000 0.061 uiso h(193) 0.2084(3) 0.5666(3) 0.9652(9) 1.000 0.061 uiso h(201) -0.1481(3) 0.5803(3) 0.6909(8) 1.000 0.049 uiso h(211) -0.2516(4) 0.4927(4) 0.9233(9) 1.000 0.071 uiso h(212) -0.2406(4) 0.4060(4) 0.8571(9) 1.000 0.071 uiso h(213) -0.1537(4) 0.4968(4) 0.9503(9) 1.000 0.071 uiso h(221) -0.2434(3) 0.4924(3) 0.4188(9) 1.000 0.061 uiso h(222) -0.3045(3) 0.4178(3) 0.5862(9) 1.000 0.061 uiso h(231) -0.3701(3) 0.4998(3) 0.5441(9) 1.000 0.057 uiso h(232) -0.3104(3) 0.5398(3) 0.7443(9) 1.000 0.057 uiso h(281) -0.2542(3) 0.6780(3) 0.7566(8) 1.000 0.062 uiso h(291) -0.2107(4) 0.7755(4) 0.428(1) 1.000 0.070 uiso h(292) -0.1828(4) 0.8159(4) 0.650(1) 1.000 0.070 uiso h(341) -0.1392(5) 0.6664(5) 1.064(1) 1.000 0.096 uiso h(342) -0.0451(5) 0.7112(5) 0.937(1) 1.000 0.096 uiso h(343) -0.0423(5) 0.7385(5) 1.167(1) 1.000 0.096 uiso h(351) -0.0383(5) 0.9213(5) 0.918(1) 1.000 0.105 uiso h(352) 0.0206(5) 0.8987(5) 1.075(1) 1.000 0.105 uiso h(353) 0.0177(5) 0.8713(5) 0.844(1) 1.000 0.105 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 c(1) 0.051(2) 0.037(2) -0.008(2) 0.066(3) 0.001(2) 0.059(3) c(2) 0.053(3) 0.030(2) 0.005(2) 0.053(3) 0.011(2) 0.070(3) c(3) 0.052(3) 0.032(2) -0.003(3) 0.049(3) -0.004(2) 0.095(4) c(4) 0.058(3) 0.033(2) 0.008(2) 0.058(3) -0.005(2) 0.069(3) c(5) 0.036(2) 0.023(2) 0.006(2) 0.047(2) 0.001(2) 0.070(3) c(6) 0.041(2) 0.024(2) 0.014(2) 0.059(3) 0.006(2) 0.068(3) c(7) 0.047(2) 0.029(2) 0.011(2) 0.060(3) 0.007(2) 0.053(3) c(8) 0.035(2) 0.016(2) 0.007(2) 0.039(2) 0.001(2) 0.052(2) c(9) 0.036(2) 0.020(2) -0.002(2) 0.042(2) -0.003(2) 0.046(2) c(10) 0.040(2) 0.022(2) -0.006(2) 0.046(2) -0.005(2) 0.057(2) c(11) 0.042(2) 0.028(2) -0.001(2) 0.054(2) -0.001(2) 0.045(2) c(12) 0.041(2) 0.026(2) 0.003(2) 0.051(2) 0.001(2) 0.046(2) c(13) 0.036(2) 0.017(2) 0.003(2) 0.037(2) 0.002(2) 0.046(2) c(14) 0.037(2) 0.017(2) 0.003(2) 0.040(2) 0.001(2) 0.044(2) c(15) 0.051(2) 0.029(2) 0.008(2) 0.055(2) 0.011(2) 0.052(3) c(16) 0.054(2) 0.036(2) 0.000(2) 0.060(3) 0.008(2) 0.052(3) c(17) 0.043(2) 0.024(2) 0.001(2) 0.043(2) 0.001(2) 0.047(2) c(18) 0.050(2) 0.028(2) -0.007(2) 0.052(3) -0.011(2) 0.062(3) c(19) 0.041(2) 0.020(2) -0.014(2) 0.055(3) -0.010(2) 0.080(3) c(20) 0.043(2) 0.024(2) -0.002(2) 0.052(2) -0.002(2) 0.051(2) c(21) 0.060(3) 0.049(3) 0.014(2) 0.100(4) 0.013(3) 0.063(3) c(22) 0.042(2) 0.027(2) -0.006(2) 0.065(3) -0.006(2) 0.070(3) c(23) 0.038(2) 0.029(2) -0.001(2) 0.068(3) -0.002(2) 0.066(3) c(24) 0.032(2) 0.027(2) -0.005(2) 0.072(3) 0.002(2) 0.061(3) o(25) 0.074(2) 0.039(2) 0.002(2) 0.057(2) -0.009(2) 0.107(3) o(26) 0.044(2) 0.014(1) -0.005(1) 0.046(2) 0.010(1) 0.065(2) o(27) 0.061(2) 0.019(2) -0.005(2) 0.080(3) 0.003(2) 0.058(2) n(28) 0.054(2) 0.032(2) -0.003(2) 0.068(3) -0.006(2) 0.063(2) c(29) 0.068(3) 0.040(3) -0.001(3) 0.065(3) 0.004(3) 0.084(4) c(30) 0.062(3) 0.027(2) -0.009(2) 0.055(3) -0.003(2) 0.065(3) o(31) 0.073(2) 0.047(2) -0.001(2) 0.081(3) 0.013(2) 0.092(3) o(32) 0.076(3) 0.047(2) 0.010(2) 0.080(3) 0.022(2) 0.108(3) c(33) 0.075(4) 0.042(3) -0.003(3) 0.082(4) -0.012(3) 0.065(3) c(34) 0.103(5) 0.068(4) -0.007(4) 0.100(5) -0.012(4) 0.099(5) c(35) 0.082(4) 0.022(4) -0.018(4) 0.098(5) 0.001(4) 0.099(5) o(36) 0.074(3) 0.049(2) -0.004(2) 0.092(3) -0.010(3) 0.105(3) # GEOMETRY ############################################### #BOND DISTANCES# 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 C(1) C(2) 1.51(1) . . yes C(1) C(10) 1.546(8) . . yes C(1) H(11) 1.080(9) . . yes C(1) H(12) 1.080(8) . . yes C(2) C(3) 1.509(9) . . yes C(2) H(21) 1.080(9) . . yes C(2) H(22) 1.080(9) . . yes C(3) C(4) 1.519(9) . . yes C(3) O(25) 1.45(1) . . yes C(3) H(31) 1.080(9) . . yes C(4) C(5) 1.54(1) . . yes C(4) H(41) 1.080(8) . . yes C(4) H(42) 1.08(1) . . yes C(5) C(6) 1.531(9) . . yes C(5) C(10) 1.562(8) . . yes C(5) H(51) 1.080(8) . . yes C(6) C(7) 1.536(8) . . yes C(6) H(61) 1.08(1) . . yes C(6) H(62) 1.080(8) . . yes C(7) C(8) 1.534(7) . . yes C(7) H(71) 1.080(9) . . yes C(7) H(72) 1.08(1) . . yes C(8) C(9) 1.548(7) . . yes C(8) C(14) 1.517(7) . . yes C(8) H(81) 1.080(9) . . yes C(9) C(10) 1.552(7) . . yes C(9) C(11) 1.536(7) . . yes C(9) H(91) 1.080(8) . . yes C(10) C(19) 1.53(1) . . yes C(11) C(12) 1.529(7) . . yes C(11) H(111) 1.080(8) . . yes C(11) H(112) 1.080(9) . . yes C(12) C(13) 1.536(7) . . yes C(12) O(26) 1.427(8) . . yes C(12) H(121) 1.080(7) . . yes C(13) C(14) 1.547(7) . . yes C(13) C(17) 1.562(7) . . yes C(13) C(18) 1.538(9) . . yes C(14) C(15) 1.522(7) . . yes C(14) H(141) 1.080(8) . . yes C(15) C(16) 1.528(8) . . yes C(15) H(151) 1.08(1) . . yes C(15) H(152) 1.080(8) . . yes C(16) C(17) 1.554(9) . . yes C(16) H(161) 1.080(8) . . yes C(16) H(162) 1.08(1) . . yes C(17) C(20) 1.534(6) . . yes C(17) H(171) 1.080(9) . . yes C(18) H(181) 1.080(9) . . yes C(18) H(182) 1.080(8) . . yes C(18) H(183) 1.080(9) . . yes C(19) H(191) 1.080(8) . . yes C(19) H(192) 1.080(9) . . yes C(19) H(193) 1.080(9) . . yes C(20) C(21) 1.534(9) . . yes C(20) C(22) 1.529(9) . . yes C(20) H(201) 1.080(9) . . yes C(21) H(211) 1.080(8) . . yes C(21) H(212) 1.08(1) . . yes C(21) H(213) 1.08(1) . . yes C(22) C(23) 1.537(7) . . yes C(22) H(221) 1.080(9) . . yes C(22) H(222) 1.08(1) . . yes C(23) C(24) 1.49(1) . . yes C(23) H(231) 1.08(1) . . yes C(23) H(232) 1.080(9) . . yes C(24) O(27) 1.242(8) . . yes C(24) N(28) 1.332(9) . . yes N(28) C(29) 1.44(1) . . yes N(28) H(281) 1.000(8) . . yes C(29) C(30) 1.53(1) . . yes C(29) H(291) 1.08(1) . . yes C(29) H(292) 1.08(1) . . yes C(30) O(31) 1.170(7) . . yes C(30) O(32) 1.31(1) . . yes C(33) C(34) 1.48(1) . . yes C(33) C(35) 1.49(2) . . yes C(33) O(36) 1.20(1) . . yes C(34) H(341) 1.08(2) . . yes C(34) H(342) 1.08(1) . . yes C(34) H(343) 1.08(1) . . yes C(35) H(351) 1.08(1) . . yes C(35) H(352) 1.08(2) . . yes C(35) H(353) 1.08(1) . . yes #BOND ANGLES# 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 H(12) C(1) C(2) 108.3(8) . . . yes C(10) C(1) C(2) 114.0(5) . . . yes C(10) C(1) H(12) 108.4(5) . . . yes H(11) C(1) C(2) 108.2(6) . . . yes H(11) C(1) H(12) 109.5(7) . . . yes H(11) C(1) C(10) 108.3(7) . . . yes H(21) C(2) C(3) 109.0(5) . . . yes C(1) C(2) C(3) 111.1(6) . . . yes C(1) C(2) H(21) 109.1(7) . . . yes H(22) C(2) C(3) 109.2(7) . . . yes H(22) C(2) H(21) 109.5(9) . . . yes H(22) C(2) C(1) 109.0(6) . . . yes C(2) C(3) H(31) 107.0(7) . . . yes C(4) C(3) H(31) 108.0(7) . . . yes C(4) C(3) C(2) 112.0(4) . . . yes O(25) C(3) H(31) 108.9(5) . . . yes O(25) C(3) C(2) 110.8(6) . . . yes O(25) C(3) C(4) 110.0(6) . . . yes H(42) C(4) C(3) 108.7(8) . . . yes H(41) C(4) C(3) 108.5(5) . . . yes H(41) C(4) H(42) 109.5(8) . . . yes C(5) C(4) C(3) 112.7(5) . . . yes C(5) C(4) H(42) 108.9(6) . . . yes C(5) C(4) H(41) 108.5(8) . . . yes C(10) C(5) C(4) 112.2(6) . . . yes C(6) C(5) C(4) 111.3(5) . . . yes C(6) C(5) C(10) 111.5(4) . . . yes H(51) C(5) C(4) 107.2(5) . . . yes H(51) C(5) C(10) 106.9(6) . . . yes H(51) C(5) C(6) 107.3(7) . . . yes C(7) C(6) H(61) 108.1(5) . . . yes C(5) C(6) H(61) 108.6(6) . . . yes C(5) C(6) C(7) 112.8(6) . . . yes H(62) C(6) H(61) 109.5(8) . . . yes H(62) C(6) C(7) 109.0(6) . . . yes H(62) C(6) C(5) 108.8(5) . . . yes C(6) C(7) H(71) 109.0(7) . . . yes H(72) C(7) H(71) 109.5(7) . . . yes H(72) C(7) C(6) 108.1(5) . . . yes C(8) C(7) H(71) 109.2(5) . . . yes C(8) C(7) C(6) 112.7(5) . . . yes C(8) C(7) H(72) 108.1(7) . . . yes C(9) C(8) C(7) 110.0(4) . . . yes H(81) C(8) C(7) 107.5(6) . . . yes H(81) C(8) C(9) 110.3(5) . . . yes C(14) C(8) C(7) 111.4(5) . . . yes C(14) C(8) C(9) 109.3(5) . . . yes C(14) C(8) H(81) 108.2(4) . . . yes C(11) C(9) C(8) 111.9(3) . . . yes H(91) C(9) C(8) 107.1(5) . . . yes H(91) C(9) C(11) 105.9(6) . . . yes C(10) C(9) C(8) 112.1(5) . . . yes C(10) C(9) C(11) 114.0(4) . . . yes C(10) C(9) H(91) 105.0(4) . . . yes C(19) C(10) C(9) 111.7(4) . . . yes C(5) C(10) C(9) 108.2(5) . . . yes C(5) C(10) C(19) 110.0(5) . . . yes C(1) C(10) C(9) 112.9(5) . . . yes C(1) C(10) C(19) 106.5(5) . . . yes C(1) C(10) C(5) 107.5(4) . . . yes C(12) C(11) C(9) 113.3(4) . . . yes H(111) C(11) C(9) 108.6(4) . . . yes H(111) C(11) C(12) 108.7(6) . . . yes H(112) C(11) C(9) 108.3(6) . . . yes H(112) C(11) C(12) 108.4(4) . . . yes H(112) C(11) H(111) 109.5(6) . . . yes C(13) C(12) C(11) 110.3(5) . . . yes H(121) C(12) C(11) 107.3(5) . . . yes H(121) C(12) C(13) 110.2(4) . . . yes O(26) C(12) C(11) 110.8(4) . . . yes O(26) C(12) C(13) 108.4(4) . . . yes O(26) C(12) H(121) 109.8(7) . . . yes C(17) C(13) C(12) 116.3(5) . . . yes C(14) C(13) C(12) 107.5(3) . . . yes C(14) C(13) C(17) 100.2(4) . . . yes C(18) C(13) C(12) 109.9(5) . . . yes C(18) C(13) C(17) 110.3(4) . . . yes C(18) C(13) C(14) 112.4(5) . . . yes C(15) C(14) C(8) 119.6(5) . . . yes C(13) C(14) C(8) 114.9(4) . . . yes C(13) C(14) C(15) 103.6(3) . . . yes H(141) C(14) C(8) 95.7(4) . . . yes H(141) C(14) C(15) 109.6(5) . . . yes H(141) C(14) C(13) 113.6(6) . . . yes H(151) C(15) C(16) 111.0(5) . . . yes H(152) C(15) C(16) 110.5(6) . . . yes H(152) C(15) H(151) 109.5(8) . . . yes C(14) C(15) C(16) 104.4(5) . . . yes C(14) C(15) H(151) 111.0(6) . . . yes C(14) C(15) H(152) 110.4(5) . . . yes H(162) C(16) C(17) 110.0(7) . . . yes H(161) C(16) C(17) 109.8(5) . . . yes H(161) C(16) H(162) 109.5(6) . . . yes C(15) C(16) C(17) 107.5(4) . . . yes C(15) C(16) H(162) 110.2(5) . . . yes C(15) C(16) H(161) 109.7(7) . . . yes H(171) C(17) C(13) 108.7(4) . . . yes C(20) C(17) C(13) 119.3(5) . . . yes C(20) C(17) H(171) 97.4(6) . . . yes C(16) C(17) C(13) 102.6(5) . . . yes C(16) C(17) H(171) 117.1(6) . . . yes C(16) C(17) C(20) 112.5(4) . . . yes C(13) C(18) H(183) 109.4(5) . . . yes H(181) C(18) H(183) 109.5(8) . . . yes H(181) C(18) C(13) 109.6(6) . . . yes H(182) C(18) H(183) 109.5(7) . . . yes H(182) C(18) C(13) 109.3(7) . . . yes H(182) C(18) H(181) 109.5(6) . . . yes C(10) C(19) H(193) 109.2(7) . . . yes H(192) C(19) H(193) 109.5(6) . . . yes H(192) C(19) C(10) 109.6(7) . . . yes H(191) C(19) H(193) 109.5(8) . . . yes H(191) C(19) C(10) 109.6(6) . . . yes H(191) C(19) H(192) 109.5(8) . . . yes H(201) C(20) C(22) 110.9(5) . . . yes C(21) C(20) C(22) 109.0(6) . . . yes C(21) C(20) H(201) 107.4(6) . . . yes C(17) C(20) C(22) 109.9(5) . . . yes C(17) C(20) H(201) 105.8(6) . . . yes C(17) C(20) C(21) 113.9(4) . . . yes H(211) C(21) H(213) 109.5(8) . . . yes H(212) C(21) H(213) 109.5(8) . . . yes H(212) C(21) H(211) 109(1) . . . yes C(20) C(21) H(213) 109.4(9) . . . yes C(20) C(21) H(211) 109.3(6) . . . yes C(20) C(21) H(212) 109.7(7) . . . yes H(222) C(22) H(221) 109.5(8) . . . yes C(20) C(22) H(221) 108.7(6) . . . yes C(20) C(22) H(222) 108.4(6) . . . yes C(23) C(22) H(221) 108.5(6) . . . yes C(23) C(22) H(222) 108.7(6) . . . yes C(23) C(22) C(20) 113.0(6) . . . yes H(232) C(23) C(22) 109.0(5) . . . yes H(231) C(23) C(22) 109.1(7) . . . yes H(231) C(23) H(232) 109.5(8) . . . yes C(24) C(23) C(22) 111.4(5) . . . yes C(24) C(23) H(232) 108.8(7) . . . yes C(24) C(23) H(231) 109.0(6) . . . yes O(27) C(24) C(23) 122.0(6) . . . yes N(28) C(24) C(23) 118.5(6) . . . yes N(28) C(24) O(27) 119.6(7) . . . yes H(281) N(28) C(24) 120.2(8) . . . yes C(29) N(28) C(24) 119.7(6) . . . yes C(29) N(28) H(281) 120.2(7) . . . yes H(291) C(29) H(292) 109.5(7) . . . yes N(28) C(29) H(292) 109.3(8) . . . yes N(28) C(29) H(291) 108.8(9) . . . yes C(30) C(29) H(292) 109.0(9) . . . yes C(30) C(29) H(291) 108.6(7) . . . yes C(30) C(29) N(28) 111.7(5) . . . yes C(29) C(30) O(32) 110.0(5) . . . yes O(31) C(30) O(32) 124.9(7) . . . yes O(31) C(30) C(29) 125.1(8) . . . yes C(35) C(33) O(36) 121.2(7) . . . yes C(34) C(33) O(36) 120(1) . . . yes C(34) C(33) C(35) 118.1(8) . . . yes H(342) C(34) H(343) 109(1) . . . yes H(341) C(34) H(343) 109(1) . . . yes H(341) C(34) H(342) 109(1) . . . yes C(33) C(34) H(343) 109(1) . . . yes C(33) C(34) H(342) 110.1(9) . . . yes C(33) C(34) H(341) 108.6(9) . . . yes H(352) C(35) H(353) 109(1) . . . yes C(33) C(35) H(353) 109(1) . . . yes C(33) C(35) H(352) 109(1) . . . yes H(351) C(35) H(353) 109(1) . . . yes H(351) C(35) H(352) 109(1) . . . yes H(351) C(35) C(33) 110(1) . . . yes #===END# # MATERIAL RELEVANT TO HTDC ##### # data_HTDC _chemical_formula_sum 'H49C26N1O8S1' _chemical_formula_weight 535.7 _computing_structure_solution 'SIR92(Altomare al.,J.Appl.Cryst.,1994,27,435)' _computing_structure_refinement 'SIR-CAOS(Camalli al.,User Guide,1986)' _cell_length_a 9.965(1) _cell_length_b 8.132(1) _cell_length_c 17.301(2) _cell_angle_alpha 90.000 _cell_angle_beta 90.90(1) _cell_angle_gamma 90.000 _cell_volume 1401.8(4) _cell_formula_units_Z 2 _cell_measurement_radiation 'CuK\a' _cell_measurement_wavelength 1.54178 _cell_measurement_temperature 293 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,1/2+y,-z' _exptl_crystal_density_diffrn 1.27 _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.396 _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 69.50 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 98 'Hydrogen ' 0.0000 0.0000 ' Int. Tab.IV, 1974' 'c ' 52 'Carbon ' 0.0170 0.0090 ' Int. Tab.IV, 1974' 'n ' 2 'Nitrogen ' 0.0290 0.0180 ' Int. Tab.IV, 1974' 'o ' 16 'Oxygen ' 0.0470 0.0320 ' Int. Tab.IV, 1974' 's ' 2 'Sulphur ' 0.3190 0.5570 ' Int. Tab.IV, 1974' _reflns_number_total 2795 _reflns_number_observed 2581 _reflns_observed_criterion ' F >5.0 sigma(F) ' _reflns_limit_h_max 12 _reflns_limit_h_min 0 _reflns_limit_k_max 9 _reflns_limit_k_min 0 _reflns_limit_l_max 20 _reflns_limit_l_min -20 _reflns_d_resolution_high 0.825 _reflns_d_resolution_low 17.299 _refine_ls_structure_factor_coef F _refine_ls_extinction_method 'none' _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment ' H atoms rigid to parent C atom ' _refine_ls_weighting_scheme 'W=(Sin(Theta)/Lambda)^P(2)' _refine_ls_number_reflns 2581 _refine_ls_number_parameters 327 _refine_ls_R_factor_obs 0.066 _refine_ls_wR_factor_obs 0.083 _refine_diff_density_max 0.519 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.185 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type c(1) 0.8344(8) 1.033(1) 0.2654(4) 1.000 0.050(2) uani c(2) 0.6943(8) 1.041(1) 0.2983(4) 1.000 0.048(2) uani c(3) 0.6728(6) 0.892(1) 0.3487(3) 1.000 0.046(2) uani c(4) 0.6886(7) 0.7337(9) 0.3022(4) 1.000 0.042(2) uani c(5) 0.8286(6) 0.724(1) 0.2654(3) 1.000 0.042(2) uani c(6) 0.8458(8) 0.564(1) 0.2206(4) 1.000 0.051(2) uani c(7) 0.7671(8) 0.5657(9) 0.1423(4) 1.000 0.046(2) uani c(8) 0.8063(6) 0.7150(9) 0.0937(3) 1.000 0.036(2) uani c(9) 0.7834(5) 0.8756(8) 0.1392(3) 1.000 0.035(2) uani c(10) 0.8645(5) 0.8775(9) 0.2170(3) 1.000 0.040(2) uani c(11) 0.8128(8) 1.026(1) 0.0884(4) 1.000 0.046(2) uani c(12) 0.7358(7) 1.0278(9) 0.0102(4) 1.000 0.041(2) uani c(13) 0.7595(5) 0.8686(8) -0.0349(3) 1.000 0.033(2) uani c(14) 0.7248(6) 0.7215(8) 0.0180(3) 1.000 0.034(2) uani c(15) 0.7312(7) 0.5730(9) -0.0364(4) 1.000 0.045(2) uani c(16) 0.6793(7) 0.6420(9) -0.1156(3) 1.000 0.042(2) uani c(17) 0.6650(5) 0.8301(9) -0.1058(3) 1.000 0.034(1) uani c(18) 0.9071(5) 0.866(1) -0.0609(3) 1.000 0.046(2) uani c(19) 1.0174(6) 0.879(1) 0.2026(4) 1.000 0.062(3) uani c(20) 0.6873(6) 0.9266(9) -0.1815(3) 1.000 0.041(2) uani c(21) 0.6666(9) 1.113(1) -0.1725(5) 1.000 0.059(3) uani c(22) 0.5931(6) 0.860(1) -0.2459(3) 1.000 0.047(2) uani c(23) 0.6357(7) 0.909(1) -0.3283(4) 1.000 0.053(2) uani c(24) 0.7743(7) 0.847(1) -0.3456(3) 1.000 0.046(2) uani o(25) 0.5425(5) 0.9026(9) 0.3837(3) 1.000 0.059(2) uani o(26) 0.5971(6) 1.0543(9) 0.0243(3) 1.000 0.064(2) uani o(27) 0.8098(6) 0.7003(8) -0.3328(3) 1.000 0.059(2) uani n(28) 0.8625(8) 0.9497(9) -0.3744(4) 1.000 0.053(2) uani c(29) 0.9966(7) 0.904(1) -0.3970(4) 1.000 0.051(2) uani c(30) 1.0023(7) 0.8578(9) -0.4827(3) 1.000 0.045(2) uani s(31) 1.1703(2) 0.8284 -0.5115(1) 1.000 0.0443(4) uani o(32) 1.1599(6) 0.7879(7) -0.5949(2) 1.000 0.051(2) uani o(33) 1.2389(7) 0.9835(9) -0.4982(3) 1.000 0.067(2) uani o(34) 1.2227(6) 0.690(1) -0.4682(3) 1.000 0.069(2) uani o(1) 0.4735(8) 0.180(1) -0.4952(5) 1.000 0.098(3) uani o(2) 0.3177(5) 0.9513(7) 0.3154(3) 1.000 0.049(1) uani h(11) 0.8457(8) 1.138(1) 0.2279(4) 1.000 0.050 uiso h(12) 0.9067(8) 1.040(1) 0.3129(4) 1.000 0.050 uiso h(21) 0.6197(8) 1.043(1) 0.2525(4) 1.000 0.048 uiso h(22) 0.6847(8) 1.151(1) 0.3325(4) 1.000 0.048 uiso h(3) 0.7485(6) 0.889(1) 0.3941(3) 1.000 0.046 uiso h(41) 0.6128(7) 0.7319(9) 0.2570(4) 1.000 0.042 uiso h(42) 0.6758(7) 0.6289(9) 0.3400(4) 1.000 0.042 uiso h(5) 0.8999(6) 0.724(1) 0.3128(3) 1.000 0.042 uiso h(61) 0.8091(8) 0.463(1) 0.2551(4) 1.000 0.051 uiso h(62) 0.9511(8) 0.545(1) 0.2101(4) 1.000 0.051 uiso h(71) 0.6603(8) 0.5694(9) 0.1535(4) 1.000 0.046 uiso h(72) 0.7903(8) 0.4554(9) 0.1105(4) 1.000 0.046 uiso h(8) 0.9112(6) 0.7022(9) 0.0811(3) 1.000 0.036 uiso h(9) 0.6787(5) 0.8827(8) 0.1543(3) 1.000 0.035 uiso h(111) 0.9187(8) 1.028(1) 0.0772(4) 1.000 0.046 uiso h(112) 0.7847(8) 1.135(1) 0.1202(4) 1.000 0.046 uiso h(12) 0.7726(7) 1.1255(9) -0.0259(4) 1.000 0.041 uiso h(14) 0.6256(6) 0.7304(8) 0.0419(3) 1.000 0.034 uiso h(151) 0.6679(7) 0.4741(9) -0.0161(4) 1.000 0.045 uiso h(152) 0.8329(7) 0.5291(9) -0.0411(4) 1.000 0.045 uiso h(161) 0.5834(7) 0.5881(9) -0.1296(3) 1.000 0.042 uiso h(162) 0.7494(7) 0.6141(9) -0.1606(3) 1.000 0.042 uiso h(17) 0.5645(5) 0.8712(9) -0.0948(3) 1.000 0.034 uiso h(181) 0.9258(5) 0.754(1) -0.0931(3) 1.000 0.046 uiso h(182) 0.9728(5) 0.871(1) -0.0111(3) 1.000 0.046 uiso h(183) 0.9258(5) 0.971(1) -0.0971(3) 1.000 0.046 uiso h(191) 1.0426(6) 0.986(1) 0.1687(4) 1.000 0.062 uiso h(192) 1.0456(6) 0.769(1) 0.1717(4) 1.000 0.062 uiso h(193) 1.0706(6) 0.884(1) 0.2577(4) 1.000 0.062 uiso h(20) 0.7914(6) 0.9080(9) -0.1961(3) 1.000 0.041 uiso h(211) 0.6841(9) 1.172(1) -0.2275(5) 1.000 0.059 uiso h(212) 0.7351(9) 1.161(1) -0.1295(5) 1.000 0.059 uiso h(213) 0.5651(9) 1.137(1) -0.1555(5) 1.000 0.059 uiso h(221) 0.4942(6) 0.907(1) -0.2361(3) 1.000 0.047 uiso h(222) 0.5922(6) 0.727(1) -0.2421(3) 1.000 0.047 uiso h(231) 0.6334(7) 1.042(1) -0.3338(4) 1.000 0.053 uiso h(232) 0.5654(7) 0.856(1) -0.3688(4) 1.000 0.053 uiso h(28) 0.84(1) 1.01(2) -0.385(7) 1.000 0.053 uiso h(291) 1.0280(7) 0.800(1) -0.3630(4) 1.000 0.051 uiso h(292) 1.0640(7) 1.006(1) -0.3860(4) 1.000 0.051 uiso h(301) 0.9570(7) 0.9541(9) -0.5171(3) 1.000 0.045 uiso h(302) 0.9480(7) 0.7441(9) -0.4921(3) 1.000 0.045 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 c(1) 0.058(4) -0.013(3) -0.006(3) 0.055(4) -0.005(3) 0.038(3) c(2) 0.061(4) 0.006(3) -0.003(3) 0.050(4) -0.005(3) 0.034(3) c(3) 0.041(3) 0.009(3) 0.001(2) 0.063(4) -0.002(3) 0.034(3) c(4) 0.044(3) 0.000(3) 0.001(2) 0.049(4) 0.004(3) 0.033(3) c(5) 0.044(3) 0.006(3) -0.005(2) 0.052(4) 0.002(3) 0.030(3) c(6) 0.064(4) 0.021(3) -0.003(3) 0.053(4) 0.003(3) 0.035(3) c(7) 0.065(4) 0.003(3) -0.004(3) 0.041(3) 0.005(3) 0.032(3) c(8) 0.034(3) 0.006(2) -0.004(2) 0.043(3) 0.003(2) 0.030(3) c(9) 0.033(2) -0.001(2) -0.004(2) 0.044(3) 0.000(2) 0.028(2) c(10) 0.031(2) -0.005(3) -0.007(2) 0.058(4) 0.000(3) 0.032(2) c(11) 0.061(4) -0.010(3) -0.007(3) 0.046(4) 0.000(3) 0.032(3) c(12) 0.048(3) 0.005(3) -0.004(2) 0.041(3) 0.001(3) 0.034(3) c(13) 0.029(2) -0.000(2) -0.001(2) 0.041(3) 0.001(2) 0.028(2) c(14) 0.034(3) 0.001(2) -0.003(2) 0.040(3) 0.002(2) 0.027(3) c(15) 0.058(4) 0.005(3) -0.004(3) 0.039(3) -0.002(3) 0.036(3) c(16) 0.054(3) 0.001(3) -0.002(2) 0.041(3) -0.001(3) 0.031(3) c(17) 0.032(2) -0.001(3) -0.002(2) 0.044(3) 0.002(3) 0.026(2) c(18) 0.032(2) -0.003(3) 0.002(2) 0.067(5) 0.006(3) 0.040(3) c(19) 0.034(3) -0.007(4) -0.006(3) 0.100(7) 0.006(4) 0.052(3) c(20) 0.039(3) -0.003(3) -0.003(2) 0.052(4) 0.009(3) 0.031(3) c(21) 0.077(5) -0.006(4) -0.013(4) 0.050(4) 0.015(3) 0.049(4) c(22) 0.040(3) 0.001(3) -0.003(2) 0.070(5) 0.004(3) 0.030(2) c(23) 0.055(4) 0.011(4) -0.001(2) 0.074(5) 0.005(3) 0.031(3) c(24) 0.056(3) 0.008(3) 0.001(2) 0.050(4) -0.000(3) 0.032(3) o(25) 0.049(2) 0.017(3) 0.010(2) 0.085(4) 0.007(3) 0.045(2) o(26) 0.061(3) 0.034(3) -0.000(2) 0.080(4) -0.006(3) 0.053(3) o(27) 0.059(3) -0.000(2) 0.001(2) 0.048(3) 0.008(3) 0.068(3) n(28) 0.071(4) 0.010(3) 0.014(3) 0.048(4) 0.005(3) 0.040(3) c(29) 0.056(4) -0.000(3) 0.004(3) 0.059(4) -0.003(3) 0.037(3) c(30) 0.051(3) -0.001(3) -0.001(2) 0.047(4) -0.005(3) 0.036(3) s(31) 0.0483(7) -0.0035(7) 0.0002(5) 0.0498(8) -0.0005(7) 0.0349(6) o(32) 0.075(3) -0.001(2) 0.007(2) 0.051(3) -0.005(2) 0.029(2) o(33) 0.073(3) -0.035(3) 0.003(3) 0.073(4) -0.014(3) 0.055(3) o(34) 0.069(3) 0.024(3) 0.002(3) 0.086(5) 0.023(3) 0.053(3) o(1) 0.085(5) -0.026(4) 0.027(4) 0.113(7) -0.059(5) 0.098(5) o(2) 0.057(3) 0.002(2) -0.000(2) 0.051(3) -0.003(2) 0.040(2) # GEOMETRY ############################################### #BOND DISTANCES# 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 C(1) C(2) 1.52(1) . . yes C(1) C(10) 1.55(1) . . yes C(1) H(11) 1.08(1) . . yes C(1) H(12) 1.08(1) . . yes C(2) C(3) 1.51(1) . . yes C(2) H(21) 1.08(1) . . yes C(2) H(22) 1.07(1) . . yes C(3) C(4) 1.53(1) . . yes C(3) O(25) 1.445(8) . . yes C(3) H(3) 1.080(9) . . yes C(4) C(5) 1.544(9) . . yes C(4) H(41) 1.078(9) . . yes C(4) H(42) 1.08(1) . . yes C(5) C(6) 1.53(1) . . yes C(5) C(10) 1.55(1) . . yes C(5) H(5) 1.076(9) . . yes C(6) C(7) 1.55(1) . . yes C(6) H(61) 1.08(1) . . yes C(6) H(62) 1.08(1) . . yes C(7) C(8) 1.53(1) . . yes C(7) H(71) 1.09(1) . . yes C(7) H(72) 1.08(1) . . yes C(8) C(9) 1.543(9) . . yes C(8) C(14) 1.532(8) . . yes C(8) H(8) 1.076(8) . . yes C(9) C(10) 1.560(8) . . yes C(9) C(11) 1.54(1) . . yes C(9) H(9) 1.081(7) . . yes C(10) C(19) 1.548(8) . . yes C(11) C(12) 1.545(9) . . yes C(11) H(111) 1.08(1) . . yes C(11) H(112) 1.09(1) . . yes C(12) C(13) 1.532(9) . . yes C(12) O(26) 1.423(9) . . yes C(12) H(12) 1.08(1) . . yes C(13) C(14) 1.549(8) . . yes C(13) C(17) 1.566(7) . . yes C(13) C(18) 1.544(7) . . yes C(14) C(15) 1.533(9) . . yes C(14) H(14) 1.080(8) . . yes C(15) C(16) 1.562(9) . . yes C(15) H(151) 1.08(1) . . yes C(15) H(152) 1.08(1) . . yes C(16) C(17) 1.55(1) . . yes C(16) H(161) 1.08(1) . . yes C(16) H(162) 1.079(9) . . yes C(17) C(20) 1.546(8) . . yes C(17) H(17) 1.076(7) . . yes C(18) H(181) 1.09(1) . . yes C(18) H(182) 1.074(8) . . yes C(18) H(183) 1.08(1) . . yes C(19) H(191) 1.08(1) . . yes C(19) H(192) 1.08(1) . . yes C(19) H(193) 1.09(1) . . yes C(20) C(21) 1.54(1) . . yes C(20) C(22) 1.544(9) . . yes C(20) H(20) 1.082(9) . . yes C(21) H(211) 1.08(1) . . yes C(21) H(212) 1.07(1) . . yes C(21) H(213) 1.08(1) . . yes C(22) C(23) 1.548(9) . . yes C(22) H(221) 1.074(9) . . yes C(22) H(222) 1.08(1) . . yes C(23) C(24) 1.51(1) . . yes C(23) H(231) 1.08(1) . . yes C(23) H(232) 1.07(1) . . yes C(24) O(27) 1.26(1) . . yes C(24) N(28) 1.32(1) . . yes N(28) C(29) 1.45(1) . . yes N(28) H(28) 0.6(1) . . yes C(29) C(30) 1.532(9) . . yes C(29) H(291) 1.08(1) . . yes C(29) H(292) 1.08(1) . . yes C(30) S(31) 1.771(7) . . yes C(30) H(301) 1.08(1) . . yes C(30) H(302) 1.08(1) . . yes S(31) O(32) 1.482(5) . . yes S(31) O(33) 1.451(7) . . yes S(31) O(34) 1.448(7) . . yes #BOND ANGLES# 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(10) C(1) C(2) 115.2(6) . . . yes H(11) C(1) C(2) 107.2(8) . . . yes H(11) C(1) C(10) 107.4(7) . . . yes H(12) C(1) C(2) 108.5(7) . . . yes H(12) C(1) C(10) 108.8(8) . . . yes H(12) C(1) H(11) 109.7(9) . . . yes H(22) C(2) C(1) 109.4(8) . . . yes C(3) C(2) C(1) 108.8(6) . . . yes C(3) C(2) H(22) 109.4(7) . . . yes H(21) C(2) C(1) 110.6(7) . . . yes H(21) C(2) H(22) 109.1(9) . . . yes H(21) C(2) C(3) 109.4(8) . . . yes O(25) C(3) C(4) 111.7(6) . . . yes C(2) C(3) C(4) 110.8(5) . . . yes C(2) C(3) O(25) 109.5(6) . . . yes H(3) C(3) C(4) 106.7(7) . . . yes H(3) C(3) O(25) 108.5(6) . . . yes H(3) C(3) C(2) 109.5(8) . . . yes C(3) C(4) C(5) 111.1(6) . . . yes H(41) C(4) C(5) 109.2(6) . . . yes H(41) C(4) C(3) 108.4(7) . . . yes H(42) C(4) C(5) 108.9(7) . . . yes H(42) C(4) C(3) 109.3(6) . . . yes H(42) C(4) H(41) 109.8(8) . . . yes C(10) C(5) C(4) 113.5(6) . . . yes C(6) C(5) C(4) 111.2(6) . . . yes C(6) C(5) C(10) 112.6(5) . . . yes H(5) C(5) C(4) 106.0(6) . . . yes H(5) C(5) C(10) 104.8(7) . . . yes H(5) C(5) C(6) 108.1(7) . . . yes H(62) C(6) C(7) 109.5(7) . . . yes C(5) C(6) C(7) 111.9(6) . . . yes C(5) C(6) H(62) 108.8(8) . . . yes H(61) C(6) C(7) 108.6(8) . . . yes H(61) C(6) H(62) 109.2(9) . . . yes H(61) C(6) C(5) 108.9(7) . . . yes C(6) C(7) H(72) 109.1(7) . . . yes C(8) C(7) H(72) 108.7(6) . . . yes C(8) C(7) C(6) 111.0(6) . . . yes H(71) C(7) H(72) 109.4(8) . . . yes H(71) C(7) C(6) 109.2(6) . . . yes H(71) C(7) C(8) 109.6(7) . . . yes H(8) C(8) C(14) 109.5(6) . . . yes C(7) C(8) C(14) 111.1(5) . . . yes C(7) C(8) H(8) 107.0(7) . . . yes C(9) C(8) C(14) 109.0(5) . . . yes C(9) C(8) H(8) 109.7(6) . . . yes C(9) C(8) C(7) 110.5(5) . . . yes C(11) C(9) C(8) 110.5(5) . . . yes H(9) C(9) C(8) 108.6(6) . . . yes H(9) C(9) C(11) 106.8(6) . . . yes C(10) C(9) C(8) 111.7(5) . . . yes C(10) C(9) C(11) 112.7(5) . . . yes C(10) C(9) H(9) 106.2(5) . . . yes C(1) C(10) C(9) 111.9(5) . . . yes C(5) C(10) C(9) 109.8(5) . . . yes C(5) C(10) C(1) 108.5(5) . . . yes C(19) C(10) C(9) 111.0(5) . . . yes C(19) C(10) C(1) 106.3(6) . . . yes C(19) C(10) C(5) 109.2(6) . . . yes H(111) C(11) C(12) 108.5(7) . . . yes C(9) C(11) C(12) 114.4(6) . . . yes C(9) C(11) H(111) 108.3(7) . . . yes H(112) C(11) C(12) 107.9(7) . . . yes H(112) C(11) H(111) 109.8(9) . . . yes H(112) C(11) C(9) 107.9(7) . . . yes O(26) C(12) C(13) 112.0(6) . . . yes C(11) C(12) C(13) 111.0(6) . . . yes C(11) C(12) O(26) 108.8(5) . . . yes H(12) C(12) C(13) 105.7(6) . . . yes H(12) C(12) O(26) 109.1(7) . . . yes H(12) C(12) C(11) 110.3(7) . . . yes C(14) C(13) C(12) 108.3(4) . . . yes C(18) C(13) C(12) 108.4(5) . . . yes C(18) C(13) C(14) 112.6(5) . . . yes C(17) C(13) C(12) 118.1(5) . . . yes C(17) C(13) C(14) 99.8(5) . . . yes C(17) C(13) C(18) 109.4(4) . . . yes C(8) C(14) H(14) 98.7(5) . . . yes C(15) C(14) H(14) 109.6(6) . . . yes C(15) C(14) C(8) 118.1(6) . . . yes C(13) C(14) H(14) 112.9(6) . . . yes C(13) C(14) C(8) 114.3(5) . . . yes C(13) C(14) C(15) 103.6(5) . . . yes H(152) C(15) H(151) 109.4(8) . . . yes C(14) C(15) H(151) 110.9(7) . . . yes C(14) C(15) H(152) 110.8(7) . . . yes C(16) C(15) H(151) 111.3(7) . . . yes C(16) C(15) H(152) 110.5(7) . . . yes C(16) C(15) C(14) 103.8(5) . . . yes H(162) C(16) C(17) 110.5(7) . . . yes C(15) C(16) C(17) 106.8(5) . . . yes C(15) C(16) H(162) 110.4(7) . . . yes H(161) C(16) C(17) 110.2(7) . . . yes H(161) C(16) H(162) 109.5(7) . . . yes H(161) C(16) C(15) 109.4(7) . . . yes C(20) C(17) H(17) 97.9(6) . . . yes C(16) C(17) H(17) 114.5(7) . . . yes C(16) C(17) C(20) 113.2(5) . . . yes C(13) C(17) H(17) 110.5(5) . . . yes C(13) C(17) C(20) 118.0(5) . . . yes C(13) C(17) C(16) 103.2(5) . . . yes H(181) C(18) H(183) 109.5(7) . . . yes C(13) C(18) H(183) 109.4(6) . . . yes C(13) C(18) H(181) 109.4(6) . . . yes H(182) C(18) H(183) 109.1(8) . . . yes H(182) C(18) H(181) 109.6(8) . . . yes H(182) C(18) C(13) 109.7(6) . . . yes H(193) C(19) H(191) 109(1) . . . yes C(10) C(19) H(191) 109.3(8) . . . yes C(10) C(19) H(193) 109.0(6) . . . yes H(192) C(19) H(191) 109.6(9) . . . yes H(192) C(19) H(193) 109(1) . . . yes H(192) C(19) C(10) 109.8(8) . . . yes H(20) C(20) C(22) 110.9(6) . . . yes C(17) C(20) C(22) 109.8(5) . . . yes C(17) C(20) H(20) 106.2(6) . . . yes C(21) C(20) C(22) 109.8(6) . . . yes C(21) C(20) H(20) 107.0(7) . . . yes C(21) C(20) C(17) 113.1(5) . . . yes C(20) C(21) H(212) 110.1(8) . . . yes H(213) C(21) H(212) 109(1) . . . yes H(213) C(21) C(20) 109.6(8) . . . yes H(211) C(21) H(212) 109(1) . . . yes H(211) C(21) C(20) 108.9(8) . . . yes H(211) C(21) H(213) 108(1) . . . yes C(23) C(22) H(221) 108.5(6) . . . yes H(222) C(22) H(221) 109.7(8) . . . yes H(222) C(22) C(23) 108.6(7) . . . yes C(20) C(22) H(221) 108.1(6) . . . yes C(20) C(22) C(23) 113.6(6) . . . yes C(20) C(22) H(222) 108.3(6) . . . yes C(24) C(23) H(231) 109.6(8) . . . yes H(232) C(23) H(231) 109.5(9) . . . yes H(232) C(23) C(24) 109.0(8) . . . yes C(22) C(23) H(231) 109.5(7) . . . yes C(22) C(23) C(24) 111.2(6) . . . yes C(22) C(23) H(232) 108.0(7) . . . yes O(27) C(24) N(28) 118.6(7) . . . yes C(23) C(24) N(28) 118.9(7) . . . yes C(23) C(24) O(27) 122.5(7) . . . yes C(24) N(28) H(28) 114(12) . . . yes C(29) N(28) H(28) 119(11) . . . yes C(29) N(28) C(24) 124.5(7) . . . yes C(30) C(29) H(291) 108.7(8) . . . yes H(292) C(29) H(291) 109.4(8) . . . yes H(292) C(29) C(30) 109.1(7) . . . yes N(28) C(29) H(291) 108.4(7) . . . yes N(28) C(29) C(30) 112.0(6) . . . yes N(28) C(29) H(292) 109.3(8) . . . yes H(302) C(30) C(29) 109.3(6) . . . yes S(31) C(30) C(29) 110.8(5) . . . yes S(31) C(30) H(302) 108.4(6) . . . yes H(301) C(30) C(29) 109.4(7) . . . yes H(301) C(30) H(302) 109.4(7) . . . yes H(301) C(30) S(31) 109.4(6) . . . yes O(34) S(31) O(32) 110.5(3) . . . yes O(33) S(31) O(32) 111.9(3) . . . yes O(33) S(31) O(34) 115.5(4) . . . yes C(30) S(31) O(32) 104.6(3) . . . yes C(30) S(31) O(34) 107.1(3) . . . yes C(30) S(31) O(33) 106.4(4) . . . yes #===END# #MATERIAL RELEVANT TO HTUDC# data_HTUDC _chemical_formula_sum 'H49C26N1O8S1' _chemical_formula_weight 535.74 _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _computing_structure_refinement 'SIR-CAOS(Camalli al.,User Guide,1986)' _cell_length_a 9.659(3) _cell_length_b 8.334(2) _cell_length_c 17.308(5) _cell_angle_alpha 90.000 _cell_angle_beta 91.18(2) _cell_angle_gamma 90.000 _cell_volume 1393.0(6) _cell_formula_units_Z 2 _cell_measurement_radiation 'MoK\a' _cell_measurement_wavelength 0.71069 _cell_measurement_temperature 293 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,1/2+y,-z' _exptl_crystal_density_diffrn 1.278 _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.167 _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'h ' 98 'Hydrogen ' 0.0000 0.0000 ' Int. Tab. IV,1974 ' 'c ' 52 'Carbon ' 0.0020 0.0020 ' Int. Tab. IV,1974 ' 'n ' 2 'Nitrogen ' 0.0040 0.0030 ' Int. Tab. IV,1974 ' 'o ' 16 'Oxygen ' 0.0080 0.0060 ' Int. Tab. IV,1974 ' 's ' 2 'Sulphur ' 0.1100 0.1240 ' Int. Tab. IV,1974 ' _reflns_number_total 5377 _reflns_number_observed 2773 _reflns_observed_criterion ' F >8.0 sigma(F)' _reflns_limit_h_max 14 _reflns_limit_h_min 0 _reflns_limit_k_max 12 _reflns_limit_k_min 0 _reflns_limit_l_max 26 _reflns_limit_l_min -26 _refine_ls_structure_factor_coef F _refine_ls_extinction_method 'none' _refine_ls_matrix_type Full _refine_ls_hydrogen_treatment 'H atoms refined independently' _refine_ls_weighting_scheme 'W=(Sin(Theta)/Lambda)^P(2)' _refine_ls_number_reflns 2773 _refine_ls_number_parameters 324 _refine_ls_R_factor_obs 0.036 _refine_ls_wR_factor_obs 0.046 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type S(31) 1.1708(1) 0.8258(3) -0.51251(4) 1.000 0.0356(2) uani C(1) 0.8378(4) 1.0318(5) 0.2614(2) 1.000 0.039(1) uani C(2) 0.6969(4) 1.0410(5) 0.2982(2) 1.000 0.040(1) uani C(3) 0.6787(3) 0.8990(5) 0.3516(2) 1.000 0.037(1) uani C(4) 0.6914(3) 0.7425(5) 0.3073(2) 1.000 0.035(1) uani C(5) 0.8309(3) 0.7294(5) 0.2661(2) 1.000 0.034(1) uani C(6) 0.8406(4) 0.5725(5) 0.2218(2) 1.000 0.039(1) uani C(7) 0.7540(4) 0.5711(4) 0.1470(2) 1.000 0.034(1) uani C(8) 0.7903(3) 0.7092(4) 0.0936(2) 1.000 0.028(1) uani C(9) 0.7708(3) 0.8691(4) 0.1388(2) 1.000 0.028(1) uani C(10) 0.8629(3) 0.8758(5) 0.2143(2) 1.000 0.033(1) uani C(11) 0.7884(5) 1.0176(5) 0.0890(2) 1.000 0.043(1) uani C(12) 0.7076(4) 1.0116(5) 0.0110(2) 1.000 0.038(1) uani C(13) 0.7408(3) 0.8606(4) -0.0341(2) 1.000 0.028(1) uani C(14) 0.7050(3) 0.7161(4) 0.0183(2) 1.000 0.027(1) uani C(15) 0.7090(4) 0.5719(5) -0.0373(2) 1.000 0.040(1) uani C(16) 0.6551(4) 0.6400(5) -0.1153(2) 1.000 0.040(1) uani C(17) 0.6466(3) 0.8259(5) -0.1062(2) 1.000 0.030(1) uani C(18) 0.8940(3) 0.8580(6) -0.0578(2) 1.000 0.043(1) uani C(19) 1.0185(3) 0.8752(7) 0.1943(2) 1.000 0.052(1) uani C(20) 0.6775(3) 0.9145(5) -0.1823(2) 1.000 0.035(1) uani C(21) 0.6699(5) 1.0974(6) -0.1747(2) 1.000 0.052(1) uani C(22) 0.5804(3) 0.8562(5) -0.2477(2) 1.000 0.039(1) uani C(23) 0.6252(4) 0.9077(6) -0.3290(2) 1.000 0.044(1) uani C(24) 0.7677(3) 0.8465(5) -0.3465(2) 1.000 0.038(1) uani O(25) 0.5472(3) 0.9118(4) 0.3885(1) 1.000 0.048(1) uani O(26) 0.7680(4) 0.4153(4) 0.1120(2) 1.000 0.051(1) uani O(27) 0.8048(3) 0.7048(4) -0.3350(2) 1.000 0.051(1) uani N(28) 0.8566(3) 0.9507(4) -0.3746(2) 1.000 0.043(1) uani C(29) 0.9957(4) 0.9064(5) -0.3974(2) 1.000 0.042(1) uani C(30) 0.9985(3) 0.8576(5) -0.4826(2) 1.000 0.036(1) uani O(32) 1.1576(3) 0.7874(4) -0.5956(1) 1.000 0.044(1) uani O(33) 1.2435(3) 0.9749(5) -0.4996(2) 1.000 0.059(1) uani O(34) 1.2237(4) 0.6889(5) -0.4695(2) 1.000 0.060(1) uani O(1) 1.5298(4) 0.6865(6) -0.5046(3) 1.000 0.089(2) uani O(2) 1.3204(3) 0.9537(4) -0.6829(1) 1.000 0.041(1) uani H(11) 1.4736(4) 0.6732(6) -0.4863(3) 1.000 0.035 uiso H(12) 1.5448(4) 0.6025(6) -0.5174(3) 1.000 0.035 uiso H(21) 1.4028(3) 0.9510(4) -0.6552(1) 1.000 0.035 uiso H(22) 1.2606(3) 0.9010(4) -0.6543(1) 1.000 0.035 uiso H(23) 1.2884(3) 1.0503(4) -0.6787(1) 1.000 0.035 uiso H(37) 0.8921(3) 0.6936(4) 0.0802(2) 1.000 0.035 uiso H(38) 0.6015(3) 0.7278(4) 0.0306(2) 1.000 0.035 uiso H(39) 0.6680(3) 0.8622(4) 0.1549(2) 1.000 0.035 uiso H(40) 0.8984(3) 0.7329(5) 0.3092(2) 1.000 0.035 uiso H(43) 0.7481(3) 0.9075(5) 0.3945(2) 1.000 0.035 uiso H(46) 1.0459(3) 0.7871(7) 0.1573(2) 1.000 0.035 uiso H(47) 0.8060(4) 0.5354(5) -0.0409(2) 1.000 0.035 uiso H(49) 0.6224(4) 1.0364(5) 0.2614(2) 1.000 0.035 uiso H(51) 0.6139(3) 0.7355(5) 0.2681(2) 1.000 0.035 uiso H(52) 0.9566(3) 0.9398(5) -0.5158(2) 1.000 0.035 uiso H(53) 1.0290(4) 0.8164(5) -0.3659(2) 1.000 0.035 uiso H(54) 0.6881(4) 1.1363(5) 0.3276(2) 1.000 0.035 uiso H(55) 0.6540(4) 0.5789(4) 0.1578(2) 1.000 0.035 uiso H(57) 0.9504(3) 0.7561(5) -0.4951(2) 1.000 0.035 uiso H(58) 0.9163(3) 0.7613(6) -0.0925(2) 1.000 0.035 uiso H(59) 0.9106(4) 1.0333(5) 0.3006(2) 1.000 0.035 uiso H(60) 0.7336(5) 1.1412(6) -0.1405(2) 1.000 0.035 uiso H(61) 0.6850(3) 0.6510(5) 0.3367(2) 1.000 0.035 uiso H(62) 0.5757(3) 0.7357(5) -0.2444(2) 1.000 0.035 uiso H(63) 0.8338(3) 1.0499(4) -0.3905(2) 1.000 0.035 uiso H(64) 0.8519(4) 1.1226(5) 0.2295(2) 1.000 0.035 uiso H(65) 0.8201(4) 0.4851(5) 0.2498(2) 1.000 0.035 uiso H(66) 0.5606(4) 0.8636(6) -0.3645(2) 1.000 0.035 uiso H(68) 0.9559(3) 0.8553(6) -0.0161(2) 1.000 0.035 uiso H(69) 0.5669(4) 0.5906(5) -0.1208(2) 1.000 0.035 uiso H(70) 0.4908(3) 0.8987(5) -0.2389(2) 1.000 0.035 uiso H(71) 0.7239(4) 1.1151(5) -0.0154(2) 1.000 0.035 uiso H(73) 0.8919(5) 1.0351(5) 0.0776(2) 1.000 0.035 uiso H(74) 0.6175(4) 1.0332(6) -0.3365(2) 1.000 0.035 uiso H(75) 0.6655(4) 0.4824(5) -0.0164(2) 1.000 0.035 uiso H(76) 1.0553(4) 1.0064(5) -0.3920(2) 1.000 0.035 uiso H(77) 0.9143(3) 0.9537(6) -0.0850(2) 1.000 0.035 uiso H(78) 0.6059(4) 1.0286(5) 0.0211(2) 1.000 0.035 uiso H(79) 0.5421(3) 0.8417(4) 0.4208(1) 1.000 0.035 uiso H(80) 0.5786(5) 1.1315(6) -0.1519(2) 1.000 0.035 uiso H(81) 0.7685(3) 0.8902(5) -0.1976(2) 1.000 0.035 uiso H(82) 0.7090(4) 0.6106(5) -0.1548(2) 1.000 0.035 uiso H(83) 0.7649(5) 1.1125(5) 0.1155(2) 1.000 0.035 uiso H(84) 0.6637(5) 1.1419(6) -0.2185(2) 1.000 0.035 uiso H(87) 1.0696(3) 0.8650(7) 0.2337(2) 1.000 0.035 uiso H(88) 1.0486(3) 0.9714(7) 0.1643(2) 1.000 0.035 uiso H(89) 0.8430(4) 0.4035(4) 0.0976(2) 1.000 0.035 uiso H(90) 0.5502(3) 0.8550(5) -0.0933(2) 1.000 0.035 uiso H(91) 0.9370(4) 0.5598(5) 0.2080(2) 1.000 0.035 uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 S(31) 0.0337(3) -0.0032(4) 0.0027(3) 0.0400(4) 0.0010(3) 0.0331(3) C(1) 0.046(2) -0.010(1) -0.006(1) 0.038(2) -0.006(1) 0.033(2) C(2) 0.053(2) 0.004(1) -0.004(1) 0.034(2) -0.004(1) 0.032(1) C(3) 0.034(1) 0.006(1) -0.000(1) 0.050(2) -0.001(1) 0.027(1) C(4) 0.036(2) 0.000(1) 0.002(1) 0.038(2) 0.001(1) 0.031(1) C(5) 0.032(1) 0.006(1) -0.003(1) 0.040(2) 0.004(1) 0.030(1) C(6) 0.044(2) 0.014(1) 0.003(1) 0.038(2) 0.006(1) 0.036(2) C(7) 0.041(2) 0.007(1) 0.004(1) 0.025(1) 0.000(1) 0.034(1) C(8) 0.026(1) 0.003(1) 0.005(1) 0.026(1) -0.001(1) 0.031(1) C(9) 0.031(1) 0.001(1) -0.0005(9) 0.025(1) -0.001(1) 0.027(1) C(10) 0.028(1) -0.003(1) -0.000(1) 0.039(2) -0.001(1) 0.033(1) C(11) 0.070(3) -0.007(2) -0.006(2) 0.025(2) 0.001(1) 0.033(2) C(12) 0.055(2) 0.003(1) -0.006(1) 0.027(2) 0.002(1) 0.032(2) C(13) 0.027(1) -0.002(1) 0.0007(9) 0.028(2) 0.002(1) 0.027(1) C(14) 0.029(1) 0.001(1) 0.006(1) 0.025(1) -0.001(1) 0.028(1) C(15) 0.051(2) 0.000(1) 0.003(1) 0.031(2) -0.004(1) 0.037(2) C(16) 0.052(2) -0.006(2) -0.000(1) 0.036(2) -0.004(1) 0.032(2) C(17) 0.026(1) -0.003(1) 0.0031(8) 0.037(1) 0.001(1) 0.027(1) C(18) 0.026(1) -0.007(2) 0.005(1) 0.060(3) 0.009(2) 0.042(1) C(19) 0.027(1) -0.007(2) -0.000(1) 0.079(3) 0.003(2) 0.051(2) C(20) 0.031(1) -0.004(1) 0.004(1) 0.046(2) 0.006(1) 0.029(1) C(21) 0.063(2) -0.013(2) -0.012(2) 0.052(2) 0.013(2) 0.041(2) C(22) 0.033(1) -0.002(2) 0.002(1) 0.056(2) 0.000(1) 0.028(1) C(23) 0.043(2) 0.007(2) 0.000(1) 0.059(2) 0.001(2) 0.031(1) C(24) 0.044(1) 0.002(2) 0.004(1) 0.042(2) 0.000(1) 0.027(1) O(25) 0.041(1) 0.014(1) 0.0089(9) 0.066(2) 0.004(1) 0.038(1) O(26) 0.076(2) 0.005(1) 0.004(1) 0.028(1) -0.003(1) 0.050(1) O(27) 0.048(1) -0.002(1) 0.008(1) 0.037(1) 0.003(1) 0.069(2) N(28) 0.053(2) 0.005(1) 0.015(1) 0.036(2) 0.004(1) 0.039(1) C(29) 0.046(2) -0.003(2) 0.006(1) 0.047(2) -0.004(1) 0.033(1) C(30) 0.034(1) -0.000(1) 0.003(1) 0.039(2) -0.004(1) 0.034(1) O(32) 0.050(1) -0.005(1) 0.007(1) 0.045(2) -0.003(1) 0.037(1) O(33) 0.054(2) -0.027(2) 0.007(1) 0.072(2) -0.015(2) 0.053(2) O(34) 0.057(2) 0.018(2) 0.006(1) 0.072(2) 0.017(2) 0.051(2) O(1) 0.068(2) 0.031(2) 0.041(2) 0.096(3) 0.058(3) 0.105(3) O(2) 0.045(1) 0.002(1) 0.005(1) 0.042(1) -0.002(1) 0.036(1) # GEOMETRY ############################################### #BOND DISTANCES# 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(31) C(30) 1.773(3) . . yes S(31) O(32) 1.477(3) . . yes S(31) O(33) 1.443(5) . . yes S(31) O(34) 1.450(5) . . yes C(1) C(2) 1.517(5) . . yes C(1) C(10) 1.556(5) . . yes C(1) H(59) 0.968(5) . . yes C(1) H(64) 0.947(6) . . yes C(2) C(3) 1.514(5) . . yes C(2) H(49) 0.952(5) . . yes C(2) H(54) 0.947(5) . . yes C(3) C(4) 1.519(5) . . yes C(3) O(25) 1.437(4) . . yes C(3) H(43) 0.992(4) . . yes C(4) C(5) 1.541(5) . . yes C(4) H(51) 1.002(5) . . yes C(4) H(61) 0.919(5) . . yes C(5) C(6) 1.520(6) . . yes C(5) C(10) 1.549(5) . . yes C(5) H(40) 0.981(5) . . yes C(6) C(7) 1.527(5) . . yes C(6) H(65) 0.899(6) . . yes C(6) H(91) 0.971(5) . . yes C(7) C(8) 1.522(5) . . yes C(7) O(26) 1.440(5) . . yes C(7) H(55) 0.989(5) . . yes C(8) C(9) 1.558(5) . . yes C(8) C(14) 1.529(4) . . yes C(8) H(37) 1.023(4) . . yes C(9) C(10) 1.566(4) . . yes C(9) C(11) 1.520(5) . . yes C(9) H(39) 1.039(4) . . yes C(10) C(19) 1.549(4) . . yes C(11) C(12) 1.546(6) . . yes C(11) H(73) 1.033(7) . . yes C(11) H(83) 0.944(6) . . yes C(12) C(13) 1.519(5) . . yes C(12) H(71) 0.990(5) . . yes C(12) H(78) 1.011(6) . . yes C(13) C(14) 1.552(4) . . yes C(13) C(17) 1.555(4) . . yes C(13) C(18) 1.544(4) . . yes C(14) C(15) 1.541(5) . . yes C(14) H(38) 1.030(4) . . yes C(15) C(16) 1.545(5) . . yes C(15) H(47) 0.988(6) . . yes C(15) H(75) 0.933(5) . . yes C(16) C(17) 1.560(6) . . yes C(16) H(69) 0.949(6) . . yes C(16) H(82) 0.902(5) . . yes C(17) C(20) 1.545(4) . . yes C(17) H(90) 0.992(4) . . yes C(18) H(58) 1.031(6) . . yes C(18) H(68) 0.927(5) . . yes C(18) H(77) 0.949(6) . . yes C(19) H(46) 1.013(7) . . yes C(19) H(87) 0.838(5) . . yes C(19) H(88) 1.003(7) . . yes C(20) C(21) 1.532(6) . . yes C(20) C(22) 1.534(5) . . yes C(20) H(81) 0.945(5) . . yes C(21) H(60) 0.921(7) . . yes C(21) H(80) 1.014(7) . . yes C(21) H(84) 0.846(6) . . yes C(22) C(23) 1.542(5) . . yes C(22) H(62) 1.007(6) . . yes C(22) H(70) 0.950(5) . . yes C(23) C(24) 1.504(5) . . yes C(23) H(66) 0.942(5) . . yes C(23) H(74) 1.056(7) . . yes C(24) O(27) 1.249(5) . . yes C(24) N(28) 1.321(5) . . yes O(25) H(79) 0.810(5) . . yes O(26) H(89) 0.777(5) . . yes N(28) C(29) 1.456(5) . . yes N(28) H(63) 0.898(5) . . yes C(29) C(30) 1.532(5) . . yes C(29) H(53) 0.978(6) . . yes C(29) H(76) 1.016(6) . . yes C(30) H(52) 0.976(5) . . yes C(30) H(57) 0.986(5) . . yes O(1) H(11) 0.644(6) . . yes O(1) H(12) 0.750(7) . . yes O(2) H(21) 0.921(4) . . yes O(2) H(22) 0.884(4) . . yes O(2) H(23) 0.866(4) . . yes #BOND ANGLES# 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(34) S(31) C(30) 106.9(2) . . . yes O(32) S(31) C(30) 104.7(2) . . . yes O(32) S(31) O(34) 110.7(2) . . . yes O(33) S(31) C(30) 106.4(2) . . . yes O(33) S(31) O(34) 115.7(2) . . . yes O(33) S(31) O(32) 111.7(2) . . . yes C(10) C(1) C(2) 114.4(3) . . . yes H(59) C(1) C(2) 110.5(4) . . . yes H(59) C(1) C(10) 105.0(4) . . . yes H(64) C(1) C(2) 110.2(4) . . . yes H(64) C(1) C(10) 109.6(4) . . . yes H(64) C(1) H(59) 106.7(5) . . . yes H(49) C(2) C(3) 106.3(4) . . . yes H(54) C(2) C(3) 108.4(4) . . . yes H(54) C(2) H(49) 108.5(5) . . . yes C(1) C(2) C(3) 109.5(3) . . . yes C(1) C(2) H(49) 112.9(4) . . . yes C(1) C(2) H(54) 111.0(4) . . . yes O(25) C(3) C(4) 111.7(3) . . . yes C(2) C(3) C(4) 110.6(3) . . . yes C(2) C(3) O(25) 109.2(3) . . . yes H(43) C(3) C(4) 112.2(4) . . . yes H(43) C(3) O(25) 104.6(3) . . . yes H(43) C(3) C(2) 108.4(4) . . . yes C(5) C(4) H(61) 105.5(4) . . . yes C(3) C(4) H(61) 115.2(4) . . . yes C(3) C(4) C(5) 112.0(3) . . . yes H(51) C(4) H(61) 105.6(5) . . . yes H(51) C(4) C(5) 109.3(3) . . . yes H(51) C(4) C(3) 108.9(4) . . . yes C(6) C(5) C(4) 111.0(3) . . . yes H(40) C(5) C(4) 102.7(3) . . . yes H(40) C(5) C(6) 111.2(4) . . . yes C(10) C(5) C(4) 113.6(3) . . . yes C(10) C(5) C(6) 111.7(3) . . . yes C(10) C(5) H(40) 106.2(4) . . . yes H(65) C(6) H(91) 105.5(5) . . . yes C(7) C(6) H(91) 107.6(4) . . . yes C(7) C(6) H(65) 109.1(4) . . . yes C(5) C(6) H(91) 106.6(4) . . . yes C(5) C(6) H(65) 114.1(4) . . . yes C(5) C(6) C(7) 113.3(3) . . . yes C(6) C(7) C(8) 112.3(3) . . . yes O(26) C(7) C(8) 113.7(3) . . . yes O(26) C(7) C(6) 108.0(3) . . . yes H(55) C(7) C(8) 107.6(4) . . . yes H(55) C(7) C(6) 111.1(4) . . . yes H(55) C(7) O(26) 103.9(4) . . . yes C(7) C(8) C(14) 114.8(3) . . . yes H(37) C(8) C(14) 108.4(3) . . . yes H(37) C(8) C(7) 106.1(3) . . . yes C(9) C(8) C(14) 109.1(3) . . . yes C(9) C(8) C(7) 108.1(2) . . . yes C(9) C(8) H(37) 110.4(3) . . . yes C(11) C(9) H(39) 108.4(3) . . . yes C(8) C(9) H(39) 102.3(3) . . . yes C(8) C(9) C(11) 113.3(3) . . . yes C(10) C(9) H(39) 107.9(3) . . . yes C(10) C(9) C(11) 112.1(3) . . . yes C(10) C(9) C(8) 112.1(3) . . . yes C(5) C(10) C(19) 109.4(3) . . . yes C(9) C(10) C(19) 110.5(3) . . . yes C(9) C(10) C(5) 109.8(3) . . . yes C(1) C(10) C(19) 106.4(3) . . . yes C(1) C(10) C(5) 108.6(3) . . . yes C(1) C(10) C(9) 112.0(3) . . . yes C(12) C(11) H(73) 108.2(4) . . . yes C(9) C(11) H(73) 110.1(4) . . . yes C(9) C(11) C(12) 114.1(3) . . . yes H(83) C(11) H(73) 102.6(5) . . . yes H(83) C(11) C(12) 109.3(5) . . . yes H(83) C(11) C(9) 112.0(4) . . . yes H(78) C(12) H(71) 97.0(5) . . . yes C(13) C(12) H(71) 116.5(4) . . . yes C(13) C(12) H(78) 114.9(4) . . . yes C(11) C(12) H(71) 107.0(4) . . . yes C(11) C(12) H(78) 108.6(4) . . . yes C(11) C(12) C(13) 111.6(3) . . . yes C(17) C(13) C(12) 116.1(3) . . . yes C(18) C(13) C(12) 111.2(3) . . . yes C(18) C(13) C(17) 109.4(2) . . . yes C(14) C(13) C(12) 106.9(2) . . . yes C(14) C(13) C(17) 101.0(2) . . . yes C(14) C(13) C(18) 111.8(3) . . . yes C(13) C(14) H(38) 106.0(3) . . . yes C(8) C(14) H(38) 109.7(3) . . . yes C(8) C(14) C(13) 113.9(3) . . . yes C(15) C(14) H(38) 103.8(3) . . . yes C(15) C(14) C(13) 103.4(2) . . . yes C(15) C(14) C(8) 118.9(3) . . . yes H(75) C(15) C(14) 111.3(4) . . . yes H(47) C(15) C(14) 108.4(4) . . . yes H(47) C(15) H(75) 102.3(5) . . . yes C(16) C(15) C(14) 104.3(3) . . . yes C(16) C(15) H(75) 119.1(4) . . . yes C(16) C(15) H(47) 111.1(4) . . . yes H(69) C(16) C(17) 113.1(4) . . . yes H(82) C(16) C(17) 112.3(4) . . . yes H(82) C(16) H(69) 109.7(5) . . . yes C(15) C(16) C(17) 107.1(3) . . . yes C(15) C(16) H(69) 102.3(4) . . . yes C(15) C(16) H(82) 112.0(4) . . . yes C(13) C(17) C(16) 103.6(3) . . . yes H(90) C(17) C(16) 108.5(4) . . . yes H(90) C(17) C(13) 108.2(3) . . . yes C(20) C(17) C(16) 112.1(3) . . . yes C(20) C(17) C(13) 118.4(3) . . . yes C(20) C(17) H(90) 105.8(3) . . . yes H(77) C(18) H(68) 105.7(5) . . . yes H(58) C(18) H(68) 107.2(5) . . . yes H(58) C(18) H(77) 108.7(4) . . . yes C(13) C(18) H(68) 113.5(4) . . . yes C(13) C(18) H(77) 109.2(4) . . . yes C(13) C(18) H(58) 112.2(4) . . . yes H(87) C(19) H(88) 109.3(6) . . . yes C(10) C(19) H(88) 114.0(4) . . . yes C(10) C(19) H(87) 112.2(4) . . . yes H(46) C(19) H(88) 99.7(5) . . . yes H(46) C(19) H(87) 106.5(6) . . . yes H(46) C(19) C(10) 114.3(4) . . . yes C(21) C(20) C(22) 110.4(3) . . . yes C(17) C(20) C(22) 110.6(3) . . . yes C(17) C(20) C(21) 113.0(3) . . . yes H(81) C(20) C(22) 106.5(3) . . . yes H(81) C(20) C(21) 106.5(4) . . . yes H(81) C(20) C(17) 109.5(4) . . . yes H(60) C(21) H(84) 116.0(7) . . . yes C(20) C(21) H(84) 111.2(5) . . . yes C(20) C(21) H(60) 114.6(5) . . . yes H(80) C(21) H(84) 100.3(6) . . . yes H(80) C(21) H(60) 102.4(6) . . . yes H(80) C(21) C(20) 110.9(5) . . . yes H(70) C(22) H(62) 108.7(5) . . . yes C(23) C(22) H(62) 110.0(4) . . . yes C(23) C(22) H(70) 108.4(4) . . . yes C(20) C(22) H(62) 107.6(3) . . . yes C(20) C(22) H(70) 108.0(4) . . . yes C(20) C(22) C(23) 113.9(3) . . . yes C(22) C(23) C(24) 111.4(3) . . . yes H(74) C(23) C(24) 112.0(4) . . . yes H(74) C(23) C(22) 111.5(4) . . . yes H(66) C(23) C(24) 109.4(4) . . . yes H(66) C(23) C(22) 107.0(4) . . . yes H(66) C(23) H(74) 105.2(5) . . . yes C(23) C(24) N(28) 117.1(4) . . . yes O(27) C(24) N(28) 119.6(3) . . . yes O(27) C(24) C(23) 123.3(3) . . . yes H(79) O(25) C(3) 108.6(4) . . . yes C(7) O(26) H(89) 110.2(4) . . . yes C(29) N(28) C(24) 122.9(3) . . . yes H(63) N(28) C(24) 124.2(4) . . . yes H(63) N(28) C(29) 111.8(4) . . . yes H(76) C(29) H(53) 113.5(5) . . . yes C(30) C(29) H(53) 108.8(4) . . . yes C(30) C(29) H(76) 106.5(4) . . . yes N(28) C(29) H(53) 109.7(4) . . . yes N(28) C(29) H(76) 107.0(4) . . . yes N(28) C(29) C(30) 111.3(3) . . . yes S(31) C(30) H(52) 108.3(3) . . . yes H(57) C(30) H(52) 106.6(4) . . . yes H(57) C(30) S(31) 104.4(3) . . . yes C(29) C(30) H(52) 111.4(4) . . . yes C(29) C(30) S(31) 110.8(2) . . . yes C(29) C(30) H(57) 114.9(3) . . . yes H(11) O(1) H(12) 99.0(8) . . . yes H(21) O(2) H(22) 105.3(4) . . . yes H(23) O(2) H(22) 100.2(4) . . . yes H(23) O(2) H(21) 106.6(4) . . . yes