#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/33/2003399.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003399 loop_ _publ_author_name 'Linden, A.' 'Lee, C. K.' _publ_section_title 2,2',3,3'-Tetra-O-benzoyl-6,6'-dideoxy-4,4'-di-O-mesyl-6,6'-dithiocyanato-\a,\a-trehalose _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 751 _journal_page_last 754 _journal_volume 51 _journal_year 1995 _chemical_compound_source 'see text' _chemical_formula_moiety 'C44 H40 N2 O17 S4' _chemical_formula_sum 'C44 H40 N2 O17 S4' _chemical_formula_weight 997.04 _chemical_name_common ; 2,2',3,3'-Tetra-O-benzoyl-6,6'-dideoxy-4,4'-di-O-mesyl- 6,6'-dithiocyanato-\a,\a-trehalose ; _chemical_name_systematic ; 2,3-di-O-benzoyl-6-deoxy-4-O-mesyl-6-thiocyanato-\a-D-glucoopyranosyl 2,3-di-O-benzoyl-6-deoxy-4-O-mesyl-6-thiocyanato-\a-D-glucoopyranoside ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.051(3) _cell_length_b 26.274(4) _cell_length_c 9.487(3) _cell_measurement_reflns_used 24 _cell_measurement_temperature 173(1) _cell_measurement_theta_max 19.5 _cell_measurement_theta_min 14 _cell_volume 4748.7(18) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991) ; _computing_data_reduction 'PROCESS TEXSAN (Molecular Structure Corporation, 1989)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'FINISH TEXSAN' _computing_structure_refinement 'LS TEXSAN' _computing_structure_solution 'SHELXS86 direct methods (Sheldrick, 1990)' _diffrn_ambient_temperature 173.0(10) _diffrn_measurement_device 'Rigaku AFC-5R diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode generator' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 14607 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% insignificant _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.394 _exptl_crystal_description prism _exptl_crystal_F_000 2072 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.33 _refine_diff_density_max 0.32 _refine_diff_density_min -0.25 _refine_ls_abs_structure_details 'see text' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_extinction_method 'not applied' _refine_ls_goodness_of_fit_obs 1.376 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 764 _refine_ls_number_reflns 8854 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_obs 0.0373 _refine_ls_shift/esd_max 0.0007 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'sigma w=1/[\s^2^(F~o~)+(0.01F~o~)^2^]' _refine_ls_wR_factor_all 0.0423 _refine_ls_wR_factor_obs 0.0381 _reflns_number_observed 8854 _reflns_number_total 11798 _reflns_observed_criterion 'I > 3\s(I)' _[local]_cod_data_source_file pa1147.cif _[local]_cod_data_source_block L9309 _cod_original_cell_volume 4749(2) _cod_database_code 2003399 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C C 'IntTabC (1992) Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 H H 'IntTabC (1992) Tables 4.2.6.8 and 6.1.1.4' 0.000 0.000 N N 'IntTabC (1992) Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033 O O 'IntTabC (1992) Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060 S S 'IntTabC (1992) Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.1234 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_type_symbol S(1) 1 0.33688(3) 0.73915(2) 0.16411(7) 0.0294(2) Uani d S S(2) 1 0.54334(4) 0.85604(2) 0.33745(8) 0.0373(2) Uani d S S(3) 1 0.81158(3) 0.54648(2) 0.59680(7) 0.0298(2) Uani d S S(4) 1 0.59571(4) 0.59573(3) 0.97648(8) 0.0423(2) Uani d S O(1) 1 0.57668(8) 0.69455(6) 0.5567(2) 0.0246(5) Uani d O O(2) 1 0.47618(8) 0.62476(6) 0.6284(2) 0.0306(5) Uani d O O(3) 1 0.38741(8) 0.63642(6) 0.3916(2) 0.0308(5) Uani d O O(4) 1 0.41283(8) 0.72325(6) 0.2209(2) 0.0267(5) Uani d O O(5) 1 0.49451(8) 0.76076(6) 0.5547(2) 0.0251(5) Uani d O O(7) 1 0.3875(1) 0.62365(8) 0.7839(3) 0.0595(8) Uani d O O(8) 1 0.32818(9) 0.79248(7) 0.1866(2) 0.0430(6) Uani d O O(9) 1 0.28539(9) 0.70647(8) 0.2221(2) 0.0461(7) Uani d O O(14) 1 0.4642(1) 0.58184(9) 0.2936(4) 0.088(1) Uani d O O(32) 1 0.68245(8) 0.73502(6) 0.4005(2) 0.0275(5) Uani d O O(33) 1 0.77891(8) 0.65215(6) 0.4140(2) 0.0269(5) Uani d O O(34) 1 0.73608(8) 0.57209(6) 0.6119(2) 0.0306(5) Uani d O O(35) 1 0.64969(8) 0.68590(6) 0.7529(2) 0.0264(5) Uani d O O(37) 1 0.78190(9) 0.78144(8) 0.4140(2) 0.0508(7) Uani d O O(38) 1 0.8103(1) 0.51902(8) 0.4682(2) 0.0518(7) Uani d O O(39) 1 0.86459(8) 0.58373(7) 0.6216(2) 0.0411(6) Uani d O O(44) 1 0.71971(9) 0.61776(8) 0.2315(2) 0.0453(7) Uani d O N(1) 1 0.6181(1) 0.8497(1) 0.5940(3) 0.061(1) Uani d N N(2) 1 0.5276(2) 0.6911(1) 0.9958(4) 0.076(1) Uani d N C(1) 1 0.5123(1) 0.71265(9) 0.6120(3) 0.0245(7) Uani d C C(2) 1 0.4555(1) 0.67415(9) 0.5782(3) 0.0266(7) Uani d C C(3) 1 0.4436(1) 0.67146(9) 0.4203(3) 0.0254(7) Uani d C C(4) 1 0.4230(1) 0.72440(9) 0.3720(3) 0.0243(7) Uani d C C(5) 1 0.4832(1) 0.76095(9) 0.4050(3) 0.0234(6) Uani d C C(6) 1 0.4671(1) 0.8157(1) 0.3640(3) 0.0292(8) Uani d C C(7) 1 0.4365(1) 0.60294(9) 0.7300(3) 0.0327(8) Uani d C C(8) 1 0.4624(1) 0.55164(9) 0.7673(3) 0.0333(8) Uani d C C(9) 1 0.5138(2) 0.5274(1) 0.6890(3) 0.046(1) Uani d C C(10) 1 0.5403(2) 0.4811(1) 0.7365(5) 0.065(1) Uani d C C(11) 1 0.5170(2) 0.4600(1) 0.8597(4) 0.062(1) Uani d C C(12) 1 0.4649(2) 0.4830(1) 0.9340(5) 0.059(1) Uani d C C(13) 1 0.4380(2) 0.5291(1) 0.8899(4) 0.047(1) Uani d C C(14) 1 0.4049(2) 0.5931(1) 0.3232(4) 0.0447(9) Uani d C C(15) 1 0.3420(2) 0.5615(1) 0.2916(3) 0.0427(9) Uani d C C(16) 1 0.3542(2) 0.5131(1) 0.2391(5) 0.069(1) Uani d C C(17) 1 0.2968(2) 0.4826(2) 0.1986(5) 0.081(2) Uani d C C(18) 1 0.2305(2) 0.5003(2) 0.2158(5) 0.069(1) Uani d C C(19) 1 0.2177(2) 0.5479(1) 0.2700(4) 0.058(1) Uani d C C(20) 1 0.2743(2) 0.5789(1) 0.3088(4) 0.044(1) Uani d C C(21) 1 0.3530(2) 0.7270(2) -0.0139(3) 0.048(1) Uani d C C(22) 1 0.5854(1) 0.8514(1) 0.4931(3) 0.0409(9) Uani d C C(31) 1 0.6366(1) 0.71354(9) 0.6285(3) 0.0240(7) Uani d C C(32) 1 0.6994(1) 0.70961(9) 0.5294(3) 0.0245(7) Uani d C C(33) 1 0.7158(1) 0.65388(9) 0.4983(3) 0.0240(7) Uani d C C(34) 1 0.7281(1) 0.62647(9) 0.6375(3) 0.0248(7) Uani d C C(35) 1 0.6631(1) 0.63258(9) 0.7320(3) 0.0261(7) Uani d C C(36) 1 0.6750(1) 0.6107(1) 0.8783(3) 0.0334(8) Uani d C C(37) 1 0.7279(1) 0.77133(9) 0.3549(3) 0.0302(7) Uani d C C(38) 1 0.7024(1) 0.79564(9) 0.2229(3) 0.0289(7) Uani d C C(39) 1 0.6581(1) 0.7701(1) 0.1307(3) 0.0358(8) Uani d C C(40) 1 0.6389(2) 0.7933(1) 0.0055(3) 0.046(1) Uani d C C(41) 1 0.6621(2) 0.8416(1) -0.0261(3) 0.049(1) Uani d C C(42) 1 0.7050(2) 0.8672(1) 0.0664(4) 0.048(1) Uani d C C(43) 1 0.7259(1) 0.8443(1) 0.1915(3) 0.0393(9) Uani d C C(44) 1 0.7731(1) 0.63459(9) 0.2794(3) 0.0280(7) Uani d C C(45) 1 0.8405(1) 0.63789(9) 0.2009(3) 0.0272(7) Uani d C C(46) 1 0.8448(1) 0.6138(1) 0.0703(3) 0.0314(8) Uani d C C(47) 1 0.9056(2) 0.6164(1) -0.0087(3) 0.0383(9) Uani d C C(48) 1 0.9630(2) 0.6425(1) 0.0433(3) 0.0419(9) Uani d C C(49) 1 0.9591(2) 0.6661(1) 0.1727(3) 0.0428(9) Uani d C C(50) 1 0.8977(1) 0.6642(1) 0.2512(3) 0.0328(8) Uani d C C(51) 1 0.8105(2) 0.5031(1) 0.7368(5) 0.057(1) Uani d C C(52) 1 0.5582(2) 0.6530(1) 0.9885(3) 0.049(1) Uani d C H(1) 1 0.514(1) 0.7187(8) 0.714(2) 0.015(6) Uiso d H H(2) 1 0.420(1) 0.6842(8) 0.625(2) 0.018(6) Uiso d H H(3) 1 0.484(1) 0.6604(9) 0.375(3) 0.028(7) Uiso d H H(4) 1 0.382(1) 0.7356(8) 0.417(2) 0.014(5) Uiso d H H(5) 1 0.523(1) 0.7501(8) 0.362(2) 0.022(6) Uiso d H H(9) 1 0.533(1) 0.543(1) 0.601(3) 0.043(8) Uiso d H H(10) 1 0.575(2) 0.466(1) 0.682(4) 0.07(1) Uiso d H H(11) 1 0.535(2) 0.432(1) 0.887(4) 0.09(1) Uiso d H H(12) 1 0.444(2) 0.468(1) 1.016(4) 0.08(1) Uiso d H H(13) 1 0.406(2) 0.546(1) 0.947(3) 0.06(1) Uiso d H H(16) 1 0.401(2) 0.500(1) 0.223(4) 0.09(1) Uiso d H H(17) 1 0.308(2) 0.449(2) 0.165(4) 0.10(1) Uiso d H H(18) 1 0.195(2) 0.480(1) 0.188(4) 0.08(1) Uiso d H H(19) 1 0.171(1) 0.561(1) 0.284(3) 0.044(8) Uiso d H H(20) 1 0.265(2) 0.614(1) 0.341(4) 0.062(9) Uiso d H H(31) 1 0.628(1) 0.7483(8) 0.654(2) 0.017(6) Uiso d H H(32) 1 0.741(1) 0.7244(9) 0.574(3) 0.035(7) Uiso d H H(33) 1 0.677(1) 0.6367(8) 0.443(3) 0.023(6) Uiso d H H(34) 1 0.768(1) 0.6380(9) 0.688(3) 0.025(6) Uiso d H H(35) 1 0.622(1) 0.6162(8) 0.692(2) 0.013(5) Uiso d H H(39) 1 0.644(1) 0.737(1) 0.142(3) 0.038(8) Uiso d H H(40) 1 0.615(1) 0.773(1) -0.059(3) 0.049(9) Uiso d H H(41) 1 0.655(1) 0.856(1) -0.111(3) 0.038(7) Uiso d H H(42) 1 0.719(1) 0.900(1) 0.046(3) 0.036(7) Uiso d H H(43) 1 0.756(2) 0.861(1) 0.247(3) 0.050(9) Uiso d H H(46) 1 0.806(1) 0.5971(8) 0.038(3) 0.024(6) Uiso d H H(47) 1 0.908(1) 0.6028(9) -0.098(3) 0.032(7) Uiso d H H(48) 1 1.010(1) 0.643(1) -0.007(3) 0.043(8) Uiso d H H(49) 1 0.999(2) 0.682(1) 0.202(3) 0.046(8) Uiso d H H(50) 1 0.895(1) 0.6797(9) 0.340(3) 0.032(7) Uiso d H H(61) 1 0.432(1) 0.8324(9) 0.432(3) 0.033(7) Uiso d H H(62) 1 0.447(1) 0.815(1) 0.275(3) 0.049(8) Uiso d H H(211) 1 0.353(2) 0.691(1) -0.023(3) 0.06(1) Uiso d H H(212) 1 0.397(2) 0.742(1) -0.040(4) 0.07(1) Uiso d H H(213) 1 0.308(2) 0.736(1) -0.060(4) 0.07(1) Uiso d H H(361) 1 0.694(1) 0.576(1) 0.873(3) 0.039(7) Uiso d H H(362) 1 0.704(1) 0.6341(9) 0.934(3) 0.031(7) Uiso d H H(511) 1 0.808(2) 0.525(1) 0.828(4) 0.06(1) Uiso d H H(512) 1 0.845(2) 0.486(1) 0.726(4) 0.07(1) Uiso d H H(513) 1 0.775(2) 0.482(1) 0.714(4) 0.07(1) Uiso d H 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 _atom_site_aniso_type_symbol S(1) 0.0215(3) 0.0011(3) -0.0048(3) 0.0374(3) -0.0003(3) 0.0294(3) S S(2) 0.0380(3) -0.0073(3) -0.0013(3) 0.0334(3) 0.0033(3) 0.0406(4) S S(3) 0.0309(3) 0.0040(3) 0.0010(3) 0.0252(3) -0.0016(3) 0.0334(3) S S(4) 0.0381(4) -0.0073(3) 0.0011(3) 0.0550(4) 0.0104(4) 0.0339(4) S O(1) 0.0178(7) 0.0032(6) -0.0010(7) 0.0286(8) -0.0018(7) 0.0274(9) O O(2) 0.0265(9) 0.0080(7) 0.0058(8) 0.0283(9) 0.0076(8) 0.037(1) O O(3) 0.0239(8) -0.0013(7) -0.0018(8) 0.0275(9) -0.0024(8) 0.041(1) O O(4) 0.0211(8) 0.0034(7) -0.0004(7) 0.0366(9) -0.0025(7) 0.0224(8) O O(5) 0.0249(8) 0.0054(7) -0.0021(7) 0.0265(8) -0.0017(7) 0.0239(9) O O(7) 0.051(1) 0.022(1) 0.030(1) 0.054(1) 0.031(1) 0.074(2) O O(8) 0.035(1) 0.0078(8) -0.007(1) 0.039(1) -0.003(1) 0.055(1) O O(9) 0.0276(9) -0.0084(9) -0.0051(9) 0.058(1) 0.013(1) 0.053(1) O O(14) 0.041(1) -0.006(1) 0.028(2) 0.061(2) -0.058(2) 0.161(3) O O(32) 0.0244(8) -0.0014(7) -0.0054(7) 0.0304(8) 0.0063(8) 0.0276(9) O O(33) 0.0217(8) -0.0016(7) 0.0005(7) 0.0335(9) -0.0024(8) 0.0254(8) O O(34) 0.0244(8) -0.0008(7) 0.0014(8) 0.0224(8) -0.0009(8) 0.045(1) O O(35) 0.0260(8) 0.0044(7) -0.0025(7) 0.0290(8) -0.0003(7) 0.0243(9) O O(37) 0.032(1) -0.0182(9) -0.015(1) 0.064(1) 0.026(1) 0.056(1) O O(38) 0.049(1) 0.012(1) -0.002(1) 0.060(1) -0.022(1) 0.046(1) O O(39) 0.0256(8) 0.0036(8) -0.0007(9) 0.034(1) -0.002(1) 0.064(1) O O(44) 0.031(1) -0.0117(9) -0.0033(9) 0.068(1) -0.016(1) 0.037(1) O N(1) 0.064(2) -0.013(1) -0.029(2) 0.051(2) 0.002(2) 0.068(2) N N(2) 0.060(2) 0.009(2) 0.037(2) 0.083(2) 0.003(2) 0.085(2) N C(1) 0.024(1) 0.008(1) 0.001(1) 0.028(1) 0.000(1) 0.022(1) C C(2) 0.020(1) 0.005(1) 0.005(1) 0.026(1) 0.006(1) 0.033(1) C C(3) 0.018(1) 0.0018(9) 0.000(1) 0.027(1) 0.000(1) 0.031(1) C C(4) 0.021(1) 0.0026(9) 0.000(1) 0.029(1) -0.002(1) 0.023(1) C C(5) 0.020(1) 0.004(1) 0.000(1) 0.029(1) 0.001(1) 0.022(1) C C(6) 0.027(1) 0.000(1) -0.005(1) 0.029(1) 0.005(1) 0.032(1) C C(7) 0.023(1) 0.001(1) 0.000(1) 0.034(1) 0.006(1) 0.040(1) C C(8) 0.030(1) -0.002(1) -0.007(1) 0.025(1) 0.002(1) 0.045(2) C C(9) 0.061(2) 0.006(1) -0.004(2) 0.035(1) -0.005(1) 0.043(2) C C(10) 0.087(3) 0.022(2) 0.001(2) 0.039(2) -0.010(2) 0.069(3) C C(11) 0.082(3) 0.010(2) -0.020(2) 0.031(2) 0.009(2) 0.074(3) C C(12) 0.068(2) -0.001(2) -0.003(2) 0.036(2) 0.017(2) 0.074(3) C C(13) 0.044(2) 0.001(1) 0.002(2) 0.037(2) 0.018(2) 0.060(2) C C(14) 0.042(2) -0.005(1) 0.007(2) 0.033(1) -0.011(1) 0.058(2) C C(15) 0.046(2) -0.010(1) 0.005(2) 0.033(1) -0.006(1) 0.049(2) C C(16) 0.063(2) -0.012(2) 0.021(2) 0.046(2) -0.025(2) 0.097(3) C C(17) 0.081(3) -0.024(2) 0.025(3) 0.049(2) -0.033(2) 0.115(4) C C(18) 0.062(2) -0.037(2) 0.007(2) 0.059(2) -0.014(2) 0.087(3) C C(19) 0.049(2) -0.017(2) 0.001(2) 0.052(2) 0.001(2) 0.073(2) C C(20) 0.044(2) -0.011(1) -0.005(1) 0.036(2) 0.003(1) 0.053(2) C C(21) 0.046(2) 0.002(2) -0.009(1) 0.067(2) -0.009(2) 0.030(2) C C(22) 0.039(1) -0.003(1) -0.008(1) 0.030(1) -0.005(1) 0.054(2) C C(31) 0.023(1) 0.0013(9) -0.003(1) 0.024(1) 0.000(1) 0.025(1) C C(32) 0.021(1) -0.001(1) -0.004(1) 0.026(1) 0.000(1) 0.027(1) C C(33) 0.018(1) 0.0002(9) 0.000(1) 0.028(1) -0.002(1) 0.026(1) C C(34) 0.021(1) 0.0011(9) -0.002(1) 0.021(1) -0.002(1) 0.032(1) C C(35) 0.023(1) -0.001(1) -0.003(1) 0.027(1) 0.002(1) 0.028(1) C C(36) 0.027(1) 0.003(1) -0.003(1) 0.042(2) 0.007(1) 0.031(1) C C(37) 0.022(1) 0.000(1) 0.001(1) 0.036(1) 0.006(1) 0.033(1) C C(38) 0.021(1) 0.005(1) 0.004(1) 0.037(1) 0.005(1) 0.030(1) C C(39) 0.033(1) 0.007(1) 0.003(1) 0.044(2) 0.001(1) 0.031(1) C C(40) 0.049(2) 0.008(2) 0.000(1) 0.059(2) 0.000(2) 0.030(2) C C(41) 0.049(2) 0.014(2) 0.004(2) 0.066(2) 0.018(2) 0.033(2) C C(42) 0.042(2) 0.005(1) 0.006(2) 0.048(2) 0.020(2) 0.053(2) C C(43) 0.029(1) -0.001(1) 0.004(1) 0.045(2) 0.009(1) 0.044(2) C C(44) 0.027(1) 0.002(1) -0.004(1) 0.030(1) 0.000(1) 0.027(1) C C(45) 0.027(1) 0.006(1) -0.002(1) 0.030(1) 0.003(1) 0.025(1) C C(46) 0.029(1) 0.003(1) -0.007(1) 0.038(1) -0.004(1) 0.027(1) C C(47) 0.041(1) 0.008(1) -0.001(1) 0.051(2) -0.003(1) 0.023(1) C C(48) 0.034(1) 0.001(1) 0.004(1) 0.061(2) 0.001(1) 0.031(1) C C(49) 0.032(1) -0.010(1) 0.000(1) 0.058(2) -0.005(2) 0.038(2) C C(50) 0.032(1) -0.005(1) 0.002(1) 0.041(1) -0.003(1) 0.025(1) C C(51) 0.065(2) 0.016(2) 0.008(2) 0.044(2) 0.020(2) 0.063(2) C C(52) 0.037(2) -0.008(2) 0.011(1) 0.067(2) -0.001(2) 0.044(2) C loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 6 -1 3 6 1 -3 3 2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(4) S(1) O(8) 108.10(10) yes O(4) S(1) O(9) 109.70(10) yes O(4) S(1) C(21) 96.80(10) yes O(8) S(1) O(9) 117.20(10) yes O(8) S(1) C(21) 110.2(2) yes O(9) S(1) C(21) 112.8(2) yes C(6) S(2) C(22) 102.50(10) yes C(2) O(2) C(7) 117.8(2) yes C(3) O(3) C(14) 116.5(2) yes S(1) O(4) C(4) 116.70(10) yes C(1) O(5) C(5) 114.7(2) yes O(1) C(1) O(5) 111.4(2) yes O(1) C(1) C(2) 108.4(2) yes O(5) C(1) C(2) 110.1(2) yes O(2) C(2) C(1) 109.7(2) yes O(2) C(2) C(3) 109.0(2) yes C(1) C(2) C(3) 110.3(2) yes O(3) C(3) C(2) 109.1(2) yes O(3) C(3) C(4) 109.7(2) yes C(2) C(3) C(4) 107.1(2) yes O(4) C(4) C(3) 108.3(2) yes O(4) C(4) C(5) 108.4(2) yes C(3) C(4) C(5) 108.6(2) yes O(5) C(5) C(4) 108.2(2) yes O(5) C(5) C(6) 106.6(2) yes C(4) C(5) C(6) 112.9(2) yes S(2) C(6) C(5) 115.2(2) yes O(2) C(7) O(7) 123.3(2) yes O(2) C(7) C(8) 111.8(2) yes O(7) C(7) C(8) 124.9(2) yes C(7) C(8) C(9) 121.8(3) ? C(7) C(8) C(13) 118.6(3) ? C(9) C(8) C(13) 119.4(3) ? C(8) C(9) C(10) 119.0(3) ? C(9) C(10) C(11) 120.9(4) ? C(10) C(11) C(12) 120.0(3) ? C(11) C(12) C(13) 120.3(4) ? C(8) C(13) C(12) 120.3(3) ? O(3) C(14) O(14) 123.5(3) yes O(3) C(14) C(15) 111.6(2) yes O(14) C(14) C(15) 124.9(3) yes C(14) C(15) C(16) 116.7(3) ? C(14) C(15) C(20) 123.1(2) ? C(16) C(15) C(20) 120.2(3) ? C(15) C(16) C(17) 119.3(4) ? C(16) C(17) C(18) 119.7(4) ? C(17) C(18) C(19) 121.4(3) ? C(18) C(19) C(20) 119.5(3) ? C(15) C(20) C(19) 119.8(3) ? S(2) C(22) N(1) 175.0(3) yes C(1) O(1) C(31) 113.6(2) yes O(34) S(3) O(38) 106.10(10) yes O(34) S(3) O(39) 109.50(10) yes O(34) S(3) C(51) 101.3(2) yes O(38) S(3) O(39) 120.20(10) yes O(38) S(3) C(51) 108.8(2) yes O(39) S(3) C(51) 109.2(2) yes C(36) S(4) C(52) 101.30(10) yes C(32) O(32) C(37) 117.1(2) yes C(33) O(33) C(44) 117.5(2) yes S(3) O(34) C(34) 121.50(10) yes C(31) O(35) C(35) 114.7(2) yes O(1) C(31) O(35) 111.3(2) yes O(1) C(31) C(32) 108.2(2) yes O(35) C(31) C(32) 110.0(2) yes O(32) C(32) C(31) 108.5(2) yes O(32) C(32) C(33) 109.2(2) yes C(31) C(32) C(33) 110.1(2) yes O(33) C(33) C(32) 107.9(2) yes O(33) C(33) C(34) 109.7(2) yes C(32) C(33) C(34) 108.5(2) yes O(34) C(34) C(33) 109.6(2) yes O(34) C(34) C(35) 106.5(2) yes C(33) C(34) C(35) 109.4(2) yes O(35) C(35) C(34) 109.0(2) yes O(35) C(35) C(36) 105.6(2) yes C(34) C(35) C(36) 111.9(2) yes S(4) C(36) C(35) 115.2(2) yes O(32) C(37) O(37) 123.5(2) yes O(32) C(37) C(38) 111.2(2) yes O(37) C(37) C(38) 125.3(2) yes C(37) C(38) C(39) 121.4(2) ? C(37) C(38) C(43) 118.1(2) ? C(39) C(38) C(43) 120.4(3) ? C(38) C(39) C(40) 119.2(3) ? C(39) C(40) C(41) 120.6(3) ? C(40) C(41) C(42) 120.2(3) ? C(41) C(42) C(43) 120.2(3) ? C(38) C(43) C(42) 119.4(3) ? O(33) C(44) O(44) 123.3(2) yes O(33) C(44) C(45) 112.3(2) yes O(44) C(44) C(45) 124.4(2) yes C(44) C(45) C(46) 118.0(2) ? C(44) C(45) C(50) 122.7(2) ? C(46) C(45) C(50) 119.3(2) ? C(45) C(46) C(47) 120.6(2) ? C(46) C(47) C(48) 119.6(3) ? C(47) C(48) C(49) 119.9(3) ? C(48) C(49) C(50) 120.6(3) ? C(45) C(50) C(49) 120.0(2) ? S(4) C(52) N(2) 175.2(3) yes O(1) C(1) H(1) 113.0(10) ? O(5) C(1) H(1) 104.0(10) ? C(2) C(1) H(1) 110.0(10) ? O(2) C(2) H(2) 109(2) ? C(1) C(2) H(2) 105(2) ? C(3) C(2) H(2) 114(2) ? O(3) C(3) H(3) 109(2) ? C(2) C(3) H(3) 111(2) ? C(4) C(3) H(3) 111(2) ? O(4) C(4) H(4) 110.0(10) ? C(3) C(4) H(4) 112.0(10) ? C(5) C(4) H(4) 109.0(10) ? O(5) C(5) H(5) 108.0(10) ? C(4) C(5) H(5) 110.0(10) ? C(6) C(5) H(5) 111.0(10) ? S(2) C(6) H(61) 111.0(10) ? S(2) C(6) H(62) 103(2) ? C(5) C(6) H(61) 112.0(10) ? C(5) C(6) H(62) 108(2) ? H(61) C(6) H(62) 107(2) ? C(8) C(9) H(9) 121(2) ? C(10) C(9) H(9) 120(2) ? C(9) C(10) H(10) 117(2) ? C(11) C(10) H(10) 122(2) ? C(10) C(11) H(11) 119(3) ? C(12) C(11) H(11) 121(3) ? C(11) C(12) H(12) 123(2) ? C(13) C(12) H(12) 117(2) ? C(8) C(13) H(13) 121(2) ? C(12) C(13) H(13) 119(2) ? C(15) C(16) H(16) 123(2) ? C(17) C(16) H(16) 118(2) ? C(16) C(17) H(17) 116(3) ? C(18) C(17) H(17) 124(2) ? C(17) C(18) H(18) 117(2) ? C(19) C(18) H(18) 121(2) ? C(18) C(19) H(19) 122(2) ? C(20) C(19) H(19) 118(2) ? C(15) C(20) H(20) 121(2) ? C(19) C(20) H(20) 119(2) ? S(1) C(21) H(211) 106(2) ? S(1) C(21) H(212) 109(2) ? S(1) C(21) H(213) 103(2) ? H(211) C(21) H(212) 112(3) ? H(211) C(21) H(213) 102(3) ? H(212) C(21) H(213) 123(3) ? O(1) C(31) H(31) 108.0(10) ? O(35) C(31) H(31) 108.0(10) ? C(32) C(31) H(31) 111.0(10) ? O(32) C(32) H(32) 112(2) ? C(31) C(32) H(32) 110(2) ? C(33) C(32) H(32) 107.0(10) ? O(33) C(33) H(33) 108.0(10) ? C(32) C(33) H(33) 112.0(10) ? C(34) C(33) H(33) 110.0(10) ? O(34) C(34) H(34) 108.0(10) ? C(33) C(34) H(34) 114.0(10) ? C(35) C(34) H(34) 109.0(10) ? O(35) C(35) H(35) 110.0(10) ? C(34) C(35) H(35) 112.0(10) ? C(36) C(35) H(35) 108.0(10) ? S(4) C(36) H(361) 98(2) ? S(4) C(36) H(362) 109.0(10) ? C(35) C(36) H(361) 111(2) ? C(35) C(36) H(362) 110(2) ? H(361) C(36) H(362) 113(2) ? C(38) C(39) H(39) 124(2) ? C(40) C(39) H(39) 116(2) ? C(39) C(40) H(40) 116(2) ? C(41) C(40) H(40) 123(2) ? C(40) C(41) H(41) 123(2) ? C(42) C(41) H(41) 117(2) ? C(41) C(42) H(42) 120(2) ? C(43) C(42) H(42) 120(2) ? C(38) C(43) H(43) 123(2) ? C(42) C(43) H(43) 118(2) ? C(45) C(46) H(46) 118(2) ? C(47) C(46) H(46) 121(2) ? C(46) C(47) H(47) 122(2) ? C(48) C(47) H(47) 119(2) ? C(47) C(48) H(48) 122(2) ? C(49) C(48) H(48) 118(2) ? C(48) C(49) H(49) 115(2) ? C(50) C(49) H(49) 124(2) ? C(45) C(50) H(50) 119(2) ? C(49) C(50) H(50) 121(2) ? S(3) C(51) H(511) 106(2) ? S(3) C(51) H(512) 106(3) ? S(3) C(51) H(513) 103(2) ? H(511) C(51) H(512) 117(3) ? H(511) C(51) H(513) 120(3) ? H(512) C(51) H(513) 104(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S(1) O(4) 1.599(2) yes S(1) O(8) 1.427(2) yes S(1) O(9) 1.415(2) yes S(1) C(21) 1.746(3) yes S(2) C(6) 1.817(3) yes S(2) C(22) 1.685(3) yes O(1) C(1) 1.416(3) yes O(2) C(2) 1.438(3) yes O(2) C(7) 1.352(3) yes O(3) C(3) 1.438(3) yes O(3) C(14) 1.351(3) yes O(4) C(4) 1.447(3) yes O(5) C(1) 1.417(3) yes O(5) C(5) 1.437(3) yes O(7) C(7) 1.197(3) yes O(14) C(14) 1.202(3) yes N(1) C(22) 1.143(4) yes C(1) C(2) 1.516(3) yes C(2) C(3) 1.517(4) yes C(3) C(4) 1.516(3) yes C(4) C(5) 1.529(3) yes C(5) C(6) 1.521(3) yes C(7) C(8) 1.478(3) yes C(8) C(9) 1.386(4) ? C(8) C(13) 1.386(4) ? C(9) C(10) 1.391(4) ? C(10) C(11) 1.369(6) ? C(11) C(12) 1.359(5) ? C(12) C(13) 1.382(4) ? C(14) C(15) 1.488(4) yes C(15) C(16) 1.386(4) ? C(15) C(20) 1.378(4) ? C(16) C(17) 1.411(5) ? C(17) C(18) 1.356(5) ? C(18) C(19) 1.375(5) ? C(19) C(20) 1.399(4) ? S(3) O(34) 1.594(2) yes S(3) O(38) 1.417(2) yes S(3) O(39) 1.426(2) yes S(3) C(51) 1.750(4) yes S(4) C(36) 1.819(3) yes S(4) C(52) 1.671(4) yes O(1) C(31) 1.420(3) yes O(32) C(32) 1.431(3) yes O(32) C(37) 1.359(3) yes O(33) C(33) 1.445(3) yes O(33) C(44) 1.363(3) yes O(34) C(34) 1.457(3) yes O(35) C(31) 1.409(3) yes O(35) C(35) 1.438(3) yes O(37) C(37) 1.201(3) yes O(44) C(44) 1.198(3) yes N(2) C(52) 1.160(4) yes C(31) C(32) 1.526(3) yes C(32) C(33) 1.526(3) yes C(33) C(34) 1.523(3) yes C(34) C(35) 1.538(3) yes C(35) C(36) 1.519(3) yes C(37) C(38) 1.487(3) yes C(38) C(39) 1.390(4) ? C(38) C(43) 1.387(4) ? C(39) C(40) 1.384(4) ? C(40) C(41) 1.376(4) ? C(41) C(42) 1.376(5) ? C(42) C(43) 1.389(4) ? C(44) C(45) 1.487(3) yes C(45) C(46) 1.394(3) ? C(45) C(50) 1.377(3) ? C(46) C(47) 1.382(4) ? C(47) C(48) 1.382(4) ? C(48) C(49) 1.378(4) ? C(49) C(50) 1.386(4) ? C(1) H(1) 0.98(2) ? C(2) H(2) 0.85(2) ? C(3) H(3) 0.92(2) ? C(4) H(4) 0.93(2) ? C(5) H(5) 0.91(2) ? C(6) H(61) 1.03(3) ? C(6) H(62) 0.93(3) ? C(9) H(9) 1.00(3) ? C(10) H(10) 0.93(3) ? C(11) H(11) 0.85(3) ? C(12) H(12) 0.96(3) ? C(13) H(13) 0.93(3) ? C(16) H(16) 0.97(4) ? C(17) H(17) 0.95(4) ? C(18) H(18) 0.90(3) ? C(19) H(19) 0.96(3) ? C(20) H(20) 0.99(3) ? C(21) H(211) 0.96(3) ? C(21) H(212) 0.96(3) ? C(21) H(213) 1.00(3) ? C(31) H(31) 0.96(2) ? C(32) H(32) 0.98(3) ? C(33) H(33) 1.01(2) ? C(34) H(34) 0.95(2) ? C(35) H(35) 0.97(2) ? C(36) H(361) 0.97(3) ? C(36) H(362) 0.98(3) ? C(39) H(39) 0.92(3) ? C(40) H(40) 0.93(3) ? C(41) H(41) 0.91(3) ? C(42) H(42) 0.94(3) ? C(43) H(43) 0.90(3) ? C(46) H(46) 0.91(2) ? C(47) H(47) 0.93(3) ? C(48) H(48) 1.02(3) ? C(49) H(49) 0.92(3) ? C(50) H(50) 0.94(3) ? C(51) H(511) 1.04(3) ? C(51) H(512) 0.82(4) ? C(51) H(513) 0.90(4) ? 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_publ_flag O(5) C(1) C(2) C(3) 56.1(3) yes O(5) C(5) C(4) C(3) -60.7(2) yes C(1) O(5) C(5) C(4) 59.9(2) yes C(1) C(2) C(3) C(4) -58.8(2) yes C(2) C(1) O(5) C(5) -57.6(2) yes C(2) C(3) C(4) C(5) 61.1(2) yes O(1) C(1) O(5) C(5) 62.8(2) yes O(1) C(1) C(2) O(2) 54.1(2) yes O(1) C(1) C(2) C(3) -66.0(2) yes O(2) C(2) C(3) O(3) 62.1(2) yes O(2) C(2) C(3) C(4) -179.2(2) yes O(2) C(7) C(8) C(9) -9.6(4) yes O(3) C(3) C(4) O(4) -63.0(2) yes O(3) C(3) C(4) C(5) 179.4(2) yes O(3) C(14) C(15) C(16) -171.4(3) yes O(4) C(4) C(5) O(5) -178.2(2) yes O(4) C(4) C(5) C(6) 63.9(3) yes O(5) C(1) O(1) C(31) 84.4(2) yes C(2) C(1) O(1) C(31) -154.3(2) yes C(1) O(5) C(5) C(6) -178.4(2) yes C(1) C(2) O(2) C(7) 116.7(2) yes C(2) O(2) C(7) C(8) 177.8(2) yes C(2) C(3) O(3) C(14) -113.1(2) yes C(3) O(3) C(14) C(15) -176.5(2) yes C(4) O(4) S(1) C(21) -176.3(2) yes S(1) O(4) C(4) C(3) 120.9(2) yes S(1) O(4) C(4) C(5) -121.4(2) yes S(2) C(6) C(5) O(5) 83.2(2) yes S(2) C(6) C(5) C(4) -158.1(2) yes O(2) C(2) C(1) O(5) 176.2(2) ? O(2) C(7) C(8) C(13) 165.5(2) ? O(3) C(3) C(2) C(1) -177.4(2) ? O(3) C(14) C(15) C(20) 10.4(4) ? O(4) C(4) C(3) C(2) 178.7(2) ? O(7) C(7) O(2) C(2) -3.5(4) ? O(7) C(7) C(8) C(9) 171.8(3) ? O(7) C(7) C(8) C(13) -13.1(4) ? O(8) S(1) O(4) C(4) 69.8(2) ? O(9) S(1) O(4) C(4) -59.1(2) ? O(14) C(14) O(3) C(3) 4.3(5) ? O(14) C(14) C(15) C(16) 7.8(5) ? O(14) C(14) C(15) C(20) -170.4(4) ? N(1) C(22) S(2) C(6) 164(3) ? C(3) C(2) O(2) C(7) -122.5(2) ? C(3) C(4) C(5) C(6) -178.5(2) ? C(4) C(3) O(3) C(14) 129.9(2) ? C(5) C(6) S(2) C(22) -57.0(2) ? C(7) C(8) C(9) C(10) 174.3(3) ? C(7) C(8) C(13) C(12) -174.9(3) ? C(8) C(9) C(10) C(11) -1.0(5) ? C(8) C(13) C(12) C(11) 1.8(5) ? C(9) C(8) C(13) C(12) 0.3(4) ? C(9) C(10) C(11) C(12) 3.0(6) ? C(10) C(9) C(8) C(13) -0.7(4) ? C(10) C(11) C(12) C(13) -3.5(6) ? C(14) C(15) C(16) C(17) -175.9(4) ? C(14) C(15) C(20) C(19) 176.6(3) ? C(15) C(16) C(17) C(18) -2.1(7) ? C(15) C(20) C(19) C(18) 0.4(6) ? C(16) C(15) C(20) C(19) -1.5(5) ? C(16) C(17) C(18) C(19) 1.1(7) ? C(17) C(16) C(15) C(20) 2.3(6) ? C(17) C(18) C(19) C(20) -0.2(7) ? O(35) C(31) C(32) C(33) 56.5(2) yes O(35) C(35) C(34) C(33) -57.7(2) yes C(31) O(35) C(35) C(34) 60.1(2) yes C(31) C(32) C(33) C(34) -56.6(2) yes C(32) C(31) O(35) C(35) -59.5(2) yes C(32) C(33) C(34) C(35) 57.3(2) yes O(1) C(31) O(35) C(35) 60.4(2) yes O(1) C(31) C(32) O(32) 54.2(2) yes O(1) C(31) C(32) C(33) -65.2(2) yes O(32) C(32) C(33) O(33) 65.6(2) yes O(32) C(32) C(33) C(34) -175.6(2) yes O(32) C(37) C(38) C(39) -26.1(3) yes O(33) C(33) C(34) O(34) -68.7(2) yes O(33) C(33) C(34) C(35) 175.0(2) yes O(33) C(44) C(45) C(46) 169.9(2) yes O(34) C(34) C(35) O(35) -176.0(2) yes O(34) C(34) C(35) C(36) 67.6(3) yes O(35) C(31) O(1) C(1) 81.3(2) yes C(32) C(31) O(1) C(1) -157.7(2) yes C(31) O(35) C(35) C(36) -179.6(2) yes C(31) C(32) O(32) C(37) 126.7(2) yes C(32) O(32) C(37) C(38) -178.1(2) yes C(32) C(33) O(33) C(44) -114.3(2) yes C(33) O(33) C(44) C(45) 176.2(2) yes C(34) O(34) S(3) C(51) 119.2(2) yes S(3) O(34) C(34) C(33) 96.2(2) yes S(3) O(34) C(34) C(35) -145.7(2) yes S(4) C(36) C(35) O(35) 82.0(2) yes S(4) C(36) C(35) C(34) -159.6(2) yes O(32) C(32) C(31) O(35) 176.0(2) ? O(32) C(37) C(38) C(43) 155.9(2) ? O(33) C(33) C(32) C(31) -175.3(2) ? O(33) C(44) C(45) C(50) -11.1(3) ? O(34) C(34) C(33) C(32) 173.7(2) ? O(37) C(37) O(32) C(32) 2.9(4) ? O(37) C(37) C(38) C(39) 152.9(3) ? O(37) C(37) C(38) C(43) -25.0(4) ? O(38) S(3) O(34) C(34) -127.3(2) ? O(39) S(3) O(34) C(34) 3.8(2) ? O(44) C(44) O(33) C(33) -4.9(4) ? O(44) C(44) C(45) C(46) -9.0(4) ? O(44) C(44) C(45) C(50) 170.0(3) ? N(2) C(52) S(4) C(36) 144(4) ? C(33) C(32) O(32) C(37) -113.3(2) ? C(33) C(34) C(35) C(36) -174.1(2) ? C(34) C(33) O(33) C(44) 127.7(2) ? C(35) C(36) S(4) C(52) -61.3(2) ? C(37) C(38) C(39) C(40) -176.5(2) ? C(37) C(38) C(43) C(42) 177.7(2) ? C(38) C(39) C(40) C(41) -1.5(4) ? C(38) C(43) C(42) C(41) -0.7(4) ? C(39) C(38) C(43) C(42) -0.4(4) ? C(39) C(40) C(41) C(42) 0.4(5) ? C(40) C(39) C(38) C(43) 1.4(4) ? C(40) C(41) C(42) C(43) 0.7(5) ? C(44) C(45) C(46) C(47) 178.8(2) ? C(44) C(45) C(50) C(49) -179.7(3) ? C(45) C(46) C(47) C(48) 0.8(4) ? C(45) C(50) C(49) C(48) 1.1(4) ? C(46) C(45) C(50) C(49) -0.7(4) ? C(46) C(47) C(48) C(49) -0.5(4) ? C(47) C(46) C(45) C(50) -0.3(4) ? C(47) C(48) C(49) C(50) -0.5(5) ?