#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003399.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003399 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 751 _journal_page_last 754 _publ_section_title ; 2,2',3,3'-Tetra-O-benzoyl-6,6'-dideoxy-4,4'-di-O-mesyl-6,6'-dithiocyanato- \a,\a-trehalose Crystal structure of trehalose derivatives, Part 9. For Part 8, see Lee & Linden (1994b). ; _chemical_formula_moiety 'C44 H40 N2 O17 S4' _chemical_formula_sum 'C44 H40 N2 O17 S4' _chemical_formula_weight 997.04 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' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 19.051(3) _cell_length_b 26.274(4) _cell_length_c 9.487(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4749(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14 _cell_measurement_theta_max 19.5 _exptl_absorpt_coefficient_mu 0.261 _cell_measurement_temperature 173(1) _exptl_crystal_description prism _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.33 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _chemical_compound_source 'see text' _diffrn_measurement_device 'Rigaku AFC-5R diffractometer' _diffrn_measurement_method '\w scans' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 14607 _reflns_number_total 11798 _reflns_number_observed 8854 _reflns_observed_criterion 'I > 3\s(I)' _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 30 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% insignificant _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_obs 0.0381 _refine_ls_wR_factor_all 0.0423 _refine_ls_goodness_of_fit_obs 1.376 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 8854 _refine_ls_number_parameters 764 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'sigma w=1/[\s^2^(F~o~)+(0.01F~o~)^2^]' _refine_ls_shift/esd_max 0.0007 _refine_diff_density_max 0.32 _refine_diff_density_min -0.25 _refine_ls_extinction_method 'not applied' _refine_ls_extinction_coef ? 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 _refine_ls_abs_structure_details 'see text' _refine_ls_abs_structure_Flack 0.04(5) ##; ##MSC/AFC Diffractometer Control Software ##(Molecular Structure Corporation, 1991) ##; 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 S(1) 1 0.33688(3) 0.73915(2) 0.16411(7) 0.0294(2) S(2) 1 0.54334(4) 0.85604(2) 0.33745(8) 0.0373(2) S(3) 1 0.81158(3) 0.54648(2) 0.59680(7) 0.0298(2) S(4) 1 0.59571(4) 0.59573(3) 0.97648(8) 0.0423(2) O(1) 1 0.57668(8) 0.69455(6) 0.5567(2) 0.0246(5) O(2) 1 0.47618(8) 0.62476(6) 0.6284(2) 0.0306(5) O(3) 1 0.38741(8) 0.63642(6) 0.3916(2) 0.0308(5) O(4) 1 0.41283(8) 0.72325(6) 0.2209(2) 0.0267(5) O(5) 1 0.49451(8) 0.76076(6) 0.5547(2) 0.0251(5) O(7) 1 0.3875(1) 0.62365(8) 0.7839(3) 0.0595(8) O(8) 1 0.32818(9) 0.79248(7) 0.1866(2) 0.0430(6) O(9) 1 0.28539(9) 0.70647(8) 0.2221(2) 0.0461(7) O(14) 1 0.4642(1) 0.58184(9) 0.2936(4) 0.088(1) O(32) 1 0.68245(8) 0.73502(6) 0.4005(2) 0.0275(5) O(33) 1 0.77891(8) 0.65215(6) 0.4140(2) 0.0269(5) O(34) 1 0.73608(8) 0.57209(6) 0.6119(2) 0.0306(5) O(35) 1 0.64969(8) 0.68590(6) 0.7529(2) 0.0264(5) O(37) 1 0.78190(9) 0.78144(8) 0.4140(2) 0.0508(7) O(38) 1 0.8103(1) 0.51902(8) 0.4682(2) 0.0518(7) O(39) 1 0.86459(8) 0.58373(7) 0.6216(2) 0.0411(6) O(44) 1 0.71971(9) 0.61776(8) 0.2315(2) 0.0453(7) N(1) 1 0.6181(1) 0.8497(1) 0.5940(3) 0.061(1) N(2) 1 0.5276(2) 0.6911(1) 0.9958(4) 0.076(1) C(1) 1 0.5123(1) 0.71265(9) 0.6120(3) 0.0245(7) C(2) 1 0.4555(1) 0.67415(9) 0.5782(3) 0.0266(7) C(3) 1 0.4436(1) 0.67146(9) 0.4203(3) 0.0254(7) C(4) 1 0.4230(1) 0.72440(9) 0.3720(3) 0.0243(7) C(5) 1 0.4832(1) 0.76095(9) 0.4050(3) 0.0234(6) C(6) 1 0.4671(1) 0.8157(1) 0.3640(3) 0.0292(8) C(7) 1 0.4365(1) 0.60294(9) 0.7300(3) 0.0327(8) C(8) 1 0.4624(1) 0.55164(9) 0.7673(3) 0.0333(8) C(9) 1 0.5138(2) 0.5274(1) 0.6890(3) 0.046(1) C(10) 1 0.5403(2) 0.4811(1) 0.7365(5) 0.065(1) C(11) 1 0.5170(2) 0.4600(1) 0.8597(4) 0.062(1) C(12) 1 0.4649(2) 0.4830(1) 0.9340(5) 0.059(1) C(13) 1 0.4380(2) 0.5291(1) 0.8899(4) 0.047(1) C(14) 1 0.4049(2) 0.5931(1) 0.3232(4) 0.0447(9) C(15) 1 0.3420(2) 0.5615(1) 0.2916(3) 0.0427(9) C(16) 1 0.3542(2) 0.5131(1) 0.2391(5) 0.069(1) C(17) 1 0.2968(2) 0.4826(2) 0.1986(5) 0.081(2) C(18) 1 0.2305(2) 0.5003(2) 0.2158(5) 0.069(1) C(19) 1 0.2177(2) 0.5479(1) 0.2700(4) 0.058(1) C(20) 1 0.2743(2) 0.5789(1) 0.3088(4) 0.044(1) C(21) 1 0.3530(2) 0.7270(2) -0.0139(3) 0.048(1) C(22) 1 0.5854(1) 0.8514(1) 0.4931(3) 0.0409(9) C(31) 1 0.6366(1) 0.71354(9) 0.6285(3) 0.0240(7) C(32) 1 0.6994(1) 0.70961(9) 0.5294(3) 0.0245(7) C(33) 1 0.7158(1) 0.65388(9) 0.4983(3) 0.0240(7) C(34) 1 0.7281(1) 0.62647(9) 0.6375(3) 0.0248(7) C(35) 1 0.6631(1) 0.63258(9) 0.7320(3) 0.0261(7) C(36) 1 0.6750(1) 0.6107(1) 0.8783(3) 0.0334(8) C(37) 1 0.7279(1) 0.77133(9) 0.3549(3) 0.0302(7) C(38) 1 0.7024(1) 0.79564(9) 0.2229(3) 0.0289(7) C(39) 1 0.6581(1) 0.7701(1) 0.1307(3) 0.0358(8) C(40) 1 0.6389(2) 0.7933(1) 0.0055(3) 0.046(1) C(41) 1 0.6621(2) 0.8416(1) -0.0261(3) 0.049(1) C(42) 1 0.7050(2) 0.8672(1) 0.0664(4) 0.048(1) C(43) 1 0.7259(1) 0.8443(1) 0.1915(3) 0.0393(9) C(44) 1 0.7731(1) 0.63459(9) 0.2794(3) 0.0280(7) C(45) 1 0.8405(1) 0.63789(9) 0.2009(3) 0.0272(7) C(46) 1 0.8448(1) 0.6138(1) 0.0703(3) 0.0314(8) C(47) 1 0.9056(2) 0.6164(1) -0.0087(3) 0.0383(9) C(48) 1 0.9630(2) 0.6425(1) 0.0433(3) 0.0419(9) C(49) 1 0.9591(2) 0.6661(1) 0.1727(3) 0.0428(9) C(50) 1 0.8977(1) 0.6642(1) 0.2512(3) 0.0328(8) C(51) 1 0.8105(2) 0.5031(1) 0.7368(5) 0.057(1) C(52) 1 0.5582(2) 0.6530(1) 0.9885(3) 0.049(1) H(1) 1 0.514(1) 0.7187(8) 0.714(2) 0.015(6) H(2) 1 0.420(1) 0.6842(8) 0.625(2) 0.018(6) H(3) 1 0.484(1) 0.6604(9) 0.375(3) 0.028(7) H(4) 1 0.382(1) 0.7356(8) 0.417(2) 0.014(5) H(5) 1 0.523(1) 0.7501(8) 0.362(2) 0.022(6) H(9) 1 0.533(1) 0.543(1) 0.601(3) 0.043(8) H(10) 1 0.575(2) 0.466(1) 0.682(4) 0.07(1) H(11) 1 0.535(2) 0.432(1) 0.887(4) 0.09(1) H(12) 1 0.444(2) 0.468(1) 1.016(4) 0.08(1) H(13) 1 0.406(2) 0.546(1) 0.947(3) 0.06(1) H(16) 1 0.401(2) 0.500(1) 0.223(4) 0.09(1) H(17) 1 0.308(2) 0.449(2) 0.165(4) 0.10(1) H(18) 1 0.195(2) 0.480(1) 0.188(4) 0.08(1) H(19) 1 0.171(1) 0.561(1) 0.284(3) 0.044(8) H(20) 1 0.265(2) 0.614(1) 0.341(4) 0.062(9) H(31) 1 0.628(1) 0.7483(8) 0.654(2) 0.017(6) H(32) 1 0.741(1) 0.7244(9) 0.574(3) 0.035(7) H(33) 1 0.677(1) 0.6367(8) 0.443(3) 0.023(6) H(34) 1 0.768(1) 0.6380(9) 0.688(3) 0.025(6) H(35) 1 0.622(1) 0.6162(8) 0.692(2) 0.013(5) H(39) 1 0.644(1) 0.737(1) 0.142(3) 0.038(8) H(40) 1 0.615(1) 0.773(1) -0.059(3) 0.049(9) H(41) 1 0.655(1) 0.856(1) -0.111(3) 0.038(7) H(42) 1 0.719(1) 0.900(1) 0.046(3) 0.036(7) H(43) 1 0.756(2) 0.861(1) 0.247(3) 0.050(9) H(46) 1 0.806(1) 0.5971(8) 0.038(3) 0.024(6) H(47) 1 0.908(1) 0.6028(9) -0.098(3) 0.032(7) H(48) 1 1.010(1) 0.643(1) -0.007(3) 0.043(8) H(49) 1 0.999(2) 0.682(1) 0.202(3) 0.046(8) H(50) 1 0.895(1) 0.6797(9) 0.340(3) 0.032(7) H(61) 1 0.432(1) 0.8324(9) 0.432(3) 0.033(7) H(62) 1 0.447(1) 0.815(1) 0.275(3) 0.049(8) H(211) 1 0.353(2) 0.691(1) -0.023(3) 0.06(1) H(212) 1 0.397(2) 0.742(1) -0.040(4) 0.07(1) H(213) 1 0.308(2) 0.736(1) -0.060(4) 0.07(1) H(361) 1 0.694(1) 0.576(1) 0.873(3) 0.039(7) H(362) 1 0.704(1) 0.6341(9) 0.934(3) 0.031(7) H(511) 1 0.808(2) 0.525(1) 0.828(4) 0.06(1) H(512) 1 0.845(2) 0.486(1) 0.726(4) 0.07(1) H(513) 1 0.775(2) 0.482(1) 0.714(4) 0.07(1) 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(1) 0.0215(3) 0.0011(3) -0.0048(3) 0.0374(3) -0.0003(3) 0.0294(3) S(2) 0.0380(3) -0.0073(3) -0.0013(3) 0.0334(3) 0.0033(3) 0.0406(4) S(3) 0.0309(3) 0.0040(3) 0.0010(3) 0.0252(3) -0.0016(3) 0.0334(3) S(4) 0.0381(4) -0.0073(3) 0.0011(3) 0.0550(4) 0.0104(4) 0.0339(4) O(1) 0.0178(7) 0.0032(6) -0.0010(7) 0.0286(8) -0.0018(7) 0.0274(9) O(2) 0.0265(9) 0.0080(7) 0.0058(8) 0.0283(9) 0.0076(8) 0.037(1) O(3) 0.0239(8) -0.0013(7) -0.0018(8) 0.0275(9) -0.0024(8) 0.041(1) O(4) 0.0211(8) 0.0034(7) -0.0004(7) 0.0366(9) -0.0025(7) 0.0224(8) O(5) 0.0249(8) 0.0054(7) -0.0021(7) 0.0265(8) -0.0017(7) 0.0239(9) O(7) 0.051(1) 0.022(1) 0.030(1) 0.054(1) 0.031(1) 0.074(2) O(8) 0.035(1) 0.0078(8) -0.007(1) 0.039(1) -0.003(1) 0.055(1) O(9) 0.0276(9) -0.0084(9) -0.0051(9) 0.058(1) 0.013(1) 0.053(1) O(14) 0.041(1) -0.006(1) 0.028(2) 0.061(2) -0.058(2) 0.161(3) O(32) 0.0244(8) -0.0014(7) -0.0054(7) 0.0304(8) 0.0063(8) 0.0276(9) O(33) 0.0217(8) -0.0016(7) 0.0005(7) 0.0335(9) -0.0024(8) 0.0254(8) O(34) 0.0244(8) -0.0008(7) 0.0014(8) 0.0224(8) -0.0009(8) 0.045(1) O(35) 0.0260(8) 0.0044(7) -0.0025(7) 0.0290(8) -0.0003(7) 0.0243(9) O(37) 0.032(1) -0.0182(9) -0.015(1) 0.064(1) 0.026(1) 0.056(1) O(38) 0.049(1) 0.012(1) -0.002(1) 0.060(1) -0.022(1) 0.046(1) O(39) 0.0256(8) 0.0036(8) -0.0007(9) 0.034(1) -0.002(1) 0.064(1) O(44) 0.031(1) -0.0117(9) -0.0033(9) 0.068(1) -0.016(1) 0.037(1) N(1) 0.064(2) -0.013(1) -0.029(2) 0.051(2) 0.002(2) 0.068(2) N(2) 0.060(2) 0.009(2) 0.037(2) 0.083(2) 0.003(2) 0.085(2) C(1) 0.024(1) 0.008(1) 0.001(1) 0.028(1) 0.000(1) 0.022(1) C(2) 0.020(1) 0.005(1) 0.005(1) 0.026(1) 0.006(1) 0.033(1) C(3) 0.018(1) 0.0018(9) 0.000(1) 0.027(1) 0.000(1) 0.031(1) C(4) 0.021(1) 0.0026(9) 0.000(1) 0.029(1) -0.002(1) 0.023(1) C(5) 0.020(1) 0.004(1) 0.000(1) 0.029(1) 0.001(1) 0.022(1) C(6) 0.027(1) 0.000(1) -0.005(1) 0.029(1) 0.005(1) 0.032(1) C(7) 0.023(1) 0.001(1) 0.000(1) 0.034(1) 0.006(1) 0.040(1) C(8) 0.030(1) -0.002(1) -0.007(1) 0.025(1) 0.002(1) 0.045(2) C(9) 0.061(2) 0.006(1) -0.004(2) 0.035(1) -0.005(1) 0.043(2) C(10) 0.087(3) 0.022(2) 0.001(2) 0.039(2) -0.010(2) 0.069(3) C(11) 0.082(3) 0.010(2) -0.020(2) 0.031(2) 0.009(2) 0.074(3) C(12) 0.068(2) -0.001(2) -0.003(2) 0.036(2) 0.017(2) 0.074(3) C(13) 0.044(2) 0.001(1) 0.002(2) 0.037(2) 0.018(2) 0.060(2) C(14) 0.042(2) -0.005(1) 0.007(2) 0.033(1) -0.011(1) 0.058(2) C(15) 0.046(2) -0.010(1) 0.005(2) 0.033(1) -0.006(1) 0.049(2) C(16) 0.063(2) -0.012(2) 0.021(2) 0.046(2) -0.025(2) 0.097(3) C(17) 0.081(3) -0.024(2) 0.025(3) 0.049(2) -0.033(2) 0.115(4) C(18) 0.062(2) -0.037(2) 0.007(2) 0.059(2) -0.014(2) 0.087(3) C(19) 0.049(2) -0.017(2) 0.001(2) 0.052(2) 0.001(2) 0.073(2) C(20) 0.044(2) -0.011(1) -0.005(1) 0.036(2) 0.003(1) 0.053(2) C(21) 0.046(2) 0.002(2) -0.009(1) 0.067(2) -0.009(2) 0.030(2) C(22) 0.039(1) -0.003(1) -0.008(1) 0.030(1) -0.005(1) 0.054(2) C(31) 0.023(1) 0.0013(9) -0.003(1) 0.024(1) 0.000(1) 0.025(1) C(32) 0.021(1) -0.001(1) -0.004(1) 0.026(1) 0.000(1) 0.027(1) C(33) 0.018(1) 0.0002(9) 0.000(1) 0.028(1) -0.002(1) 0.026(1) C(34) 0.021(1) 0.0011(9) -0.002(1) 0.021(1) -0.002(1) 0.032(1) C(35) 0.023(1) -0.001(1) -0.003(1) 0.027(1) 0.002(1) 0.028(1) C(36) 0.027(1) 0.003(1) -0.003(1) 0.042(2) 0.007(1) 0.031(1) C(37) 0.022(1) 0.000(1) 0.001(1) 0.036(1) 0.006(1) 0.033(1) C(38) 0.021(1) 0.005(1) 0.004(1) 0.037(1) 0.005(1) 0.030(1) C(39) 0.033(1) 0.007(1) 0.003(1) 0.044(2) 0.001(1) 0.031(1) C(40) 0.049(2) 0.008(2) 0.000(1) 0.059(2) 0.000(2) 0.030(2) C(41) 0.049(2) 0.014(2) 0.004(2) 0.066(2) 0.018(2) 0.033(2) C(42) 0.042(2) 0.005(1) 0.006(2) 0.048(2) 0.020(2) 0.053(2) C(43) 0.029(1) -0.001(1) 0.004(1) 0.045(2) 0.009(1) 0.044(2) C(44) 0.027(1) 0.002(1) -0.004(1) 0.030(1) 0.000(1) 0.027(1) C(45) 0.027(1) 0.006(1) -0.002(1) 0.030(1) 0.003(1) 0.025(1) C(46) 0.029(1) 0.003(1) -0.007(1) 0.038(1) -0.004(1) 0.027(1) C(47) 0.041(1) 0.008(1) -0.001(1) 0.051(2) -0.003(1) 0.023(1) C(48) 0.034(1) 0.001(1) 0.004(1) 0.061(2) 0.001(1) 0.031(1) C(49) 0.032(1) -0.010(1) 0.000(1) 0.058(2) -0.005(2) 0.038(2) C(50) 0.032(1) -0.005(1) 0.002(1) 0.041(1) -0.003(1) 0.025(1) C(51) 0.065(2) 0.016(2) 0.008(2) 0.044(2) 0.020(2) 0.063(2) C(52) 0.037(2) -0.008(2) 0.011(1) 0.067(2) -0.001(2) 0.044(2) _cod_database_code 2003399