#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003363.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_2003363 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 758 _journal_page_last 759 _publ_section_title ; p-Chlorophenyl 3,4,6-Tri-O-benzyl-2-deoxy-2-methylene-\b-D-glucopyranoside ; _chemical_formula_moiety 'C34 H33 Cl O5' _chemical_formula_sum 'C34 H33 Cl O5' _chemical_formula_structural 'C34 H33 Cl O5' _chemical_formula_weight 558.093 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 8.236(3) _cell_length_b 14.967(4) _cell_length_c 24.032(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2962(1) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_meas 1.25(2) _exptl_crystal_density_method flotation _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 1.4 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _chemical_compound_source ;recrystallized from a mixture of chloroform and ethanol ; _diffrn_measurement_device 'Enraf Nonius diffractometer' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2538 _reflns_number_total 2538 _reflns_number_observed 2214 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 60 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <3 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.042 _refine_ls_wR_factor_obs 0.047 _refine_ls_wR_factor_all 0.085 _refine_ls_goodness_of_fit_obs 0.62 _refine_ls_goodness_of_fit_all 0.65 _refine_ls_number_reflns 1548 _refine_ls_number_parameters 361 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme '1/[\s^2^(F)+0.009(F)^2^]' _refine_ls_shift/esd_max 0.113 _refine_diff_density_max 0.18 _refine_diff_density_min -0.17 _refine_ls_extinction_method none _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 ? 'SHELXS86 (Sheldrick, 1985)' ? ? O ? 'SHELXS86 (Sheldrick, 1985)' ? ? Cl ? 'SHELXS86 (Sheldrick, 1985)' ? ? H ? 'SHELXS86 (Sheldrick, 1985)' ? ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cl 0.1544(3) 0.2906(1) 0.9885(1) 0.109(1) O1 0.3531(5) 0.7406(2) 0.9660(1) 0.058(2) O2 0.3093(6) 0.7285(3) 0.8489(1) 0.079(3) O3 0.3344(5) 0.6593(3) 1.0454(1) 0.067(2) O4 0.2687(5) 0.9776(3) 1.0469(1) 0.072(2) O5 0.2428(5) 0.9662(2) 0.9254(1) 0.064(2) C1 0.2655(7) 0.7331(4) 1.0169(2) 0.058(3) C2 0.2866(7) 0.8164(4) 1.0498(2) 0.062(3) C3 0.2341(7) 0.8980(4) 1.0181(2) 0.060(3) C4 0.3122(7) 0.8997(4) 0.9604(2) 0.059(3) C5 0.2880(6) 0.8113(3) 0.9320(2) 0.053(3) C6 0.3733(8) 0.8036(4) 0.8769(2) 0.061(3) C7 0.4147(8) 0.6887(4) 0.8102(2) 0.070(4) C8 0.3332(8) 0.6070(4) 0.7858(2) 0.058(3) C9 0.3783(9) 0.5775(4) 0.7340(2) 0.081(4) C10 0.3079(12) 0.5008(6) 0.7116(3) 0.098(5) C11 0.1987(12) 0.4550(5) 0.7400(3) 0.099(5) C12 0.1537(12) 0.4822(5) 0.7911(3) 0.103(6) C13 0.2186(9) 0.5578(4) 0.8148(2) 0.077(4) C14 0.2927(7) 0.5745(4) 1.0283(2) 0.059(3) C15 0.2171(8) 0.5549(4) 0.9785(2) 0.065(3) C16 0.1769(8) 0.4680(4) 0.9663(2) 0.069(4) C17 0.2155(8) 0.4011(4) 1.0025(2) 0.076(4) C18 0.2975(10) 0.4202(5) 1.0518(3) 0.091(5) C19 0.3340(8) 0.5074(5) 1.0636(2) 0.078(4) C20 0.3489(9) 0.8195(5) 1.1015(2) 0.091(5) C21 0.1348(8) 1.0160(5) 1.0762(2) 0.077(4) C22 0.1986(7) 1.0756(4) 1.1204(2) 0.062(3) C23 0.1587(10) 1.0599(4) 1.1756(2) 0.082(4) C24 0.2198(12) 1.1161(5) 1.2160(2) 0.098(5) C25 0.3134(9) 1.1867(5) 1.2040(3) 0.079(4) C26 0.3545(10) 1.2030(4) 1.1500(3) 0.086(5) C27 0.2986(10) 1.1480(4) 1.1088(2) 0.079(4) C28 0.3165(11) 1.0506(5) 0.9274(2) 0.095(5) C29 0.2799(9) 1.1044(4) 0.8758(2) 0.069(4) C30 0.3445(10) 1.1887(4) 0.8714(3) 0.078(4) C31 0.3156(12) 1.2408(4) 0.8246(4) 0.102(6) C32 0.2216(12) 1.2070(5) 0.7818(4) 0.099(6) C33 0.1592(10) 1.1250(5) 0.7870(3) 0.087(5) C34 0.1829(8) 1.0717(4) 0.8327(2) 0.071(4) H6a 0.497(6) 0.788(3) 0.884(2) 0.022(4) H6b 0.347(6) 0.860(3) 0.851(2) 0.020(4) H1 0.146(5) 0.723(2) 1.008(1) 0.018(3) H4 0.431(6) 0.917(3) 0.966(2) 0.022(4) H3 0.123(5) 0.897(2) 1.012(1) 0.017(3) H15 0.163(7) 0.606(3) 0.954(2) 0.030(5) H19 0.385(6) 0.523(3) 1.096(2) 0.021(4) H21a 0.076(7) 0.957(3) 1.092(2) 0.033(6) H21b 0.062(9) 1.052(4) 1.043(2) 0.043(7) H34 0.161(6) 1.008(3) 0.839(1) 0.020(4) H24 0.198(7) 1.102(4) 1.253(2) 0.035(6) H9 0.453(6) 0.611(3) 0.716(2) 0.017(4) H30 0.408(6) 1.212(3) 0.899(2) 0.026(5) H5 0.183(5) 0.798(2) 0.925(1) 0.013(3) H25 0.345(6) 1.229(3) 1.236(2) 0.025(4) H18 0.315(7) 0.372(3) 1.076(2) 0.027(5) H16 0.128(6) 0.460(3) 0.933(2) 0.025(4) H20b 0.299(6) 0.856(4) 1.136(2) 0.099(5) H20c 0.346(7) 0.749(4) 1.109(2) 0.087(6) H23 0.067(7) 1.009(4) 1.184(2) 0.039(6) H13 0.181(6) 0.581(3) 0.851(2) 0.023(4) H32 0.204(8) 1.253(4) 0.753(2) 0.043(7) H33 0.099(5) 1.101(3) 0.755(2) 0.024(4) H31 0.347(8) 1.297(4) 0.825(2) 0.035(6) H7a 0.428(6) 0.740(3) 0.775(2) 0.025(4) H7b 0.508(7) 0.672(3) 0.839(2) 0.028(5) H10 0.346(6) 0.482(3) 0.677(2) 0.022(4) H11 0.159(7) 0.404(3) 0.726(2) 0.028(5) H12 0.090(6) 0.451(3) 0.813(2) 0.025(5) H28a 0.316(7) 1.083(3) 0.958(2) 0.027(5) H28b 0.457(9) 1.037(4) 0.928(2) 0.044(6) H27 0.317(6) 1.156(3) 1.072(2) 0.021(4) H26 0.421(6) 1.249(3) 1.134(2) 0.021(4) 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 Cl 0.135(2) 0.005(1) -0.003(1) 0.083(1) 0.025(1) 0.108(1) O1 0.042(2) 0.007(2) 0.002(2) 0.081(2) 0.005(2) 0.051(2) O2 0.072(3) -0.029(2) 0.019(2) 0.094(3) -0.013(3) 0.071(2) O3 0.046(2) 0.013(2) -0.011(2) 0.101(3) -0.004(2) 0.056(2) O4 0.041(2) -0.030(2) 0.009(2) 0.101(3) -0.010(2) 0.072(2) O5 0.056(3) 0.000(2) -0.007(2) 0.064(2) -0.010(2) 0.072(2) C1 0.034(3) 0.014(3) -0.002(2) 0.098(4) -0.006(3) 0.042(3) C2 0.033(3) -0.002(3) 0.007(2) 0.106(4) 0.002(3) 0.046(2) C3 0.038(3) -0.014(3) 0.001(3) 0.084(4) -0.009(3) 0.059(3) C4 0.047(4) -0.002(2) -0.003(3) 0.076(3) -0.015(3) 0.054(3) C5 0.041(3) 0.005(2) -0.005(2) 0.070(3) -0.005(3) 0.048(2) C6 0.069(4) -0.005(2) 0.006(3) 0.065(3) -0.010(3) 0.050(3) C7 0.075(5) -0.007(3) -0.002(3) 0.077(4) 0.004(4) 0.057(3) C8 0.051(4) 0.007(3) -0.007(3) 0.065(3) 0.003(3) 0.058(3) C9 0.087(5) 0.000(3) 0.008(4) 0.086(4) -0.011(4) 0.069(4) C10 0.126(7) -0.020(4) -0.002(5) 0.090(5) 0.015(6) 0.077(4) C11 0.134(8) 0.005(4) -0.029(6) 0.060(4) -0.013(5) 0.103(5) C12 0.125(7) 0.020(4) 0.002(5) 0.079(4) -0.033(5) 0.105(5) C13 0.092(5) 0.007(3) 0.004(4) 0.076(4) -0.010(4) 0.063(3) C14 0.033(3) 0.013(3) 0.002(2) 0.091(4) 0.001(3) 0.053(3) C15 0.059(4) 0.015(3) 0.009(3) 0.082(4) 0.011(3) 0.054(3) C16 0.064(4) 0.014(3) -0.001(3) 0.088(4) 0.009(4) 0.054(3) C17 0.060(4) 0.006(3) 0.009(3) 0.098(4) 0.015(4) 0.068(3) C18 0.086(5) 0.034(4) 0.010(4) 0.104(5) 0.032(5) 0.083(4) C19 0.064(5) 0.019(4) -0.003(3) 0.105(5) 0.010(4) 0.065(3) C20 0.062(5) -0.001(4) -0.004(3) 0.156(7) -0.007(5) 0.056(3) C21 0.048(4) -0.027(4) 0.001(3) 0.108(5) 0.012(4) 0.075(3) C22 0.051(4) -0.007(3) 0.004(3) 0.073(3) 0.015(4) 0.063(3) C23 0.085(5) -0.009(3) 0.015(4) 0.083(4) -0.008(4) 0.077(4) C24 0.120(7) -0.009(4) 0.024(4) 0.112(5) -0.009(6) 0.062(3) C25 0.069(5) -0.023(4) -0.007(4) 0.085(4) 0.007(4) 0.085(4) C26 0.082(5) 0.010(4) -0.014(4) 0.067(4) -0.010(4) 0.110(5) C27 0.092(6) 0.014(3) 0.001(4) 0.086(4) 0.001(4) 0.058(3) C28 0.134(8) -0.008(3) -0.023(4) 0.086(4) -0.034(5) 0.067(3) C29 0.072(5) -0.012(3) 0.014(3) 0.073(4) -0.003(4) 0.064(3) C30 0.084(5) -0.012(3) 0.007(4) 0.057(3) -0.005(4) 0.094(4) C31 0.105(7) 0.004(4) 0.041(6) 0.062(4) -0.003(5) 0.138(7) C32 0.102(7) 0.021(4) 0.027(5) 0.075(5) 0.015(5) 0.120(6) C33 0.076(5) 0.006(4) 0.005(4) 0.106(6) 0.009(5) 0.079(4) C34 0.062(4) 0.005(3) -0.001(3) 0.076(4) -0.009(4) 0.074(4)