#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000348.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_4000348 _publ_section_title ; E,E-2,5-Bis[2-hydroxyethoxy]-1,4- bis[2-(3,4,5-trimethoxyphenyl)ethoxy]benzene ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm034708z _journal_year 2004 _chemical_formula_sum 'C34 H44 O11 S' _chemical_formula_weight 660.75 _chemical_melting_point 246.0(10) _chemical_name_common ; E,E-2,5-Bis[2-hydroxyethoxy]-1,4- bis[2-(3,4,5-trimethoxyphenyl)ethoxy]benzene ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.3582(16) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.3009(2) _cell_length_b 24.0823(10) _cell_length_c 13.0444(6) _cell_measurement_reflns_used 1577 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 21.97 _cell_measurement_theta_min 4.08 _cell_volume 1665.19(12) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2995 _diffrn_reflns_theta_max 22.01 _diffrn_reflns_theta_min 4.14 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_T_max 0.9845 _exptl_absorpt_correction_T_min 0.8913 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 1967 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.181 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0498 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.7319P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.1183 _reflns_number_gt 1697 _reflns_number_total 1967 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_chemical_melting_point' value '245-247' was changed to '246.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 4000348 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.8261(4) 0.31660(9) 0.22414(16) 0.0410(6) Uani 1 1 d . . . O2 O 0.4780(4) 0.31350(9) 0.07123(16) 0.0355(6) Uani 1 1 d . . . O3 O 0.1906(4) 0.22536(9) 0.04052(15) 0.0355(6) Uani 1 1 d . . . O4 O 0.8087(4) 0.01382(9) 0.66949(15) 0.0359(6) Uani 1 1 d . . . O5 O 1.0438(5) 0.06607(11) 0.84963(17) 0.0561(7) Uani 1 1 d . . . H5 H 1.0313 0.0401 0.8899 0.084 Uiso 1 1 calc R . . C1 C 0.7060(6) 0.22378(13) 0.2797(2) 0.0320(8) Uani 1 1 d . . . H1 H 0.8239 0.2243 0.3327 0.038 Uiso 1 1 calc R . . C2 C 0.6862(6) 0.26891(13) 0.2151(2) 0.0310(8) Uani 1 1 d . . . C3 C 0.5111(5) 0.26847(12) 0.1345(2) 0.0282(7) Uani 1 1 d . . . C4 C 0.3565(5) 0.22207(13) 0.1217(2) 0.0289(7) Uani 1 1 d . . . C5 C 0.3738(5) 0.17709(13) 0.1871(2) 0.0287(7) Uani 1 1 d . . . H5 H 0.2675 0.1467 0.1784 0.034 Uiso 1 1 calc R . . C6 C 0.5526(5) 0.17757(13) 0.2667(2) 0.0303(8) Uani 1 1 d . . . C7 C 0.5843(6) 0.13134(14) 0.3388(2) 0.0347(8) Uani 1 1 d . . . H7 H 0.7093 0.1360 0.3884 0.042 Uiso 1 1 calc R . . C8 C 0.4585(6) 0.08379(13) 0.3428(2) 0.0298(8) Uani 1 1 d . . . H8 H 0.3435 0.0770 0.2901 0.036 Uiso 1 1 calc R . . C9 C 0.4833(5) 0.04100(12) 0.4220(2) 0.0266(7) Uani 1 1 d . . . C10 C 0.6406(5) 0.04777(13) 0.5083(2) 0.0299(8) Uani 1 1 d . . . H10 H 0.7358 0.0800 0.5146 0.036 Uiso 1 1 calc R . . C11 C 0.6576(5) 0.00810(13) 0.5838(2) 0.0288(8) Uani 1 1 d . . . C12 C 1.0003(6) 0.05559(13) 0.6674(2) 0.0323(8) Uani 1 1 d . . . H12A H 0.9243 0.0922 0.6691 0.039 Uiso 1 1 calc R . . H12B H 1.0983 0.0524 0.6051 0.039 Uiso 1 1 calc R . . C13 C 1.1655(6) 0.04752(15) 0.7586(2) 0.0401(9) Uani 1 1 d . . . H13A H 1.2075 0.0085 0.7653 0.048 Uiso 1 1 calc R . . H13B H 1.3213 0.0680 0.7494 0.048 Uiso 1 1 calc R . . C14 C 1.0172(6) 0.31769(15) 0.3019(2) 0.0420(9) Uani 1 1 d . . . H14A H 1.1017 0.3529 0.3007 0.063 Uiso 1 1 calc R . . H14B H 1.1369 0.2886 0.2894 0.063 Uiso 1 1 calc R . . H14C H 0.9413 0.3123 0.3677 0.063 Uiso 1 1 calc R . . C15 C 0.6852(6) 0.32392(15) 0.0034(3) 0.0430(9) Uani 1 1 d . . . H15A H 0.6479 0.3557 -0.0383 0.065 Uiso 1 1 calc R . . H15B H 0.7108 0.2921 -0.0398 0.065 Uiso 1 1 calc R . . H15C H 0.8353 0.3308 0.0429 0.065 Uiso 1 1 calc R . . C16 C 0.0258(6) 0.17954(14) 0.0235(2) 0.0412(9) Uani 1 1 d . . . H16A H -0.0796 0.1869 -0.0350 0.062 Uiso 1 1 calc R . . H16B H -0.0776 0.1741 0.0828 0.062 Uiso 1 1 calc R . . H16C H 0.1237 0.1467 0.0113 0.062 Uiso 1 1 calc R . . S1 S 0.4726(4) -0.00274(12) 1.04717(15) 0.0550(6) Uani 0.50 1 d P . . O1S O 0.2010(9) 0.0113(3) 1.0227(4) 0.0718(18) Uani 0.50 1 d P . . C1S C 0.6346(15) 0.0593(4) 1.0472(7) 0.067(2) Uani 0.50 1 d P . . H1S1 H 0.5838 0.0812 1.1050 0.100 Uiso 0.50 1 calc PR . . H1S2 H 0.5978 0.0792 0.9850 0.100 Uiso 0.50 1 calc PR . . H1S3 H 0.8125 0.0521 1.0514 0.100 Uiso 0.50 1 calc PR . . C2S C 0.610(2) -0.0337(4) 0.9316(7) 0.066(3) Uani 0.50 1 d P . . H2S1 H 0.5387 -0.0698 0.9204 0.100 Uiso 0.50 1 calc PR . . H2S2 H 0.7896 -0.0370 0.9405 0.100 Uiso 0.50 1 calc PR . . H2S3 H 0.5746 -0.0104 0.8735 0.100 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0485(14) 0.0337(14) 0.0408(13) 0.0052(11) -0.0096(11) -0.0124(11) O2 0.0399(13) 0.0290(13) 0.0376(13) 0.0111(10) 0.0032(10) 0.0006(10) O3 0.0393(12) 0.0349(14) 0.0321(12) 0.0051(10) -0.0097(10) -0.0026(11) O4 0.0415(13) 0.0371(14) 0.0289(12) 0.0089(10) -0.0104(10) -0.0101(11) O5 0.0772(18) 0.0595(18) 0.0317(14) -0.0041(12) -0.0001(13) 0.0052(15) C1 0.0367(18) 0.033(2) 0.0265(17) 0.0041(15) -0.0026(13) -0.0060(16) C2 0.0347(18) 0.0258(18) 0.0325(18) -0.0018(15) 0.0032(14) -0.0046(15) C3 0.0345(17) 0.0248(18) 0.0254(16) 0.0029(15) 0.0036(14) 0.0033(15) C4 0.0315(17) 0.0320(19) 0.0231(16) 0.0020(15) 0.0016(14) 0.0042(15) C5 0.0311(17) 0.0261(19) 0.0289(17) 0.0021(14) 0.0005(13) -0.0036(14) C6 0.0333(17) 0.034(2) 0.0240(17) 0.0050(15) 0.0009(14) -0.0004(15) C7 0.0359(18) 0.040(2) 0.0280(18) 0.0068(16) -0.0061(14) -0.0025(16) C8 0.0370(18) 0.0294(19) 0.0231(17) -0.0003(14) -0.0016(13) 0.0014(15) C9 0.0294(17) 0.0278(18) 0.0226(17) 0.0016(14) 0.0021(13) 0.0009(14) C10 0.0344(18) 0.0267(19) 0.0287(18) 0.0026(15) 0.0000(14) -0.0033(14) C11 0.0303(17) 0.035(2) 0.0214(17) 0.0018(15) -0.0007(14) 0.0027(15) C12 0.0377(19) 0.0306(19) 0.0285(18) 0.0000(14) -0.0007(14) -0.0039(15) C13 0.046(2) 0.041(2) 0.0325(19) -0.0014(16) -0.0046(16) -0.0037(17) C14 0.0401(19) 0.045(2) 0.041(2) -0.0044(17) -0.0040(16) -0.0099(17) C15 0.045(2) 0.047(2) 0.0373(19) 0.0135(17) 0.0029(16) -0.0040(17) C16 0.042(2) 0.044(2) 0.038(2) -0.0021(17) -0.0106(15) -0.0032(17) S1 0.0383(11) 0.0875(19) 0.0390(10) 0.0153(12) -0.0057(9) 0.0040(12) O1S 0.037(3) 0.130(6) 0.049(3) 0.027(3) 0.002(2) 0.009(3) C1S 0.056(5) 0.070(6) 0.075(6) -0.017(5) 0.011(4) 0.021(5) C2S 0.078(7) 0.037(5) 0.084(7) -0.019(5) 0.002(6) 0.025(5)