#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2009056.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_2009056 loop_ _publ_author_name 'Foxon, S. P.' 'Semlyen, J. A.' 'Wood, B. R.' _publ_section_title ; A cyclic dimer of ethyleneglycol maleate ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900115 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C12 H12 O8' _chemical_formula_structural '[CH2CH2O.CO.CHCH.CO.O]2' _chemical_formula_sum 'C12 H12 O8' _chemical_formula_weight 284.22 _chemical_name_systematic ; ENTER SYSTEMATIC NAME ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.929(3) _cell_length_b 8.895(2) _cell_length_c 14.482(4) _cell_measurement_reflns_used 19 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 6.4 _cell_measurement_theta_min 4.6 _cell_volume 1279.0(6) _computing_cell_refinement 'MSC/AFC6S Diffractometer Control Software' _computing_data_collection 'MSC/AFC-6S Diffractometer Control Software (MSC, 1992a)' _computing_data_reduction 'TEXSAN (MSC, 1992b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 1127 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.05 _diffrn_standards_decay_% 0.11 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.175 _refine_diff_density_min -0.179 _refine_ls_extinction_coef 0.021(3) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1127 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0361 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.1215P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1085 _reflns_number_gt 854 _reflns_number_total 1127 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qa0166.cif _[local]_cod_data_source_block QA0166 _cod_database_code 2009056 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2-y,1/2+z '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' 1/2+x,1/2+y,1/2-z '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 0.44670(13) -0.03168(14) 0.62584(9) 0.0348(4) Uani d . 1 O O2 0.63888(12) 0.10046(15) 0.60779(8) 0.0309(4) Uani d . 1 O O3 0.25295(12) 0.16158(15) 0.72149(8) 0.0323(4) Uani d . 1 O O4 0.11998(13) 0.09292(15) 0.60202(9) 0.0362(4) Uani d . 1 O C1 0.71508(19) -0.0141(2) 0.65669(14) 0.0356(5) Uani d . 1 C H1A 0.7583 -0.0812 0.6130 0.043 Uiso calc R 1 H H1B 0.6556 -0.0729 0.6956 0.043 Uiso calc R 1 H C2 0.50478(18) 0.0808(2) 0.60149(11) 0.0250(4) Uani d . 1 C C3 0.44016(18) 0.2151(2) 0.56003(12) 0.0280(4) Uani d . 1 C H3 0.4913 0.2785 0.5229 0.034 Uiso calc R 1 H C4 0.31079(18) 0.2475(2) 0.57447(11) 0.0282(4) Uani d . 1 C H4 0.2765 0.3332 0.5462 0.034 Uiso calc R 1 H C5 0.21725(17) 0.1577(2) 0.63198(12) 0.0262(4) Uani d . 1 C C6 0.18116(18) 0.0638(2) 0.78561(13) 0.0361(5) Uani d . 1 C H6A 0.1278 -0.0092 0.7520 0.043 Uiso calc R 1 H H6B 0.1214 0.1226 0.8244 0.043 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0315(7) 0.0281(7) 0.0448(8) 0.0000(6) -0.0024(6) -0.0008(6) O2 0.0231(7) 0.0414(8) 0.0283(7) 0.0040(6) -0.0020(5) -0.0001(6) O3 0.0260(6) 0.0453(9) 0.0255(6) -0.0007(6) -0.0006(5) -0.0062(6) O4 0.0300(8) 0.0394(8) 0.0391(8) 0.0012(6) -0.0101(6) -0.0018(6) C1 0.0309(10) 0.0412(11) 0.0347(10) -0.0033(9) -0.0039(8) 0.0104(9) C2 0.0251(9) 0.0298(9) 0.0201(9) -0.0053(7) 0.0014(7) 0.0007(8) C3 0.0313(9) 0.0301(10) 0.0225(9) 0.0013(7) -0.0005(7) -0.0002(8) C4 0.0332(9) 0.0276(9) 0.0238(9) 0.0004(7) -0.0060(7) 0.0055(8) C5 0.0227(9) 0.0267(9) 0.0292(9) -0.0032(7) -0.0036(7) 0.0089(8) C6 0.0222(9) 0.0547(12) 0.0316(10) 0.0017(9) 0.0032(8) -0.0082(9) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -1 2 0 1 2 0 4 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O2 C1 . 117.19(14) yes C5 O3 C6 . 118.04(14) ? O2 C1 C6 4_656 107.82(16) yes O1 C2 O2 . 124.08(16) yes O1 C2 C3 . 125.39(17) yes O2 C2 C3 . 110.53(15) ? C4 C3 C2 . 121.83(17) yes C3 C4 C5 . 125.19(16) yes O4 C5 O3 . 124.78(17) ? O4 C5 C4 . 123.89(16) ? O3 C5 C4 . 111.30(14) ? O3 C6 C1 4_656 107.16(14) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 . 1.207(2) yes O2 C2 . 1.346(2) yes O2 C1 . 1.453(2) yes O3 C5 . 1.344(2) no O3 C6 . 1.458(2) no O4 C5 . 1.206(2) no C1 C6 4_656 1.496(3) no C2 C3 . 1.483(2) yes C3 C4 . 1.333(3) yes C4 C5 . 1.481(3) no C6 C1 4_656 1.497(3) yes 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_site_symmetry_4 _geom_torsion C2 O2 C1 C6 4_656 -139.00(15) C1 O2 C2 O1 . -7.4(2) C1 O2 C2 C3 . 173.11(14) O1 C2 C3 C4 . 24.0(3) O2 C2 C3 C4 . -156.51(16) C2 C3 C4 C5 . 0.3(3) C6 O3 C5 O4 . 9.2(2) C6 O3 C5 C4 . -172.48(15) C3 C4 C5 O4 . -115.4(2) C3 C4 C5 O3 . 66.2(2) C5 O3 C6 C1 4_656 132.47(16)