#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/38/2103817.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_2103817 loop_ _publ_author_name 'Small, Ronald W. H.' _publ_section_title ; An X-ray diffraction study of partially ordered electron density in clathrates of Dianin's compound that include simple carboxylic acids ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 141 _journal_page_last 148 _journal_paper_doi 10.1107/S0108768102022395 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety '6(C18 H20 O2),(C7 H14 O2)' _chemical_formula_structural 'C18 H20 O2, 1/6(C7 H14 O2)' _chemical_formula_sum 'C115 H134 O14' _chemical_formula_weight 1740.3 _chemical_name_common 'Dianins compound-butyric acid' _chemical_name_systematic ; [4-p-hydroxyphenyl-2,2,4-trimethylchroman]-heptanoic acid ; _space_group_IT_number 148 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 27.30(2) _cell_length_b 27.30(2) _cell_length_c 11.070(10) _cell_measurement_reflns_used 15 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 5 _cell_volume 7145(10) _computing_cell_refinement local _computing_data_collection 'Stoe STADI-2' _computing_data_reduction SMALL _computing_molecular_graphics SNOOPI _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement SHELX76 _computing_structure_solution MULTAN87 _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Stoe STADI-2 two circle diffractometer' _diffrn_measurement_method ; variable \w scan 2\q'fixed, where the angle \q' is the projection of \q on the equatorial plane ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4458 _diffrn_reflns_reduction_process ; ? ; _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% 'maximum 5% corrected by interpolation' _diffrn_standards_interval_count 20 _diffrn_standards_number 'one per layer' _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description 'acicular,hexagonal prism' _exptl_crystal_F_000 2808 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.45 _refine_diff_density_min -0.27 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.28 _refine_ls_hydrogen_treatment ' see text ' _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 215 _refine_ls_number_reflns 1350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.071 _refine_ls_R_factor_gt 0.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.00 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ' w = 1/[\s^2^(F) + 0.00012F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.058 _refine_ls_wR_factor_ref 0.058 _reflns_number_gt 1350 _reflns_number_total 1626 _reflns_threshold_expression refl_obs_if_F_>_6.0_sigma(F) _cod_data_source_file bm0059.cif _cod_data_source_block DIE _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. '_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 2103817 loop_ _symmetry_equiv_pos_as_xyz x,y,z -y,x-y,z -x+y,-x,z -x,-y,-z y,-x+y,-z x-y,x,-z 1/3+x,2/3+y,2/3+z 1/3-y,2/3+x-y,2/3+z 1/3-x+y,2/3-x,2/3+z 1/3-x,2/3-y,2/3-z 1/3+y,2/3-x+y,2/3-z 1/3+x-y,2/3+x,2/3-z 2/3+x,1/3+y,1/3+z 2/3-y,1/3+x-y,1/3+z 2/3-x+y,1/3-x,1/3+z 2/3-x,1/3-y,1/3-z 2/3+y,1/3-x+y,1/3-z 2/3+x-y,1/3+x,1/3-z 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 0.076(3) 0.085(3) 0.0615(19) 0.030(2) -0.018(2) -0.0116(19) O2 0.051(2) 0.044(2) 0.0561(15) 0.0201(17) 0.0072(15) -0.0067(15) C1 0.050(4) 0.059(3) 0.042(2) 0.017(3) -0.001(3) 0.000(2) C2 0.060(4) 0.039(3) 0.056(3) 0.012(3) 0.001(3) -0.011(3) C3 0.054(3) 0.043(3) 0.054(2) 0.021(3) 0.002(2) -0.001(2) C4 0.040(3) 0.033(3) 0.0387(19) 0.014(2) 0.006(2) -0.004(2) C5 0.047(3) 0.046(3) 0.046(2) 0.022(3) -0.002(2) -0.002(2) C6 0.053(3) 0.049(3) 0.051(2) 0.022(3) -0.001(3) 0.001(2) C7 0.038(3) 0.032(3) 0.045(2) 0.019(2) 0.005(2) 0.003(2) C8 0.041(3) 0.037(3) 0.052(2) 0.023(2) 0.001(2) -0.001(2) C9 0.038(3) 0.034(3) 0.047(2) 0.014(3) -0.001(2) 0.000(2) C10 0.038(3) 0.043(3) 0.046(2) 0.021(2) -0.001(2) 0.003(2) C11 0.038(3) 0.037(3) 0.043(2) 0.019(2) -0.005(2) -0.001(2) C12 0.045(3) 0.040(3) 0.050(2) 0.015(3) -0.002(2) 0.001(2) C13 0.052(3) 0.038(3) 0.065(3) 0.015(3) -0.006(3) 0.004(3) C14 0.049(3) 0.034(3) 0.082(3) 0.019(3) -0.019(3) -0.007(3) C15 0.049(3) 0.039(3) 0.065(3) 0.025(3) -0.007(2) -0.010(3) C16 0.043(3) 0.067(3) 0.065(3) 0.030(3) -0.001(3) -0.004(3) C17 0.065(4) 0.064(4) 0.055(2) 0.031(3) 0.016(3) 0.013(3) C18 0.053(3) 0.053(3) 0.066(3) 0.033(3) 0.011(2) 0.000(3) loop_ _atom_site_label _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_occupancy _atom_site_type_symbol O1 0.12390(10) 0.0571(3) 0.0187(3) 0.0787(15) Uani 1.000 O O2 0.26330(10) 0.1754(2) 0.6261(2) 0.0520(11) Uani 1.000 O C1 0.1650(2) 0.0747(4) 0.1108(4) 0.0549(18) Uani 1.000 C C2 0.1784(2) 0.0370(4) 0.1649(4) 0.0573(19) Uani 1.000 C C3 0.2183(2) 0.0557(4) 0.2581(3) 0.0518(16) Uani 1.000 C C4 0.2453(2) 0.1119(4) 0.2984(3) 0.0391(15) Uani 1.000 C C5 0.2308(2) 0.1482(4) 0.2397(3) 0.0469(16) Uani 1.000 C C6 0.1911(2) 0.1302(4) 0.1467(3) 0.0526(16) Uani 1.000 C C7 0.2884(2) 0.1305(4) 0.4032(3) 0.0377(16) Uani 1.000 C C8 0.2613(2) 0.0964(4) 0.5196(3) 0.0418(16) Uani 1.000 C C9 0.2270(2) 0.1158(4) 0.5926(3) 0.0414(16) Uani 1.000 C C10 0.2996(2) 0.2117(4) 0.5389(3) 0.0420(16) Uani 1.000 C C11 0.3135(2) 0.1937(4) 0.4332(3) 0.0392(16) Uani 1.000 C C12 0.3531(2) 0.2356(4) 0.3563(3) 0.0478(16) Uani 1.000 C C13 0.3770(2) 0.2928(4) 0.3818(4) 0.0550(17) Uani 1.000 C C14 0.3620(2) 0.3096(4) 0.4870(4) 0.0558(17) Uani 1.000 C C15 0.3236(2) 0.2691(4) 0.5657(4) 0.0497(17) Uani 1.000 C C16 0.1752(2) 0.1107(4) 0.5286(4) 0.0572(17) Uani 1.000 C C17 0.2101(2) 0.0842(4) 0.7141(4) 0.062(2) Uani 1.000 C C18 0.3365(2) 0.1189(4) 0.3683(4) 0.0544(17) Uani 1.000 C O3 0.00060 -0.01600 0.09610 0.1631 Uiso 0.167 O O4 0.04100 0.06690 0.18970 0.1883 Uiso 0.167 O C20 0.00890 0.01310 0.19230 0.1115 Uiso 0.167 C C21 0.00650 -0.01510 0.31440 0.2211 Uiso 0.167 C C22 0.01630 0.02680 0.41730 0.1254 Uiso 0.167 C C23 0.01750 -0.00010 0.53870 0.1049 Uiso 0.167 C C24 0.02050 0.03890 0.64250 0.1059 Uiso 0.167 C C25 0.02840 0.01540 0.76290 0.1235 Uiso 0.167 C C26 -0.02280 -0.04390 0.78410 0.2679 Uiso 0.167 C H1 0.128(3) 0.023(5) 0.021(6) 0.14(3) Uiso 1.000 H H2 0.1581(2) -0.0065(4) 0.1353(4) 0.090(15) Uiso 1.000 H H3 0.2285(2) 0.0262(4) 0.3000(3) 0.059(12) Uiso 1.000 H H4 0.2509(2) 0.1920(4) 0.2680(3) 0.072(13) Uiso 1.000 H H5 0.1817(2) 0.1599(4) 0.1027(3) 0.080(14) Uiso 1.000 H H6 0.2338(2) 0.0527(4) 0.4946(3) 0.048(11) Uiso 1.000 H H7 0.2949(2) 0.0996(4) 0.5766(3) 0.042(10) Uiso 1.000 H H8 0.3655(2) 0.2231(4) 0.2745(3) 0.055(11) Uiso 1.000 H H9 0.4066(2) 0.3240(4) 0.3196(4) 0.057(11) Uiso 1.000 H H10 0.3805(2) 0.3540(4) 0.5082(4) 0.072(13) Uiso 1.000 H H11 0.3119(2) 0.2820(4) 0.6479(4) 0.049(10) Uiso 1.000 H H12 0.1475(2) 0.0672(4) 0.5030(4) 0.095(17) Uiso 1.000 H H13 0.1530(2) 0.1241(4) 0.5888(4) 0.093(15) Uiso 1.000 H H14 0.1882(2) 0.1369(4) 0.4488(4) 0.116(18) Uiso 1.000 H H15 0.1829(2) 0.0396(4) 0.6981(4) 0.085(15) Uiso 1.000 H H16 0.2476(2) 0.0911(4) 0.7614(4) 0.110(19) Uiso 1.000 H H17 0.1879(2) 0.0999(4) 0.7681(4) 0.078(14) Uiso 1.000 H H18 0.3568(2) 0.1419(4) 0.2869(4) 0.068(12) Uiso 1.000 H H19 0.3672(2) 0.1325(4) 0.4405(4) 0.073(13) Uiso 1.000 H H20 0.3189(2) 0.0741(4) 0.3529(4) 0.091(16) Uiso 1.000 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 l 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 C9 O2 C10 117.6(3) no C2 C1 C6 120.7(5) no O1 C1 C6 118.1(6) yes O1 C1 C2 121.2(6) yes C1 C2 C3 119.6(6) no C2 C3 C4 121.4(6) no C5 C4 C7 123.7(6) no C3 C4 C7 119.7(6) no C3 C4 C5 116.6(5) no C4 C5 C6 122.6(6) no C1 C6 C5 119.1(6) no C8 C7 C11 107.8(4) no C11 C7 C18 109.6(6) no C4 C7 C11 111.6(5) no C8 C7 C18 106.6(5) no C4 C7 C8 111.8(5) no C4 C7 C18 109.3(4) no C7 C8 C9 115.3(5) no C8 C9 C17 109.5(5) no C16 C9 C17 110.5(5) no O2 C9 C17 104.3(4) no C8 C9 C16 115.2(4) no O2 C9 C16 107.5(5) no O2 C9 C8 109.2(5) no O2 C10 C15 115.0(4) no O2 C10 C11 123.9(6) no C11 C10 C15 121.1(5) no C10 C11 C12 117.2(6) no C7 C11 C10 121.9(5) no C7 C11 C12 120.8(4) no C11 C12 C13 122.1(5) no C12 C13 C14 119.5(6) no C13 C14 C15 119.7(6) no C10 C15 C14 120.4(5) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 1.411(7) no O2 C9 1.468(8) no O2 C10 1.383(6) no C1 C2 1.389(9) no C1 C6 1.372(10) no C2 C3 1.398(8) no C3 C4 1.402(10) no C4 C5 1.398(9) no C4 C7 1.546(7) no C5 C6 1.394(8) no C7 C18 1.546(10) no C7 C11 1.541(10) no C7 C8 1.545(7) no C8 C9 1.519(9) no C9 C17 1.539(7) no C9 C16 1.525(9) no C10 C11 1.393(7) no C10 C15 1.395(10) no C11 C12 1.402(9) no C12 C13 1.387(10) no C13 C14 1.386(8) no C14 C15 1.386(9) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O1 2.961(8) 5_555 yes O1 O1 2.961(7) 6_555 yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O1 5_555 0.99(10) 2.28(9) 2.961(8) 125(7) 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 _geom_torsion_publ_flag C10 O2 C9 C8 42.3(6) no C10 O2 C9 C16 -83.3(5) no C10 O2 C9 C17 159.3(5) no C9 O2 C10 C11 -15.6(8) no C9 O2 C10 C15 166.4(5) no O1 C1 C2 C3 -178.3(5) no C2 C1 C6 C5 -0.9(9) no C6 C1 C2 C3 0.9(9) no O1 C1 C6 C5 178.4(5) no C1 C2 C3 C4 -0.1(9) no C2 C3 C4 C5 -0.8(8) no C2 C3 C4 C7 179.0(5) no C3 C4 C5 C6 0.8(8) no C3 C4 C7 C11 179.6(5) no C3 C4 C7 C18 58.2(7) no C5 C4 C7 C8 120.2(6) no C5 C4 C7 C11 -0.6(8) no C5 C4 C7 C18 -122.0(6) no C3 C4 C7 C8 -59.5(7) no C7 C4 C5 C6 -178.9(5) no C4 C5 C6 C1 0.0(9) no C4 C7 C8 C9 -80.0(7) no C4 C7 C11 C10 108.8(6) no C4 C7 C11 C12 -73.5(7) no C8 C7 C11 C10 -14.4(8) no C8 C7 C11 C12 163.3(6) no C18 C7 C11 C10 -130.0(6) no C11 C7 C8 C9 43.0(7) no C18 C7 C8 C9 160.6(5) no C18 C7 C11 C12 47.7(6) no C7 C8 C9 C17 -171.7(5) no C7 C8 C9 C16 63.0(8) no C7 C8 C9 O2 -58.0(6) no O2 C10 C11 C7 0.9(9) no C15 C10 C11 C12 0.9(9) no O2 C10 C11 C12 -176.9(5) no C15 C10 C11 C7 178.7(6) no C11 C10 C15 C14 0.0(10) no O2 C10 C15 C14 178.0(5) no C10 C11 C12 C13 -1.3(9) no C7 C11 C12 C13 -179.1(6) no C11 C12 C13 C14 0.6(10) no C12 C13 C14 C15 0.4(9) no C13 C14 C15 C10 -0.7(10) no