#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/21/2102135.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_2102135 loop_ _publ_author_name 'Katrusiak, A.' _publ_section_title ; Conformational transformation coupled with the order--disorder phase transition in 2-methyl-1,3-cyclohexanedione crystals ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 872 _journal_page_last 881 _journal_paper_doi 10.1107/S0108768100005905 _journal_volume 56 _journal_year 2000 _chemical_formula_sum 'C7 H10 O2' _chemical_formula_weight 126.15 _chemical_name_common 2-methyl-1,3-cyclohexanedione _chemical_name_systematic ; ? ; _space_group_IT_number 56 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.427(3) _cell_length_b 13.689(3) _cell_length_c 6.946(2) _cell_measurement_temperature 123.0(3) _cell_volume 1276.7(5) _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device KUMA-4-CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0547 _diffrn_reflns_av_sigmaI/netI .0231 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 6596 _diffrn_reflns_theta_max 29.72 _diffrn_reflns_theta_min 2.98 _exptl_absorpt_coefficient_mu .095 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.313 _exptl_crystal_description plate _exptl_crystal_F_000 544 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _refine_diff_density_max .437 _refine_diff_density_min -.311 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_obs 1.127 _refine_ls_matrix_type full _refine_ls_number_parameters 117 _refine_ls_number_reflns 1616 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.104 _refine_ls_restrained_S_obs 1.127 _refine_ls_R_factor_all .0673 _refine_ls_R_factor_obs .0531 _refine_ls_shift/esd_max -.014 _refine_ls_shift/esd_mean .002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .1565 _refine_ls_wR_factor_obs .1439 _reflns_number_observed 1322 _reflns_number_total 1616 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file hr0044.cif _[local]_cod_data_source_block 123 _[local]_cod_cif_authors_sg_H-M 'P ccn' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2102135 _cod_database_fobs_code 2102135 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' 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 .0196(5) .0104(5) .0313(7) .0016(3) .0001(4) -.0018(3) O2 .0272(5) .0104(5) .0367(7) -.0005(3) -.0032(4) -.0010(4) C1 .0189(6) .0118(6) .0156(7) .0010(4) -.0012(4) .0006(4) C2 .0171(6) .0112(6) .0212(7) .0003(4) -.0021(4) .0005(4) C7 .0179(6) .0170(7) .0411(9) -.0027(4) -.0009(5) -.0008(5) C3 .0211(6) .0117(6) .0196(8) .0002(4) -.0028(5) -.0003(4) C4 .0211(6) .0153(6) .0250(8) .0034(4) .0030(5) -.0017(5) C5 .0169(6) .0166(6) .0249(8) .0018(4) -.0005(5) -.0002(5) C6 .0164(6) .0129(6) .0249(8) -.0019(4) -.0004(4) .0009(5) 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O1 .56748(7) .45070(6) .23059(14) .0204(3) Uani d . 1 O H1 .5274(18) .3894(17) .229(3) .046(7) Uiso d . 1 H O2 .52702(8) .78702(7) .2790(2) .0248(3) Uani d . 1 O C1 .50884(10) .52910(9) .2458(2) .0155(3) Uani d . 1 C C2 .55143(10) .61931(9) .2478(2) .0165(3) Uani d . 1 C C7 .66143(10) .63485(10) .2226(2) .0253(4) Uani d . 1 C H7A .67266(10) .6811(6) .1210(10) .033 Uiso calc R 1 H H7B .69266(15) .5739(2) .1905(15) .033 Uiso calc R 1 H H7C .6893(2) .6595(7) .3403(5) .033 Uiso calc R 1 H C3 .48991(10) .70373(9) .2796(2) .0175(3) Uani d . 1 C C4 .37998(9) .68976(9) .3210(2) .0205(3) Uani d . 1 C H4A .3435(13) .7508(13) .289(2) .025 Uiso d . 1 H H4B .3761(11) .6800(10) .459(3) .025 Uiso d . 1 H C5 .33758(9) .60178(9) .2154(2) .0195(3) Uani d . 1 C H5A .2630(15) .5867(13) .254(2) .023 Uiso d . 1 H H5B .3401(11) .6117(11) .079(2) .023 Uiso d . 1 H C6 .39853(10) .51077(9) .2618(2) .0181(3) Uani d . 1 C H6A .3857(11) .4891(11) .397(2) .022 Uiso d . 1 H H6B .3817(12) .4569(12) .179(3) .022 Uiso d . 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 O1 H1 111.1(13) O1 C1 C2 118.84(12) O1 C1 C6 116.85(11) C2 C1 C6 124.30(12) C1 C2 C3 119.31(12) C1 C2 C7 122.71(12) C3 C2 C7 117.96(11) C2 C7 H7A 109.47(7) C2 C7 H7B 109.47(7) H7A C7 H7B 109.5 C2 C7 H7C 109.47(7) H7A C7 H7C 109.5 H7B C7 H7C 109.5 O2 C3 C2 120.40(12) O2 C3 C4 120.41(11) C2 C3 C4 119.16(10) C3 C4 C5 111.90(11) C3 C4 H4A 109.4(10) C5 C4 H4A 112.0(10) C3 C4 H4B 104.9(9) C5 C4 H4B 110.3(9) H4A C4 H4B 108.0(13) C4 C5 C6 110.11(11) C4 C5 H5A 112.8(9) C6 C5 H5A 107.2(10) C4 C5 H5B 110.6(9) C6 C5 H5B 107.8(9) H5A C5 H5B 108.1(12) C1 C6 C5 112.08(10) C1 C6 H6A 106.7(9) C5 C6 H6A 110.4(9) C1 C6 H6B 108.3(10) C5 C6 H6B 111.9(10) H6A C6 H6B 107.2(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.3353(15) O1 H1 1.00(2) O2 C3 1.2443(15) C1 C2 1.361(2) C1 C6 1.506(2) C2 C3 1.438(2) C2 C7 1.502(2) C7 H7A .96 C7 H7B .96 C7 H7C .96 C3 C4 1.516(2) C4 C5 1.521(2) C4 H4A .99(2) C4 H4B .97(2) C5 C6 1.525(2) C5 H5A 1.06(2) C5 H5B .96(2) C6 H6A 1.00(2) C6 H6B .96(2) 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 O1 C1 C2 C3 -175.04(11) C6 C1 C2 C3 4.3(2) O1 C1 C2 C7 3.5(2) C6 C1 C2 C7 -177.20(11) C1 C2 C3 O2 -178.86(11) C7 C2 C3 O2 2.6(2) C1 C2 C3 C4 3.3(2) C7 C2 C3 C4 -175.28(12) O2 C3 C4 C5 148.88(13) C2 C3 C4 C5 -33.3(2) C3 C4 C5 C6 54.4(2) O1 C1 C6 C5 -162.03(12) C2 C1 C6 C5 18.6(2) C4 C5 C6 C1 -47.0(2)