#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/21/2102137.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_2102137 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 13.466(4) _cell_length_b 13.691(4) _cell_length_c 7.053(2) _cell_measurement_temperature 180.0(2) _cell_volume 1300.3(7) _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 .0773 _diffrn_reflns_av_sigmaI/netI .0563 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 7637 _diffrn_reflns_theta_max 29.72 _diffrn_reflns_theta_min 2.12 _exptl_absorpt_coefficient_mu .093 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.289 _exptl_crystal_description plate _exptl_crystal_F_000 544 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _refine_diff_density_max .660 _refine_diff_density_min -.295 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.148 _refine_ls_goodness_of_fit_obs 1.220 _refine_ls_matrix_type full _refine_ls_number_parameters 117 _refine_ls_number_reflns 1712 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.148 _refine_ls_restrained_S_obs 1.220 _refine_ls_R_factor_all .1421 _refine_ls_R_factor_obs .0923 _refine_ls_shift/esd_max .007 _refine_ls_shift/esd_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .2777 _refine_ls_wR_factor_obs .2356 _reflns_number_observed 1088 _reflns_number_total 1712 _reflns_observed_criterion >2sigma(I) _cod_data_source_file hr0044.cif _cod_data_source_block 180 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.1519P)^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^)+(0.1519P)^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_original_sg_symbol_H-M 'P ccn' _cod_database_code 2102137 _cod_database_fobs_code 2102137 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 .0263(10) .0326(11) .0665(14) .0017(7) -.0011(8) -.0016(8) O2 .0361(11) .0329(11) .078(2) -.0010(8) -.0051(9) .0006(9) C1 .0236(11) .0334(14) .0453(14) .0022(9) -.0023(10) .0010(10) C2 .0252(12) .0315(14) .048(2) .0025(9) -.0051(10) -.0024(10) C7 .0238(13) .042(2) .085(3) -.0038(11) .0018(14) -.002(2) C3 .0292(13) .0337(14) .046(2) .0017(10) -.0035(10) -.0021(10) C4 .0292(14) .0381(15) .066(2) .0066(10) .0021(13) -.0010(14) C5 .0203(12) .043(2) .058(2) .0020(10) .0025(11) .0003(13) C6 .0233(12) .0362(14) .055(2) -.0022(10) -.0026(11) .0013(12) 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_occupancy _atom_site_type_symbol O1 .56745(13) .45111(14) .2322(3) .0418(6) Uani d 1 O H1 .528(3) .378(3) .232(5) .075(14) Uiso d 1 H O2 .52617(15) .78690(15) .2775(3) .0489(7) Uani d 1 O C1 .5088(2) .5297(2) .2461(3) .0341(6) Uani d 1 C C2 .5514(2) .6194(2) .2484(4) .0349(7) Uani d 1 C C7 .6615(2) .6352(3) .2258(6) .0503(9) Uani d 1 C H7A .678(3) .683(3) .109(6) .090(8) Uiso d 1 H H7B .686(3) .583(4) .195(6) .090(8) Uiso d 1 H H7C .684(3) .665(3) .330(6) .090(8) Uiso d 1 H C3 .4900(2) .7042(2) .2776(4) .0362(7) Uani d 1 C C4 .3796(2) .6895(2) .3176(5) .0443(8) Uani d 1 C H4A .347(2) .754(3) .283(4) .056(6) Uiso d 1 H H4B .377(2) .679(2) .463(5) .056(6) Uiso d 1 H C5 .3383(2) .6008(2) .2154(4) .0405(7) Uani d 1 C H5A .339(2) .612(2) .070(4) .047(6) Uiso d 1 H H5B .265(3) .586(3) .258(4) .047(6) Uiso d 1 H C6 .3984(2) .5109(2) .2609(4) .0383(7) Uani d 1 C H6A .385(3) .486(3) .404(5) .063(7) Uiso d 1 H H6B .381(3) .456(3) .173(5) .063(7) 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 116(2) O1 C1 C2 118.7(2) O1 C1 C6 116.6(2) C2 C1 C6 124.7(2) C1 C2 C3 119.3(2) C1 C2 C7 123.0(3) C3 C2 C7 117.7(2) C2 C7 H7A 112(2) C2 C7 H7B 108(3) H7A C7 H7B 104(4) C2 C7 H7C 108(3) H7A C7 H7C 107(4) H7B C7 H7C 119(4) O2 C3 C2 120.9(2) O2 C3 C4 120.4(2) C2 C3 C4 118.7(2) C5 C4 C3 112.0(2) C5 C4 H4A 115.1(19) C3 C4 H4A 105.3(19) C5 C4 H4B 109.9(17) C3 C4 H4B 103.9(17) H4A C4 H4B 110(2) C6 C5 C4 110.8(2) C6 C5 H5A 109.3(15) C4 C5 H5A 110.4(15) C6 C5 H5B 106.3(19) C4 C5 H5B 111.6(17) H5A C5 H5B 108(2) C5 C6 C1 111.9(2) C5 C6 H6A 111.4(18) C1 C6 H6A 106.7(18) C5 C6 H6B 111(2) C1 C6 H6B 108(2) H6A C6 H6B 108(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.338(3) O1 H1 1.13(4) O2 C3 1.233(3) C1 C2 1.355(4) C1 C6 1.513(4) C2 C3 1.440(3) C2 C7 1.507(4) C7 H7A 1.07(4) C7 H7B .82(5) C7 H7C .89(4) C3 C4 1.525(4) C4 C5 1.518(4) C4 H4A 1.02(4) C4 H4B 1.03(3) C5 C6 1.508(4) C5 H5A 1.04(3) C5 H5B 1.05(4) C6 H6A 1.08(3) C6 H6B 1.00(4) 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 -175.4(2) C6 C1 C2 C3 3.7(4) O1 C1 C2 C7 3.3(4) C6 C1 C2 C7 -177.6(3) C1 C2 C3 O2 -178.8(2) C7 C2 C3 O2 2.4(4) C1 C2 C3 C4 3.9(4) C7 C2 C3 C4 -174.9(3) O2 C3 C4 C5 149.6(3) C2 C3 C4 C5 -33.1(4) C3 C4 C5 C6 54.0(3) C4 C5 C6 C1 -46.5(3) O1 C1 C6 C5 -162.3(2) C2 C1 C6 C5 18.5(4)