#------------------------------------------------------------------------------ #$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/59/2105936.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_2105936 loop_ _publ_author_name 'Jahangiri, Amita' 'Fleckhaus, Andre' 'Lidin, Sven' 'Strand, Daniel' _publ_section_title ; Allotwinning in a molecular crystal: (1R,3S)-dimethyl 2-oxocyclohexane-1,3-dicarboxylate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 509 _journal_page_last 513 _journal_paper_doi 10.1107/S2052519213018605 _journal_volume 69 _journal_year 2013 _chemical_formula_sum 'C10 H14 O5' _chemical_formula_weight 214.2 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall Xmc21 _symmetry_space_group_name_H-M Xmc21 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 37.8883 _cell_length_b 4.7233 _cell_length_c 11.6835 _cell_measurement_reflns_used 5939 _cell_measurement_temperature 293 _cell_measurement_theta_max 29.22 _cell_measurement_theta_min 2.69 _cell_volume 2090.854 _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET) (compiled Jan 27 2011,13:34:29) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET) (compiled Jan 27 2011,13:34:29) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET) (compiled Jan 27 2011,13:34:29) ; _computing_structure_refinement ; Petricek, V., Dusek, M. & Palatinus, L. (2006). Jana2006. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. ; _computing_structure_solution 'Palatinus L., Chapuis G. (2007). J. Appl. Cryst. 40, 786-790' _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 16.1829 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 31649 _diffrn_reflns_theta_full 28.81 _diffrn_reflns_theta_max 29.23 _diffrn_reflns_theta_min 3.23 _exptl_absorpt_coefficient_mu 0.11 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET) (compiled Jan 27 2011,13:34:29) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.3606 _exptl_crystal_description cube _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _refine_diff_density_max 0.16 _refine_diff_density_min -0.12 _refine_ls_abs_structure_details ' 3002 of Friedel pairs used in the refinement' _refine_ls_extinction_coef 81E2(7) _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_ref 1.34 _refine_ls_hydrogen_treatment constr _refine_ls_number_constraints 120 _refine_ls_number_parameters 281 _refine_ls_number_reflns 7281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0497 _refine_ls_shift/su_max 0.0421 _refine_ls_shift/su_mean 0.0046 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/(\s^2^(I)+0.0016I^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.1229 _refine_ls_wR_factor_ref 0.1450 _reflns_number_gt 3986 _reflns_number_total 7281 _reflns_threshold_expression I>3\s(I) _cod_data_source_file dk5017.cif _cod_data_source_block Phase_II _cod_database_code 2105936 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,z 3 x,-y,z+1/2 4 -x,-y,z+1/2 5 x+1/2,y,z 6 -x+1/2,y,z 7 x+1/2,-y,z+1/2 8 -x+1/2,-y,z+1/2 loop_ _atom_site_type_symbol _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_occupancy C C1-2_1 -0.1033(3) -0.0196(13) 0.818(3) 0.070(4) Uani d 1 C C1-2_2 0.1451(3) 0.4871(12) 1.562(3) 0.078(4) Uani d 1 O O1-2_1 -0.07522(6) 0.1618(6) 0.774(3) 0.0363(11) Uani d 1 O O1-2_2 0.17446(8) 0.3180(6) 1.523(3) 0.0432(11) Uani d 1 C C2-2_1 -0.06536(10) 0.1036(10) 0.668(3) 0.0256(13) Uani d 1 C C2-2_2 0.18476(11) 0.3747(10) 1.414(3) 0.0306(15) Uani d 1 O O2-2_1 -0.07768(12) -0.0813(10) 0.611(3) 0.0491(15) Uani d 1 O O2-2_2 0.17179(16) 0.5564(11) 1.357(3) 0.0578(17) Uani d 1 C C3-2_1 -0.03404(8) 0.2859(7) 0.631(3) 0.0226(11) Uani d 1 C C3-2_2 0.21646(9) 0.1961(7) 1.379(3) 0.0251(12) Uani d 1 C C4-2_1 0 0.1331(13) 0.671(3) 0.0180(16) Uani d 1 C C4-2_2 0.25 0.3457(12) 1.417(3) 0.0232(17) Uani d 1 O O3-2_1 0 -0.0778(11) 0.726(3) 0.0291(15) Uani d 1 O O3-2_2 0.25 0.5617(11) 1.470(3) 0.0331(16) Uani d 1 C C5-2_1 -0.03323(10) 0.3396(8) 0.502(3) 0.0267(12) Uani d 1 C C5-2_2 0.21710(10) 0.1505(8) 1.249(3) 0.0325(13) Uani d 1 C C6-2_1 0 0.4923(10) 0.464(3) 0.027(3) Uani d 1 C C6-2_2 0.25 -0.0079(12) 1.212(3) 0.038(4) Uani d 1 H H1c1-2_1 -0.095366 -0.212697 0.818709 0.0838 Uiso d 1 H H2c1-2_1 -0.109257 0.037768 0.894352 0.0838 Uiso d 1 H H3c1-2_1 -0.123696 -0.003354 0.769713 0.0838 Uiso d 1 H H1c1-2_2 0.129257 0.370329 1.605571 0.094 Uiso d 1 H H2c1-2_2 0.153743 0.637664 1.609787 0.094 Uiso d 1 H H3c1-2_2 0.132863 0.565514 1.497679 0.094 Uiso d 1 H H1c3-2_1 -0.036051 0.469391 0.665924 0.0271 Uiso d 1 H H1c3-2_2 0.214823 0.013452 1.414308 0.0301 Uiso d 1 H H1c5-2_1 -0.035114 0.162647 0.461877 0.0321 Uiso d 1 H H2c5-2_1 -0.053547 0.44848 0.480065 0.0321 Uiso d 1 H H1c5-2_2 0.19657 0.045406 1.226384 0.039 Uiso d 1 H H2c5-2_2 0.216275 0.330476 1.211001 0.039 Uiso d 1 H H1c6-2_1 0 0.681188 0.494109 0.0326 Uiso d 1 H H2c6-2_1 0 0.510037 0.381888 0.0326 Uiso d 1 H H1c6-2_2 0.25 -0.029698 1.130796 0.0461 Uiso d 1 H H2c6-2_2 0.25 -0.193055 1.246399 0.0461 Uiso d 1 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 _atom_site_aniso_type_symbol C1-2_1 0.033(5) 0.097(7) 0.079(6) -0.010(3) 0.025(5) 0.015(3) C C1-2_2 0.039(6) 0.095(7) 0.101(8) 0.008(3) 0.034(5) -0.022(3) C O1-2_1 0.0190(14) 0.051(2) 0.039(2) -0.0044(13) 0.0063(13) -0.0039(14) O O1-2_2 0.0375(17) 0.052(2) 0.0397(19) 0.0045(14) 0.0084(14) 0.0106(15) O C2-2_1 0.0145(19) 0.034(3) 0.028(2) -0.0027(16) -0.0039(17) 0.001(2) C C2-2_2 0.033(2) 0.032(3) 0.027(2) -0.0019(18) -0.0052(18) 0.0000(19) C O2-2_1 0.035(2) 0.054(2) 0.059(3) -0.014(2) 0.005(2) -0.011(3) O O2-2_2 0.060(3) 0.059(2) 0.054(3) 0.019(3) 0.002(2) 0.022(3) O C3-2_1 0.0126(16) 0.0245(19) 0.031(2) 0.0063(13) 0.0005(16) 0.0022(15) C C3-2_2 0.030(2) 0.021(2) 0.024(2) -0.0017(15) -0.0016(16) -0.0020(14) C C4-2_1 0.012(2) 0.031(3) 0.011(3) 0 0 -0.008(2) C C4-2_2 0.035(3) 0.020(3) 0.014(3) 0 0 0.005(2) C O3-2_1 0.028(2) 0.022(2) 0.037(3) 0 0 0.010(3) O O3-2_2 0.050(3) 0.018(2) 0.032(3) 0 0 0.001(3) O C5-2_1 0.0177(18) 0.034(2) 0.028(2) 0.0063(15) -0.0058(15) 0.0018(16) C C5-2_2 0.039(2) 0.031(2) 0.027(2) -0.0067(17) -0.0066(19) -0.0025(16) C C6-2_1 0.025(6) 0.038(6) 0.019(5) 0 0 0.0054(19) C C6-2_2 0.059(9) 0.038(7) 0.017(5) 0 0 -0.008(2) C loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1-2_1 O1-2_1 1.46(2) C1-2_1 H1c1-2_1 0.96 C1-2_1 H2c1-2_1 0.96 C1-2_1 H3c1-2_1 0.96 C1-2_2 O1-2_2 1.45(2) C1-2_2 H1c1-2_2 0.96 C1-2_2 H2c1-2_2 0.96 C1-2_2 H3c1-2_2 0.96 O1-2_1 C2-2_1 1.32(5) O1-2_2 C2-2_2 1.35(5) C2-2_1 O2-2_1 1.19(3) C2-2_1 C3-2_1 1.527(17) C2-2_2 O2-2_2 1.20(3) C2-2_2 C3-2_2 1.524(16) C3-2_1 C4-2_1 1.550(17) C3-2_1 C5-2_1 1.53(6) C3-2_1 H1c3-2_1 0.96 C3-2_2 C4-2_2 1.522(17) C3-2_2 C5-2_2 1.53(6) C3-2_2 H1c3-2_2 0.96 C4-2_1 O3-2_1 1.18(3) C4-2_2 O3-2_2 1.19(3) C5-2_1 C6-2_1 1.517(17) C5-2_1 H1c5-2_1 0.96 C5-2_1 H2c5-2_1 0.96 C5-2_2 C6-2_2 1.515(17) C5-2_2 H1c5-2_2 0.96 C5-2_2 H2c5-2_2 0.96 C6-2_1 H1c6-2_1 0.96 C6-2_1 H2c6-2_1 0.96 C6-2_2 H1c6-2_2 0.96 C6-2_2 H2c6-2_2 0.96 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C1-2_2 H3c1-2_2 O2-2_2 0.96 2.21 2.63(5) 104.81