#------------------------------------------------------------------------------ #$Date: 2013-12-28 14:58:47 +0100 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100344.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_2100344 loop_ _publ_author_name 'Hao, Xiang' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; The unusual phases of anhydrous and hydrated pinacol ; _journal_coeditor_code WS5034 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 689 _journal_page_last 699 _journal_volume 61 _journal_year 2005 _chemical_formula_moiety 'C6 H14 O2, 0.5(H2 O)' _chemical_formula_sum 'C6 H15 O2.5' _chemical_formula_weight 127.18 _chemical_melting_point 301.0(10) _chemical_name_common 'pinacol hemihydrate' _chemical_name_systematic ; 2,3-dimethyl-2,3-butanediol hemihydrate ; _space_group_IT_number 179 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 65 2 (0 0 1)' _symmetry_space_group_name_H-M 'P 65 2 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 12 _cell_length_a 14.696(2) _cell_length_b 14.696(2) _cell_length_c 13.686(3) _cell_measurement_reflns_used 3031 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 1.02 _cell_volume 2559.8(7) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4442 _diffrn_reflns_theta_full 22.48 _diffrn_reflns_theta_max 22.48 _diffrn_reflns_theta_min 2.19 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 0.9926 _exptl_absorpt_correction_T_min 0.9635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.250 _refine_diff_density_min -0.157 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 95 _refine_ls_number_reflns 1121 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0715 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1531P)^2^+0.2175P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1948 _refine_ls_wR_factor_ref 0.2144 _reflns_number_gt 836 _reflns_number_total 1121 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ws5034.cif _[local]_cod_data_source_block k01235 _[local]_cod_cif_authors_sg_H-M P6(5)22 _[local]_cod_chemical_formula_sum_orig 'C6 H15 O2.50' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' 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 '300-302' was changed to '301.0(10)' - the average value was taken and precision was estimated. 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 '300-302' was changed to '301.0(10)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2100344 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' 'y, x, -z+2/3' 'x-y, -y, -z' '-x, -x+y, -z+1/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 0.7636(3) 0.2018(3) 0.9135(3) 0.0750(12) Uani d . 1 . . C C2 0.8251(5) 0.1428(4) 0.9278(4) 0.1050(18) Uani d . 1 . . C H2A 0.8197 0.1207 0.9961 0.158 Uiso calc R 1 . . H H2B 0.8991 0.1894 0.9110 0.158 Uiso calc R 1 . . H H2C 0.7955 0.0808 0.8853 0.158 Uiso calc R 1 . . H C3 0.6445(4) 0.1272(4) 0.9263(4) 0.1070(18) Uani d . 1 . . C H3A 0.6081 0.1676 0.9227 0.161 Uiso calc R 1 . . H H3B 0.6311 0.0924 0.9900 0.161 Uiso calc R 1 . . H H3C 0.6187 0.0742 0.8744 0.161 Uiso calc R 1 . . H C4 0.7889(3) 0.2588(3) 0.8147(2) 0.0726(12) Uani d . 1 . . C C5 0.9050(3) 0.3387(4) 0.8069(4) 0.0887(14) Uani d . 1 . . C H5A 0.9264 0.3862 0.8633 0.133 Uiso calc R 1 . . H H5B 0.9181 0.3794 0.7467 0.133 Uiso calc R 1 . . H H5C 0.9455 0.3023 0.8059 0.133 Uiso calc R 1 . . H C6 0.7521(4) 0.1832(4) 0.7280(3) 0.0944(16) Uani d . 1 . . C H6A 0.7708 0.2233 0.6669 0.142 Uiso calc R 1 . . H H6B 0.6757 0.1372 0.7313 0.142 Uiso calc R 1 . . H H6C 0.7861 0.1404 0.7302 0.142 Uiso calc R 1 . . H O1 0.7982(2) 0.2787(2) 0.98827(17) 0.0755(9) Uani d D 1 . . O H1OA 0.780(7) 0.325(6) 0.974(7) 0.120 Uiso d PD 0.50 . . H H1OB 0.749(6) 0.236(6) 1.028(6) 0.120 Uiso d PD 0.50 . . H O2 0.7290(3) 0.3116(2) 0.8107(2) 0.0873(11) Uani d D 1 . . O H2OA 0.744(9) 0.374(5) 0.830(6) 0.120 Uiso d PD 0.50 . . H H2OB 0.693(7) 0.302(7) 0.758(5) 0.120 Uiso d PD 0.50 . . H O1W 1.045(4) 0.0225(18) 0.9167 0.63(3) Uani d S 1 . . O 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 C1 0.107(3) 0.077(3) 0.050(2) 0.053(3) -0.005(2) 0.000(2) C2 0.166(5) 0.119(4) 0.074(3) 0.104(4) 0.007(3) 0.011(3) C3 0.100(4) 0.084(3) 0.109(4) 0.025(3) 0.028(3) 0.017(3) C4 0.099(3) 0.082(3) 0.047(2) 0.054(2) -0.008(2) -0.0049(19) C5 0.077(3) 0.091(3) 0.084(3) 0.032(3) 0.009(2) 0.013(3) C6 0.132(4) 0.102(3) 0.056(3) 0.063(3) -0.018(2) -0.021(2) O1 0.094(2) 0.096(2) 0.0406(14) 0.0503(18) -0.0018(13) -0.0054(13) O2 0.119(3) 0.100(2) 0.0673(19) 0.073(2) -0.0138(16) 0.0029(15) O1W 0.81(5) 0.46(2) 0.72(7) 0.41(3) 0.000 -0.23(4) 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 C1 O1 . 1.417(5) no C1 C4 . 1.535(5) no C1 C3 . 1.541(7) no C1 C2 . 1.547(6) no C2 H2A . 0.9800 no C2 H2B . 0.9800 no C2 H2C . 0.9800 no C3 H3A . 0.9800 no C3 H3B . 0.9800 no C3 H3C . 0.9800 no C4 O2 . 1.437(5) no C4 C5 . 1.515(6) no C4 C6 . 1.527(5) no C5 H5A . 0.9800 no C5 H5B . 0.9800 no C5 H5C . 0.9800 no C6 H6A . 0.9800 no C6 H6B . 0.9800 no C6 H6C . 0.9800 no O1 H1OA . 0.87(5) no O1 H1OB . 0.87(5) no O2 H2OA . 0.87(5) no O2 H2OB . 0.87(5) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' O O 0.0106 0.0060 '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 _geom_angle_publ_flag O1 C1 C4 108.0(3) no O1 C1 C3 108.2(4) no C4 C1 C3 111.6(4) no O1 C1 C2 106.1(3) no C4 C1 C2 111.5(4) no C3 C1 C2 111.2(4) no C1 C2 H2A 109.5 no C1 C2 H2B 109.5 no H2A C2 H2B 109.5 no C1 C2 H2C 109.5 no H2A C2 H2C 109.5 no H2B C2 H2C 109.5 no C1 C3 H3A 109.5 no C1 C3 H3B 109.5 no H3A C3 H3B 109.5 no C1 C3 H3C 109.5 no H3A C3 H3C 109.5 no H3B C3 H3C 109.5 no O2 C4 C5 109.6(3) no O2 C4 C6 105.9(3) no C5 C4 C6 111.2(4) no O2 C4 C1 106.3(3) no C5 C4 C1 110.9(3) no C6 C4 C1 112.7(3) no C4 C5 H5A 109.5 no C4 C5 H5B 109.5 no H5A C5 H5B 109.5 no C4 C5 H5C 109.5 no H5A C5 H5C 109.5 no H5B C5 H5C 109.5 no C4 C6 H6A 109.5 no C4 C6 H6B 109.5 no H6A C6 H6B 109.5 no C4 C6 H6C 109.5 no H6A C6 H6C 109.5 no H6B C6 H6C 109.5 no C1 O1 H1OA 109(7) no C1 O1 H1OB 92(6) no H1OA O1 H1OB 104(7) no C4 O2 H2OA 131(7) no C4 O2 H2OB 115(6) no H2OA O2 H2OB 105(7) no 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 O1 C1 C4 O2 -62.8(4) no C3 C1 C4 O2 56.0(4) no C2 C1 C4 O2 -179.1(4) no O1 C1 C4 C5 56.2(4) no C3 C1 C4 C5 175.0(4) no C2 C1 C4 C5 -60.0(4) no O1 C1 C4 C6 -178.4(4) no C3 C1 C4 C6 -59.6(5) no C2 C1 C4 C6 65.4(5) no _cod_database_fobs_code 2100344 _journal_paper_doi 10.1107/S0108768105031356