#------------------------------------------------------------------------------ #$Date: 2012-02-03 18:16:24 +0100 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100342.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_2100342 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, H2 O' _chemical_formula_sum 'C6 H16 O3' _chemical_formula_weight 136.19 _chemical_melting_point 314.4 _chemical_name_common 'pinacol monohydrate' _chemical_name_systematic ; 2,3-dimethyl-2,3-butanediol monohydrate ; _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yac' _symmetry_space_group_name_H-M 'P 1 2/n 1' _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 92.13(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.582(2) _cell_length_b 7.3637(15) _cell_length_c 10.587(2) _cell_measurement_reflns_used 5559 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.02 _cell_volume 824.4(3) _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 'SHELXD (Sheldrick, 2002)' _diffrn_ambient_temperature 90.0(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.098 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2125 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.67 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 304 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.200 _refine_diff_density_min -0.234 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 97 _refine_ls_number_reflns 2125 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0528 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.1650P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.1226 _reflns_number_gt 1666 _reflns_number_total 2125 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file ws5034.cif _[local]_cod_data_source_block k03227p _[local]_cod_cif_authors_sg_H-M 'P 2/n' _cod_database_code 2100342 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' 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 0.0141(3) 0.0722(3) 0.4515(3) 0.0301(7) Uani d . 1 . . C C2 0.1380(4) 0.0329(3) 0.3833(3) 0.0383(9) Uani d . 1 . . C H2A 0.1489 0.1233 0.3166 0.057 Uiso calc R 1 . . H H2B 0.1338 -0.0887 0.3458 0.057 Uiso calc R 1 . . H H2C 0.2098 0.0393 0.4443 0.057 Uiso calc R 1 . . H C3 -0.0955(3) 0.0956(4) 0.3546(3) 0.0442(8) Uani d . 1 . . C H3A -0.1719 0.1309 0.3980 0.066 Uiso calc R 1 . . H H3B -0.1106 -0.0193 0.3098 0.066 Uiso calc R 1 . . H H3C -0.0742 0.1902 0.2938 0.066 Uiso calc R 1 . . H O1 0.0351(2) 0.2411(2) 0.51800(19) 0.0372(5) Uani d . 1 . . O H1 0.0842 0.3068 0.4774 0.056 Uiso calc R 1 . . H C4 0.0052(3) 0.5590(4) 0.0606(3) 0.0303(7) Uani d . 1 . . C C5 0.0449(3) 0.7541(3) 0.0291(3) 0.0385(9) Uani d . 1 . . C H5A 0.0533 0.8253 0.1072 0.058 Uiso calc R 1 . . H H5B -0.0194 0.8095 -0.0276 0.058 Uiso calc R 1 . . H H5C 0.1262 0.7519 -0.0123 0.058 Uiso calc R 1 . . H C6 -0.1150(3) 0.5629(4) 0.1330(3) 0.0328(7) Uani d . 1 . . C H6A -0.1413 0.4383 0.1513 0.049 Uiso calc R 1 . . H H6B -0.1817 0.6238 0.0822 0.049 Uiso calc R 1 . . H H6C -0.1001 0.6290 0.2125 0.049 Uiso calc R 1 . . H O2 0.1026(2) 0.4796(2) 0.14287(19) 0.0337(5) Uani d . 1 . . O H2 0.1737 0.4974 0.1124 0.051 Uiso calc R 1 . . H O3 0.1415(2) 0.5241(2) 0.3925(2) 0.0314(5) Uani d D 1 . . O H31 0.105(2) 0.498(3) 0.3230(15) 0.047 Uiso d D 1 . . H H32 0.0915(19) 0.596(3) 0.427(2) 0.047 Uiso d D 1 . . H 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 0.047(2) 0.0172(12) 0.0271(15) 0.0013(13) 0.0111(14) -0.0006(11) C2 0.055(3) 0.0238(12) 0.038(2) -0.0003(15) 0.0223(18) 0.0022(12) C3 0.064(2) 0.0321(17) 0.0364(17) 0.0093(16) 0.0027(15) 0.0036(14) O1 0.0576(15) 0.0184(10) 0.0369(12) -0.0027(9) 0.0176(10) 0.0000(7) C4 0.040(2) 0.0216(13) 0.0299(17) -0.0002(12) 0.0096(15) 0.0014(12) C5 0.054(2) 0.0194(14) 0.0427(18) -0.0015(14) 0.0062(16) -0.0009(12) C6 0.039(2) 0.0338(16) 0.0262(16) 0.0037(15) 0.0061(14) 0.0020(13) O2 0.0377(15) 0.0352(11) 0.0284(12) 0.0006(10) 0.0037(10) 0.0038(8) O3 0.0391(16) 0.0250(9) 0.0305(14) 0.0028(9) 0.0081(9) -0.0041(8) 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 . 1.442(3) no C1 C1 3_556 1.516(5) no C1 C3 . 1.529(4) no C1 C2 . 1.547(5) 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 O1 H1 . 0.8400 no C4 O2 . 1.447(4) no C4 C6 . 1.510(4) no C4 C5 . 1.537(4) no C4 C4 3_565 1.551(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 O2 H2 . 0.8400 no O3 H31 . 0.842(5) no O3 H32 . 0.842(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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 C1 C1 . 3_556 107.7(3) no O1 C1 C3 . . 109.2(2) no C1 C1 C3 3_556 . 111.7(4) no O1 C1 C2 . . 105.8(2) no C1 C1 C2 3_556 . 112.2(3) no C3 C1 C2 . . 110.0(3) 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 C1 O1 H1 . . 109.5 no O2 C4 C6 . . 107.3(2) no O2 C4 C5 . . 108.3(3) no C6 C4 C5 . . 109.6(2) no O2 C4 C4 . 3_565 107.4(3) no C6 C4 C4 . 3_565 113.2(3) no C5 C4 C4 . 3_565 110.9(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 C4 O2 H2 . . 109.5 no H31 O3 H32 . . 104.1(8) no