#------------------------------------------------------------------------------ #$Date: 2013-12-28 14:58:47 +0100 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/03/2100343.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_2100343 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, 6(H2 O)' _chemical_formula_sum 'C6 H26 O8' _chemical_formula_weight 226.27 _chemical_melting_point 318.6 _chemical_name_common 'pinacol hexahydrate' _chemical_name_systematic ; 2,3-dimethyl-2,3-butanediol hexahydrate ; _space_group_IT_number 58 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2 2n' _symmetry_space_group_name_H-M 'P n n m' _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 90.00 _cell_formula_units_Z 2 _cell_length_a 6.308(2) _cell_length_b 6.321(2) _cell_length_c 15.759(3) _cell_measurement_reflns_used 1360 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 628.4(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 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90.0(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _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 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 3531 _diffrn_reflns_theta_full 27.47 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 1.29 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_correction_T_min 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 252 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.276 _refine_diff_density_min -0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 87 _refine_ls_number_reflns 734 _refine_ls_number_restraints 103 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0363 _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^)+(0.0432P)^2^+0.1463P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.0941 _reflns_number_gt 559 _reflns_number_total 734 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file ws5034.cif _[local]_cod_data_source_block k03226o _[local]_cod_cif_authors_sg_H-M Pnnm _cod_database_code 2100343 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 0.3792(12) 0.5259(13) 0.5000 0.0216(15) Uani d SPDU 0.428(4) . 1 C C2 0.3069(18) 0.678(2) 0.4327(6) 0.041(2) Uani d PDU 0.428(4) . 1 C H2A 0.1557 0.7082 0.4403 0.062 Uiso calc PR 0.428(4) . 1 H H2B 0.3297 0.6151 0.3765 0.062 Uiso calc PR 0.428(4) . 1 H H2C 0.3881 0.8097 0.4372 0.062 Uiso calc PR 0.428(4) . 1 H O1 0.2599(15) 0.3322(14) 0.5000 0.0257(17) Uani d SPDU 0.428(4) . 1 O H1O 0.26(3) 0.27(2) 0.463(4) 0.039 Uiso d PD 0.2140(19) . 1 H C1' 0.5260(10) 0.3828(10) 0.5000 0.0261(13) Uani d SPDU 0.572(4) . 2 C C2' 0.6451(13) 0.3393(17) 0.4141(4) 0.0407(16) Uani d PDU 0.572(4) . 2 C H2'1 0.5571 0.3871 0.3666 0.061 Uiso calc PR 0.572(4) . 2 H H2'2 0.6726 0.1874 0.4085 0.061 Uiso calc PR 0.572(4) . 2 H H2'3 0.7799 0.4164 0.4137 0.061 Uiso calc PR 0.572(4) . 2 H O1' 0.3309(10) 0.2651(12) 0.5000 0.0277(14) Uani d SPDU 0.572(4) . 2 O H1O' 0.277(13) 0.246(16) 0.461(3) 0.042 Uiso d PD 0.2860(19) . 2 H O2 0.1568(3) 0.1567(3) 0.34129(5) 0.0256(3) Uani d D 1 . . O H2W1 0.064(6) 0.066(6) 0.3459(13) 0.038 Uiso d PD 0.50 . . H H2W2 0.195(6) 0.194(6) 0.3886(9) 0.038 Uiso d PD 0.50 . . H H2W3 0.109(7) 0.258(4) 0.316(3) 0.038 Uiso d PD 0.50 . . H H2W4 0.257(4) 0.107(7) 0.315(3) 0.038 Uiso d PD 0.50 . . H O3 0.0000 0.5000 0.2506(2) 0.0259(3) Uani d SD 1 . . O H3W1 0.051(4) 0.396(5) 0.277(3) 0.039 Uiso d PD 0.50 . . H H3W2 0.102(5) 0.549(5) 0.223(3) 0.039 Uiso d PD 0.50 . . 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 0.017(3) 0.025(4) 0.022(3) -0.001(3) 0.000 0.000 C2 0.040(5) 0.041(4) 0.043(4) 0.012(3) 0.003(3) 0.018(3) O1 0.026(4) 0.026(3) 0.025(4) -0.007(3) 0.000 0.000 C1' 0.024(3) 0.033(3) 0.021(2) -0.001(2) 0.000 0.000 C2' 0.032(3) 0.051(4) 0.039(3) 0.006(3) 0.012(3) -0.016(3) O1' 0.029(3) 0.030(3) 0.024(3) -0.006(2) 0.000 0.000 O2 0.0308(10) 0.0296(11) 0.0164(4) -0.0008(4) -0.0001(7) -0.0003(7) O3 0.0320(14) 0.0285(15) 0.0171(6) 0.0006(14) 0.000 0.000 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 . 1.437(10) no C1 C2 . 1.503(10) no C1 C2 6_556 1.503(10) no C1 C1 5_666 1.559(15) no C2 H2A . 0.9800 no C2 H2B . 0.9800 no C2 H2C . 0.9800 no O1 H1O . 0.72(5) no O1 H1O' . 0.83(9) no C1' O1' . 1.438(8) no C1' C1' 5_666 1.517(13) no C1' C2' . 1.572(7) no C1' C2' 6_556 1.572(7) no C2' H2'1 . 0.9800 no C2' H2'2 . 0.9800 no C2' H2'3 . 0.9800 no O1' H1O . 0.74(15) no O1' H1O' . 0.72(5) no O2 H2W1 . 0.821(13) no O2 H2W2 . 0.817(12) no O2 H2W3 . 0.816(12) no O2 H2W4 . 0.816(12) no O3 H3W1 . 0.838(13) no O3 H3W2 . 0.838(13) 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 C2 . . 112.7(8) no O1 C1 C2 . 6_556 112.7(8) no C2 C1 C2 . 6_556 89.9(9) no O1 C1 C1 . 5_666 109.4(8) no C2 C1 C1 . 5_666 115.5(7) no C2 C1 C1 6_556 5_666 115.5(7) no C1 O1 H1O . . 120(3) no C1 O1 H1O' . . 119(3) no O1' C1' C1' . 5_666 108.7(7) no O1' C1' C2' . . 108.6(5) no C1' C1' C2' 5_666 . 105.9(5) no O1' C1' C2' . 6_556 108.6(5) no C1' C1' C2' 5_666 6_556 105.9(5) no C2' C1' C2' . 6_556 118.8(6) no C1' C2' H2'1 . . 109.5 no C1' C2' H2'2 . . 109.5 no H2'1 C2' H2'2 . . 109.5 no C1' C2' H2'3 . . 109.5 no H2'1 C2' H2'3 . . 109.5 no H2'2 C2' H2'3 . . 109.5 no C1' O1' H1O . . 121(3) no C1' O1' H1O' . . 120(3) no H2W1 O2 H2W2 . . 109.0(8) no H2W1 O2 H2W3 . . 109.1(8) no H2W2 O2 H2W3 . . 109.7(8) no H2W1 O2 H2W4 . . 109.2(8) no H2W2 O2 H2W4 . . 109.8(8) no H2W3 O2 H2W4 . . 110.1(8) no H3W1 O3 H3W2 . . 104.5(9) no _cod_database_fobs_code 2100343 _journal_paper_doi 10.1107/S0108768105031356