#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/03/2200365.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_2200365 loop_ _publ_author_name 'Nie, Jing-Jing' 'Xu, Duan-Jun' 'Wu, Jing-Yun' 'Chiang, Michael Y.' _publ_section_title ; Redetermination of racemic tartaric acid monohydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o428 _journal_page_last o429 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C4 H6 O6, H2 O' _chemical_formula_sum 'C4 H8 O7' _chemical_formula_weight 168.10 _chemical_name_common 'Tartaric acid monohydrate' _chemical_name_systematic ; 2,3-Dihydroxysuccinic acid monohydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 109.260(5) _cell_angle_beta 99.862(5) _cell_angle_gamma 96.108(5) _cell_formula_units_Z 2 _cell_length_a 4.869(5) _cell_length_b 8.052(5) _cell_length_c 9.153(5) _cell_measurement_reflns_used 16 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 9.9 _cell_measurement_theta_min 4.7 _cell_volume 328.6(4) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992a) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1992b)' _computing_molecular_graphics 'XP (Siemens, 1994)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS93 (Sheldrick, 1993)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Rigaku AFC-7S' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .014 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1145 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.9 _diffrn_standards_decay_% 1.4 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time none _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .17 _exptl_absorpt_correction_T_max .934 _exptl_absorpt_correction_T_min .888 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 176 _exptl_crystal_size_max .70 _exptl_crystal_size_mid .60 _exptl_crystal_size_min .40 _refine_diff_density_max .34 _refine_diff_density_min -.16 _refine_ls_extinction_coef .64(7) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.07 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 102 _refine_ls_number_reflns 1145 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.07 _refine_ls_restrained_S_obs 1.09 _refine_ls_R_factor_all .043 _refine_ls_R_factor_gt .040 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.1479P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .119 _refine_ls_wR_factor_ref .114 _reflns_number_gt 1040 _reflns_number_total 1145 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6020.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200365 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 .0561(9) .0253(7) .0478(9) .0146(6) .0253(7) .0135(6) O2 .0543(9) .0266(7) .0416(8) .0103(6) .0268(7) .0051(6) O3 .0352(7) .0278(7) .0337(7) .0128(5) .0151(5) .0108(5) O4 .0334(7) .0343(7) .0291(7) .0128(5) .0047(5) .0034(5) O5 .0548(9) .0314(8) .0342(8) .0158(6) .0069(6) -.0007(6) O6 .0482(8) .0288(7) .0372(8) .0177(6) .0089(6) .0099(6) OW .0588(9) .0295(8) .0555(10) .0183(6) .0282(7) .0156(7) C1 .0308(9) .0229(9) .0232(8) .0054(7) .0046(7) .0039(7) C2 .0306(9) .0234(9) .0239(8) .0077(7) .0060(7) .0071(7) C3 .0321(9) .0236(9) .0269(9) .0080(7) .0091(7) .0079(7) C4 .0343(9) .0206(8) .0326(10) .0052(7) .0119(7) .0089(7) 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol O1 .2091(3) .4357(2) .3708(2) .0406(4) Uani d . 1 . O O2 -.0110(3) .2696(2) .4835(2) .0403(5) Uani d . 1 . O O3 .4040(3) .1621(2) .19547(15) .0307(4) Uani d . 1 . O O4 -.1667(3) -.0229(2) .14076(15) .0340(4) Uani d . 1 . O O5 .1126(3) -.2886(2) .0393(2) .0430(5) Uani d . 1 . O O6 .3946(3) -.2208(2) .2797(2) .0378(4) Uani d . 1 . O OW .6175(3) .5052(2) .1831(2) .0450(5) Uani d . 1 . O C1 .1529(4) .2952(2) .3925(2) .0268(4) Uani d . 1 . C C2 .2829(3) .1338(2) .3169(2) .0260(5) Uani d . 1 . C C3 .0594(4) -.0375(2) .2524(2) .0272(5) Uani d . 1 . C C4 .1918(4) -.1979(2) .1776(2) .0287(5) Uani d . 1 . C H2 -.0691 .3666 .5268 .080 Uiso d . 1 . H H2C .4305 .1231 .3964 .080 Uiso d . 1 . H H3 .5380 .1021 .1814 .080 Uiso d . 1 . H H3C -.0136 -.0532 .3395 .080 Uiso d . 1 . H H4 -.1660 -.0954 .0391 .080 Uiso d . 1 . H H6 .4477 -.3273 .2410 .080 Uiso d . 1 . H H1W .7133 .4556 .0990 .080 Uiso d . 1 . H H2W .5156 .4088 .2015 .080 Uiso d . 1 . H 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 O1 C1 . 1.223(2) yes O2 C1 . 1.296(2) yes O2 H2 . .8536 ? O3 C2 . 1.413(2) yes O3 H3 . .8545 ? O4 C3 . 1.411(2) yes O4 H4 . .9217 ? O5 C4 . 1.203(2) yes O6 C4 . 1.311(2) yes O6 H6 . .8980 ? OW H1W . .9641 ? OW H2W . .9535 ? C1 C2 . 1.516(2) yes C2 C3 . 1.536(3) yes C2 H2C . .964 ? C3 C4 . 1.516(2) ? C3 H3C . .965 ? 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 _geom_angle_publ_flag C1 O2 H2 109.1 ? C2 O3 H3 109.5 ? C3 O4 H4 111.4 ? C4 O6 H6 111.9 ? H1W OW H2W 108.2 ? O1 C1 O2 124.9(2) yes O1 C1 C2 121.6(2) ? O2 C1 C2 113.54(15) ? O3 C2 C1 108.47(14) yes O3 C2 C3 111.51(14) yes C1 C2 C3 110.67(15) yes O3 C2 H2C 108.8 ? C1 C2 H2C 108.6 ? C3 C2 H2C 108.7 ? O4 C3 C4 110.43(14) yes O4 C3 C2 110.15(14) yes C4 C3 C2 110.20(15) yes O4 C3 H3C 108.6 ? C4 C3 H3C 108.8 ? C2 C3 H3C 108.7 ? O5 C4 O6 126.4(2) yes O5 C4 C3 121.3(2) ? O6 C4 C3 112.24(15) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H2 O1 2_566 .854 1.828 2.680(2) 175.0 yes O3 H3 O4 1_655 .854 1.861 2.714(3) 176.4 yes O6 H6 OW 1_545 .898 1.643 2.526(2) 167.0 yes OW H2W O3 . .954 1.983 2.891(2) 158.5 yes OW H1W O5 2_655 .964 1.902 2.824(2) 159.2 yes