X-ray Diffraction and Solid-State NMR Investigation of the Single-Crystal to Single-Crystal Dehydration of Thiamine Hydrochloride Monohydrate
Te, Ruth L.; Griesser, Ulrich J.; Morris, Kenneth R.; Byrn, Stephen R.; Stowell, Joseph G.; Crystal Growth & Design 3 (2003) 997–; doi:10.1021/cg0340749

data_4505736
_publ_section_title
;
 X-ray Diffraction and Solid-State NMR Investigation of the Single-Crystal
 to Single-Crystal Dehydration of Thiamine Hydrochloride Monohydrate
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              997
_journal_paper_doi               10.1021/cg0340749
_journal_volume                  3
_journal_year                    2003
_chemical_compound_source
'crystallized in-house from material from Sigma (USA)'
_chemical_formula_structural     'C12 H18 N4 O1 S1 2+, 2(Cl1 1-), H2 O1'
_chemical_formula_sum            'C12 H20 Cl2 N4 O2 S'
_chemical_formula_weight         355.30
_chemical_name_common            'vitamine B1'
_chemical_name_systematic
;3-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-5-(2-hydroxyethyl)-4-
methylthiazolium chloride monohydrochloride'
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.699(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9928(2)
_cell_length_b                   20.6631(10)
_cell_length_c                   11.7695(5)
_cell_measurement_reflns_used    11310
_cell_measurement_temperature    296
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     1681.05(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski, 1996)'
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
Xtal_GX (Hall, 1995)
PLUTON (Spek, 1991)
;
_computing_publication_material  'CIF VAX MolEN (Fair, 1990)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution
'Direct methods (SIR97, Altomare et al., 1997)'
_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11310
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.9141
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       0.12E-01
_refine_ls_extinction_method     'SHELXL97 (Sheldrick 1997)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4307
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.1219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.138
_reflns_number_gt                2767
_reflns_number_total             4307
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            cg0340749si20030509_015708.cif
_cod_data_source_block           Thiamine_Hydrochloride_Monohydrate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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_original_cell_volume        1681.0(2)
_cod_original_formula_sum        'C12 H20 Cl2 N4 O2 S1'
_cod_database_code               4505736