Two hydrate pseudopolymorphs of thiamine pyrophosphate: a dihydrate and a trihydrate
Li, Shu-Qiang; Hu, Ning-Hai; Acta Crystallographica Section C 69 (2013) 794–797; doi:10.1107/S0108270113015783

data_2019066
_publ_section_title
;
 Two hydrate pseudopolymorphs of thiamine pyrophosphate: a dihydrate and a
 trihydrate
;
_journal_coeditor_code           WQ3039
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              794
_journal_page_last               797
_journal_paper_doi               10.1107/S0108270113015783
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C12 H18 N4 O7 P2 S , 3H2 O'
_chemical_formula_moiety         'C12 H18 N4 O7 P2 S, 3(H2 O)'
_chemical_formula_sum            'C12 H24 N4 O10 P2 S'
_chemical_formula_weight         478.35
_chemical_name_common            'Thiamine pyrophosphate trihydrate'
_chemical_name_systematic
'3-[(4-Amino-2-methylpyrimidin-1-ium-5-yl)methyl]-4-methyl-1,3-thiazol-3-ium-5-yl hydrogen pyrophosphate trihydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                87.896(11)
_cell_angle_beta                 74.324(13)
_cell_angle_gamma                75.559(11)
_cell_formula_units_Z            2
_cell_length_a                   8.3776(12)
_cell_length_b                   9.2397(13)
_cell_length_c                   14.208(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      19.86
_cell_measurement_theta_min      9.67
_cell_volume                     1024.9(3)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       '2\q and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4473
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.9532
_exptl_absorpt_correction_T_min  0.8444
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0566P)^2^+0.4384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                2953
_reflns_number_total             3593
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3039.cif
_cod_data_source_block           II
_cod_original_cell_volume        1024.8(3)
_cod_database_code               2019066
_cod_database_fobs_code          2019066