Hydrogen-Bonding Schemes of Galactonic Acid Hydrazide and its Hemihydrate
André, C.; Luger, P.; Fuhrhop, J.-H.; Hahn, F.; Acta Crystallographica Section B 53 (1997) 490–497; doi:10.1107/S0108768196012906

data_2101861
_publ_section_title
;
 Hydrogen-Bonding Schemes of Galactonic Acid Hydrazide and its
 Hemihydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              490
_journal_page_last               497
_journal_paper_doi               10.1107/S0108768196012906
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         '2C6 H14 N2 O6 , H2 O'
_chemical_formula_sum            'C12 H30 N4 O13'
_chemical_formula_weight         438.40
_chemical_name_systematic
;
 L-galactonic acid  hydrazide hemihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.7800(10)
_cell_length_b                   13.603(2)
_cell_length_c                   14.822(3)
_cell_measurement_reflns_used    1561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      4.25
_cell_volume                     952.3(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE Imaging Plate Diffraction System'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4399
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         5.26
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.227
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.6(13)
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.123
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment
;
It was found necessary only for H(O4), H(O6), H(O32) and H(O42), as well
as the two water H atoms, to introduce a DFIX restraint of
0.90 \%A (esd = 0.02). The isotropic displacement parameters of the
two latter atoms had to be held fixed at an U value of 0.072 \%A^2^
[= 1.2U~eq~(Ow)]
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4252
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_obs          0.0441
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.7754P], where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0981
_refine_ls_wR_factor_obs         0.0802
_reflns_number_observed          3214
_reflns_number_total             4254
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka0031.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w =
1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.7754P], where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.7754P], where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2101861
_cod_database_fobs_code          2101861