A hydrate of carbamoylmethyl 3,4,5-trihydroxybenzoate with three different molecular conformations
Andrew Parkin; Simon Parsons; Johanna H. Robertson; Peter A. Tasker; Acta Crystallographica Section E 58 (2002) o1348–o1350; doi:10.1107/S1600536802020147

data_2201532
_publ_section_title
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 A hydrate of carbamoylmethyl 3,4,5-trihydroxybenzoate with three
 different molecular conformations
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_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1348
_journal_page_last               o1350
_journal_paper_doi               10.1107/S1600536802020147
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C9 H9 N O6, 0.33H2 O'
_chemical_formula_moiety         'C9 H9 N O6, 0.33H2O'
_chemical_formula_sum            'C9 H9.67 N O6.33'
_chemical_formula_weight         233.18
_chemical_name_systematic
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carbamoylmethyl 3,4,5-trihydroxybenzoate hydrate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.08(3)
_cell_angle_beta                 86.56(3)
_cell_angle_gamma                78.32(3)
_cell_formula_units_Z            6
_cell_length_a                   8.266(5)
_cell_length_b                   8.515(4)
_cell_length_c                   20.614(7)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     1417.2(12)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1990)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990)'
_computing_molecular_graphics    'SHELXTL and CAMERON (Watkin et al., 1993)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       \w--\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8429
_diffrn_reflns_theta_full        69.94
_diffrn_reflns_theta_max         69.94
_diffrn_reflns_theta_min         4.30
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.262
_refine_ls_extinction_coef       0.0019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         5000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0803P)^2^+0.3171P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                4192
_reflns_number_total             5000
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6179.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               2201532
_cod_database_fobs_code          2201532