Comparison of conventional and synchrotron X-ray structure determinations of the adduct 1,2,4,5-tetrahydroxybenzene–2,5-dihydroxy-1,4-benzoquinone (1/1) and a conventional X-ray structure determination of 1,2,4,5-tetrahydroxybenzene monohydrate
Jene, Paul G.; Pernin, Christopher G.; Ibers, James A.; Acta Crystallographica Section C 57 (2001) 730–734; doi:10.1107/S0108270101003353

data_2012013
_publ_section_title
;
 Comparison of conventional and synchrotron X-ray structure
 determinations of the adduct
 1,2,4,5-tetrahydroxybenzene--2,5-dihydroxy-1,4-benzoquinone (1/1) and
 a conventional X-ray structure determination of
 1,2,4,5-tetrahydroxybenzene monohydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              730
_journal_page_last               734
_journal_paper_doi               10.1107/S0108270101003353
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C6 H6 O4 , H2 O'
_chemical_formula_sum            'C6 H8 O5'
_chemical_formula_weight         160.12
_chemical_melting_point          490.5(5)
_chemical_name_systematic
;
1,2,4,5-Tetrahydroxybenzene monohydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 102.33(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.487(3)
_cell_length_b                   3.6470(10)
_cell_length_c                   13.506(3)
_cell_measurement_reflns_used    623
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.94
_cell_volume                     649.0(3)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full .977
_diffrn_measured_fraction_theta_max .977
_diffrn_measurement_device_type  'Bruker Smart1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_sigmaI/netI    .029
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3708
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    .146
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         .39
_refine_diff_density_min         -.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.22
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.22
_refine_ls_R_factor_all          .055
_refine_ls_R_factor_gt           .045
_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^)+(0.036P)^2^+1.0778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .149
_reflns_number_gt                1270
_reflns_number_total             1578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1173.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07

The following automatic conversions were performed:

'_chemical_melting_point' value '490-491' was changed to '490.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '490-491' was changed to '490.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        649.1(2)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2012013
_cod_database_fobs_code          2012013