Structure and hydrogen bonding in 2,4-dihydroxybenzoic acid at 90, 100, 110 and 150K; a theoretical and single-crystal X-ray diffraction study
Parkin, Andrew; Adam, Martin; Cooper, Richard I.; Middlemiss, Derek S.; Wilson, Chick C.; Acta Crystallographica Section B 63 (2007) 303–308; doi:10.1107/S0108768106055212

data_2102782
_publ_section_title
;
 Structure and hydrogen bonding in 2,4-dihydroxybenzoic acid at 90,
 100, 110 and 150K; a theoretical and single-crystal X-ray diffraction
 study
;
_journal_coeditor_code           BS5037
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              303
_journal_page_last               308
_journal_paper_doi               10.1107/S0108768106055212
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'C7 H6 O4'
_chemical_formula_sum            'C7 H6 O4'
_chemical_formula_weight         154.12
_chemical_name_systematic        '2,4-dihydroxybenzoic acid'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 99.630(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.6686(5)
_cell_length_b                   22.333(3)
_cell_length_c                   8.0046(11)
_cell_measurement_reflns_used    10028
_cell_measurement_temperature    90
_cell_measurement_theta_max      35
_cell_measurement_theta_min      0
_cell_volume                     646.58(15)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.775
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5714
_diffrn_reflns_theta_full        26.040
_diffrn_reflns_theta_max         33.818
_diffrn_reflns_theta_min         1.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       12(7)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.9636
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000164
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^
 Method = SHELXL 97 (Sheldrick, 1997)
 W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ]
 P(i) are:
 0.322E-01 0.690 0.00 0.00 0.00 0.333
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1317
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                1301
_reflns_number_total             2022
_reflns_threshold_expression     I>2.00s(I)
_cod_data_source_file            bs5037.cif
_cod_data_source_block           90k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               2102782