Crystal structure and Hirshfeld surface analysis of 4,4'-di-meth-oxy-biphenyl-3,3',5,5'-tetra-carb-oxy-lic acid dihydrate.
Hanauer, Thomas; Seichter, Wilhelm; Mazik, Monika; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 413–417; doi:10.1107/S2056989024002305

data_2023071
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 4,4'-di-meth-oxy-biphenyl-3,3',5,5'-tetra-carb-oxy-lic acid dihydrate.
;
_journal_coeditor_code           EX2080
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              413
_journal_page_last               417
_journal_paper_doi               10.1107/S2056989024002305
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C18 H14 O10, 2H2 O'
_chemical_formula_moiety         'C18 H14 O10, 2(H2 O)'
_chemical_formula_sum            'C18 H18 O12'
_chemical_formula_weight         426.32
_chemical_name_systematic
;
4,4'-Dimethoxybiphenyl-3,3',5,5'-tetracarboxylic acid dihydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.069(3)
_cell_length_b                   24.069(3)
_cell_length_c                   6.4468(8)
_cell_measurement_reflns_used    1164
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      3.67
_cell_volume                     3734.7(8)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012), <i>publCIF</i> (Westrip, 2010),
<i>ShelXle</i>
(H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14573
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.481
_diffrn_reflns_theta_min         2.676
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.196
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 575 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -2.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+2.9912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                1502
_reflns_number_total             1914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2080.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023071.cif.'
_cod_original_cell_volume        3734.6(9)
_cod_database_code               2023071
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              88795
_shelx_res_checksum              32021