Crystal structure of 4-(4′-(pyridin-4-yl)-[1,1′-biphenyl]-4-yl)pyridin-1-ium 2-carboxy-4-(3,5-dicarboxyphenoxy)benzoate hydrate, C38H28N2O10
Hu, Xu-Ze; Zhao, Yan; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1125–1127; doi:10.1515/ncrs-2020-0198

data_8105397
_publ_section_title
;
 Crystal structure of
 4-(4&#x2032;-(pyridin-4-yl)-[1,1&#x2032;-biphenyl]-4-yl)pyridin-1-ium
 2-carboxy-4-(3,5-dicarboxyphenoxy)benzoate hydrate, C38H28N2O10
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1125
_journal_page_last               1127
_journal_paper_doi               10.1515/ncrs-2020-0198
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C22 H17 N2, H2 O, C16 H9 O9'
_chemical_formula_sum            'C38 H28 N2 O10'
_chemical_formula_weight         672.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.195(5)
_cell_angle_beta                 103.259(5)
_cell_angle_gamma                97.356(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3207(6)
_cell_length_b                   11.9296(6)
_cell_length_c                   13.6079(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1564.57(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18117
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.9584
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                4276
_reflns_number_total             5833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0198_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1564.58(15)
_cod_database_code               8105397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C4(H4), C6(H6), C8(H8A), C11(H11), C12(H12), C17(H17),
 C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29),
  C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38)
2.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.224
_oxdiff_exptl_absorpt_empirical_full_min 0.595