Crystal structure of trans-1,2-bis(pyridinium-4-yl) ethylene bis(2-carboxy-4-bromobenzoate) – water (1/4), C14H14BrNO6
Wei-Wei, Yuan; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 289–291; doi:10.1515/ncrs-2022-0002

data_8105207
_publ_section_title
;
 Crystal structure of trans-1,2-bis(pyridinium-4-yl) ethylene
 bis(2-carboxy-4-bromobenzoate) -- water (1/4), C14H14BrNO6
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              289
_journal_page_last               291
_journal_paper_doi               10.1515/ncrs-2022-0002
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C8 H4 Br O4, 2(H2 O), C6 H6 N'
_chemical_formula_sum            'C14 H14 Br N O6'
_chemical_formula_weight         372.174
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_cell_angle_alpha                72.774(5)
_cell_angle_beta                 81.547(4)
_cell_angle_gamma                74.370(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9693(3)
_cell_length_b                   8.6514(5)
_cell_length_c                   13.6726(8)
_cell_measurement_reflns_used    4076
_cell_measurement_temperature    290.7(3)
_cell_measurement_theta_max      25.0180
_cell_measurement_theta_min      4.0110
_cell_volume                     756.26(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.7(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9839
_diffrn_measured_fraction_theta_max 0.9839
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -4.00  46.00   1.00    6.22    --   12.34  38.00  30.00   50
  2  \w     -2.00  80.00   1.00    6.22    --   12.34  57.00  60.00   82
  3  \w     13.00  80.00   1.00    6.22    --   12.34  57.00 -90.00   67
  4  \w     53.00  79.00   1.00    6.22    --   12.34  57.00-150.00   26
  5  \w     -3.00  79.00   1.00    6.22    --   12.34  57.00-180.00   82
  6  \w    -27.00  58.00   1.00    6.22    --  -11.32  38.00 -60.00   85
  7  \w    -20.00  30.00   1.00    6.22    --   12.34 -38.00  60.00   50
  8  \w    -20.00  51.00   1.00    6.22    --   12.34 -99.00  60.00   71
  9  \w     25.00  51.00   1.00    6.22    --   12.34 -99.00 -60.00   26
 10  \w    -20.00  51.00   1.00    6.22    --   12.34 -99.00-150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0111924000
_diffrn_orient_matrix_UB_12      -0.0699951000
_diffrn_orient_matrix_UB_13      -0.0190924000
_diffrn_orient_matrix_UB_21      -0.0101405000
_diffrn_orient_matrix_UB_22      0.0532846000
_diffrn_orient_matrix_UB_23      -0.0505382000
_diffrn_orient_matrix_UB_31      0.1048850000
_diffrn_orient_matrix_UB_32      -0.0087339000
_diffrn_orient_matrix_UB_33      -0.0068687000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.9839
_diffrn_reflns_Laue_measured_fraction_max 0.9839
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9713
_diffrn_reflns_point_group_measured_fraction_full 0.9839
_diffrn_reflns_point_group_measured_fraction_max 0.9839
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             375.870
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.6234
_refine_diff_density_min         -0.7303
_refine_diff_density_rms         0.0837
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             6.1386
_refine_ls_goodness_of_fit_ref   1.0562
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0562
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.3771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -9
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2234
_reflns_number_total             2621
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2022-0002_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105207
_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 Riding coordinates:
 O4(H4), O5(H5a,H5b), O6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), N1(H1), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14)
;
_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 1.718
_oxdiff_exptl_absorpt_empirical_full_min 0.463