Strong supramolecular synthons assembled by hydrogen bonds and chalcogen bonds
Zhang, Yu; Sun, Xiaotian; Wang, Weizhou; CrystEngComm 27 (2025) 3439–3443; doi:10.1039/D5CE00262A

data_1574556
_publ_section_title
;
 Strong supramolecular synthons assembled by hydrogen bonds and chalcogen
 bonds
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3439
_journal_page_last               3443
_journal_paper_doi               10.1039/D5CE00262A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C6 H4 N2 Se, C8 H5 N O6'
_chemical_formula_sum            'C14 H9 N3 O6 Se'
_chemical_formula_weight         394.203
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_Int_Tables_number      13
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.02.24 svn.r684696ac for OlexSys, GUI svn.r6476)
;
_audit_update_record
;
2025-03-09 deposited with the CCDC.	2025-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.648(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3555(4)
_cell_length_b                   9.1502(3)
_cell_length_c                   7.1692(4)
_cell_measurement_reflns_used    2894
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7560
_cell_measurement_theta_min      4.2550
_cell_volume                     734.38(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9610
_diffrn_measured_fraction_theta_max 0.8717
_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    -10.00  42.00   1.00    4.46    --   17.09  77.00  60.00   52
  2  \w      0.00  84.00   1.00    4.46    --   17.09  57.00  30.00   84
  3  \w     39.00  89.00   1.00    4.46    --   17.09 178.00-180.00   50
  4  \w     39.00  89.00   1.00    4.46    --   17.09 178.00 -90.00   50
  5  \w     -2.00  86.00   1.00    4.46    --   17.09  38.00  60.00   88
  6  \w    -10.00  42.00   1.00    4.46    --   17.09  77.00-180.00   52
  7  \w    -10.00  42.00   1.00    4.46    --   17.09  77.00-120.00   52
  8  \w    -52.00  -2.00   1.00    4.46    --   17.09 -38.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0165948000
_diffrn_orient_matrix_UB_12      0.0650636000
_diffrn_orient_matrix_UB_13      0.0515279000
_diffrn_orient_matrix_UB_21      -0.0566694000
_diffrn_orient_matrix_UB_22      0.0306300000
_diffrn_orient_matrix_UB_23      -0.0353878000
_diffrn_orient_matrix_UB_31      -0.0228537000
_diffrn_orient_matrix_UB_32      -0.0288839000
_diffrn_orient_matrix_UB_33      0.0786227000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.9610
_diffrn_reflns_Laue_measured_fraction_max 0.8717
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7626
_diffrn_reflns_point_group_measured_fraction_full 0.9610
_diffrn_reflns_point_group_measured_fraction_max 0.8717
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.64
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             392.270
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.7491
_refine_diff_density_min         -0.4957
_refine_diff_density_rms         0.1089
_refine_ls_d_res_high            0.7284
_refine_ls_d_res_low             5.5974
_refine_ls_goodness_of_fit_ref   1.0756
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    10
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0756
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.2925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                1484
_reflns_number_total             1733
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00262a2.cif
_cod_data_source_block           WWZ2023041201_auto
_cod_depositor_comments
'Adding full bibliography for 1574556--1574561.cif.'
_cod_database_code               1574556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.809