Benzo[1,2-<i>d</i>:4,5-<i>d</i>']bis([1,2,3]thiadiazole) and Its Bromo Derivatives: Molecular Structure and Reactivity.
Chmovzh, Timofey N.; Alekhina, Daria A.; Kudryashev, Timofey A.; Aysin, Rinat R.; Korlyukov, Alexander A.; Rakitin, Oleg A.; International journal of molecular sciences 24 (2023) 8835–; doi:10.3390/ijms24108835

data_1569282
_publ_section_title
;
 Benzo[1,2-<i>d</i>:4,5-<i>d</i>']bis([1,2,3]thiadiazole) and Its Bromo
 Derivatives: Molecular Structure and Reactivity.
;
_journal_issue                   10
_journal_name_full               'International journal of molecular sciences'
_journal_page_first              8835
_journal_paper_doi               10.3390/ijms24108835
_journal_volume                  24
_journal_year                    2023
_chemical_formula_moiety         'C6 H Br N4 S2'
_chemical_formula_sum            'C6 H Br N4 S2'
_chemical_formula_weight         273.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.562(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5976(3)
_cell_length_b                   9.2941(2)
_cell_length_c                   6.9912(2)
_cell_measurement_reflns_used    10519
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      35.7150
_cell_measurement_theta_min      2.7300
_cell_volume                     795.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.914
_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    -48.00   9.00   0.50    8.00    --  -17.65  95.00   7.00  114
  2  \w    -31.00  48.00   0.50    8.00    --   17.96 -95.00-102.00  158
  3  \w    -28.00  55.00   0.50    8.00    --  -17.65  38.00-150.00  166
  4  \w      4.00  90.00   0.50    8.00    --   17.96  57.00   0.00  172
  5  \w    -56.00   5.00   0.50    8.00    --   17.96 -19.00-180.00  122
  6  \w    -56.00   5.00   0.50    8.00    --   17.96 -19.00 -60.00  122
  7  \w     -4.00  90.00   0.50    8.00    --   17.96  77.00 120.00  188
  8  \w     42.00  73.00   0.50    8.00    --   17.96 178.00-150.00   62
  9  \w      7.00  90.00   0.50    8.00    --   17.96  38.00 -90.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0438338000
_diffrn_orient_matrix_UB_12      0.0480339000
_diffrn_orient_matrix_UB_13      0.0005976000
_diffrn_orient_matrix_UB_21      0.0375680000
_diffrn_orient_matrix_UB_22      -0.0526701000
_diffrn_orient_matrix_UB_23      0.0484324000
_diffrn_orient_matrix_UB_31      0.0046575000
_diffrn_orient_matrix_UB_32      -0.0272748000
_diffrn_orient_matrix_UB_33      -0.0924293000
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.819
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         3403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0338P)^2^+0.6678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2983
_reflns_number_total             3403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2256390.cif
_cod_data_source_block           tim-47
_cod_database_code               1569282
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6HBrN4S2
_chemical_oxdiff_usercomment     Tim-47
_olex2_refinement_description
;
;
_shelx_res_checksum              23838
_shelx_hkl_checksum              48231
_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 1.689
_oxdiff_exptl_absorpt_empirical_full_min 0.485