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_1569281
_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         '2(C3 H N2 S)'
_chemical_formula_sum            'C6 H2 N4 S2'
_chemical_formula_weight         194.24
_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     dual
_audit_creation_date             2023-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                82.88(4)
_cell_angle_beta                 87.48(4)
_cell_angle_gamma                83.96(4)
_cell_formula_units_Z            2
_cell_length_a                   3.738(3)
_cell_length_b                   9.027(5)
_cell_length_c                   10.156(9)
_cell_measurement_reflns_used    2249
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.632
_cell_measurement_theta_min      2.867
_cell_volume                     338.0(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon III area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2024
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.627
_diffrn_reflns_theta_min         2.022
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.746072
_exptl_absorpt_correction_T_min  0.480154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1576 before and 0.0556 after correction.
 
For component 2:
 wR2(int) was 0.1709 before and 0.0769 after correction.
 The Ratio of minimum to maximum transmission is 0.64.

Final HKLF 4 output contains 8915 reflections, Rint = 0.0557
 (6431 with I > 3sig(I), Rint = 0.0536)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       prism
_exptl_crystal_F_000             196
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.2740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1881
_reflns_number_total             2024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2255420.cif
_cod_data_source_block           tim3
_cod_database_code               1569281
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6673(15)
 0.3327(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A)
;
_shelx_res_checksum              64105
_shelx_hkl_checksum              37866
_olex2_submission_special_instructions 'No special instructions were received'