Azophotoswitches containing thiazole, isothiazole, thiadiazole, and isothiadiazole.
Cheruthu, Nusaiba Madappuram; Hashim, P. K.; Sahu, Saugata; Takahashi, Kiyonori; Nakamura, Takayoshi; Mitomo, Hideyuki; Ijiro, Kuniharu; Tamaoki, Nobuyuki; Organic & biomolecular chemistry 23 (2024) 207–212; doi:10.1039/d4ob01573h

data_7160213
_publ_section_title
;
 Azophotoswitches containing thiazole, isothiazole, thiadiazole, and
 isothiadiazole.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              207
_journal_page_last               212
_journal_paper_doi               10.1039/d4ob01573h
_journal_volume                  23
_journal_year                    2024
_chemical_formula_moiety         'C8 H6 N4 S'
_chemical_formula_sum            'C8 H6 N4 S'
_chemical_formula_weight         190.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-07-16 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.039(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1698(4)
_cell_length_b                   5.5451(3)
_cell_length_c                   19.2296(9)
_cell_measurement_reflns_used    7106
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      71.9670
_cell_measurement_theta_min      2.3440
_cell_volume                     864.58(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -89.00  89.00   0.50    1.37    --    0.00  46.00 -90.00  356
  2  \w    -84.00  94.00   0.50    5.48    --    5.00  37.00-180.00  356
  3  \w   -185.00  -6.00   0.50    5.48    --  -95.70  49.00 -17.48  358
  4  \w   -185.00  -6.00   0.50    5.48    --  -95.70  46.00 150.00  358
  5  \w   -185.00  -6.00   0.50    5.48    --  -95.70  55.00-104.90  358
  6  \w   -185.00  -6.00   0.50    5.48    --  -95.70  55.00-104.90  358
  7  \w   -185.00  -6.00   0.50    5.48    --  -95.70  54.00  89.06  358
  8  \w   -185.00  -6.00   0.50    5.48    --  -95.70  38.00-140.93  358
  9  \w   -185.00  -6.00   0.50    5.48    --  -95.70  55.00  41.60  358
 10  \w   -185.00  -6.00   0.50    5.48    --  -95.70  46.00 150.00  358
 11  \w   -185.00  -6.00   0.50    5.48    --  -95.70  52.00 140.44  358
 12  \w   -185.00  -6.00   0.50    5.48    --  -95.70  55.00 -37.38  358
 13  \w    -89.00  89.00   0.50    1.37    --    0.00  18.00  60.00  356
 14  \w    -89.00  89.00   0.50    1.37    --    0.00  46.00-180.00  356
 15  \w   -185.00  -6.00   0.50    5.48    --  -95.70   0.00 -90.00  358
 16  \w   -185.00 -74.00   0.50    5.48    --  -95.70  46.00  60.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180777000
_diffrn_orient_matrix_UB_12      0.0364390000
_diffrn_orient_matrix_UB_13      0.0800177000
_diffrn_orient_matrix_UB_21      0.1837785000
_diffrn_orient_matrix_UB_22      -0.0682352000
_diffrn_orient_matrix_UB_23      0.0047537000
_diffrn_orient_matrix_UB_31      0.0445926000
_diffrn_orient_matrix_UB_32      0.2667297000
_diffrn_orient_matrix_UB_33      -0.0098369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.627
_diffrn_reflns_theta_min         4.634
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       plate
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0808P)^2^+0.2122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4535
_reflns_number_total             5133
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9170\% 
around [-0.00 0.00 1.00] (reciprocal) or [0.27 -0.00 0.96] (direct)
;
_cod_data_source_file            d4ob01573h2.cif
_cod_data_source_block           exp_867_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7160210--7160217.cif.'
_cod_database_code               7160213
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4H2N6S2
_chemical_oxdiff_usercomment     200K
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.620(2)
 0.380(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
4. Rigid bond restraints
 C8A, C7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C8A) = Uanis(S1)
6. Others
 Sof(N1A)=Sof(N2A)=Sof(C7A)=Sof(S1A)=Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(S1)=Sof(C8)=Sof(H8)=Sof(N1)=Sof(N2)=Sof(C7)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C6(H6), C4(H4), C3(H3), C2(H2), C8A(H8A)
;
_shelx_res_checksum              30557
_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 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2