One-pot synthesis of unsubstituted and methyl substituted-pyrazinyl diselenides and monoselenides: structural, optical property characterization and DFT calculations
Kushwah, Nisha; Chopade, Suresh M.; Wadawale, Amey; Sharma, P.; Kedarnath, G.; RSC Advances 13 (2023) 36392–36402; doi:10.1039/D3RA06591J

data_7247872
_publ_section_title
;
 One-pot synthesis of unsubstituted and methyl substituted-pyrazinyl
 diselenides and monoselenides: structural, optical property
 characterization and DFT calculations
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              36392
_journal_page_last               36402
_journal_paper_doi               10.1039/D3RA06591J
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C8 H6 N4 Se2'
_chemical_formula_weight         316.09
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2023-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                63.530(5)
_cell_angle_beta                 87.994(8)
_cell_angle_gamma                69.991(8)
_cell_formula_units_Z            1
_cell_length_a                   5.8558(6)
_cell_length_b                   6.9698(4)
_cell_length_c                   6.9700(3)
_cell_measurement_reflns_used    1473
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.9100
_cell_measurement_theta_min      7.1900
_cell_volume                     236.93(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'OLEX 1.2'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.896
_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   -109.00 -83.00   0.50    0.05    --  -47.70-136.00 114.00   52
  2  \w    -81.00 -56.00   0.50    0.05    --  -47.70 136.00 178.00   50
  3  \w    -97.00 -72.00   0.50    0.05    --  -47.70-132.00 -68.00   50
  4  \w     41.00  72.00   0.50    0.05    --   47.70-132.00 -68.00   62
  5  \w     56.00  82.00   0.50    0.05    --   47.70-136.00 114.00   52
  6  \w    -63.00 -17.00   0.50    0.05    --  -86.25 132.00   0.00   92
  7  \w    -94.00 -66.00   0.50    0.05    --  -86.25 136.00 178.00   56
  8  \w     94.00 130.00   0.50    0.05    --  107.74 132.00   0.00   72
  9  \w     77.00 102.00   0.50    0.05    --  107.74-132.00 -68.00   50
 10  \w     80.00 118.00   0.50    0.05    --  107.74-136.00 114.00   76
 11  \w    109.00 135.00   0.50    0.05    --  107.74 136.00 178.00   52
 12  \w   -109.00 -83.00   0.50    0.05    --  -47.70-125.00  30.00   52
 13  \w    -81.00 -31.00   0.50    0.05    --  -47.70 -77.00-180.00  100
 14  \w   -110.00 -84.00   0.50    0.05    --  -47.70 -77.00-180.00   52
 15  \w    -26.00  25.00   0.50    0.05    --   47.70 -19.00   0.00  102
 16  \w    -42.00 -17.00   0.50    0.05    --  -86.25  37.00 -60.00   50
 17  \w   -157.00-123.00   0.50    0.05    --  -86.25 -57.00 -60.00   68
 18  \w    -39.00 -14.00   0.50    0.05    --  -86.25  37.00   0.00   50
 19  \w   -159.00-122.00   0.50    0.05    --  -86.25 -37.00 -30.00   74
 20  \w    -38.00 -13.00   0.50    0.05    --  -86.25  37.00-120.00   50
 21  \w    -66.00 -41.00   0.50    0.05    --  -86.25  57.00-120.00   50
 22  \w    -42.00 -17.00   0.50    0.05    --  -86.25  37.00-150.00   50
 23  \w   -110.00 -75.00   0.50    0.05    --  -86.25 -37.00 -30.00   70
 24  \w   -116.00 -78.00   0.50    0.05    --  -86.25 -57.00 -60.00   76
 25  \w     38.00  63.00   0.50    0.05    --  107.74 -57.00   0.00   50
 26  \w     42.00 102.00   0.50    0.05    --  107.74 -99.00 -60.00  120
 27  \w     70.00  96.00   0.50    0.05    --  107.74 -99.00 120.00   52
 28  \w     40.00  66.00   0.50    0.05    --  107.74 -99.00 120.00   52
 29  \w     39.00  64.00   0.50    0.05    --  107.74 -57.00 150.00   50
 30  \w     39.00  65.00   0.50    0.05    --  107.74 -57.00 120.00   52
 31  \w     50.00  76.00   0.50    0.05    --  107.74 -77.00 -30.00   52
 32  \w    136.00 162.00   0.50    0.05    --  107.74  57.00 -90.00   52
 33  \w     93.00 121.00   0.50    0.05    --  107.74  57.00 -90.00   56
 34  \w     78.00 105.00   0.50    0.05    --  107.74 -77.00 -30.00   54
 35  \w     37.00  63.00   0.50    0.05    --  107.74 -99.00 150.00   52
 36  \w     81.00 106.00   0.50    0.05    --  107.74 -99.00 150.00   50
 37  \w     35.00  62.00   0.50    0.05    --  107.74 -57.00-150.00   54
 38  \w     36.00  61.00   0.50    0.05    --  107.74 -57.00  60.00   50
 39  \w    153.00 178.00   0.50    0.05    --  107.74  77.00 150.00   50
 40  \w     95.00 146.00   0.50    0.05    --  107.74  77.00 150.00  102
;
_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      0.0844461000
_diffrn_orient_matrix_UB_12      -0.2319382000
_diffrn_orient_matrix_UB_13      0.2079772000
_diffrn_orient_matrix_UB_21      0.0504401000
_diffrn_orient_matrix_UB_22      -0.1285351000
_diffrn_orient_matrix_UB_23      -0.1375292000
_diffrn_orient_matrix_UB_31      0.2650936000
_diffrn_orient_matrix_UB_32      -0.0049188000
_diffrn_orient_matrix_UB_33      -0.0029311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2005
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.212
_diffrn_reflns_theta_min         7.168
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             150
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0710P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                852
_reflns_number_total             904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra06591j2.cif
_cod_data_source_block           SMC-08d
_cod_original_cell_volume        236.93(3)
_cod_database_code               7247872
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.451
_shelx_estimated_absorpt_t_max   0.649
_oxdiff_exptl_absorpt_empirical_full_min 0.464
_oxdiff_exptl_absorpt_empirical_full_max 2.464
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01971a9481dbc9edd4bf0532ae455d72d8000528f4b
;
_diffrn_oxdiff_digest_hkl
;
01e7c01dcc564b9677f12782b244a9fcdfb2b7
;
_shelx_res_checksum              34611
_shelx_hkl_checksum              19874