Synthesis of photo-responsive indium selenides (InSe and In2Se3) from tris(4,6-dimethyl-2-pyrimidylselenolato)indium(iii) as a molecular precursor
Karmakar, Gourab; Shah, Alpa Y.; Tyagi, Adish; Wadawale, A. P.; Kedarnath, G.; Kumar, N. Naveen; Bahadur, Jitendra; New Journal of Chemistry 46 (2022) 3871–3881; doi:10.1039/D1NJ06167D

data_7061250
_publ_section_title
;
 Synthesis of photo-responsive indium selenides (InSe and In2Se3) from
 tris(4,6-dimethyl-2-pyrimidylselenolato)indium(iii) as a molecular
 precursor
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3871
_journal_page_last               3881
_journal_paper_doi               10.1039/D1NJ06167D
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C18 H21 In N6 Se3'
_chemical_formula_weight         673.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9248(2)
_cell_length_b                   14.9880(2)
_cell_length_c                   22.0289(3)
_cell_measurement_reflns_used    18685
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.5920
_cell_measurement_theta_min      3.5950
_cell_volume                     4927.71(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.962
_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   -118.00 -75.00   0.50    0.99    --  -48.29-123.00  62.00   86
  2  \w   -118.00 -91.00   0.50    0.99    --  -48.29-149.00-100.00   54
  3  \w     48.00  73.00   0.50    0.99    --   48.29-123.00  62.00   50
  4  \w     64.00  89.00   0.50    4.50    --  107.39-149.00-100.00   50
  5  \w     66.00 110.00   0.50    4.50    --  107.39-123.00  62.00   88
  6  \w     84.00 145.00   0.50    4.50    --  107.39 149.00 -53.00  122
  7  \w    -20.00  23.00   0.50    0.99    --  -48.29  19.00-180.00   86
  8  \w   -112.00 -75.00   0.50    0.99    --  -48.29-125.00 120.00   74
  9  \w    -17.00   8.00   0.50    0.99    --  -48.29  19.00 -90.00   50
 10  \w    -20.00  21.00   0.50    0.99    --  -48.29  19.00 -60.00   82
 11  \w    -42.00 -17.00   0.50    4.50    --  -86.25  37.00 -30.00   50
 12  \w    -42.00 -14.00   0.50    4.50    --  -86.25  37.00 -90.00   56
 13  \w    -41.00 -16.00   0.50    4.50    --  -86.25  37.00 -60.00   50
 14  \w    -41.00 -16.00   0.50    4.50    --  -86.25  37.00   0.00   50
 15  \w     98.00 123.00   0.50    4.50    --  107.39 125.00  60.00   50
 16  \w    114.00 170.00   0.50    4.50    --  107.39  19.00 150.00  112
 17  \w     35.00  63.00   0.50    4.50    --  107.39 -57.00  60.00   56
 18  \w     41.00  66.00   0.50    4.50    --  107.39 -57.00-180.00   50
 19  \w     43.00  99.00   0.50    4.50    --  107.39 -77.00  30.00  112
 20  \w    147.00 173.00   0.50    4.50    --  107.39 125.00  60.00   52
 21  \w     38.00  63.00   0.50    4.50    --  107.39 -57.00  30.00   50
 22  \w     36.00  62.00   0.50    4.50    --  107.39 -57.00-120.00   52
;
_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      0.0995131000
_diffrn_orient_matrix_UB_12      -0.0124088000
_diffrn_orient_matrix_UB_13      -0.0165795000
_diffrn_orient_matrix_UB_21      0.0229355000
_diffrn_orient_matrix_UB_22      -0.0129685000
_diffrn_orient_matrix_UB_23      0.0676079000
_diffrn_orient_matrix_UB_31      -0.0150803000
_diffrn_orient_matrix_UB_32      -0.1012130000
_diffrn_orient_matrix_UB_33      -0.0066087000
_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  0.0980
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22624
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.925
_diffrn_reflns_theta_min         4.014
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13463
_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            colourless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+3.6640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4648
_reflns_number_total             5013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj06167d3.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7061250.cif.'
_cod_database_code               7061250
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.249
_shelx_estimated_absorpt_t_max   0.360
_oxdiff_exptl_absorpt_empirical_full_min 0.327
_oxdiff_exptl_absorpt_empirical_full_max 3.195
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01140c1adf916017c7d541fcd34bce322c000291d39
;
_diffrn_oxdiff_digest_hkl
;
013ba77f3fc972b1a2836e5d78a6458475ade4
;
_shelx_res_checksum              36775
_shelx_fab_checksum              12942