Novel bismuth-selone molecular precursor based selective synthesis of Bi<sub>2</sub>Se<sub>3</sub> nanoplates and nanosheets: a promising electrocatalyst for hydrogen evolution in a neutral medium.
Kulkarni, Atharva Yeshwant; Majumder, Dwaipayan; Nigam, Sandeep; Tripathi, Vaidehi S.; Wadawale, Amey P.; Bahadur, Jitendra; Pathak, Ankita; Karmakar, Gourab; Chauhan, Rohit Singh; Tyagi, Adish; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3570–3585; doi:10.1039/d6dt00093b

data_7720087
_publ_section_title
;
 Novel bismuth-selone molecular precursor based selective synthesis of
 Bi<sub>2</sub>Se<sub>3</sub> nanoplates and nanosheets: a promising
 electrocatalyst for hydrogen evolution in a neutral medium.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3570
_journal_page_last               3585
_journal_paper_doi               10.1039/d6dt00093b
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C44 H48 Bi2 Cl6 N8 Se4, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H54 Bi2 Cl6 N10 Se4'
_chemical_formula_weight         1717.51
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-02-06 deposited with the CCDC.	2026-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                64.1150(10)
_cell_angle_beta                 67.9020(10)
_cell_angle_gamma                89.3250(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0388(2)
_cell_length_b                   11.96160(10)
_cell_length_c                   13.6884(2)
_cell_measurement_reflns_used    16886
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.6830
_cell_measurement_theta_min      3.9550
_cell_volume                     1481.24(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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.955
_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   -121.00 -50.00   0.50    0.16    --  -47.82 -33.00   2.00  142
  2  \w    -31.00  24.00   0.50    0.16    --  -47.82  33.00 161.00  110
  3  \w    -20.00  37.00   0.50    0.16    --   47.82 -33.00   2.00  114
  4  \w     67.00 119.00   0.50    0.16    --   47.82  33.00 161.00  104
  5  \w   -151.00-112.00   0.50    0.66    --  -86.25 -33.00   2.00   78
  6  \w    -38.00 -13.00   0.50    0.66    --  -86.25  33.00 161.00   50
  7  \w     98.00 172.00   0.50    0.66    --  107.74  33.00 161.00  148
  8  \w    -16.00  28.00   0.50    0.16    --  -47.82  19.00 -60.00   88
  9  \w    -81.00 -30.00   0.50    0.16    --  -47.82 125.00  30.00  102
 10  \w    -16.00  22.00   0.50    0.16    --  -47.82  19.00 -90.00   76
 11  \w     57.00  91.00   0.50    0.16    --   47.82-125.00  60.00   68
 12  \w    -13.00  26.00   0.50    0.16    --   47.82 -19.00-120.00   78
 13  \w    -42.00 -13.00   0.50    0.66    --  -86.25  37.00   0.00   58
 14  \w    -42.00 -17.00   0.50    0.66    --  -86.25  37.00-180.00   50
 15  \w    -40.00 -15.00   0.50    0.66    --  -86.25  37.00-150.00   50
 16  \w   -147.00-121.00   0.50    0.66    --  -86.25 -37.00-120.00   52
 17  \w    -42.00 -17.00   0.50    0.66    --  -86.25  37.00 -60.00   50
 18  \w    -79.00 -13.00   0.50    0.66    --  -86.25 125.00-150.00  132
 19  \w    -63.00 -15.00   0.50    0.66    --  -86.25  57.00  60.00   96
 20  \w    -42.00 -17.00   0.50    0.66    --  -86.25  37.00 -30.00   50
 21  \w     41.00  67.00   0.50    0.66    --  107.74-108.00-154.31   52
 22  \w     35.00  61.00   0.50    0.66    --  107.74 -99.00 -90.00   52
 23  \w     35.00  64.00   0.50    0.66    --  107.74 -57.00-180.00   58
 24  \w     35.00  66.00   0.50    0.66    --  107.74 -57.00 -60.00   62
 25  \w     49.00  75.00   0.50    0.66    --  107.74 -99.00-120.00   52
 26  \w     82.00 107.00   0.50    0.66    --  107.74-110.00   9.04   50
 27  \w     35.00  65.00   0.50    0.66    --  107.74 -57.00 -90.00   60
 28  \w     36.00  61.00   0.50    0.66    --  107.74 -57.00-120.00   50
 29  \w    132.00 165.00   0.50    0.66    --  107.74  19.00  90.00   66
 30  \w    100.00 178.00   0.50    0.66    --  107.74  57.00   0.00  156
 31  \w     98.00 151.00   0.50    0.66    --  107.74 125.00  90.00  106
 32  \w     40.00 106.00   0.50    0.66    --  107.74 -99.00-150.00  132
 33  \w     35.00 106.00   0.50    0.66    --  107.74 -99.00  90.00  142
 34  \w     41.00  82.00   0.50    0.66    --  107.74-107.00  51.91   82
 35  \w     95.00 120.00   0.50    0.66    --  107.74  19.00  90.00   50
 36  \w     64.00 103.00   0.50    0.66    --  107.74 -99.00 -90.00   78
 37  \w     64.00 103.00   0.50    0.66    --  107.74 -99.00 150.00   78
 38  \w     49.00  75.00   0.50    0.66    --  107.74-110.00   9.04   52
 39  \w     63.00 105.00   0.50    0.66    --  107.74 -99.00   0.00   84
 40  \w     40.00 105.00   0.50    0.66    --  107.74 -99.00 -60.00  130
 41  \w     38.00 100.00   0.50    0.66    --  107.74 -77.00  90.00  124
 42  \w    132.00 171.00   0.50    0.66    --  107.74  57.00-150.00   78
 43  \w     95.00 138.00   0.50    0.66    --  107.74 125.00-120.00   86
 44  \w     78.00 107.00   0.50    0.66    --  107.74-108.00-154.31   58
 45  \w     35.00  66.00   0.50    0.66    --  107.74 -57.00 150.00   62
 46  \w     51.00 107.00   0.50    0.66    --  107.74-102.00  79.61  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1345540000
_diffrn_orient_matrix_UB_12      0.0117904000
_diffrn_orient_matrix_UB_13      0.0077240000
_diffrn_orient_matrix_UB_21      -0.0127199000
_diffrn_orient_matrix_UB_22      -0.1448503000
_diffrn_orient_matrix_UB_23      0.0572544000
_diffrn_orient_matrix_UB_31      0.0721512000
_diffrn_orient_matrix_UB_32      0.0090200000
_diffrn_orient_matrix_UB_33      -0.1245738000
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18923
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.933
_diffrn_reflns_theta_min         3.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26174
_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            orange
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.598
_refine_diff_density_min         -2.628
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5967
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0269P)^2^+3.9617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             5967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00093b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7720087.cif.'
_cod_database_code               7720087
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.725
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_exptl_absorpt_empirical_full_max 2.154
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              96476
_shelx_hkl_checksum              85061