Molecular Precursor Mediated Selective Synthesis of Phase Pure Cubic InSe and Hexagonal In2Se3 Nanostructures: New Anode Materials for Li-ion Batteries
Karmakar, Gourab; Dutta Pathak, Dipa; Tyagi, Adish; Mandal, Balaji P.; Wadawale, Amey; Gotluru, Kedarnath; Dalton Transactions  (2023) –; doi:10.1039/D3DT00234A

data_7712809
_publ_section_title
;
 Molecular Precursor Mediated Selective Synthesis of Phase Pure Cubic InSe
 and Hexagonal In2Se3 Nanostructures: New Anode Materials for Li-ion
 Batteries
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00234A
_journal_year                    2023
_chemical_formula_moiety         'C18 H18 In N3 Se3'
_chemical_formula_sum            'C18 H18 In N3 Se3'
_chemical_formula_weight         628.05
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-02-16 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   12.69060(10)
_cell_length_b                   12.69060(10)
_cell_length_c                   44.8678(5)
_cell_measurement_reflns_used    24466
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.8600
_cell_measurement_theta_min      2.9630
_cell_volume                     6257.92(10)
_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_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SIR-2014 (Burla et al., 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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     27.00 120.00   0.50    0.49    --   47.82  73.00 -48.00  186
  2  \w    105.00 178.00   0.50    1.96    --  107.75 107.00-102.00  146
  3  \w    146.00 178.00   0.50    1.96    --  107.75  73.00 -48.00   64
  4  \w    152.00 178.00   0.50    1.96    --  107.75  30.00 -60.00   52
  5  \w    128.00 177.00   0.50    1.96    --  107.75  30.00 -90.00   98
  6  \w    110.00 178.00   0.50    1.96    --  107.75  45.00-150.00  136
  7  \w    112.00 138.00   0.50    1.96    --  107.75 125.00   0.00   52
  8  \w     85.00 178.00   0.50    1.96    --  107.75  77.00  30.00  186
  9  \w    145.00 177.00   0.50    1.96    --  107.75  45.00 150.00   64
 10  \w    108.00 137.00   0.50    1.96    --  107.75  15.00 120.00   58
 11  \w     97.00 123.00   0.50    1.96    --  107.75  45.00 150.00   52
 12  \w     85.00 178.00   0.50    1.96    --  107.75  77.00 120.00  186
 13  \w     96.00 154.00   0.50    1.96    --  107.75  30.00  30.00  116
 14  \w     85.00 178.00   0.50    1.96    --  107.75  77.00 -90.00  186
 15  \w     89.00 169.00   0.50    1.96    --  107.75  77.00-120.00  160
 16  \w     92.00 174.00   0.50    1.96    --  107.75  61.00 -60.00  164
 17  \w     89.00 138.00   0.50    1.96    --  107.75  73.00 -48.00   98
 18  \w     35.00  79.00   0.50    1.96    --  107.75 -66.00-156.00   88
 19  \w     76.00 106.00   0.50    1.96    --  107.75 -77.00-150.00   60
 20  \w     43.00  70.00   0.50    1.96    --  107.75 -61.00 -60.00   54
 21  \w     35.00  71.00   0.50    1.96    --  107.75 -61.00-120.00   72
 22  \w     35.00  85.00   0.50    1.96    --  107.75 -94.00-150.00  100
 23  \w     36.00  67.00   0.50    1.96    --  107.75 -61.00-150.00   62
 24  \w     36.00 121.00   0.50    0.49    --   47.82  37.00 -90.00  170
 25  \w     35.00  71.00   0.50    1.96    --  107.75 -61.00  30.00   72
 26  \w     37.00  71.00   0.50    1.96    --  107.75 -61.00  60.00   68
 27  \w     35.00 105.00   0.50    1.96    --  107.75 -89.00 167.00  140
 28  \w    -42.00  25.00   0.50    0.49    --  -47.82  37.00 120.00  134
 29  \w    -51.00 -14.00   0.50    1.96    --  -86.25  45.00 -30.00   74
 30  \w    -80.00 -13.00   0.50    1.96    --  -86.25  90.00  38.00  134
 31  \w    -26.00  28.00   0.50    0.49    --  -47.82  19.00-180.00  108
 32  \w   -119.00 -73.00   0.50    0.49    --  -47.82-125.00-150.00   92
 33  \w   -159.00 -65.00   0.50    1.96    --  -86.25 -73.00-177.00  188
 34  \w   -159.00 -79.00   0.50    1.96    --  -86.25 -90.00 -76.00  160
 35  \w   -159.00 -63.00   0.50    1.96    --  -86.25 -77.00 -60.00  192
 36  \w   -119.00 -73.00   0.50    0.49    --  -47.82-125.00 120.00   92
;
_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      -0.0019640000
_diffrn_orient_matrix_UB_12      0.1190872000
_diffrn_orient_matrix_UB_13      -0.0050808000
_diffrn_orient_matrix_UB_21      0.1061564000
_diffrn_orient_matrix_UB_22      0.0660845000
_diffrn_orient_matrix_UB_23      0.0221223000
_diffrn_orient_matrix_UB_31      0.0914885000
_diffrn_orient_matrix_UB_32      0.0332467000
_diffrn_orient_matrix_UB_33      -0.0257598000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            26964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.069
_diffrn_reflns_theta_min         4.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17309
_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    2.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0227P)^2^+23.7760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1462
_reflns_number_total             1476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00234a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        6257.91(12)
_cod_database_code               7712809
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.211
_shelx_estimated_absorpt_t_max   0.314
_oxdiff_exptl_absorpt_empirical_full_min 0.413
_oxdiff_exptl_absorpt_empirical_full_max 13.104
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
010219db2a2d69689e7aa1f7ae6a55b693000303047
;
_diffrn_oxdiff_digest_hkl
;
01403167101b4d6de734d1347946895b01bade
;
_shelx_res_checksum              80614
_shelx_hkl_checksum              40914