A molecular precursor approach for the synthesis of hollow nanotubes and nanorods of antimonselite (Sb<sub>2</sub>Se<sub>3</sub>): an efficient electrocatalyst for hydrogen evolution reactions.
Kulkarni, Atharva Y.; Majumder, Dwaipayan; Tripathi, Vaidehi S.; Kedarnath, G.; Wadawale, Amey P.; Singh, Vishal; Chauhan, Rohit Singh; Karmakar, Gourab; Tyagi, Adish; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6550–6562; doi:10.1039/d4dt03435j

data_7718332
_publ_section_title
;
 A molecular precursor approach for the synthesis of hollow nanotubes and
 nanorods of antimonselite (Sb<sub>2</sub>Se<sub>3</sub>): an efficient
 electrocatalyst for hydrogen evolution reactions.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6550
_journal_page_last               6562
_journal_paper_doi               10.1039/d4dt03435j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C11 H12 Cl3 N2 Sb Se)'
_chemical_formula_sum            'C22 H24 Cl6 N4 Sb2 Se2'
_chemical_formula_weight         958.616
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-12-03 deposited with the CCDC.	2025-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                111.195(1)
_cell_angle_beta                 103.242(1)
_cell_angle_gamma                94.756(1)
_cell_formula_units_Z            1
_cell_length_a                   6.4400(1)
_cell_length_b                   11.6756(2)
_cell_length_c                   11.8559(2)
_cell_measurement_reflns_used    13763
_cell_measurement_temperature    298
_cell_measurement_theta_max      76.1520
_cell_measurement_theta_min      4.1450
_cell_volume                     795.45(2)
_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    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9715
_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    -99.00 -52.00   0.50    0.05    --  -47.82 144.00  -6.00   94
  2  \w   -114.00 -89.00   0.50    0.05    --  -47.82-144.00 -60.00   50
  3  \w   -118.00 -77.00   0.50    0.05    --  -47.82-126.00 108.00   82
  4  \w    -74.00 -49.00   0.50    0.05    --  -47.82 126.00-175.00   50
  5  \w     47.00  99.00   0.50    0.05    --   47.82-144.00 -60.00  104
  6  \w     37.00  93.00   0.50    0.05    --   47.82-126.00 108.00  112
  7  \w    -75.00 -49.00   0.50    0.05    --  -86.25 126.00-175.00   52
  8  \w   -131.00-106.00   0.50    0.05    --  -86.25-144.00 -60.00   50
  9  \w   -126.00 -95.00   0.50    0.05    --  -86.25-126.00 108.00   62
 10  \w    113.00 139.00   0.50    0.05    --  107.74 144.00  -6.00   52
 11  \w     79.00 111.00   0.50    0.05    --  107.74-126.00 108.00   64
 12  \w    101.00 126.00   0.50    0.05    --  107.74-144.00 -60.00   50
 13  \w    101.00 147.00   0.50    0.05    --  107.74 126.00-175.00   92
 14  \w    -58.00 -31.00   0.50    0.05    --   10.00 158.00 -95.40   54
 15  \w     -7.00  18.00   0.50    0.05    --   26.00  99.00 131.56   50
 16  \w    -50.00 -25.00   0.50    0.05    --  -47.82 -77.00  30.00   50
 17  \w    -63.00 -35.00   0.50    0.05    --  -47.82 -37.00 120.00   56
 18  \w    -77.00 -26.00   0.50    0.05    --  -47.82 -77.00 120.00  102
 19  \w     37.00  69.00   0.50    0.05    --   47.82  37.00 -30.00   64
 20  \w     45.00 120.00   0.50    0.05    --   47.82  19.00 -90.00  150
 21  \w     37.00  63.00   0.50    0.05    --   47.82  57.00   0.00   52
 22  \w   -101.00 -75.00   0.50    0.05    --  -50.00 -80.00-136.29   52
 23  \w    -60.00 -26.00   0.50    0.05    --  -50.00 -79.00  89.40   68
 24  \w    -52.00 -26.00   0.50    0.05    --  -50.00 -80.00-136.29   52
 25  \w     26.00  51.00   0.50    0.05    --   50.00  80.00-116.71   50
 26  \w   -111.00 -85.00   0.50    0.05    --  -54.00 -78.00 -42.11   52
 27  \w    -62.00 -31.00   0.50    0.05    --  -54.00 -78.00 -11.72   62
 28  \w    -56.00 -31.00   0.50    0.05    --  -54.00 -78.00 -42.11   50
 29  \w     34.00  61.00   0.50    0.05    --   54.00  70.00 -87.72   54
 30  \w     32.00  57.00   0.50    0.05    --   54.00  75.00-164.89   50
 31  \w     89.00 126.00   0.50    0.05    --   54.00  78.00 113.31   74
 32  \w     30.00  56.00   0.50    0.05    --   54.00  79.00  78.91   52
 33  \w     31.00  57.00   0.50    0.05    --   54.00  78.00 113.31   52
 34  \w     71.00  96.00   0.50    0.05    --   54.00  77.00 -43.19   50
 35  \w     31.00  56.00   0.50    0.05    --   54.00  77.00 -43.19   50
 36  \w     36.00  61.00   0.50    0.05    --   58.00  75.00 -13.53   50
 37  \w    -72.00 -47.00   0.50    0.05    --  -62.00 -61.00-131.48   50
 38  \w     39.00  64.00   0.50    0.05    --   62.00  77.00  65.64   50
 39  \w   -123.00 -98.00   0.50    0.05    --  -66.00 -65.00-105.76   50
 40  \w    -73.00 -47.00   0.50    0.05    --  -66.00 -68.00 -66.15   52
 41  \w    -73.00 -48.00   0.50    0.05    --  -66.00 -65.00-105.76   50
 42  \w    -69.00 -43.00   0.50    0.05    --  -66.00 -77.00-165.09   52
 43  \w    -76.00 -50.00   0.50    0.05    --  -66.00 -63.00 108.55   52
 44  \w   -139.00-113.00   0.50    0.05    --  -66.00 -63.00 108.55   52
 45  \w     45.00  71.00   0.50    0.05    --   66.00  73.00 124.73   52
 46  \w    -80.00 -55.00   0.50    0.05    --  -70.00 -60.00 138.38   50
 47  \w    -74.00 -48.00   0.50    0.05    --  -70.00 -80.00   2.63   52
 48  \w    -88.00 -49.00   0.50    0.05    --  -70.00 -72.00  60.32   78
 49  \w    -91.00 -59.00   0.50    0.05    --  -74.00 -60.00-143.52   64
 50  \w    -85.00 -55.00   0.50    0.05    --  -74.00 -67.00 -34.33   60
 51  \w    -83.00 -58.00   0.50    0.05    --  -74.00 -60.00 127.83   50
 52  \w   -122.00 -89.00   0.50    0.05    --  -74.00 -60.00 127.83   66
 53  \w    -84.00 -56.00   0.50    0.05    --  -74.00 -66.00 -46.27   56
 54  \w    -91.00 -66.00   0.50    0.05    --  -82.00 -60.00 101.87   50
 55  \w   -157.00-131.00   0.50    0.05    --  -86.25 -77.00  30.00   52
 56  \w    -97.00 -66.00   0.50    0.05    --  -86.25 -70.00  68.23   62
 57  \w   -158.00-100.00   0.50    0.05    --  -86.25 -71.00  36.58  116
 58  \w   -148.00-123.00   0.50    0.05    --  -86.25 -77.00 120.00   50
 59  \w   -107.00 -66.00   0.50    0.05    --  -86.25 -71.00 -29.73   82
 60  \w    -97.00 -66.00   0.50    0.05    --  -86.25 -72.00   1.53   62
 61  \w    -89.00 -64.00   0.50    0.05    --  -86.25 -77.00  90.00   50
 62  \w   -101.00 -67.00   0.50    0.05    --  -86.25 -68.00  96.44   68
 63  \w    -93.00 -63.00   0.50    0.05    --  -86.25 -77.00 120.00   60
 64  \w   -100.00 -63.00   0.50    0.05    --  -86.25 -77.00 -60.00   74
 65  \w   -137.00 -67.00   0.50    0.05    --  -86.25 -69.00 -49.27  140
 66  \w    -88.00 -63.00   0.50    0.05    --  -86.25 -77.00-150.00   50
 67  \w    -99.00 -65.00   0.50    0.05    --  -86.25 -77.00 150.00   68
 68  \w   -157.00-116.00   0.50    0.05    --  -86.25 -77.00 150.00   82
 69  \w   -159.00-111.00   0.50    0.05    --  -86.25 -77.00-150.00   96
 70  \w    -88.00 -63.00   0.50    0.05    --  -86.25 -77.00 -30.00   50
 71  \w   -129.00 -66.00   0.50    0.05    --  -86.25 -73.00  12.03  126
 72  \w    -89.00 -63.00   0.50    0.05    --  -86.25 -77.00  60.00   52
 73  \w   -112.00 -65.00   0.50    0.05    --  -86.25 -77.00-120.00   94
 74  \w   -129.00 -66.00   0.50    0.05    --  -86.25 -78.00 -74.33  126
 75  \w    -42.00 -16.00   0.50    0.05    --  -86.25  37.00 -60.00   52
 76  \w    -88.00 -63.00   0.50    0.05    --  -86.25 -77.00 -90.00   50
 77  \w    -96.00 -66.00   0.50    0.05    --  -86.25 -71.00  36.58   60
 78  \w   -102.00 -73.00   0.50    0.05    --  -86.25 -71.00-167.98   58
 79  \w   -158.00-124.00   0.50    0.05    --  -86.25 -71.00-167.98   68
 80  \w    -88.00 -63.00   0.50    0.05    --  -86.25 -77.00  30.00   50
 81  \w    -93.00 -67.00   0.50    0.05    --  -86.25 -77.00-180.00   52
 82  \w     92.00 178.00   0.50    0.05    --  107.74  77.00-150.00  172
 83  \w     79.00 105.00   0.50    0.05    --  107.74-125.00-120.00   52
 84  \w    118.00 172.00   0.50    0.05    --  107.74  37.00 -60.00  108
 85  \w     36.00  70.00   0.50    0.05    --  107.74-125.00-120.00   68
 86  \w     90.00 155.00   0.50    0.05    --  107.74  77.00  30.00  130
 87  \w     37.00 103.00   0.50    0.05    --  107.74 -99.00 -30.00  132
 88  \w     71.00  99.00   0.50    0.05    --  107.74-125.00 -30.00   56
 89  \w     40.00  91.00   0.50    0.05    --  107.74 -99.00-180.00  102
 90  \w     38.00  64.00   0.50    0.05    --  107.74-125.00 -30.00   52
 91  \w     77.00 108.00   0.50    0.05    --  107.74-125.00  60.00   62
 92  \w     81.00 106.00   0.50    0.05    --  107.74 -77.00 -60.00   50
 93  \w     38.00  63.00   0.50    0.05    --  107.74 -57.00 -60.00   50
 94  \w     72.00 106.00   0.50    0.05    --  107.74 -77.00-150.00   68
 95  \w     35.00  74.00   0.50    0.05    --  107.74-125.00  60.00   78
 96  \w    140.00 167.00   0.50    0.05    --  107.74  77.00-180.00   54
 97  \w    104.00 142.00   0.50    0.05    --  107.74  37.00   0.00   76
 98  \w    108.00 177.00   0.50    0.05    --  107.74  37.00 -90.00  138
 99  \w     87.00 130.00   0.50    0.05    --  107.74  77.00-180.00   86
100  \w     43.00  69.00   0.50    0.05    --  107.74 -77.00 -60.00   52
101  \w     39.00  70.00   0.50    0.05    --  107.74 -99.00-120.00   62
102  \w    150.00 178.00   0.50    0.05    --  107.74  37.00   0.00   56
103  \w     94.00 124.00   0.50    0.05    --  107.74  57.00 150.00   60
104  \w    104.00 129.00   0.50    0.05    --  107.74  19.00  30.00   50
105  \w     35.00  66.00   0.50    0.05    --  107.74 -57.00  90.00   62
106  \w    113.00 177.00   0.50    0.05    --  107.74  37.00-180.00  128
107  \w     68.00 101.00   0.50    0.05    --  107.74 -77.00  90.00   66
108  \w    127.00 170.00   0.50    0.05    --  107.74 125.00-150.00   86
109  \w     95.00 120.00   0.50    0.05    --  107.74 125.00-150.00   50
110  \w     76.00 101.00   0.50    0.05    --  107.74 -77.00   0.00   50
111  \w     95.00 166.00   0.50    0.05    --  107.74  19.00 120.00  142
112  \w     38.00  64.00   0.50    0.05    --  107.74 -77.00   0.00   52
113  \w     37.00  63.00   0.50    0.05    --  107.74 -57.00-120.00   52
114  \w     36.00  66.00   0.50    0.05    --  107.74 -57.00 120.00   60
;
_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      0.0149825000
_diffrn_orient_matrix_UB_12      -0.1200231000
_diffrn_orient_matrix_UB_13      0.0251491000
_diffrn_orient_matrix_UB_21      0.0785117000
_diffrn_orient_matrix_UB_22      0.0789260000
_diffrn_orient_matrix_UB_23      0.1427911000
_diffrn_orient_matrix_UB_31      -0.2368329000
_diffrn_orient_matrix_UB_32      -0.0091701000
_diffrn_orient_matrix_UB_33      0.0062250000
_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  0.1424
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9715
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22734
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9715
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.01
_diffrn_reflns_theta_min         4.13
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08491
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_description       block
_exptl_crystal_F_000             457.902
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.5151
_refine_diff_density_min         -3.3365
_refine_diff_density_rms         0.5523
_refine_ls_d_res_high            0.7912
_refine_ls_d_res_low             10.7028
_refine_ls_goodness_of_fit_ref   1.1082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    22
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1082
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.2535
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2798
_reflns_number_total             3273
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03435j2.cif
_cod_data_source_block           AT-777b-d
_cod_depositor_comments          'Adding full bibliography for 7718332.cif.'
_cod_database_code               7718332
_chemical_oxdiff_formula         'Sb2 Cl6 N4 C20 Se2 H20'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C10(H10), C9(H9), C8(H8), C7(H7)
2.c Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11)
2.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c)
;
_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 6.513
_oxdiff_exptl_absorpt_empirical_full_min 0.347