Molecular precursor mediated facile synthesis of photo-responsive stibnite Sb2S3 nanorods and tetrahedrite Cu12Sb4S13 nanocrystals
Thomas, Agnes; Karmakar, Gourab; Shah, Alpa Y.; Lokhande, Saili Vikram; Kulkarni, Atharva Yeshwant; Tyagi, Adish; Chauhan, Rohit Singh; Kumar, N. Naveen; Singh, Avadhesh Pratap; Dalton Transactions  (2022) –; doi:10.1039/D2DT01814D

data_7710757
_publ_section_title
;
 Molecular precursor mediated facile synthesis of photo-responsive
 stibnite Sb2S3 nanorods and tetrahedrite Cu12Sb4S13 nanocrystals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01814D
_journal_year                    2022
_chemical_formula_moiety         'C18 H22 N6 S3 Sb'
_chemical_formula_sum            'C18 H22 N6 S3 Sb'
_chemical_formula_weight         540.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.704(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.315(3)
_cell_length_b                   11.378(3)
_cell_length_c                   15.490(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.317
_cell_volume                     2253.9(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18931
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         2.396
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1489 before and 0.0966 after correction.
The Ratio of minimum to maximum transmission is 0.5435.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0076P)^2^+4.6171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3146
_reflns_number_total             4106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01814d2.cif
_cod_data_source_block           saili1_0m_a
_cod_original_cell_volume        2253.8(9)
_cod_database_code               7710757
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.565
_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:
 C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C),
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              50983
_shelx_hkl_checksum              76419
_olex2_submission_special_instructions 'No special instructions were received'