Selective synthesis of the missing tiara-like Ni<sub>10</sub>, Ni<sub>5</sub> and Ni<sub>6</sub> thiolates by the C-S bond cleavage of bis(thioether) molecules with a DFT study.
Debnath, Suparno; Giri, Sandip; Mani, Ganesan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14875–14886; doi:10.1039/d4dt02047b

data_7716831
_publ_section_title
;
 Selective synthesis of the missing tiara-like Ni<sub>10</sub>,
 Ni<sub>5</sub> and Ni<sub>6</sub> thiolates by the C-S bond cleavage of
 bis(thioether) molecules with a DFT study.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14875
_journal_page_last               14886
_journal_paper_doi               10.1039/d4dt02047b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C84 H84 Ni6 S12'
_chemical_formula_weight         1830.49
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-12 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8191(8)
_cell_length_b                   18.8191(8)
_cell_length_c                   23.116(3)
_cell_measurement_reflns_used    216649
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.329
_cell_measurement_theta_min      2.068
_cell_volume                     8186.7(12)
_computing_molecular_graphics    ortep
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 QUEST'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            216649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.329
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.6048
_exptl_absorpt_correction_T_min  0.4920
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       needle
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.006(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0201P)^2^+2.4514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6994
_reflns_number_total             7478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02047b2.cif
_cod_data_source_block           Ni6
_cod_depositor_comments
'Adding full bibliography for 7716829--7716831.cif.'
_cod_original_cell_volume        8186.7(13)
_cod_database_code               7716831
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              55651