Supramolecular and electrocatalytic OER properties of new heteroleptic fluoro- and trifluoromethyl-substituted Ni(ii)-dithiolates: effects of substituents and dihedral angle on the electrocatalytic performance
Kushwaha, Aparna; Srivastava, Devyani; Kociok-Köhn, Gabriele; Gosavi, Suresh W.; Chauhan, Ratna; Ahmed, Sarfaraz; Kumar, Abhinav; New Journal of Chemistry 48 (2024) 15856–15865; doi:10.1039/D4NJ03502J

data_7063415
_publ_section_title
;
 Supramolecular and electrocatalytic OER properties of new heteroleptic
 fluoro- and trifluoromethyl-substituted Ni(ii)-dithiolates: effects of
 substituents and dihedral angle on the electrocatalytic performance
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15856
_journal_page_last               15865
_journal_paper_doi               10.1039/D4NJ03502J
_journal_volume                  48
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C35 H28 F N Ni P2 S2'
_chemical_formula_sum            'C35 H28 F N Ni P2 S2'
_chemical_formula_weight         666.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.4415(2)
_cell_length_b                   12.8011(2)
_cell_length_c                   59.9701(7)
_cell_measurement_reflns_used    62851
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9040
_cell_measurement_theta_min      3.6210
_cell_volume                     9551.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2019/2 (Sheldrick, 2019)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2300
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_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  0.0930
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            181098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.700
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1176
_refine_ls_number_reflns         19179
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0809
_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^)+50.4574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                18730
_reflns_number_total             19179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03502j2.cif
_cod_data_source_block           s23gkk4
_cod_depositor_comments
'Adding full bibliography for 7063415--7063416.cif.'
_cod_database_code               7063415
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.642
_oxdiff_exptl_absorpt_empirical_full_min 0.689
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              13588
_shelx_hkl_checksum              93980