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_7063416
_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_formula_moiety         'C36 H28 F3 N Ni P2 S2 [+ solvent]'
_chemical_formula_sum            'C36 H28 F3 N Ni P2 S2'
_chemical_formula_weight         716.36
_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_method           SHELXL-2019/3
_audit_update_record
;
2024-08-14 deposited with the CCDC.	2024-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.714(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   14.9884(4)
_cell_length_c                   19.4818(5)
_cell_measurement_reflns_used    7468
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1100
_cell_measurement_theta_min      3.2740
_cell_volume                     3361.71(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.94a (release 21-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.522
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 / MeOH'
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7365
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0572P)^2^+5.7237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5183
_reflns_number_total             7365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03502j2.cif
_cod_data_source_block           e24gkk8_sq
_cod_depositor_comments
'Adding full bibliography for 7063415--7063416.cif.'
_cod_original_cell_volume        3361.70(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063416
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.891
_oxdiff_exptl_absorpt_empirical_full_min 0.908
_oxdiff_exptl_absorpt_empirical_full_max 1.128
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              70351
_shelx_hkl_checksum              45284
_shelx_fab_checksum              53525