Insights into the supramolecular and molecular electrocatalytic properties of 1,2-bis(diphenylphosphine)ethane appended nickel(ii) 1,2-dithiosquarate for oxygen and hydrogen evolution reactions
Kushwaha, Aparna; Srivastava, Devyani; Kociok-Köhn, Gabriele; Padwal, Yogita; Chauhan, Ratna; Gosavi, Suresh W.; Muddassir, Mohd.; Kumar, Abhinav; New Journal of Chemistry 48 (2024) 3717–3728; doi:10.1039/D4NJ00247D

data_7062986
_publ_section_title
;
 Insights into the supramolecular and molecular electrocatalytic
 properties of 1,2-bis(diphenylphosphine)ethane appended nickel(ii)
 1,2-dithiosquarate for oxygen and hydrogen evolution reactions
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3717
_journal_page_last               3728
_journal_paper_doi               10.1039/D4NJ00247D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C30 H24 Ni O2 P2 S2'
_chemical_formula_sum            'C30 H24 Ni O2 P2 S2'
_chemical_formula_weight         601.26
_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
;
2024-01-12 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.425(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3624(4)
_cell_length_b                   14.1583(4)
_cell_length_c                   17.0895(6)
_cell_measurement_reflns_used    11586
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5430
_cell_measurement_theta_min      3.1700
_cell_volume                     2726.17(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44123
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.541
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83530
_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    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl2, MeOH 1:1'
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0422P)^2^+4.1141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5371
_reflns_number_total             6929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00247d2.cif
_cod_data_source_block           e23gkk12
_cod_depositor_comments          'Adding full bibliography for 7062986.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7062986
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.937
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_oxdiff_exptl_absorpt_empirical_full_max 1.222
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              77197
_shelx_hkl_checksum              15317