Supramolecular and homogeneous electrocatalytic HER properties of new heteroleptic cyanoacetamide dithiolate-based Ni(ii) tertiary phosphanes: effect of co-ligand flexibility on electrocatalytic performance
Srivastava, Shreya; Omoding, Daniel; Kushwaha, Aparna; Kociok-Köhn, Gabriele; Ahmed, Sarfaraz; Kumar, Abhinav; New Journal of Chemistry 48 (2024) 20268–20279; doi:10.1039/D4NJ04282D

data_7063538
_publ_section_title
;
 Supramolecular and homogeneous electrocatalytic HER properties of new
 heteroleptic cyanoacetamide dithiolate-based Ni(ii) tertiary phosphanes:
 effect of co-ligand flexibility on electrocatalytic performance
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20268
_journal_page_last               20279
_journal_paper_doi               10.1039/D4NJ04282D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C40 H32 N2 Ni O P2 S2 [+ solvent]'
_chemical_formula_sum            'C40 H32 N2 Ni O P2 S2'
_chemical_formula_weight         741.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-30 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.5021(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5993(3)
_cell_length_b                   16.68773(12)
_cell_length_c                   19.7885(2)
_cell_measurement_reflns_used    36041
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.6790
_cell_measurement_theta_min      3.2710
_cell_volume                     7449.44(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution
;
 SHELXT 2018/2 (Sheldrick, 2018)
 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.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.271
_diffrn_reflns_theta_min         3.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane-methanol (1:1)'
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         15543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0789P)^2^+5.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12600
_reflns_number_total             15543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04282d2.cif
_cod_data_source_block           Ni-3
_cod_depositor_comments
'Adding full bibliography for 7063536--7063538.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063538
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.745
_oxdiff_exptl_absorpt_empirical_full_min 0.743
_oxdiff_exptl_absorpt_empirical_full_max 1.471
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              95992
_shelx_hkl_checksum              68357
_shelx_fab_checksum              62320