New heteroleptic bis-(diphenylphosphino)ethane appended dialkyldithiophosphate cobalt(iii) cations: apt electrocatalysts for the heterogeneous oxygen evolution reaction and homogeneous hydrogen evolution reaction
Srivastava, Devyani; Daniel, Omoding; Kushwaha, Aparna; Kociok-Köhn, Gabriele; Gosavi, Suresh W.; Chauhan, Ratna; Muddassir, Mohd.; Kumar, Abhinav; New Journal of Chemistry 48 (2024) 12217–12226; doi:10.1039/D4NJ02358G

data_7063262
_publ_section_title
;
 New heteroleptic bis-(diphenylphosphino)ethane appended
 dialkyldithiophosphate cobalt(iii) cations: apt electrocatalysts for the
 heterogeneous oxygen evolution reaction and homogeneous hydrogen
 evolution reaction
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12217
_journal_page_last               12226
_journal_paper_doi               10.1039/D4NJ02358G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'2(C38 H52 Co O4 P4 S4), C26 H24 O0.32 P2 S1.68, 2(C24 H20 B)'
_chemical_formula_sum            'C75 H84 B Co O4.16 P5 S4.84'
_chemical_formula_weight         1431.72
_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-2018/3
_audit_update_record
;
2024-05-17 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6417(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4413(2)
_cell_length_b                   30.6056(6)
_cell_length_c                   21.3033(4)
_cell_measurement_reflns_used    19325
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5730
_cell_measurement_theta_min      3.2680
_cell_volume                     7375.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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-2018/3 (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.
;
_computing_structure_solution
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_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 0.883
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.826
_diffrn_reflns_theta_min         2.911
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             3007
_exptl_crystal_size_max          0.608
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         17034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.9249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12707
_reflns_number_total             17034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02358g2.cif
_cod_data_source_block           e22gkk7
_cod_depositor_comments
'Adding full bibliography for 7063261--7063262.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063262
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.741
_shelx_estimated_absorpt_t_max   0.917
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_exptl_absorpt_empirical_full_max 1.657
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              9789