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_7063261
_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         'C34 H44 Co O4 P4 S4, C24 H20 B'
_chemical_formula_sum            'C58 H64 B Co O4 P4 S4'
_chemical_formula_weight         1146.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                90.966(6)
_cell_angle_beta                 93.440(6)
_cell_angle_gamma                98.915(5)
_cell_formula_units_Z            4
_cell_length_a                   11.4920(7)
_cell_length_b                   18.9820(13)
_cell_length_c                   25.9740(19)
_cell_measurement_reflns_used    4300
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.2550
_cell_measurement_theta_min      3.3500
_cell_volume                     5585.5(7)
_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 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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_unetI/netI     0.1353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.965
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         24627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15849
_reflns_number_total             24627
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9921\% 
around [0.00 0.00 1.00] (reciprocal) or [0.14 0.04 0.99] (direct)
;
_cod_data_source_file            d4nj02358g2.cif
_cod_data_source_block           e22gkk5
_cod_depositor_comments
'Adding full bibliography for 7063261--7063262.cif.'
_cod_database_code               7063261
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.926
_oxdiff_exptl_absorpt_empirical_full_min 0.558
_oxdiff_exptl_absorpt_empirical_full_max 1.647
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              59572