1,2-Bis-(diphenylphosphino)ethane (dppe) appended cobalt(iii)-dithiocarbamates as single source precursors of cobalt sulfide/cobalt phosphide composites: apt electrocatalytic materials for water splitting reactions
Srivastava, Devyani; Kushwaha, Aparna; Sudheer,; Kociok-Köhn, Gabriele; Singh, Ashish Kumar; Muddassir, Mohd.; Kumar, Abhinav; New Journal of Chemistry 48 (2024) 9366–9375; doi:10.1039/D4NJ01285B

data_7063196
_publ_section_title
;
 1,2-Bis-(diphenylphosphino)ethane (dppe) appended
 cobalt(iii)-dithiocarbamates as single source precursors of cobalt
 sulfide/cobalt phosphide composites: apt electrocatalytic materials for
 water splitting reactions
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9366
_journal_page_last               9375
_journal_paper_doi               10.1039/D4NJ01285B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C40 H52 Co N2 P2 S4, F6 P'
_chemical_formula_sum            'C40 H52 Co F6 N2 P3 S4'
_chemical_formula_weight         954.91
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
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_cell_measurement_temperature    150(2)
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_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
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_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~
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.265
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5124
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+12.9530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4285
_reflns_number_total             5124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01285b1.cif
_cod_data_source_block           e22gkk10
_cod_depositor_comments
'Adding full bibliography for 7063195--7063197.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7063196
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.830
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.073
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              76971