Phase-controlled solvothermal syntheses and oxygen evolution reaction (OER) activity of nickel sulfide nanoparticles obtained from 1,2-bis(diphenylphosphino)ethane nickel(ii) acetylacetonatedithiolate
Singh, Ayushi; Singh, Amita; Kociok-Köhn, Gabriele; Chauhan, Ratna; Gosavi, Suresh W.; Singh, Anar; Singh, Ashish Kumar; Kumar, Abhinav; Muddassir, Mohd.; New Journal of Chemistry 46 (2022) 10246–10255; doi:10.1039/D2NJ01177H

data_7061466
_publ_section_title
;
 Phase-controlled solvothermal syntheses and oxygen evolution reaction
 (OER) activity of nickel sulfide nanoparticles obtained from
 1,2-bis(diphenylphosphino)ethane nickel(ii) acetylacetonatedithiolate
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10246
_journal_page_last               10255
_journal_paper_doi               10.1039/D2NJ01177H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C32 H30 Ni O2 P2 S2, C H Cl3'
_chemical_formula_sum            'C33 H31 Cl3 Ni O2 P2 S2'
_chemical_formula_weight         750.70
_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-2014/7
_audit_update_record
;
2022-01-26 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                89.198(2)
_cell_angle_beta                 74.574(2)
_cell_angle_gamma                81.894(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6800(3)
_cell_length_b                   12.5165(3)
_cell_length_c                   13.2741(4)
_cell_measurement_reflns_used    10932
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.8750
_cell_measurement_theta_min      3.9820
_cell_volume                     1692.90(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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-2014/7 (Sheldrick, 2014)
 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 
G.M.Sheldrick,Acta Crystallogr.,Sect. A: Found.Crystallogr., 2008, 64,112-122.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_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 0.881
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25119
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.280
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0275P)^2^+0.7457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7300
_reflns_number_total             8921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01177h2.cif
_cod_data_source_block           e16gkk4
_cod_depositor_comments          'Adding full bibliography for 7061466.cif.'
_cod_database_code               7061466
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.620
_shelx_estimated_absorpt_t_max   0.816
_oxdiff_exptl_absorpt_empirical_full_min 0.870
_oxdiff_exptl_absorpt_empirical_full_max 1.270
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              35944