New heteroleptic [Ni(ii) 1,1-dithiolate-phosphine] complexes: synthesis, characterization and electrocatalytic oxygen evolution studies.
Anamika, ?; Yadav, Dharmendra Kumar; Manar, Krishna K.; Yadav, Chote Lal; Kumar, Kamlesh; Ganesan, Vellaichamy; Drew, Michael G. B.; Singh, Nanhai; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3592–3605; doi:10.1039/c9dt04923a

data_7703593
_publ_section_title
;
 New heteroleptic [Ni(ii) 1,1-dithiolate-phosphine] complexes: synthesis,
 characterization and electrocatalytic oxygen evolution studies.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3592
_journal_page_last               3605
_journal_paper_doi               10.1039/c9dt04923a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C35 H34 Ni O2 P2 S2, H2 O'
_chemical_formula_sum            'C35 H36 Ni O3 P2 S2'
_chemical_formula_weight         689.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-24 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7845(9)
_cell_length_b                   15.2433(6)
_cell_length_c                   22.3400(9)
_cell_measurement_temperature    100(2)
_cell_volume                     6737.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103324
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_min         2.094
_exptl_absorpt_coefficient_mu    0.828
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8373
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0664P)^2^+8.4018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5963
_reflns_number_total             8373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04923a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7703591--7703594.cif.'
_cod_database_code               7703593
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1W-H1WB = O1W-H1WA
 0.85 with sigma of 0.02
 H1WB-H1WA
 1.375 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C16(H16A,H16B), C18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
3.c Idealised Me refined as rotating group:
 C171(H17A,H17B,H17C), C172(H17D,H17E,H17F)
;
_shelx_res_checksum              29840
_olex2_submission_special_instructions 'No special instructions were received'