Neutral heteroleptic nickel complexes incorporating maleonitriledithiolate and bis(diphenylphosphanyl)amine as robust molecular electrocatalysts for hydrogen evolution
Mou, Wen-Yu; Li, Tao; Xie, Bin; Zhang, Dong-Liang; Lai, Chuan; Deng, Cheng-Long; Cao, Jia-Xi; Bai, Xiao-Xue; Liu, Xiao-Qiang; Inorganica Chimica Acta 507 (2020) 119587–; doi:10.1016/j.ica.2020.119587

data_1564745
_publ_section_title
;
 Neutral heteroleptic nickel complexes incorporating
 maleonitriledithiolate and bis(diphenylphosphanyl)amine as robust
 molecular electrocatalysts for hydrogen evolution
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119587
_journal_paper_doi               10.1016/j.ica.2020.119587
_journal_volume                  507
_journal_year                    2020
_chemical_formula_sum            'C33 H31 N3 Ni P2 S2'
_chemical_formula_weight         654.38
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.184(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.34370(10)
_cell_length_b                   18.2134(2)
_cell_length_c                   18.7553(3)
_cell_measurement_reflns_used    4695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.3590
_cell_measurement_theta_min      4.8250
_cell_volume                     3107.66(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9672
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.988
_diffrn_reflns_theta_min         3.427
_exptl_absorpt_coefficient_mu    3.342
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00213(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0769P)^2^+0.3849P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4655
_reflns_number_total             5370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-507-119587.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564745
_shelx_estimated_absorpt_t_min   0.585
_shelx_estimated_absorpt_t_max   0.617
_shelxl_version_number           2013-2
_shelx_res_checksum              13223
_shelx_hkl_checksum              52530