Studies of a Series of [Ni(PR2NPh2)2(CH3CN)]2+ Complexes as Electrocatalysts for H2 Production: Substituent Variation at the Phosphorus Atom of the P2N2 Ligand
Uriah J. Kilgore; Michael P. Stewart; Monte L. Helm; William G. Dougherty; W. Scott Kassel; Mary Rakowski DuBois; Daniel L. DuBois; R. Morris Bullock; Inorganic Chemistry 50 (2011) 10908–10918; doi:10.1021/ic201461a

data_4326678
_publ_section_title
;
 Studies of a Series of [Ni(PR2NPh2)2(CH3CN)]2+ Complexes as
 Electrocatalysts for H2 Production: Substituent Variation at the
 Phosphorus Atom of the P2N2 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10908
_journal_page_last               10918
_journal_paper_doi               10.1021/ic201461a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C60 H64 N4 Ni P4'
_chemical_formula_sum            'C60 H64 N4 Ni P4'
_chemical_formula_weight         1023.74
_chemical_name_common            Ni(PBz2NPh2)2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.048(2)
_cell_angle_beta                 83.100(2)
_cell_angle_gamma                87.433(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1225(4)
_cell_length_b                   13.6857(5)
_cell_length_c                   19.1016(6)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.82
_cell_measurement_theta_min      2.42
_cell_volume                     2512.77(16)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57371
_diffrn_reflns_theta_full        31.82
_diffrn_reflns_theta_max         31.82
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.7676
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         17001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+1.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                14963
_reflns_number_total             17001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201461a_si_002_3.cif
_cod_data_source_block           helm071
_cod_database_code               4326678