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_4326677
_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_sum            'C64 H102 B2 F8 N6 Ni O3 P4'
_chemical_formula_weight         1359.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.139(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7991(11)
_cell_length_b                   30.863(2)
_cell_length_c                   15.7859(10)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.46
_cell_volume                     6787.5(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            105527
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.21
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.9152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Squeeze result consistent with 3 THF and 1 acetonitrile solvent 
molecules in the asymmetric unit.  These were located from the difference
map but were disordered and would not adequately refine so they were removed.
They had no interaction with the main molecule of the crystal.

PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
                     Spek, A.L. (2009). Acta Cryst. D65, 148-155. 
;
_refine_diff_density_max         2.338
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         25697
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                15054
_reflns_number_total             25697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201461a_si_002_2.cif
_cod_data_source_block           pnl090s
_cod_database_code               4326677