Organometallic Ni Pincer Complexes for the Electrocatalytic Production of Hydrogen
Oana R. Luca; James D. Blakemore; Steven J. Konezny; Jeremy M. Praetorius; Timothy J. Schmeier; Glendon B. Hunsinger; Victor S. Batista; Gary W. Brudvig; Nilay Hazari; Robert H. Crabtree; Inorganic Chemistry 51 (2012) 8704–8709; doi:10.1021/ic300009a

data_4329994
_publ_contact_author
;
 Dr R. H. Crabtree           
 The Department of Chemistry 
 Yale University 
 P. O. Box 208107 
 New Haven 
 Connecticut 06520 USA.
;
_publ_contact_author_email       nilay.hazari@yale.edu
_publ_contact_author_fax         '+1 203 432 6144'
_publ_contact_author_phone       '+1 203 432 0885'
_publ_section_title
;
 Organometallic Ni Pincer Complexes for the Electrocatalytic Production of
 Hydrogen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8704
_journal_page_last               8709
_journal_paper_doi               10.1021/ic300009a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'P2 N2 C28 H49 Ni B F4'
_chemical_formula_sum            'C28 H49 B F4 N2 Ni P2'
_chemical_formula_weight         621.16
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-12-23
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.242(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   10.4927(18)
_cell_length_b                   15.606(3)
_cell_length_c                   10.6505(18)
_cell_measurement_reflns_used    12093
_cell_measurement_temperature    223
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      3.32
_cell_volume                     1625.5(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD (SCX mini)'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12989
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             660.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.340
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3023 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.003(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                5183
_reflns_number_total             6348
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300009a_si_001.cif
_cod_data_source_block           '_Compound3-ACN+'
_cod_original_formula_sum        'P2 N2 C28 H49 Ni B F4'
_cod_database_code               4329994