Production of H2 at fast rates using a nickel electrocatalyst in water-acetonitrile solutions
Wesley A. Hoffert; John A. S. Roberts; R. Morris Bullock; Monte L. Helm; Chem.Commun. 49 (2013) 7767–; doi:10.1039/c3cc43203c

data_7109661
_publ_section_title
;
 Production of H2 at fast rates using a nickel electrocatalyst in
 water-acetonitrile solutions
;
_journal_name_full               Chem.Commun.
_journal_page_first              7767
_journal_paper_doi               10.1039/c3cc43203c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C58 H59 N5 Ni O4 P4, 2(B F4), 1.6(C4 H10 O)'
_chemical_formula_sum            'C64.4 H75 B2 F8 N5 Ni O5.6 P4'
_chemical_formula_weight         1364.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           21
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2 2'
_symmetry_space_group_name_H-M   'C 2 2 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1339(14)
_cell_length_b                   23.3855(14)
_cell_length_c                   20.0338(15)
_cell_measurement_reflns_used    5565
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.59
_cell_volume                     7090.2(9)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0130
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6038
_diffrn_reflns_theta_full        24.84
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.9195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2845
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Platon SQUEEZE was used to remove the contribution of 1.6 
heavily disordered exogeneous diethyl ether molecules that 
could not be modeled in the difference map.
A total of 304  electrons in 1754 cubic angstroms of 
accessible unit cell void volume were removed. Since Z = 4, 
this translates to an average of 69 e- per whole complex 
molecule, consistent with approximately 1.6 exogenous diethyl 
ether molecules (42 e- each). This roughly matches the 
obtained elemental analysis of a crystalline sample 
see main text).
;
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.1879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                4871
_reflns_number_total             5920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43203c.txt
_cod_data_source_block           wh044z_sq_d
_cod_original_sg_symbol_H-M      C222
_cod_original_formula_sum        'C64.40 H75 B2 F8 N5 Ni O5.60 P4'
_cod_database_code               7109661