Dual Homogeneous and Heterogeneous Pathways in Photo- and Electrocatalytic Hydrogen Evolution with Nickel(II) Catalysts Bearing Tetradentate Macrocyclic Ligands
Chen, Lingjing; Chen, Gui; Leung, Chi-Fai; Yiu, Shek-Man; Ko, Chi-Chiu; Anxolabéhère-Mallart, Elodie; Robert, Marc; Lau, Tai-Chu; ACS Catalysis 5 (2015) 356–; doi:10.1021/cs501534h

data_4512457
_publ_section_title
;
 Dual Homogeneous and Heterogeneous Pathways in Photo- and
 Electrocatalytic Hydrogen Evolution with Nickel(II) Catalysts Bearing
 Tetradentate Macrocyclic Ligands
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              356
_journal_paper_doi               10.1021/cs501534h
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C21 H26 N3 Ni P, 2(Cl O4), 0.5(C2 H3 N)'
_chemical_formula_sum            'C22 H27.5 Cl2 N3.5 Ni O8 P'
_chemical_formula_weight         629.55
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-08
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.390(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.443(2)
_cell_length_b                   8.4569(7)
_cell_length_c                   22.9631(16)
_cell_measurement_reflns_used    7585
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5533
_cell_measurement_theta_min      3.2531
_cell_volume                     5271.1(7)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'CU K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15276
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    3.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0574
_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^)+(0.1026P)^2^+15.9655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                4116
_reflns_number_total             4652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501534h_si_004.cif
_cod_data_source_block           060512a_chen
_cod_depositor_comments
'Adding full bibliography for 4512457--4512460.cif.'
_cod_original_cell_volume        5271.0(7)
_cod_original_formula_sum        'C22 H27.50 Cl2 N3.50 Ni O8 P'
_cod_database_code               4512457