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_4512460
_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         '2(Cl O4), C21 H30 N3 Ni P, C3 H6 O'
_chemical_formula_sum            'C24 H36 Cl2 N3 Ni O9 P'
_chemical_formula_weight         671.14
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2013-11-04
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;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                79.943(4)
_cell_angle_beta                 89.364(4)
_cell_angle_gamma                73.953(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3883(4)
_cell_length_b                   13.0308(6)
_cell_length_c                   13.0930(6)
_cell_measurement_reflns_used    5541
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5639
_cell_measurement_theta_min      3.4281
_cell_volume                     1514.52(12)
_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      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10621
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69419
_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_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.691
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         5379
_refine_ls_number_restraints     301
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.1106
_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^)+(0.0790P)^2^+17.7542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2796
_refine_ls_wR_factor_ref         0.2828
_reflns_number_gt                4895
_reflns_number_total             5379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501534h_si_005.cif
_cod_data_source_block           100213a_chen
_cod_depositor_comments
'Adding full bibliography for 4512457--4512460.cif.'
_cod_database_code               4512460