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_4512458
_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         'C15 H25 N3 Ni S, 2(Cl O4)'
_chemical_formula_sum            'C15 H25 Cl2 N3 Ni O8 S'
_chemical_formula_weight         537.05
_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             2012-03-09
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                93.470(7)
_cell_angle_beta                 106.608(7)
_cell_angle_gamma                93.681(7)
_cell_formula_units_Z            2
_cell_length_a                   8.7289(7)
_cell_length_b                   8.7999(7)
_cell_length_c                   13.9708(11)
_cell_measurement_reflns_used    4032
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5558
_cell_measurement_theta_min      3.3096
_cell_volume                     1022.76(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -41.00    8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -120.0000 49

  2 omega  -25.00   24.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 49

  3 omega   35.00   67.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 32

  4 omega -117.00  -88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000 -155.0000    3.0000 29

  5 omega  -97.00  -54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  155.0000 -139.0000 43

  6 omega   29.00  122.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   37.0000 -150.0000 93

  7 omega   86.00  113.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -120.0000 27

  8 omega   38.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   37.0000  -60.0000 82

  9 omega   26.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -77.0000 -180.0000 40

 10 omega   79.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 45

 11 omega   19.00  112.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -155.0000  139.0000 93

 12 omega   38.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 34

 13 omega  108.00  137.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000   30.0000 29

 14 omega   38.00   71.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 33

 15 omega   41.00   79.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 38

 16 omega   37.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 35

 17 omega   86.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -82.0000 27

 18 omega   95.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  103.0000 27

 19 omega   42.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 30

 20 omega   40.00  143.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   13.0000 103

 21 omega   37.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 31

 22 omega   37.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 35

 23 omega   76.00  152.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000  -30.0000 76

 24 omega   38.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 34

 25 omega   74.00  129.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  155.0000   40.0000 55

 26 omega   42.00   81.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 39

 27 omega   49.00   77.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  150.0000 28

 28 omega   45.00   70.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 25

 29 omega   40.00   72.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 32

 30 omega  142.00  169.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000   30.0000 27

 31 omega   42.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  168.0000 67

 32 omega  129.00  172.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -180.0000 43

 33 omega   42.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  103.0000 25

 34 omega   40.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -113.0000 67
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1015039000
_diffrn_orient_matrix_UB_12      0.0599533000
_diffrn_orient_matrix_UB_13      0.1066425000
_diffrn_orient_matrix_UB_21      -0.1364143000
_diffrn_orient_matrix_UB_22      -0.0580743000
_diffrn_orient_matrix_UB_23      0.0417150000
_diffrn_orient_matrix_UB_31      0.0724956000
_diffrn_orient_matrix_UB_32      -0.1549796000
_diffrn_orient_matrix_UB_33      0.0148048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6453
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    5.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0680P)^2^+2.2530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                3438
_reflns_number_total             3610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501534h_si_002.cif
_cod_data_source_block           030612a_gchen
_cod_depositor_comments
'Adding full bibliography for 4512457--4512460.cif.'
_cod_original_cell_volume        1022.76(14)
_cod_database_code               4512458
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13