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_4512459
_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         'C30 H42 Cl2 N6 Ni2 S2, 2(Cl O4)'
_chemical_formula_sum            'C30 H42 Cl4 N6 Ni2 O8 S2'
_chemical_formula_weight         938.04
_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             2012-05-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                91.373(5)
_cell_angle_beta                 99.117(5)
_cell_angle_gamma                93.388(5)
_cell_formula_units_Z            2
_cell_length_a                   8.0156(5)
_cell_length_b                   12.2115(8)
_cell_length_c                   19.7215(12)
_cell_measurement_reflns_used    6425
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      73.7093
_cell_measurement_theta_min      3.6249
_cell_volume                     1901.6(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -24.00   26.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 50

  2 omega  -47.00   16.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  -30.0000 63

  3 omega   31.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 41

  4 omega -105.00  -32.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000 -150.0000 73

  5 omega   26.00  123.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000 -180.0000 97

  6 omega  -14.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000   30.0000 77

  7 omega   81.00  106.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000    0.0000 25

  8 omega   19.00   83.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -77.0000  -30.0000 64

  9 omega   77.00  123.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   30.0000 46

 10 omega  -61.00    9.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000   30.0000 70

 11 omega  -52.00   -5.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   50.0000 -180.0000 47

 12 omega -105.00  -79.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000 -180.0000 26

 13 omega   38.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 32

 14 omega   94.00  178.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 84

 15 omega   94.00  168.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000  -30.0000 74

 16 omega   44.00   78.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -60.0000 34

 17 omega   41.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 30

 18 omega   39.00  141.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -132.0000 102

 19 omega   85.00  146.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 61

 20 omega   42.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 29

 21 omega   38.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 34

 22 omega   81.00  141.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   41.0000 60

 23 omega   45.00   76.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 31

 24 omega   41.00   83.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 42

 25 omega   38.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 34

 26 omega   37.00   62.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 25

 27 omega   39.00   64.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 25

 28 omega   37.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 30

 29 omega   55.00   83.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   60.0000 28

 30 omega  135.00  170.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  111.0000 -150.0000 35

 31 omega  137.00  175.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -180.0000 38

 32 omega   44.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   41.0000 26

 33 omega   38.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 32

 34 omega   87.00  116.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  116.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1282282000
_diffrn_orient_matrix_UB_12      0.0358005000
_diffrn_orient_matrix_UB_13      -0.0608075000
_diffrn_orient_matrix_UB_21      -0.0690329000
_diffrn_orient_matrix_UB_22      -0.1201575000
_diffrn_orient_matrix_UB_23      -0.0142826000
_diffrn_orient_matrix_UB_31      -0.1297550000
_diffrn_orient_matrix_UB_32      0.0164348000
_diffrn_orient_matrix_UB_33      0.0486295000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12668
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    5.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52611
_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            red
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.445
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6732
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0551P)^2^+11.6310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                5879
_reflns_number_total             6732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501534h_si_003.cif
_cod_data_source_block           051412a_chen
_cod_depositor_comments
'Adding full bibliography for 4512457--4512460.cif.'
_cod_database_code               4512459
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13