Metallosupramolecular Ni2L3 and Ni4L6 complexes of bis-bidentate pyridine-containing ligands: X-ray structures and catalytic proton reduction.
Tsang, Chui-Shan; Chen, Lingjing; Li, Lu-Wei; Yiu, Shek-Man; Lau, Tai-Chu; Kwong, Hoi-Lun; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13087–13092; doi:10.1039/c5dt01706h

data_7035334
_publ_section_title
;
 Metallosupramolecular Ni2L3 and Ni4L6 complexes of bis-bidentate
 pyridine-containing ligands: X-ray structures and catalytic proton
 reduction.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13087
_journal_page_last               13092
_journal_paper_doi               10.1039/c5dt01706h
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C78 H90 N12 Ni2, 4(Cl O4), 4.5(C2 H3 N)'
_chemical_formula_sum            'C87 H103.5 Cl4 N16.5 Ni2 O16'
_chemical_formula_weight         1895.58
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
;
'Thu Mar 12 10:56:41 2015'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                89.099(2)
_cell_angle_beta                 81.233(3)
_cell_angle_gamma                76.182(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5581(5)
_cell_length_b                   12.6724(4)
_cell_length_c                   29.7591(9)
_cell_measurement_reflns_used    17632
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6697
_cell_measurement_theta_min      3.0032
_cell_volume                     4544.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -72.00   19.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000 -120.0000 91

  2 omega  -29.00    1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   30.0000 30

  3 omega   36.00   63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -155.0000  143.0000 27

  4 omega   30.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   30.0000 35

  5 omega  -71.00   -4.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000   37.0000  -90.0000 67

  6 omega -109.00  -82.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000 -155.0000  143.0000 27

  7 omega  -76.00  -21.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000    0.0000 55

  8 omega   38.00   69.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000  150.0000 31

  9 omega   82.00  122.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  155.0000 -143.0000 40

 10 omega   74.00  108.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  150.0000 34

 11 omega -112.00  -15.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000  -60.0000 97

 12 omega -137.00   -9.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000    0.0000 -120.0000 128

 13 omega   92.00  164.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   90.0000 72

 14 omega   37.00   64.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 27

 15 omega   37.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 33

 16 omega   46.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 26

 17 omega   57.00  110.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -78.0000 53

 18 omega   79.00  104.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -131.0000 25

 19 omega   41.00   82.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 41

 20 omega   38.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 33

 21 omega   41.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 28

 22 omega   37.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 34

 23 omega   87.00  134.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  136.0000 47

 24 omega   48.00   74.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 26

 25 omega   41.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 30

 26 omega   42.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 25

 27 omega   41.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  150.0000 25

 28 omega   37.00   63.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 26

 29 omega   50.00   83.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   30.0000 33

 30 omega  108.00  134.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   -5.0000 26

 31 omega   47.00  104.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   -5.0000 57

 32 omega   39.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 33

 33 omega   43.00   83.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 40

 34 omega   88.00  178.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000    0.0000 90

 35 omega   39.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  136.0000 31

 36 omega   40.00   65.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -131.0000 25

 37 omega  108.00  134.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  -90.0000 26

 38 omega  142.00  168.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  -90.0000 26

 39 omega   43.00  120.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   60.0000 77
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0003540000
_diffrn_orient_matrix_UB_12      -0.0335961000
_diffrn_orient_matrix_UB_13      -0.0494937000
_diffrn_orient_matrix_UB_21      0.0953903000
_diffrn_orient_matrix_UB_22      0.0553520000
_diffrn_orient_matrix_UB_23      -0.0161540000
_diffrn_orient_matrix_UB_31      0.0851088000
_diffrn_orient_matrix_UB_32      -0.1071810000
_diffrn_orient_matrix_UB_33      0.0058523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
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_diffrn_reflns_theta_full        71.81
_diffrn_reflns_theta_max         71.81
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75333
_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            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1986
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.482
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2396
_refine_ls_number_reflns         20982
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+3.3350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                20270
_reflns_number_total             20982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01706h2.cif
_cod_data_source_block           021512a_luwei
_cod_depositor_comments
'Adding full bibliography for 7035333--7035334.cif.'
_cod_original_cell_volume        4544.0(3)
_cod_original_formula_sum        'C87 H103.50 Cl4 N16.50 Ni2 O16'
_cod_database_code               7035334
_cell_oxdiff_angle_alpha         89.099(2)
_cell_oxdiff_angle_beta          81.233(3)
_cell_oxdiff_angle_gamma         76.182(3)
_cell_oxdiff_length_a            12.5581(5)
_cell_oxdiff_length_b            12.6724(4)
_cell_oxdiff_length_c            29.7591(9)
_cell_oxdiff_measurement_reflns_used 17633
_cell_oxdiff_volume              4544.0(3)
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13