Efficient photocatalytic water reduction by a cobalt(ii) tripodal iminopyridine complex
Leung, C.-F.; Cheng, S.-C.; Yang, Y.; Xiang, J.; Yiu, S.-M.; Ko, C.-C.; Lau, T.-C.; Catalysis Science & Technology 8 (2018) 307–; doi:10.1039/C7CY01524K

data_1548133
_publ_section_title
;
 Efficient photocatalytic water reduction by a cobalt(ii) tripodal
 iminopyridine complex
;
_journal_issue                   1
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              307
_journal_paper_doi               10.1039/C7CY01524K
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C24 H27 Co N7, 2(Cl O4)'
_chemical_formula_sum            'C24 H27 Cl2 Co N7 O8'
_chemical_formula_weight         671.36
_chemical_name_common            '[Co(trenpy3)](ClO4)2'
_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
;
'Tue Sep 29 09:40:27 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
;
2017-07-27 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 100.453(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   27.9963(7)
_cell_length_b                   10.5409(3)
_cell_length_c                   19.1609(5)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.7029
_cell_measurement_theta_min      3.6135
_cell_volume                     5560.7(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)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   38.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000    0.0000 38

  2 omega  -57.00  -12.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 45

  3 omega   47.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -90.0000 29

  4 omega   -2.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -110.0000  113.0000 49

  5 omega  -15.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000    0.0000 83

  6 omega   74.00  125.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -60.0000 51

  7 omega   79.00  110.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 31

  8 omega  -56.00   -5.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000 -180.0000 51

  9 omega  -76.00    4.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   63.0000  -30.0000 80

 10 omega   46.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 26

 11 omega   47.00   84.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -110.0000  -28.0000 37

 12 omega   46.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 26

 13 omega   38.00   67.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 29

 14 omega   44.00   69.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 25

 15 omega   42.00  119.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000   90.0000 77

 16 omega   89.00  176.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000 -150.0000 87

 17 omega   38.00   64.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 26

 18 omega   38.00   63.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 25

 19 omega   42.00   68.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 26

 20 omega   38.00   69.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 31

 21 omega   38.00   63.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 25

 22 omega   42.00  137.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -77.0000  -30.0000 95

 23 omega   39.00   69.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 30
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0518049000
_diffrn_orient_matrix_UB_12      0.0449731000
_diffrn_orient_matrix_UB_13      0.0314586000
_diffrn_orient_matrix_UB_21      0.0173914000
_diffrn_orient_matrix_UB_22      -0.0416354000
_diffrn_orient_matrix_UB_23      -0.0682950000
_diffrn_orient_matrix_UB_31      -0.0121389000
_diffrn_orient_matrix_UB_32      0.1326453000
_diffrn_orient_matrix_UB_33      -0.0320723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.1397
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12270
_diffrn_reflns_theta_full        71.84
_diffrn_reflns_theta_max         71.84
_diffrn_reflns_theta_min         4.49
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38977
_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            orange
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                4272
_reflns_number_total             5357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cy01524k2.cif
_cod_data_source_block           092515a_fai
_cod_depositor_comments          'Adding full bibliography for 1548133.cif.'
_cod_database_code               1548133
_cell_oxdiff_angle_alpha         90.025(5)
_cell_oxdiff_angle_beta          100.467(5)
_cell_oxdiff_angle_gamma         89.965(5)
_cell_oxdiff_length_a            27.9864(16)
_cell_oxdiff_length_b            10.5432(6)
_cell_oxdiff_length_c            19.1645(13)
_cell_oxdiff_measurement_reflns_used 3797
_cell_oxdiff_volume              5560.7(6)
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.70
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B),
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22)
;