A noble metal-free photocatalytic system based on a novel cobalt tetrapyridyl catalyst for hydrogen production in fully aqueous medium
Queyriaux, N.; Giannoudis, E.; Windle, C. D.; Roy, S.; Pécaut, J.; Coutsolelos, A. G.; Artero, V.; Chavarot-Kerlidou, M.; Sustainable Energy & Fuels 2 (2018) 553–; doi:10.1039/C7SE00428A

data_1553989
_publ_section_title
;
 A noble metal-free photocatalytic system based on a novel cobalt
 tetrapyridyl catalyst for hydrogen production in fully aqueous medium
;
_journal_issue                   3
_journal_name_full               'Sustainable Energy &amp; Fuels'
_journal_page_first              553
_journal_paper_doi               10.1039/C7SE00428A
_journal_volume                  2
_journal_year                    2018
_chemical_formula_moiety         'C20 H20 Co N6 O2, 2(B F4)'
_chemical_formula_sum            'C20 H20 B2 Co F8 N6 O2'
_chemical_formula_weight         608.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2016-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.096(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3282(2)
_cell_length_b                   14.2177(3)
_cell_length_c                   14.6725(3)
_cell_measurement_reflns_used    3758
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      32.4350
_cell_measurement_theta_min      2.3090
_cell_volume                     2339.61(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  98.00   1.00   10.00    --   25.72  37.00  30.00   98
  2  \w     16.00  76.00   1.00   10.00    --   25.72-126.00 134.00   60
  3  \w     -9.00  90.00   1.00   10.00    --   25.72  19.00 150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005906000
_diffrn_orient_matrix_UB_12      0.0019135000
_diffrn_orient_matrix_UB_13      -0.0483800000
_diffrn_orient_matrix_UB_21      0.0618958000
_diffrn_orient_matrix_UB_22      -0.0101669000
_diffrn_orient_matrix_UB_23      0.0059091000
_diffrn_orient_matrix_UB_31      -0.0129337000
_diffrn_orient_matrix_UB_32      -0.0487984000
_diffrn_orient_matrix_UB_33      -0.0031409000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense orange'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.7437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5598
_reflns_number_total             7081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7se00428a2.cif
_cod_data_source_block           cw213
_cod_original_cell_volume        2339.63(8)
_cod_database_code               1553989
_chemical_oxdiff_formula         'Co N6 O2 C20 H20 B2 F8'
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Others
 Sof(F13B)=Sof(F14B)=1-FVAR(1)
 Sof(F13)=Sof(F14)=FVAR(1)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.049
_oxdiff_exptl_absorpt_empirical_full_min 0.948