Homogeneous Photocatalytic Water Oxidation with a Dinuclear Co(III)-Pyridylmethylamine Complex.
Ishizuka, Tomoya; Watanabe, Atsuko; Kotani, Hiroaki; Hong, Dachao; Satonaka, Kenta; Wada, Tohru; Shiota, Yoshihito; Yoshizawa, Kazunari; Ohara, Kazuaki; Yamaguchi, Kentaro; Kato, Satoshi; Fukuzumi, Shunichi; Kojima, Takahiko; Inorganic chemistry 55 (2016) 1154–1164; doi:10.1021/acs.inorgchem.5b02336

data_4344711
_publ_section_title
;
 Homogeneous Photocatalytic Water Oxidation with a Dinuclear
 Co(III)-Pyridylmethylamine Complex.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1154
_journal_page_last               1164
_journal_paper_doi               10.1021/acs.inorgchem.5b02336
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C36 H38 Cl4 Co2 N8 O18'
_chemical_formula_weight         1130.40
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                76.576(5)
_cell_angle_beta                 83.789(5)
_cell_angle_gamma                67.032(5)
_cell_formula_units_Z            1
_cell_length_a                   10.317(5)
_cell_length_b                   12.086(5)
_cell_length_c                   12.301(5)
_cell_measurement_temperature    120(2)
_cell_volume                     1373.4(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'APEX2 v2009.11-0'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7584
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.421
_diffrn_reflns_theta_min         1.702
_exptl_absorpt_coefficient_mu    0.867
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
Two acetone molecules per the asymmetri unit were deleted with the sqeeze program.
;
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5812
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0908P)^2^+0.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3810
_reflns_number_total             5812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02336_si_003.cif
_cod_data_source_block           NABE1
_cod_database_code               4344711
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.983
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              15657
_shelx_hkl_checksum              15415