Dinuclear Co(II)Co(III) Mixed-Valence and Co(III)Co(III) Complexes with N- and O-Donor Ligands: Characterization and Water Oxidation Studies
Jia Luo; Nigam P. Rath; Liviu M. Mirica; Inorganic Chemistry 50 (2011) 6152–6157; doi:10.1021/ic201031s

data_4325569
_publ_section_title
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 Dinuclear Co(II)Co(III) Mixed-Valence and Co(III)Co(III) Complexes with
 N- and O-Donor Ligands: Characterization and Water Oxidation Studies
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6152
_journal_page_last               6157
_journal_paper_doi               10.1021/ic201031s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H39 Cl2 Co2 N6 O12'
_chemical_formula_weight         864.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.908(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3731(8)
_cell_length_b                   12.9829(8)
_cell_length_c                   20.4445(13)
_cell_measurement_reflns_used    9005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.21
_cell_measurement_theta_min      2.54
_cell_volume                     3530.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            171558
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.52
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_correction_T_min  0.6699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2008/1'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         14974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+2.1117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                12503
_reflns_number_total             14974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201031s_si_002_1.cif
_cod_data_source_block           l2010
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4325569