Catalysis of proton reduction by a [BO4]-bridged dicobalt glyoxime.
Laga, Stephanie M.; Blakemore, James D.; Henling, Lawrence M.; Brunschwig, Bruce S.; Gray, Harry B.; Inorganic chemistry 53 (2014) 12668–12670; doi:10.1021/ic501804h

data_4350704
_publ_section_title
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 Catalysis of proton reduction by a [BO4]-bridged dicobalt glyoxime.
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_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12668
_journal_page_last               12670
_journal_paper_doi               10.1021/ic501804h
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C16 H26 B Cl4 Co2 N8 O8, C2 H3 N, C8 H20 N'
_chemical_formula_sum            'C26 H49 B Cl4 Co2 N10 O8'
_chemical_formula_weight         900.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                109.121(2)
_cell_angle_beta                 102.053(2)
_cell_angle_gamma                90.025(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5189(7)
_cell_length_b                   12.7064(7)
_cell_length_c                   13.0978(8)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.97
_cell_measurement_theta_min      2.29
_cell_volume                     1919.78(19)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            288113
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         43.747
_diffrn_reflns_theta_min         1.668
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8420.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       blade
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.284
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         29359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.284
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22276
_reflns_number_total             29359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501804h_si_002.cif
_cod_data_source_block           a14113
_cod_original_cell_volume        1919.77(19)
_cod_database_code               4350704
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Others
 Sof(H3)=1-FVAR(1)
 Sof(H1)=FVAR(1)
 Sof(H6)=1-FVAR(2)
 Sof(H8)=FVAR(2)
;