Electrocatalytic proton reduction by a dicobalt tetrakis-schiff base macrocycle in nonaqueous electrolyte.
Kal, Subhadeep; Filatov, Alexander S.; Dinolfo, Peter H.; Inorganic chemistry 53 (2014) 7137–7145; doi:10.1021/ic500121f

data_4340104
_publ_section_title
;
 Electrocatalytic proton reduction by a dicobalt tetrakis-schiff base
 macrocycle in nonaqueous electrolyte.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7137
_journal_page_last               7145
_journal_paper_doi               10.1021/ic500121f
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C36 H51 Co2 N6 O4), 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C74 H105 Cl2 Co4 N13 O16'
_chemical_formula_weight         1739.33
_chemical_name_common            '[Co2LAc](ClO4)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 106.425(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.290(3)
_cell_length_b                   15.936(4)
_cell_length_c                   21.465(5)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.15
_cell_volume                     4032.4(17)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41963
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.8556
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0763P)^2^+4.3188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                7804
_reflns_number_total             9431
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic500121f_si_002.cif
_cod_data_source_block           '[Co2LAc](ClO4)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340104.cif.
;
_cod_original_cell_volume        4032.2(18)
_cod_original_sg_symbol_Hall     '-P 2yn      '
_cod_original_sg_symbol_H-M      'P 1 21/n 1  '
_cod_database_code               4340104