Ligand and Metal Based Multielectron Redox Chemistry of Cobalt Supported by Tetradentate Schiff Bases.
Andrez, Julie; Guidal, Valentin; Scopelliti, Rosario; Pécaut, Jacques; Gambarelli, Serge; Mazzanti, Marinella; Journal of the American Chemical Society 139 (2017) 8628–8638; doi:10.1021/jacs.7b03604

data_4126215
_publ_section_title
;
 Ligand and Metal Based Multielectron Redox Chemistry of Cobalt Supported
 by Tetradentate Schiff Bases.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8628
_journal_page_last               8638
_journal_paper_doi               10.1021/jacs.7b03604
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C46 H36 Co2 N4 Na2 O12, 2(C18 H36 N2 Na O6), 2(C4 H8 O)'
_chemical_formula_sum            'C90 H124 Co2 N8 Na4 O26'
_chemical_formula_weight         1943.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-10
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.568(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0036(13)
_cell_length_b                   14.5281(6)
_cell_length_c                   28.4397(14)
_cell_measurement_reflns_used    7768
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      21.6620
_cell_measurement_theta_min      3.3730
_cell_volume                     9062.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.905
_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    -13.00  14.00   1.00   75.00    --  -10.00 -99.00-120.00   27
  2  \w    -12.00  15.00   1.00   75.00    --  -10.00 -99.00  30.00   27
  3  \w    -19.00  31.00   1.00   75.00    --  -10.00 -99.00 150.00   50
  4  \w    -34.00  52.00   1.00   75.00    --  -10.00  37.00 150.00   86
  5  \w     -8.00  17.00   1.00   75.00    --  -10.00 -57.00 -60.00   25
  6  \w    -20.00   9.00   1.00   75.00    --  -10.00 -99.00 120.00   29
  7  \w    -38.00  23.00   1.00   75.00    --  -10.00  77.00 -90.00   61
  8  \w    -51.00  65.00   1.00   75.00    --  -10.00  19.00  60.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1984
_diffrn_reflns_av_unetI/netI     0.2479
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            104214
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.528
_diffrn_reflns_theta_min         3.296
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            black
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         22915
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2553
_refine_ls_R_factor_gt           0.0972
_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^)+(0.0859P)^2^+4.5930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9237
_reflns_number_total             22915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03604_si_007.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4126214--4126217.cif.'
_cod_database_code               4126215
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81238
_shelx_hkl_checksum              53257