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_4126217
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H22 Co K N2 O3'
_chemical_formula_sum            'C24 H22 Co K N2 O3'
_chemical_formula_weight         484.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.098(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.650(2)
_cell_length_b                   15.4996(18)
_cell_length_c                   7.5174(9)
_cell_measurement_reflns_used    2204
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.3270
_cell_measurement_theta_min      3.5290
_cell_volume                     2169.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -93.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -180.0000 93

  2 omega  -55.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  -60.0000 91

  3 omega  -96.00   -6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000   60.0000 90

  4 omega  -52.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000   30.0000 90

  5 omega -103.00  -65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  177.0000   61.0000 38

  6 omega  -96.00   -6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  -60.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0328442000
_diffrn_orient_matrix_UB_12      -0.0229062000
_diffrn_orient_matrix_UB_13      0.0023529000
_diffrn_orient_matrix_UB_21      0.0179545000
_diffrn_orient_matrix_UB_22      -0.0387914000
_diffrn_orient_matrix_UB_23      -0.0204378000
_diffrn_orient_matrix_UB_31      0.0069122000
_diffrn_orient_matrix_UB_32      -0.0080067000
_diffrn_orient_matrix_UB_33      0.0922851000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11150
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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)
;
_exptl_crystal_colour            'lustrous dark black'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.079
_refine_diff_density_max         2.188
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2272
_reflns_number_gt                3933
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b03604_si_003.cif
_cod_data_source_block           vg352
_cod_depositor_comments
'Adding full bibliography for 4126214--4126217.cif.'
_cod_database_code               4126217
_chemical_oxdiff_formula         'Co C20 H20 N2 O2 K'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C14(H14), C5(H5), C12(H12), C3(H3), C16(H16), C9(H9), C19(H19),
 C17(H17), C2(H2), C4(H4), C18(H18), C11(H11), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'