Co(III) Imidos Exhibiting Spin Crossover and C-H Bond Activation
Evan R. King; Graham T. Sazama; Theodore A. Betley; Journal of the American Chemical Society 134 (2012) 17858–17861; doi:10.1021/ja307699u

data_4118846
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02139
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Professor Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Co(III) Imidos Exhibiting Spin Crossover and C-H Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17858
_journal_page_last               17861
_journal_paper_doi               10.1021/ja307699u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C74 H67 Co N6, C4 H10 O'
_chemical_formula_sum            'C78 H77 Co N6 O'
_chemical_formula_weight         1173.39
_chemical_name_common            ArDpmeCo(N4tBu2)
_chemical_name_systematic
; 
5-mesityl-1,9-bis(2,4,6-triphenylphenyl)dipyrrinatocobalt(III) 
di-tert-butyltetrazene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.842(6)
_cell_angle_beta                 102.272(4)
_cell_angle_gamma                101.405(4)
_cell_formula_units_Z            2
_cell_length_a                   11.464(3)
_cell_length_b                   14.775(5)
_cell_length_c                   18.824(4)
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      11.6932
_cell_measurement_theta_min      2.1581
_cell_volume                     3034.2(15)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker D8 goniometer with CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1510
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9629
_diffrn_reflns_theta_full        13.90
_diffrn_reflns_theta_max         13.90
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9963
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2009)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.1122
_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^)+(0.1450P)^2^+10.8382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2797
_refine_ls_wR_factor_ref         0.3127
_reflns_number_gt                5230
_reflns_number_total             9629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307699u_si_002_6.cif
_cod_data_source_block           ArDpmeCoN4tBu2
_cod_original_cell_volume        3034.5(13)
_cod_database_code               4118846