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_4118845
_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         '2(C75 H60 Co N3), 3(C4 H10 O)'
_chemical_formula_sum            'C81 H75 Co N3 O1.5'
_chemical_formula_weight         1173.37
_chemical_name_common            ArDpmeCo(NH(C6H2-2,4-Me2)-6-CH2)
_chemical_name_systematic
; 
5-mesityl-1,9-bis(2,4,6-triphenylphenyl)dipyrrinato
-5,7-dimethyl-2-cobalt(III)-metallacycloindoline 
;
_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                70.312(2)
_cell_angle_beta                 70.894(2)
_cell_angle_gamma                78.788(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7041(13)
_cell_length_b                   16.763(2)
_cell_length_c                   17.822(2)
_cell_measurement_reflns_used    12043
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.8607
_cell_measurement_theta_min      2.1617
_cell_volume                     3096.9(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer with CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58807
_diffrn_reflns_theta_full        14.60
_diffrn_reflns_theta_max         14.60
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.9964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2009)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         11272
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0955P)^2^+3.4069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1928
_reflns_number_gt                7462
_reflns_number_total             11272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307699u_si_002_5.cif
_cod_data_source_block           ArDpmeCoNMes
_cod_original_formula_sum        'C81 H75 Co N3 O1.50'
_cod_database_code               4118845