Unusual Electronic Structure of First Row Transition Metal Complexes Featuring Redox-Active Dipyrromethane Ligands
Evan R. King; Theodore A. Betley; Journal of the American Chemical Society 131 (2009) 14374–14380; doi:10.1021/ja903997a

data_4105099
_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
;
 Unusual Electronic Structure of First Row Transition Metal Complexes
 Featuring Redox-Active Dipyrromethane Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14374
_journal_page_last               14380
_journal_paper_doi               10.1021/ja903997a
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C41 H56 Cl Co Li N2 O3'
_chemical_formula_sum            'C41 H56 Cl Co Li N2 O3'
_chemical_formula_weight         726.20
_chemical_name_common            '[(dmpm)CoCl(THF)][Li(THF)2]'
_chemical_name_systematic
;   
(mono-tetrahydrofuran)(1,9-dimesitly-5,5-dimethyldipyrromethanato)cobalt(II)
chloride (bis-tetrahydrofuran)lithiate
;
_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                 103.487(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7199(7)
_cell_length_b                   12.6669(5)
_cell_length_c                   22.8413(12)
_cell_measurement_reflns_used    1172
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.3587
_cell_measurement_theta_min      2.2170
_cell_volume                     3860.1(3)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'SMART V5.625 (Bruker AXS, 2001a)'
_computing_data_reduction
; 
SAINT V7.34A (Bruker AXS, 2006), SADABS (Bruker AXS, 2004) 
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'omega scans 0.5%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_sigmaI/netI    0.2071
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23487
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.9158
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent light blue'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       prism
_exptl_crystal_F_000             1548
_exptl_crystal_recrystallization_method tetrahydrofuran
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8650
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1955
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                3702
_reflns_number_total             8650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903997a_si_001_6.cif
_cod_data_source_block           compound8-erk001
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105099