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_4105100
_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         'C39 H40 Fe N4, 2 (C4 H8 O)'
_chemical_formula_sum            'C47 H56 Fe N4 O2'
_chemical_formula_weight         764.81
_chemical_name_common            (dmpm)Fe(bpy)
_chemical_name_systematic
;        
bipyridine (1,9-dimesityl-5,5-dimethyldipyrromethanato)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7737(3)
_cell_length_b                   23.0411(5)
_cell_length_c                   16.5575(4)
_cell_measurement_reflns_used    20294
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.42
_cell_volume                     4110.19(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72435
_diffrn_reflns_theta_full        29.68
_diffrn_reflns_theta_max         29.68
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.7824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method tetrahydrofuran
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         11617
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0520P)^2^+2.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                8922
_reflns_number_total             11617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903997a_si_001_7.cif
_cod_data_source_block           compound9-erk037
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105100