C-H Bond Amination from a Ferrous Dipyrromethene Complex
Evan R. King; Theodore A. Betley; Inorganic Chemistry 48 (2009) 2361–2363; doi:10.1021/ic900219b

data_4301752
_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
;
C-H Bond Amination from a Ferrous Dipyrromethene Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2361
_journal_page_last               2363
_journal_paper_doi               10.1021/ic900219b
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C40 H45 Cl Fe N2 O'
_chemical_formula_sum            'C40 H45 Cl Fe N2 O'
_chemical_formula_weight         661.08
_chemical_name_common            PyacFeCl(THF)
_chemical_name_systematic
'(1,5,9-trimesityldipyrromethenato)iron(II) chloride tetrahydrofuran adduct)'
_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                 96.779(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0636(15)
_cell_length_b                   26.792(4)
_cell_length_c                   16.566(3)
_cell_measurement_reflns_used    1701
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.71
_cell_measurement_theta_min      2.48
_cell_volume                     3553.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.1157
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13433
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.7675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent light red'
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method 'diethyl ether'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                3413
_reflns_number_total             6253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900219b_si_002_1.cif
_cod_data_source_block           erk012
_cod_original_cell_volume        3553.8(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301752