Oxygen Activation and Intramolecular C-H Bond Activation by an Amidate-Bridged Diiron(II) Complex
Matthew B. Jones; Kenneth I. Hardcastle; Karl S. Hagen; Cora E. MacBeth; Inorganic Chemistry 50 (2011) 6402–6404; doi:10.1021/ic2007183

data_4325678
_publ_contact_author_address
;1515 Dickey Drive
Department of Chemistry
Emory University
Atlanta, GA 30322
;
_publ_contact_author_email       cmacbet@emory.edu
_publ_contact_author_name        'Cora E. MacBeth'
_publ_contact_author_phone       404-727-7033
_publ_section_title
;
 Oxygen Activation and Intramolecular C-H Bond Activation by an
 Amidate-Bridged Diiron(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6402
_journal_page_last               6404
_journal_paper_doi               10.1021/ic2007183
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H32 Fe N4 O4, C24 H20 P'
_chemical_formula_sum            'C54 H52 Fe N4 O4 P'
_chemical_formula_weight         907.82
_chemical_name_common            (PPh4)[Fe(L-O)]
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-04-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.3796(5)
_cell_length_b                   13.1251(2)
_cell_length_c                   35.6256(8)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      66.73
_cell_measurement_theta_min      3.64
_cell_volume                     11361.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23082
_diffrn_reflns_theta_full        66.92
_diffrn_reflns_theta_max         66.92
_diffrn_reflns_theta_min         3.64
_diffrn_source                   'sealed tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.4
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2007/2 (Bruker,2007) was used for absorption correction.
 R(int) was 0.0726 before and 0.0379 after correction.
 The Ratio of minimum to maximum transmission is 0.854031079825.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_recrystallization_method
'slow diffusion of diethyl ether into conc. DMF solution of the product'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0563
_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^)+(0.1122P)^2^+2.6909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                6633
_reflns_number_total             8854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2007183_si_002_1.cif
_cod_data_source_block           mbj_0124s
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4325678