Oxidative N-Dealkylation of a Carboxylate-Bridged Diiron(II) Precursor Complex by Reaction with O2 Affords the Elusive {Fe2(μ-OH)2(μ-O2CR)}3+ Core of Soluble Methane Monooxygenase Hydroxylase
Dongwhan Lee; Stephen J. Lippard; Journal of the American Chemical Society 123 (2001) 4611–4612; doi:10.1021/ja0100930

data_4115545
_publ_section_title
;
 Oxidative N-Dealkylation of a Carboxylate-Bridged Diiron(II) Precursor
 Complex by Reaction with O2 Affords the Elusive {Fe2(\m-OH)2(\m-O2CR)}3+
 Core of Soluble Methane Monooxygenase Hydroxylase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4611
_journal_page_last               4612
_journal_paper_doi               10.1021/ja0100930
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C123.5 H109 Cl2 Fe2 N4 O10'
_chemical_formula_weight         1991.75
_chemical_name_common
'[Fe2(m-OH)2(m-O2CArTol)(O2CArTol)3(N-Bnen)(N,N-Bn2en)]'
_chemical_name_systematic
; 
 ? 
;
_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                95.570(2)
_cell_angle_beta                 108.017(2)
_cell_angle_gamma                104.939(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0043(18)
_cell_length_b                   16.907(2)
_cell_length_c                   24.019(3)
_cell_measurement_temperature    188(2)
_cell_volume                     5493.9(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      188(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48676
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.932736
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         24430
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+2.9076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                17220
_reflns_number_total             24430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0100930_4.cif
_cod_data_source_block           5
_cod_original_cell_volume        5493.8(11)
_cod_original_formula_sum        'C123.50 H109 Cl2 Fe2 N4 O10'
_cod_database_code               4115545