Evidence for a Nonheme Fe(IV)O Species in the Intramolecular Hydroxylation of a Phenyl Moiety
Steven J. Lange; Hiroyuki Miyake; Lawrence Que; Journal of the American Chemical Society 121 (1999) 6330–6331; doi:10.1021/ja990233u

data_4116429
_publ_section_title
;
 Evidence for a Nonheme Fe(IV)O Species in the Intramolecular
 Hydroxylation of a Phenyl Moiety
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6330
_journal_page_last               6331
_journal_paper_doi               10.1021/ja990233u
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        'S. Lange / Prof. L. Que'
_chemical_formula_sum            'C48 H41 B Fe N4 O1.5'
_chemical_formula_weight         764.51
_chemical_name_common            99074a
_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
_cell_angle_alpha                64.763(1)
_cell_angle_beta                 77.158(1)
_cell_angle_gamma                88.792(1)
_cell_formula_units_Z            2
_cell_length_a                   9.8427(7)
_cell_length_b                   13.9820(9)
_cell_length_c                   15.5076(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1875.6(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12988
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       Plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1048
_refine_ls_wR_factor_obs         0.0993
_reflns_number_observed          5368
_reflns_number_total             6590
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990233u_2.cif
_cod_data_source_block
JA990233U_complex_2_[Fe(III)2(mu-O)(6-C6H4O-TPA)2](BPh4)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C48 H41 B Fe N4 O1.50'
_cod_database_code               4116429