Formation, Structure, and EPR Detection of a High Spin FeIV-Oxo Species Derived from Either an FeIII-Oxo or FeIII-OH Complex
David C. Lacy; Rupal Gupta; Kari L. Stone; John Greaves; Joseph W. Ziller; Michael P. Hendrich; A. S. Borovik; Journal of the American Chemical Society 132 (2010) 12188–12190; doi:10.1021/ja1047818

data_4103011
_publ_section_title
;
 Formation, Structure, and EPR Detection of a High Spin FeIV-Oxo Species
 Derived from Either an FeIII-Oxo or FeIII-OH Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12188
_journal_page_last               12190
_journal_paper_doi               10.1021/ja1047818
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C27 H56 Fe K N9 O6'
_chemical_formula_weight         697.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6596(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9007(5)
_cell_length_b                   13.6243(5)
_cell_length_c                   20.2360(8)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.19
_cell_volume                     3707.7(2)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43813
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.8240
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0373P)^2^+1.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                8281
_reflns_number_total             9198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1047818_si_002.cif
_cod_data_source_block           asb178
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4103011