Characterization of a paramagnetic mononuclear nonheme iron-superoxo complex.
Chiang, Chien-Wei; Kleespies, Scott T.; Stout, Heather D.; Meier, Katlyn K.; Li, Po-Yi; Bominaar, Emile L.; Que, Jr, Lawrence; Münck, Eckard; Lee, Way-Zen; Journal of the American Chemical Society 136 (2014) 10846–10849; doi:10.1021/ja504410s

data_4122315
_publ_section_title
;
 Characterization of a paramagnetic mononuclear nonheme iron-superoxo
 complex.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10846
_journal_page_last               10849
_journal_paper_doi               10.1021/ja504410s
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C41 H41 Fe N3 O2'
_chemical_formula_sum            'C41 H41 Fe N3 O2'
_chemical_formula_weight         663.62
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.1630(5)
_cell_length_b                   8.5919(2)
_cell_length_c                   10.0756(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1832.05(8)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15293
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.7904
_exptl_absorpt_correction_T_min  0.7295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.55
_platon_squeeze_details
; 
Squeeze Void volume and electron count are consistent with CH2Cl2 moluecules which are 
dissordered with 1 on one position and 2 on the second as well as being located on a 2-fold access. 
This is consistent with the elemental analysis which required the inclusion of CH2Cl2.
;
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0995P)^2^+1.4213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                3057
_reflns_number_total             3217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja504410s_si_002.cif
_cod_data_source_block           a9567
_cod_depositor_comments          'Adding full bibliography for 4122315.cif.'
_cod_database_code               4122315