#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:49:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179025 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/23/4122315.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4122315
loop_
_publ_author_name
'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'
_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
_chemical_name_systematic
;
 ?
;
_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/[σ²(Fo²)+(0.0995P)²+1.4213P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 1.12891(15) 0.9475(4) 0.8567(3) 0.0277(7) Uani 1 1 d .
C2 C 1.16614(15) 0.8575(3) 0.7494(3) 0.0289(7) Uani 1 1 d .
C3 C 1.13559(18) 0.7415(4) 0.6756(4) 0.0368(8) Uani 1 1 d .
H3 H 1.0925 0.7187 0.6931 0.044 Uiso 1 1 calc R
C4 C 1.1672(2) 0.6599(4) 0.5777(4) 0.0434(9) Uani 1 1 d .
H4 H 1.1453 0.5839 0.5270 0.052 Uiso 1 1 calc R
C5 C 1.2309(2) 0.6881(5) 0.5530(4) 0.0474(10) Uani 1 1 d .
H5 H 1.2528 0.6309 0.4866 0.057 Uiso 1 1 calc R
C6 C 1.26214(19) 0.8014(5) 0.6271(4) 0.0425(9) Uani 1 1 d .
H6 H 1.3057 0.8216 0.6116 0.051 Uiso 1 1 calc R
C7 C 1.22987(16) 0.8847(4) 0.7232(4) 0.0348(7) Uani 1 1 d .
H7 H 1.2517 0.9622 0.7725 0.042 Uiso 1 1 calc R
C8 C 1.16370(15) 0.9226(4) 0.9894(3) 0.0311(7) Uani 1 1 d .
C9 C 1.14083(19) 0.8129(4) 1.0766(4) 0.0394(8) Uani 1 1 d .
H9 H 1.1046 0.7536 1.0534 0.047 Uiso 1 1 calc R
C10 C 1.1704(2) 0.7874(5) 1.2000(4) 0.0546(11) Uani 1 1 d .
H10 H 1.1540 0.7123 1.2600 0.066 Uiso 1 1 calc R
C11 C 1.2233(2) 0.8719(5) 1.2329(4) 0.0516(10) Uani 1 1 d .
H11 H 1.2434 0.8553 1.3160 0.062 Uiso 1 1 calc R
C12 C 1.24709(19) 0.9806(5) 1.1460(4) 0.0451(9) Uani 1 1 d .
H12 H 1.2839 1.0377 1.1689 0.054 Uiso 1 1 calc R
C13 C 1.21786(15) 1.0071(5) 1.0259(3) 0.0369(7) Uani 1 1 d .
H13 H 1.2345 1.0833 0.9671 0.044 Uiso 1 1 calc R
C14 C 1.12854(15) 1.1262(4) 0.8242(4) 0.0337(8) Uani 1 1 d .
H14 H 1.1715 1.1608 0.7955 0.040 Uiso 1 1 calc R
C15 C 1.10500(18) 1.2273(5) 0.9425(5) 0.0449(9) Uani 1 1 d .
H15A H 1.0841 1.1611 1.0099 0.054 Uiso 1 1 calc R
H15B H 1.1410 1.2815 0.9850 0.054 Uiso 1 1 calc R
C16 C 1.0587(2) 1.3442(5) 0.8866(5) 0.0567(12) Uani 1 1 d .
H16A H 1.0152 1.3211 0.9168 0.068 Uiso 1 1 calc R
H16B H 1.0700 1.4512 0.9143 0.068 Uiso 1 1 calc R
C17 C 1.0000 1.0000 0.2898(7) 0.076(2) Uani 1 2 d S
H17 H 1.0000 1.0000 0.1955 0.091 Uiso 1 2 calc SR
C18 C 0.9499(3) 0.9390(6) 0.3594(5) 0.0604(12) Uani 1 1 d .
H18 H 0.9144 0.8984 0.3134 0.072 Uiso 1 1 calc R
C19 C 0.95146(18) 0.9368(5) 0.4988(4) 0.0412(9) Uani 1 1 d .
C20 C 0.89827(18) 0.8743(5) 0.5830(4) 0.0438(9) Uani 1 1 d .
H20A H 0.8637 0.9517 0.5857 0.053 Uiso 1 1 calc R
H20B H 0.8815 0.7782 0.5419 0.053 Uiso 1 1 calc R
C21 C 0.93599(18) 0.6735(4) 0.7381(5) 0.0529(11) Uani 1 1 d .
H21A H 0.9767 0.6492 0.6942 0.063 Uiso 1 1 calc R
H21B H 0.9029 0.6040 0.7020 0.063 Uiso 1 1 calc R
N1 N 1.0000 1.0000 0.5651(4) 0.0371(8) Uani 1 2 d S
N2 N 0.91872(13) 0.8399(3) 0.7187(3) 0.0368(7) Uani 1 1 d .
O1 O 1.06754(11) 0.8943(3) 0.8648(3) 0.0345(6) Uani 1 1 d .
Fe Fe 1.0000 1.0000 0.77356(7) 0.0313(2) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 C1 C8 110.7(3) . .
O1 C1 C2 110.8(3) . .
C8 C1 C2 107.1(2) . .
O1 C1 C14 109.4(3) . .
C8 C1 C14 108.6(3) . .
C2 C1 C14 110.3(3) . .
C7 C2 C3 117.7(3) . .
C7 C2 C1 122.8(3) . .
C3 C2 C1 119.5(3) . .
C4 C3 C2 121.0(4) . .
C4 C3 H3 119.5 . .
C2 C3 H3 119.5 . .
C3 C4 C5 120.5(4) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C6 C5 C4 119.0(4) . .
C6 C5 H5 120.5 . .
C4 C5 H5 120.5 . .
C7 C6 C5 120.2(4) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C6 C7 C2 121.5(3) . .
C6 C7 H7 119.2 . .
C2 C7 H7 119.2 . .
C9 C8 C13 118.3(3) . .
C9 C8 C1 118.8(3) . .
C13 C8 C1 123.0(3) . .
C8 C9 C10 120.9(4) . .
C8 C9 H9 119.5 . .
C10 C9 H9 119.5 . .
C11 C10 C9 119.5(4) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
C10 C11 C12 120.2(4) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C11 C12 C13 120.5(4) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C12 C13 C8 120.7(4) . .
C12 C13 H13 119.7 . .
C8 C13 H13 119.7 . .
N2 C14 C15 102.9(3) 2_775 .
N2 C14 C1 110.1(3) 2_775 .
C15 C14 C1 112.8(3) . .
N2 C14 H14 110.3 2_775 .
C15 C14 H14 110.3 . .
C1 C14 H14 110.3 . .
C16 C15 C14 107.0(4) . .
C16 C15 H15A 110.3 . .
C14 C15 H15A 110.3 . .
C16 C15 H15B 110.3 . .
C14 C15 H15B 110.3 . .
H15A C15 H15B 108.6 . .
C21 C16 C15 104.7(4) 2_775 .
C21 C16 H16A 110.8 2_775 .
C15 C16 H16A 110.8 . .
C21 C16 H16B 110.8 2_775 .
C15 C16 H16B 110.8 . .
H16A C16 H16B 108.9 . .
C18 C17 C18 118.6(6) 2_775 .
C18 C17 H17 120.7 2_775 .
C18 C17 H17 120.7 . .
C17 C18 C19 119.9(5) . .
C17 C18 H18 120.1 . .
C19 C18 H18 120.1 . .
N1 C19 C18 120.7(4) . .
N1 C19 C20 115.8(3) . .
C18 C19 C20 123.4(4) . .
N2 C20 C19 112.1(3) . .
N2 C20 H20A 109.2 . .
C19 C20 H20A 109.2 . .
N2 C20 H20B 109.2 . .
C19 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
N2 C21 C16 104.2(3) . 2_775
N2 C21 H21A 110.9 . .
C16 C21 H21A 110.9 2_775 .
N2 C21 H21B 110.9 . .
C16 C21 H21B 110.9 2_775 .
H21A C21 H21B 108.9 . .
C19 N1 C19 120.2(5) . 2_775
C19 N1 Fe 119.9(2) . .
C19 N1 Fe 119.9(2) 2_775 .
C20 N2 C14 115.4(3) . 2_775
C20 N2 C21 112.9(3) . .
C14 N2 C21 105.0(3) 2_775 .
C20 N2 Fe 109.2(2) . .
C14 N2 Fe 102.5(2) 2_775 .
C21 N2 Fe 111.3(2) . .
C1 O1 Fe 120.93(19) . .
O1 Fe O1 123.03(16) 2_775 .
O1 Fe N1 118.48(8) 2_775 .
O1 Fe N1 118.48(8) . .
O1 Fe N2 80.79(10) 2_775 .
O1 Fe N2 113.10(11) . .
N1 Fe N2 75.91(9) . .
O1 Fe N2 113.10(11) 2_775 2_775
O1 Fe N2 80.79(10) . 2_775
N1 Fe N2 75.91(9) . 2_775
N2 Fe N2 151.81(18) . 2_775
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.379(4) .
C1 C8 1.541(5) .
C1 C2 1.545(4) .
C1 C14 1.570(5) .
C2 C7 1.394(5) .
C2 C3 1.401(5) .
C3 C4 1.383(6) .
C3 H3 0.9500 .
C4 C5 1.392(6) .
C4 H4 0.9500 .
C5 C6 1.394(6) .
C5 H5 0.9500 .
C6 C7 1.384(5) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C9 1.376(5) .
C8 C13 1.406(5) .
C9 C10 1.409(6) .
C9 H9 0.9500 .
C10 C11 1.373(7) .
C10 H10 0.9500 .
C11 C12 1.376(6) .
C11 H11 0.9500 .
C12 C13 1.378(5) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 N2 1.489(5) 2_775
C14 C15 1.557(6) .
C14 H14 1.0000 .
C15 C16 1.512(6) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C21 1.507(7) 2_775
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.375(6) 2_775
C17 C18 1.375(6) .
C17 H17 0.9500 .
C18 C19 1.405(6) .
C18 H18 0.9500 .
C19 N1 1.340(4) .
C19 C20 1.508(6) .
C20 N2 1.464(5) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 N2 1.488(5) .
C21 C16 1.507(7) 2_775
C21 H21A 0.9900 .
C21 H21B 0.9900 .
N1 C19 1.340(4) 2_775
N1 Fe 2.100(4) .
N2 C14 1.489(5) 2_775
N2 Fe 2.271(3) .
O1 Fe 1.927(2) .
Fe O1 1.927(2) 2_775
Fe N2 2.271(3) 2_775
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.000 0.293 143.9 62.7
2 1.000 0.500 0.707 144.0 63.0
