#------------------------------------------------------------------------------
#$Date: 2016-03-26 11:50:16 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180216 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/02/7110236.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_7110236
loop_
_publ_author_name
'Olga V. Makhlynets'
'Williamson N. Oloo'
'Yurii S. Moroz'
'Irina G. Belaya'
'Taryn D. Palluccio'
'Alexander S. Filatov'
'Peter Muller'
'Matthew A. Cranswick'
'Lawrence Que'
'Elena V. Rybak-Akimova'
_publ_section_title
;
 H2O2 activation with biomimetic non-haem iron complexes and AcOH:
 connecting the g = 2.7 EPR signal with a visible chromophore
;
_journal_name_full               Chem.Commun.
_journal_page_first              645
_journal_paper_doi               10.1039/c3cc47632d
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H40 Fe N6 O2, 2(Cl O4)'
_chemical_formula_sum            'C26 H40 Cl2 Fe N6 O10'
_chemical_formula_weight         723.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 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            8
_cell_length_a                   21.9192(14)
_cell_length_b                   15.5820(10)
_cell_length_c                   19.0923(12)
_cell_measurement_reflns_used    9290
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.26
_cell_volume                     6520.9(7)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13899
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9098
_exptl_absorpt_correction_T_min  0.8633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.105
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3863
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0621
_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/[σ²(Fo²)+(0.1083P)²+26.1139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                3633
_reflns_number_total             3863
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3cc47632d.txt
_cod_data_source_block           FeBPMEN
_cod_database_code               7110236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.2500 0.2500 0.59991(3) 0.02482(19) Uani 1 2 d SU . .
N1 N 0.22744(15) 0.3734(2) 0.59905(18) 0.0261(6) Uani 1 1 d . A .
N2 N 0.18662(19) 0.2472(2) 0.5225(2) 0.0275(8) Uani 1 1 d . A .
O1 O 0.15657(16) 0.6190(2) 0.6045(2) 0.0419(7) Uani 1 1 d . A .
C1 C 0.25738(18) 0.4379(3) 0.6300(2) 0.0293(8) Uani 1 1 d . . .
H1 H 0.2953 0.4255 0.6518 0.035 Uiso 1 1 calc R A .
C2 C 0.23631(19) 0.5216(3) 0.6321(2) 0.0309(8) Uani 1 1 d . A .
C3 C 0.2722(2) 0.5900(3) 0.6697(3) 0.0393(10) Uani 1 1 d . . .
H3A H 0.2544 0.5996 0.7162 0.059 Uiso 1 1 calc R A .
H3B H 0.2707 0.6434 0.6427 0.059 Uiso 1 1 calc R . .
H3C H 0.3146 0.5713 0.6748 0.059 Uiso 1 1 calc R . .
C4 C 0.18122(18) 0.5383(2) 0.5991(2) 0.0298(7) Uani 1 1 d . . .
C5 C 0.1703(3) 0.6730(3) 0.5464(3) 0.0553(14) Uani 1 1 d . . .
H5A H 0.2138 0.6873 0.5468 0.083 Uiso 1 1 calc R A .
H5B H 0.1462 0.7259 0.5497 0.083 Uiso 1 1 calc R . .
H5C H 0.1602 0.6431 0.5028 0.083 Uiso 1 1 calc R . .
C6 C 0.14873(18) 0.4740(2) 0.5657(2) 0.0263(7) Uani 1 1 d . A .
C7 C 0.0884(2) 0.4883(3) 0.5300(2) 0.0337(9) Uani 1 1 d . . .
H7A H 0.0735 0.5461 0.5410 0.051 Uiso 1 1 calc R A .
H7B H 0.0589 0.4457 0.5466 0.051 Uiso 1 1 calc R . .
H7C H 0.0935 0.4826 0.4792 0.051 Uiso 1 1 calc R . .
C8 C 0.17362(18) 0.3919(2) 0.56780(19) 0.0260(7) Uani 1 1 d . . .
C9 C 0.14120(18) 0.3146(3) 0.5379(2) 0.0302(8) Uani 1 1 d . A .
H9A H 0.1109 0.2928 0.5721 0.036 Uiso 1 1 calc R . .
H9B H 0.1193 0.3308 0.4945 0.036 Uiso 1 1 calc R . .
C10 C 0.2198(2) 0.2719(3) 0.4575(2) 0.0319(8) Uani 1 1 d . . .
H10A H 0.2255 0.3349 0.4560 0.038 Uiso 1 1 calc R A .
H10B H 0.1960 0.2545 0.4158 0.038 Uiso 1 1 calc R . .
C11 C 0.1533(2) 0.1658(3) 0.5126(3) 0.0375(9) Uani 1 1 d . . .
H11A H 0.1325 0.1503 0.5563 0.056 Uiso 1 1 calc R A .
H11B H 0.1821 0.1204 0.4998 0.056 Uiso 1 1 calc R . .
H11C H 0.1230 0.1727 0.4752 0.056 Uiso 1 1 calc R . .
N3 N 0.1865(11) 0.231(2) 0.6717(9) 0.024(3) Uani 0.60 1 d PDU A 1
C12 C 0.1552(9) 0.2115(17) 0.7173(8) 0.038(4) Uani 0.60 1 d PDU A 1
C13 C 0.1167(7) 0.1843(10) 0.7741(9) 0.063(4) Uani 0.60 1 d PDU A 1
H13A H 0.1168 0.1215 0.7768 0.094 Uiso 0.60 1 calc PR A 1
H13B H 0.0750 0.2047 0.7661 0.094 Uiso 0.60 1 calc PR A 1
H13C H 0.1322 0.2081 0.8182 0.094 Uiso 0.60 1 calc PR A 1
N3X N 0.1976(18) 0.236(3) 0.6757(17) 0.033(7) Uani 0.40 1 d PDU A 2
C12X C 0.1700(13) 0.225(3) 0.7254(13) 0.037(5) Uani 0.40 1 d PDU A 2
C13X C 0.1375(8) 0.2079(11) 0.7893(11) 0.046(4) Uani 0.40 1 d PDU A 2
H13D H 0.1398 0.1465 0.8001 0.069 Uiso 0.40 1 calc PR A 2
H13E H 0.0947 0.2248 0.7838 0.069 Uiso 0.40 1 calc PR A 2
H13F H 0.1559 0.2408 0.8276 0.069 Uiso 0.40 1 calc PR A 2
Cl1 Cl 0.24033(8) 0.0325(2) 0.87333(9) 0.0904(8) Uani 1 1 d D B 1
O2 O 0.1798(6) 0.049(2) 0.8967(19) 0.0836(19) Uani 0.60 1 d PD B 1
O3 O 0.2468(14) 0.0508(14) 0.8031(7) 0.096(6) Uani 0.60 1 d PD B 1
O4 O 0.2739(5) -0.0152(7) 0.9135(8) 0.100(3) Uani 0.60 1 d PD B 1
O5 O 0.2766(7) 0.1216(9) 0.8951(9) 0.132(4) Uani 0.60 1 d PD B 1
O2X O 0.1794(9) 0.044(3) 0.895(3) 0.0836(19) Uani 0.40 1 d PD C 2
O3X O 0.257(2) 0.073(2) 0.8141(11) 0.096(6) Uani 0.40 1 d PD C 2
O4X O 0.2452(7) -0.0648(8) 0.8576(11) 0.100(3) Uani 0.40 1 d PD C 2
O5X O 0.2862(10) 0.0412(15) 0.9279(11) 0.132(4) Uani 0.40 1 d PD C 2
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
N3X Fe1 N3X 78(3) 14 . yes
N3X Fe1 N3 7(2) 14 14 yes
N3X Fe1 N3 85.0(8) . 14 yes
N3X Fe1 N3 85.0(8) 14 . yes
N3X Fe1 N3 7(2) . . yes
N3 Fe1 N3 92.2(15) 14 . yes
N3X Fe1 N1 87.9(15) 14 14 yes
N3X Fe1 N1 92.9(16) . 14 yes
N3 Fe1 N1 88.8(10) 14 14 yes
N3 Fe1 N1 91.9(10) . 14 yes
N3X Fe1 N1 92.9(16) 14 . yes
N3X Fe1 N1 87.9(16) . . yes
N3 Fe1 N1 91.9(10) 14 . yes
N3 Fe1 N1 88.8(10) . . yes
N1 Fe1 N1 179.0(2) 14 . yes
N3X Fe1 N2 172.9(15) 14 . yes
N3X Fe1 N2 98.2(14) . . yes
N3 Fe1 N2 172.1(9) 14 . yes
N3 Fe1 N2 91.2(8) . . yes
N1 Fe1 N2 98.28(13) 14 . yes
N1 Fe1 N2 81.02(13) . . yes
N3X Fe1 N2 98.2(14) 14 14 yes
N3X Fe1 N2 172.9(15) . 14 yes
N3 Fe1 N2 91.2(8) 14 14 yes
N3 Fe1 N2 172.1(9) . 14 yes
N1 Fe1 N2 81.02(13) 14 14 yes
N1 Fe1 N2 98.28(13) . 14 yes
N2 Fe1 N2 86.4(2) . 14 yes
C1 N1 C8 117.5(3) . . ?
C1 N1 Fe1 127.0(3) . . ?
C8 N1 Fe1 115.3(2) . . ?
C11 N2 C9 107.6(3) . . ?
C11 N2 C10 111.0(4) . . ?
C9 N2 C10 108.2(3) . . ?
C11 N2 Fe1 116.7(3) . . ?
C9 N2 Fe1 107.5(3) . . ?
C10 N2 Fe1 105.5(3) . . ?
C4 O1 C5 113.5(4) . . ?
N1 C1 C2 123.9(4) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C4 117.0(4) . . ?
C1 C2 C3 120.4(4) . . ?
C4 C2 C3 122.6(4) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 C6 119.7(4) . . ?
O1 C4 C2 118.7(4) . . ?
C6 C4 C2 121.4(4) . . ?
O1 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 C8 116.8(3) . . ?
C4 C6 C7 123.6(4) . . ?
C8 C6 C7 119.6(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 123.4(3) . . ?
N1 C8 C9 114.0(3) . . ?
C6 C8 C9 122.5(3) . . ?
N2 C9 C8 109.0(3) . . ?
N2 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
N2 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N2 C10 C10 108.4(3) . 14 ?
N2 C10 H10A 110.0 . . ?
C10 C10 H10A 110.0 14 . ?
N2 C10 H10B 110.0 . . ?
C10 C10 H10B 110.0 14 . ?
H10A C10 H10B 108.4 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 N3 Fe1 171(3) . . ?
N3 C12 C13 178(3) . . ?
C12X N3X Fe1 174(4) . . ?
N3X C12X C13X 177(4) . . ?
C12X C13X H13D 109.5 . . ?
C12X C13X H13E 109.5 . . ?
H13D C13X H13E 109.5 . . ?
C12X C13X H13F 109.5 . . ?
H13D C13X H13F 109.5 . . ?
H13E C13X H13F 109.5 . . ?
O4 Cl1 O3 129.5(13) . . ?
O4 Cl1 O2 116.4(15) . . ?
O3 Cl1 O2 111.3(12) . . ?
O4 Cl1 O5 93.4(8) . . ?
O3 Cl1 O5 91.2(10) . . ?
O2 Cl1 O5 102.8(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3X 1.86(2) 14 yes
Fe1 N3X 1.86(2) . yes
Fe1 N3 1.977(14) 14 yes
Fe1 N3 1.977(14) . yes
Fe1 N1 1.985(3) 14 yes
Fe1 N1 1.985(3) . yes
Fe1 N2 2.030(4) . yes
Fe1 N2 2.030(4) 14 yes
N1 C1 1.338(5) . ?
N1 C8 1.353(5) . ?
N2 C11 1.476(5) . ?
N2 C9 1.477(5) . ?
N2 C10 1.487(6) . ?
O1 C4 1.373(4) . ?
O1 C5 1.425(7) . ?
C1 C2 1.384(6) . ?
C1 H1 0.9500 . ?
C2 C4 1.387(6) . ?
C2 C3 1.506(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C6 1.385(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C8 1.391(5) . ?
C6 C7 1.504(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.510(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C10 1.491(8) 14 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N3 C12 1.147(11) . ?
C12 C13 1.438(11) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N3X C12X 1.140(15) . ?
C12X C13X 1.437(15) . ?
C13X H13D 0.9800 . ?
C13X H13E 0.9800 . ?
C13X H13F 0.9800 . ?
Cl1 O4 1.297(9) . ?
Cl1 O3 1.378(11) . ?
Cl1 O2 1.422(9) . ?
Cl1 O5 1.653(13) . ?
