#------------------------------------------------------------------------------
#$Date: 2015-07-05 11:17:49 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140088 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/32/4343252.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_4343252
loop_
_publ_author_name
'Chantarojsiri, Teera'
'Sun, Yujie'
'Long, Jeffrey R.'
'Chang, Christopher J.'
_publ_section_title
;
 Water-Soluble Iron(IV)-Oxo Complexes Supported by Pentapyridine Ligands:
 Axial Ligand Effects on Hydrogen Atom and Oxygen Atom Transfer
 Reactivity.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5879
_journal_page_last               5887
_journal_paper_doi               10.1021/acs.inorgchem.5b00658
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C29 H27 B2 F8 Fe N5 O S0'
_chemical_formula_weight         691.02
_chemical_name_common            tc32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 119.82(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.930(11)
_cell_length_b                   12.259(3)
_cell_length_c                   12.759(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2840.2(18)
_computing_cell_refinement       'Bruker APEX2 v.2009.1'
_computing_data_collection       'Bruker APEX2 v.2009.1'
_computing_data_reduction        'Bruker APEX2 v.2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29258
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.702
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+4.3146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2516
_reflns_number_total             2699
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00658_si_007.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343251--4343257.cif.'
_cod_original_cell_volume        2840.2(17)
_cod_database_code               4343252
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.952
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C -0.05734(9) 0.29054(13) 0.40497(14) 0.0161(3) Uani 1 1 d . . .
H1 H -0.0225 0.3469 0.4210 0.019 Uiso 1 1 calc R U .
C2 C -0.10021(9) 0.29693(13) 0.45939(14) 0.0187(3) Uani 1 1 d . . .
H2 H -0.0950 0.3562 0.5111 0.022 Uiso 1 1 calc R U .
C3 C -0.15080(9) 0.21519(14) 0.43689(14) 0.0189(3) Uani 1 1 d . . .
H3 H -0.1798 0.2156 0.4752 0.023 Uiso 1 1 calc R U .
C4 C -0.15842(9) 0.13255(13) 0.35737(14) 0.0169(3) Uani 1 1 d . . .
H4 H -0.1933 0.0760 0.3401 0.020 Uiso 1 1 calc R U .
C5 C -0.11506(8) 0.13233(12) 0.30276(13) 0.0140(3) Uani 1 1 d . . .
C6 C -0.12952(8) 0.05311(13) 0.19967(13) 0.0137(3) Uani 1 1 d . . .
C7 C -0.19390(9) -0.02334(13) 0.17374(15) 0.0173(3) Uani 1 1 d . . .
H7A H -0.2377 0.0201 0.1544 0.026 Uiso 1 1 calc R U .
H7B H -0.2042 -0.0706 0.1051 0.026 Uiso 1 1 calc R U .
H7C H -0.1808 -0.0683 0.2451 0.026 Uiso 1 1 calc R U .
C8 C -0.14875(8) 0.12329(12) 0.08732(13) 0.0132(3) Uani 1 1 d . . .
C9 C -0.21576(8) 0.11232(13) -0.01859(14) 0.0149(3) Uani 1 1 d . . .
H9 H -0.2499 0.0584 -0.0240 0.018 Uiso 1 1 calc R U .
C10 C -0.23320(9) 0.17973(13) -0.11674(14) 0.0170(3) Uani 1 1 d . . .
H10 H -0.2786 0.1720 -0.1900 0.020 Uiso 1 1 calc R U .
C11 C -0.18286(9) 0.25814(13) -0.10508(14) 0.0172(3) Uani 1 1 d . . .
H11 H -0.1933 0.3066 -0.1697 0.021 Uiso 1 1 calc R U .
C12 C -0.11696(9) 0.26494(13) 0.00223(14) 0.0164(3) Uani 1 1 d . . .
H12 H -0.0829 0.3198 0.0095 0.020 Uiso 1 1 calc R U .
C13 C -0.06059(8) -0.01314(13) 0.23005(13) 0.0135(3) Uani 1 1 d . . .
C14 C -0.06112(9) -0.12661(13) 0.23297(14) 0.0175(3) Uani 1 1 d . . .
H14 H -0.1034 -0.1644 0.2233 0.021 Uiso 1 1 calc R U .
C15 C 0.0000 -0.18386(19) 0.2500 0.0188(5) Uani 1 2 d S T P
H15 H 0.0000 -0.2614 0.2500 0.023 Uiso 1 2 calc R U P
N1 N -0.06220(7) 0.20860(10) 0.33013(11) 0.0131(3) Uani 1 1 d . . .
N2 N -0.09802(7) 0.19816(10) 0.09764(12) 0.0128(3) Uani 1 1 d . . .
N3 N 0.0000 0.04360(15) 0.2500 0.0121(4) Uani 1 2 d S T P
O1 O 0.0000 0.36657(13) 0.2500 0.0180(3) Uani 1 2 d S T P
F1 F 0.82986(6) 0.51623(8) 0.26701(10) 0.0258(2) Uani 1 1 d . . .
F2 F 0.83023(6) 0.65537(8) 0.14986(10) 0.0294(2) Uani 1 1 d . . .
F3 F 0.88085(5) 0.49203(8) 0.14702(9) 0.0255(2) Uani 1 1 d . . .
F4 F 0.93735(6) 0.60021(10) 0.31456(10) 0.0346(3) Uani 1 1 d . . .
Fe01 Fe 0.0000 0.20286(2) 0.2500 0.01143(10) Uani 1 2 d S T P
B1 B 0.86990(10) 0.56734(15) 0.22095(17) 0.0186(4) Uani 1 1 d . . .
H101 H -0.0388(11) 0.4020(18) 0.2204(19) 0.028 Uiso 1 1 d . U .
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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 '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
N1 C1 C2 123.78(15) . .
N1 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C3 C2 C1 118.45(15) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C2 C3 C4 118.69(15) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C3 C4 C5 120.11(15) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
N1 C5 C4 121.44(14) . .
N1 C5 C6 116.36(13) . .
C4 C5 C6 121.93(14) . .
C13 C6 C7 110.29(13) . .
C13 C6 C5 111.04(12) . .
C7 C6 C5 110.34(12) . .
C13 C6 C8 107.99(12) . .
C7 C6 C8 110.14(12) . .
C5 C6 C8 106.96(12) . .
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 . .
N2 C8 C9 121.47(14) . .
N2 C8 C6 117.13(13) . .
C9 C8 C6 121.38(13) . .
C8 C9 C10 120.35(15) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C11 C10 C9 118.26(15) . .
C11 C10 H10 120.9 . .
C9 C10 H10 120.9 . .
C10 C11 C12 118.83(15) . .
C10 C11 H11 120.6 . .
C12 C11 H11 120.6 . .
N2 C12 C11 123.87(15) . .
N2 C12 H12 118.1 . .
C11 C12 H12 118.1 . .
N3 C13 C14 121.82(15) . .
N3 C13 C6 116.88(14) . .
C14 C13 C6 121.26(14) . .
C15 C14 C13 119.61(16) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C14 118.8(2) 2 .
C14 C15 H15 120.6 2 .
C14 C15 H15 120.6 . .
C1 N1 C5 117.32(13) . .
C1 N1 Fe01 122.83(11) . .
C5 N1 Fe01 119.69(10) . .
C12 N2 C8 117.14(13) . .
C12 N2 Fe01 123.75(11) . .
C8 N2 Fe01 119.10(10) . .
C13 N3 C13 118.22(19) . 2
C13 N3 Fe01 120.89(9) . .
C13 N3 Fe01 120.89(9) 2 .
Fe01 O1 H101 121.6(15) . .
N3 Fe01 N2 88.36(4) . .
N3 Fe01 N2 88.36(4) . 2
N2 Fe01 N2 176.71(7) . 2
N3 Fe01 O1 180.0 . .
N2 Fe01 O1 91.64(4) . .
N2 Fe01 O1 91.64(4) 2 .
N3 Fe01 N1 92.00(4) . 2
N2 Fe01 N1 96.70(6) . 2
N2 Fe01 N1 83.42(6) 2 2
O1 Fe01 N1 88.00(4) . 2
N3 Fe01 N1 92.00(4) . .
N2 Fe01 N1 83.42(6) . .
N2 Fe01 N1 96.70(6) 2 .
O1 Fe01 N1 88.00(4) . .
N1 Fe01 N1 176.00(7) 2 .
F4 B1 F2 111.13(15) . .
F4 B1 F1 109.76(15) . .
F2 B1 F1 109.66(14) . .
F4 B1 F3 109.37(14) . .
F2 B1 F3 108.27(14) . .
F1 B1 F3 108.60(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.354(2) .
C1 C2 1.383(2) .
C1 H1 0.9500 .
C2 C3 1.380(2) .
C2 H2 0.9500 .
C3 C4 1.386(2) .
C3 H3 0.9500 .
C4 C5 1.392(2) .
C4 H4 0.9500 .
C5 N1 1.355(2) .
C5 C6 1.539(2) .
C6 C13 1.528(2) .
C6 C7 1.536(2) .
C6 C8 1.544(2) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 N2 1.359(2) .
C8 C9 1.388(2) .
C9 C10 1.389(2) .
C9 H9 0.9500 .
C10 C11 1.378(2) .
C10 H10 0.9500 .
C11 C12 1.380(2) .
C11 H11 0.9500 .
C12 N2 1.352(2) .
C12 H12 0.9500 .
C13 N3 1.3550(19) .
C13 C14 1.392(2) .
C14 C15 1.378(2) .
C14 H14 0.9500 .
C15 C14 1.378(2) 2
C15 H15 0.9500 .
N1 Fe01 2.0171(14) .
N2 Fe01 2.0062(16) .
N3 C13 1.3550(18) 2
N3 Fe01 1.9523(19) .
O1 Fe01 2.0069(17) .
O1 H101 0.83(2) .
F1 B1 1.389(2) .
F2 B1 1.388(2) .
F3 B1 1.418(2) .
F4 B1 1.380(2) .
Fe01 N2 2.0062(16) 2
Fe01 N1 2.0171(15) 2
