#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314942.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_4314942
loop_
_publ_author_name
'Ashis K. Patra'
'Koustubh S. Dube'
'Georgia C. Papaefthymiou'
'Jeanet Conradie'
'Abhik Ghosh'
'Todd C. Harrop'
_publ_contact_author_address
;Department of Chemistry, The University of Georgia, 1001 Ceadr St,
 Athens, GA 30602,USA
;
_publ_contact_author_email       tharrop@chem.uga.edu
_publ_contact_author_fax         1-706-542-9454
_publ_contact_author_name        'Todd C. Harrop'
_publ_contact_author_phone       1-706-542-3486
_publ_section_title
;
 Stable Eight-Coordinate Iron(III/II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2032
_journal_page_last               2034
_journal_paper_doi               10.1021/ic1001336
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C20 H22 B2 F8 Fe N8'
_chemical_formula_sum            'C20 H22 B2 F8 Fe N8'
_chemical_formula_weight         603.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.0570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0023(8)
_cell_length_b                   13.7671(10)
_cell_length_c                   17.9551(12)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.32
_cell_volume                     2659.7(3)
_computing_cell_refinement       'Bruker APEX II V2008.6-1'
_computing_data_collection       'Bruker APEX II V2008.6-1'
_computing_data_reduction        'Bruker APEX II V2008.6-1'
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart CCD Area Detector'
_diffrn_measurement_method       'omega 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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36316
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.8921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0707
_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)+(0.1176P)²+1.6003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                3342
_reflns_number_total             6631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1001336_si_004.cif
_cod_data_source_block           JACScif2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314942
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.21429(6) 0.67512(5) 0.22608(4) 0.0476(2) Uani 1 1 d . . .
N1 N 0.0971(4) 0.7814(3) 0.1604(2) 0.0509(9) Uani 1 1 d . . .
N2 N 0.0669(4) 0.9371(3) 0.1350(2) 0.0579(11) Uani 1 1 d . . .
N3 N 0.3196(4) 0.8094(2) 0.2525(2) 0.0455(9) Uani 1 1 d . . .
N4 N 0.3845(3) 0.6388(3) 0.30640(19) 0.0428(8) Uani 1 1 d . . .
N5 N 0.1961(3) 0.5228(3) 0.2444(2) 0.0493(9) Uani 1 1 d . . .
N6 N 0.2835(4) 0.3907(3) 0.3023(2) 0.0474(9) Uani 1 1 d . . .
N7 N 0.1287(4) 0.7150(3) 0.3219(2) 0.0579(10) Uani 1 1 d . . .
N8 N 0.3036(4) 0.6469(3) 0.1297(3) 0.0646(12) Uani 1 1 d . . .
B1 B 0.3067(5) 0.5681(4) 0.5133(3) 0.0515(13) Uani 1 1 d . . .
B2 B 0.2123(8) 1.0632(6) 0.3700(6) 0.090(2) Uani 1 1 d . . .
C1 C -0.0137(5) 0.7942(4) 0.1116(3) 0.0634(14) Uani 1 1 d . . .
H1 H -0.0685 0.7445 0.0922 0.076 Uiso 1 1 calc R . .
C2 C -0.0333(5) 0.8896(5) 0.0951(3) 0.0662(15) Uani 1 1 d . . .
H2 H -0.1019 0.9169 0.0628 0.079 Uiso 1 1 calc R . .
C3 C 0.0876(6) 1.0418(4) 0.1348(4) 0.0796(18) Uani 1 1 d . . .
H3A H 0.0175 1.0728 0.1029 0.119 Uiso 1 1 calc R . .
H3B H 0.1611 1.0552 0.1156 0.119 Uiso 1 1 calc R . .
H3C H 0.0980 1.0664 0.1858 0.119 Uiso 1 1 calc R . .
C4 C 0.1459(4) 0.8707(3) 0.1737(3) 0.0489(11) Uani 1 1 d . . .
C5 C 0.2646(5) 0.8863(3) 0.2229(2) 0.0492(11) Uani 1 1 d . . .
H5 H 0.2991 0.9478 0.2327 0.059 Uiso 1 1 calc R . .
C6 C 0.4349(4) 0.8059(3) 0.3042(2) 0.0426(10) Uani 1 1 d . . .
C7 C 0.5130(5) 0.8848(3) 0.3273(3) 0.0536(12) Uani 1 1 d . . .
H7 H 0.4905 0.9463 0.3079 0.064 Uiso 1 1 calc R . .
C8 C 0.6228(5) 0.8718(4) 0.3784(3) 0.0617(13) Uani 1 1 d . . .
H8 H 0.6747 0.9247 0.3933 0.074 Uiso 1 1 calc R . .
C9 C 0.6575(5) 0.7802(4) 0.4083(3) 0.0633(14) Uani 1 1 d . . .
H9 H 0.7322 0.7724 0.4432 0.076 Uiso 1 1 calc R . .
C10 C 0.5816(4) 0.7010(4) 0.3864(3) 0.0539(12) Uani 1 1 d . . .
H10 H 0.6046 0.6399 0.4066 0.065 Uiso 1 1 calc R . .
C11 C 0.4695(4) 0.7133(3) 0.3335(2) 0.0433(10) Uani 1 1 d . . .
C12 C 0.3958(4) 0.5490(3) 0.3279(3) 0.0449(10) Uani 1 1 d . . .
H12 H 0.4637 0.5260 0.3634 0.054 Uiso 1 1 calc R . .
C13 C 0.2946(4) 0.4878(3) 0.2924(2) 0.0434(10) Uani 1 1 d . . .
C14 C 0.3717(5) 0.3274(3) 0.3507(3) 0.0652(14) Uani 1 1 d . . .
H14A H 0.3406 0.2621 0.3466 0.098 Uiso 1 1 calc R . .
H14B H 0.3831 0.3488 0.4026 0.098 Uiso 1 1 calc R . .
H14C H 0.4498 0.3296 0.3349 0.098 Uiso 1 1 calc R . .
C15 C 0.1737(5) 0.3632(4) 0.2570(3) 0.0566(12) Uani 1 1 d . . .
H15 H 0.1415 0.3006 0.2508 0.068 Uiso 1 1 calc R . .
C16 C 0.1205(5) 0.4449(4) 0.2228(3) 0.0582(13) Uani 1 1 d . . .
H16 H 0.0436 0.4475 0.1894 0.070 Uiso 1 1 calc R . .
C17 C 0.1007(5) 0.7503(4) 0.3730(3) 0.0578(12) Uani 1 1 d . . .
C18 C 0.0638(7) 0.7949(5) 0.4399(3) 0.0844(19) Uani 1 1 d . . .
C19 C 0.3549(5) 0.6417(4) 0.0813(3) 0.0609(13) Uani 1 1 d . . .
C20 C 0.4215(7) 0.6354(5) 0.0189(4) 0.0877(19) Uani 1 1 d . . .
F1 F 0.3776(5) 0.6362(4) 0.4887(3) 0.1308(18) Uani 1 1 d . . .
F2 F 0.1832(4) 0.5920(3) 0.4988(2) 0.1096(14) Uani 1 1 d . . .
F3 F 0.3473(3) 0.5518(3) 0.59023(17) 0.0807(10) Uani 1 1 d . . .
F4 F 0.3151(4) 0.4833(3) 0.4754(2) 0.1114(14) Uani 1 1 d . . .
F5 F 0.3127(7) 1.0821(5) 0.3338(6) 0.223(4) Uani 1 1 d . . .
F6 F 0.1976(5) 0.9681(3) 0.3649(3) 0.1286(16) Uani 1 1 d . . .
F7 F 0.2415(7) 1.1092(5) 0.4323(3) 0.186(3) Uani 1 1 d . . .
F8 F 0.1227(7) 1.1067(5) 0.3206(3) 0.195(3) Uani 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Fe1 N5 133.75(15) . . ?
N1 Fe1 N4 149.64(15) . . ?
N5 Fe1 N4 76.55(14) . . ?
N1 Fe1 N3 76.78(15) . . ?
N5 Fe1 N3 149.38(14) . . ?
N4 Fe1 N3 72.87(13) . . ?
N1 Fe1 N7 87.32(15) . . ?
N5 Fe1 N7 93.18(15) . . ?
N4 Fe1 N7 89.34(15) . . ?
N3 Fe1 N7 85.01(15) . . ?
N1 Fe1 N8 90.21(15) . . ?
N5 Fe1 N8 91.12(16) . . ?
N4 Fe1 N8 90.98(15) . . ?
N3 Fe1 N8 90.93(16) . . ?
N7 Fe1 N8 175.64(16) . . ?
C4 N1 C1 105.5(4) . . ?
C4 N1 Fe1 110.9(3) . . ?
C1 N1 Fe1 143.5(4) . . ?
C4 N2 C2 108.1(4) . . ?
C4 N2 C3 125.9(5) . . ?
C2 N2 C3 126.0(5) . . ?
C5 N3 C6 125.8(4) . . ?
C5 N3 Fe1 115.3(3) . . ?
C6 N3 Fe1 118.7(3) . . ?
C12 N4 C11 125.4(4) . . ?
C12 N4 Fe1 115.8(3) . . ?
C11 N4 Fe1 118.8(3) . . ?
C13 N5 C16 105.4(4) . . ?
C13 N5 Fe1 111.5(3) . . ?
C16 N5 Fe1 143.1(3) . . ?
C13 N6 C15 106.8(4) . . ?
C13 N6 C14 127.1(4) . . ?
C15 N6 C14 126.2(4) . . ?
C17 N7 Fe1 166.5(4) . . ?
C19 N8 Fe1 172.9(5) . . ?
F1 B1 F4 109.0(5) . . ?
F1 B1 F2 112.9(5) . . ?
F4 B1 F2 106.2(5) . . ?
F1 B1 F3 110.7(5) . . ?
F4 B1 F3 108.6(4) . . ?
F2 B1 F3 109.3(5) . . ?
F7 B2 F6 124.2(9) . . ?
F7 B2 F8 112.4(7) . . ?
F6 B2 F8 109.8(7) . . ?
F7 B2 F5 103.6(8) . . ?
F6 B2 F5 104.3(7) . . ?
F8 B2 F5 98.8(9) . . ?
C2 C1 N1 110.4(5) . . ?
C2 C1 H1 124.8 . . ?
N1 C1 H1 124.8 . . ?
N2 C2 C1 106.2(5) . . ?
N2 C2 H2 126.9 . . ?
C1 C2 H2 126.9 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 N2 109.8(4) . . ?
N1 C4 C5 121.7(4) . . ?
N2 C4 C5 128.5(5) . . ?
N3 C5 C4 115.1(4) . . ?
N3 C5 H5 122.5 . . ?
C4 C5 H5 122.5 . . ?
C7 C6 C11 119.6(4) . . ?
C7 C6 N3 125.8(4) . . ?
C11 C6 N3 114.5(4) . . ?
C8 C7 C6 120.1(4) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.7(5) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 120.3(5) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 119.5(5) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C6 119.7(4) . . ?
C10 C11 N4 125.1(4) . . ?
C6 C11 N4 115.2(4) . . ?
N4 C12 C13 114.2(4) . . ?
N4 C12 H12 122.9 . . ?
C13 C12 H12 122.9 . . ?
N5 C13 N6 111.1(4) . . ?
N5 C13 C12 121.9(4) . . ?
N6 C13 C12 127.0(4) . . ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N6 106.6(4) . . ?
C16 C15 H15 126.7 . . ?
N6 C15 H15 126.7 . . ?
C15 C16 N5 110.2(4) . . ?
C15 C16 H16 124.9 . . ?
N5 C16 H16 124.9 . . ?
N7 C17 C18 179.2(6) . . ?
N8 C19 C20 179.7(7) . . ?
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 N1 2.135(4) . ?
Fe1 N5 2.138(4) . ?
Fe1 N4 2.170(4) . ?
Fe1 N3 2.180(4) . ?
Fe1 N7 2.196(4) . ?
Fe1 N8 2.196(5) . ?
N1 C4 1.343(6) . ?
N1 C1 1.356(6) . ?
N2 C4 1.350(6) . ?
N2 C2 1.351(7) . ?
N2 C3 1.459(7) . ?
N3 C5 1.279(5) . ?
N3 C6 1.407(6) . ?
N4 C12 1.294(5) . ?
N4 C11 1.405(6) . ?
N5 C13 1.327(5) . ?
N5 C16 1.362(6) . ?
N6 C13 1.358(5) . ?
N6 C15 1.361(6) . ?
N6 C14 1.450(6) . ?
N7 C17 1.137(6) . ?
N8 C19 1.133(7) . ?
B1 F1 1.352(7) . ?
B1 F4 1.364(7) . ?
B1 F2 1.369(6) . ?
B1 F3 1.379(6) . ?
B2 F7 1.267(9) . ?
B2 F6 1.320(9) . ?
B2 F8 1.323(9) . ?
B2 F5 1.418(11) . ?
C1 C2 1.353(8) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.432(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(6) . ?
C6 C11 1.402(6) . ?
C7 C8 1.367(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.393(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.401(6) . ?
C10 H10 0.9300 . ?
C12 C13 1.435(6) . ?
C12 H12 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.355(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.480(8) . ?
C19 C20 1.464(8) . ?
