#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:04:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180002 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/96/7029602.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_7029602
loop_
_publ_author_name
'Onaka, Satoru'
'Sakai, Yoichi'
'Ozeki, Tomoji'
'Nakamoto, Tadahiro'
'Kobayashi, Yusuke'
'Takahashi, Masashi'
'Ogiso, Ryo'
'Takayama, Tsutomu'
'Shiotsuka, Michito'
_publ_section_title
;
 Synthesis, structure and valence-trapping vs. detrapping for new
 trinuclear iron pentafluoro benzoate complexes: possible recognition of
 organic molecules by (57)Fe Mössbauer spectroscopy.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6711
_journal_page_last               6719
_journal_paper_doi               10.1039/c3dt53623h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C57 H15 F30 Fe3 N3 O13, 0.735(C H2 Cl2)'
_chemical_formula_sum            'C57.74 H16.47 Cl1.47 F30 Fe3 N3 O13'
_chemical_formula_weight         1749.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.458(1)
_cell_length_b                   13.458(1)
_cell_length_c                   20.967(1)
_cell_measurement_reflns_used    1643
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      1.94
_cell_volume                     3288.7(4)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'Crystal Clear (Molecular Struture Corporation,2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;DIAMOND 3.2i (Brandenburg, 2011),
 ORTEP for Windows (Farrugia, 2012),
 and Mercury 3.1 (Macrae et al, 2008)
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       'oscillation method, ω and π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15970
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.986
_diffrn_reflns_theta_min         1.943
_diffrn_source                   'rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.9337
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON MULABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0941P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2114
_reflns_number_total             2775
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt53623h2.cif
_cod_data_source_block           c57h15f30fe3n3o13ch2cl2
_cod_original_cell_volume        3288.7(5)
_cod_database_code               7029602
#BEGIN Tags that were not found in dictionaries:
_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   0.847
_shelx_estimated_absorpt_t_max   0.958
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -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 0.15049(16) 0.22583(17) 0.33881(9) 0.0280(4) Uani 1 1 d . . .
C2 C 0.20954(17) 0.31496(18) 0.39013(10) 0.0312(4) Uani 1 1 d . . .
C3 C 0.15361(19) 0.31462(18) 0.44605(10) 0.0350(5) Uani 1 1 d . . .
C4 C 0.2090(2) 0.3953(2) 0.49335(10) 0.0424(5) Uani 1 1 d . . .
C5 C 0.3204(2) 0.4788(2) 0.48499(12) 0.0475(6) Uani 1 1 d . . .
C6 C 0.3784(2) 0.4827(2) 0.43034(13) 0.0527(7) Uani 1 1 d . . .
C7 C 0.32266(19) 0.4008(2) 0.38386(11) 0.0452(6) Uani 1 1 d . . .
C8 C 0.40062(17) 0.12333(16) 0.30485(10) 0.0305(4) Uani 1 1 d . . .
H8 H 0.3620 0.1162 0.3440 0.037 Uiso 1 1 calc R U .
C9 C 0.51257(17) 0.14556(17) 0.30667(10) 0.0331(4) Uani 1 1 d . . .
H9 H 0.5501 0.1541 0.3463 0.040 Uiso 1 1 calc R U .
C10 C 0.5691(3) 0.1551(2) 0.2500 0.0351(7) Uani 1 2 d S T P
H10 H 0.6453 0.1681 0.2500 0.042 Uiso 1 2 calc R U P
N1 N 0.34442(19) 0.11139(19) 0.2500 0.0274(5) Uani 1 2 d S T P
O1 O 0.0000 0.0000 0.2500 0.0235(6) Uani 1 6 d S T P
O2 O 0.20234(12) 0.17601(13) 0.32008(7) 0.0359(4) Uani 1 1 d . . .
O3 O 0.05626(13) 0.21130(13) 0.32015(7) 0.0355(4) Uani 1 1 d . . .
F1 F 0.04516(12) 0.23297(12) 0.45583(7) 0.0522(4) Uani 1 1 d . . .
F2 F 0.15380(16) 0.39105(14) 0.54723(7) 0.0637(5) Uani 1 1 d . . .
F3 F 0.37475(15) 0.55874(15) 0.53063(8) 0.0673(5) Uani 1 1 d . . .
F4 F 0.48814(14) 0.56577(17) 0.42243(10) 0.0888(7) Uani 1 1 d . . .
F5 F 0.38003(13) 0.40733(15) 0.33072(8) 0.0756(6) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.3189(3) 0.271(4) Uani 0.735(7) 3 d S T P
Fe1 Fe 0.16102(3) 0.05455(3) 0.2500 0.02863(16) Uani 1 2 d S T P
C11 C 0.249(3) 0.571(3) 0.2500 0.152(15) Uani 0.245(2) 2 d S T P
H11A H 0.2496 0.4981 0.2500 0.183 Uiso 0.245(2) 2 calc R U P
H11B H 0.1682 0.5547 0.2500 0.183 Uiso 0.245(2) 2 calc R U P
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'
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
O3 C1 O2 127.99(19) . .
O3 C1 C2 116.05(17) . .
O2 C1 C2 115.97(16) . .
C7 C2 C3 116.77(19) . .
C7 C2 C1 121.27(18) . .
C3 C2 C1 121.96(18) . .
F1 C3 C4 118.4(2) . .
F1 C3 C2 119.99(19) . .
C4 C3 C2 121.6(2) . .
F2 C4 C5 120.2(2) . .
F2 C4 C3 120.2(2) . .
C5 C4 C3 119.6(2) . .
F3 C5 C4 120.0(2) . .
F3 C5 C6 119.4(2) . .
C4 C5 C6 120.6(2) . .
F4 C6 C5 120.1(2) . .
F4 C6 C7 120.7(2) . .
C5 C6 C7 119.2(2) . .
F5 C7 C6 118.2(2) . .
F5 C7 C2 119.60(19) . .
C6 C7 C2 122.2(2) . .
N1 C8 C9 122.55(19) . .
N1 C8 H8 118.7 . .
C9 C8 H8 118.7 . .
C10 C9 C8 119.1(2) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
C9 C10 C9 118.6(3) 8_556 .
C9 C10 H10 120.7 8_556 .
C9 C10 H10 120.7 . .
C8 N1 C8 118.1(2) 8_556 .
C8 N1 Fe1 120.78(12) 8_556 .
C8 N1 Fe1 120.78(12) . .
Fe1 O1 Fe1 120.0 3 4
Fe1 O1 Fe1 120.0 3 .
Fe1 O1 Fe1 120.0 4 .
C1 O2 Fe1 130.53(13) . .
C1 O3 Fe1 131.37(13) . 3
C11 Cl1 C11 67.9(13) . 4_565
C11 Cl1 C11 67.9(13) . 3_665
C11 Cl1 C11 67.9(13) 4_565 3_665
O1 Fe1 O2 96.29(4) . .
O1 Fe1 O2 96.29(4) . 8_556
O2 Fe1 O2 91.18(9) . 8_556
O1 Fe1 O3 95.47(4) . 11_556
O2 Fe1 O3 168.24(6) . 11_556
O2 Fe1 O3 87.85(7) 8_556 11_556
O1 Fe1 O3 95.47(4) . 4
O2 Fe1 O3 87.85(7) . 4
O2 Fe1 O3 168.24(6) 8_556 4
O3 Fe1 O3 90.71(9) 11_556 4
O1 Fe1 N1 178.16(6) . .
O2 Fe1 N1 84.99(6) . .
O2 Fe1 N1 84.99(6) 8_556 .
O3 Fe1 N1 83.25(6) 11_556 .
O3 Fe1 N1 83.25(6) 4 .
Cl1 C11 Cl1 99.7(16) 8_556 .
Cl1 C11 H11A 111.8 8_556 .
Cl1 C11 H11A 111.8 . .
Cl1 C11 H11B 111.8 8_556 .
Cl1 C11 H11B 111.8 . .
H11A C11 H11B 109.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O3 1.246(2) .
C1 O2 1.248(2) .
C1 C2 1.508(3) .
C2 C7 1.382(3) .
C2 C3 1.392(3) .
C3 F1 1.333(3) .
C3 C4 1.382(3) .
C4 F2 1.337(3) .
C4 C5 1.362(4) .
C5 F3 1.349(3) .
C5 C6 1.373(4) .
C6 F4 1.345(3) .
C6 C7 1.378(3) .
C7 F5 1.333(3) .
C8 N1 1.341(2) .
C8 C9 1.382(3) .
C8 H8 0.9500 .
C9 C10 1.382(3) .
C9 H9 0.9500 .
C10 C9 1.382(3) 8_556
C10 H10 0.9500 .
N1 C8 1.341(2) 8_556
N1 Fe1 2.188(2) .
O1 Fe1 1.9088(4) 3
O1 Fe1 1.9089(4) 4
O1 Fe1 1.9089(4) .
O2 Fe1 2.0569(14) .
O3 Fe1 2.0674(14) 3
Cl1 C11 1.89(2) .
Cl1 C11 1.89(2) 4_565
Cl1 C11 1.89(2) 3_665
Fe1 O2 2.0570(14) 8_556
Fe1 O3 2.0674(14) 11_556
Fe1 O3 2.0674(14) 4
C11 Cl1 1.89(2) 8_556
C11 H11A 0.9900 .
C11 H11B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 C1 C2 C7 -128.9(2) . .
O2 C1 C2 C7 50.8(3) . .
O3 C1 C2 C3 51.5(3) . .
O2 C1 C2 C3 -128.8(2) . .
C7 C2 C3 F1 -178.7(2) . .
C1 C2 C3 F1 0.9(3) . .
C7 C2 C3 C4 -0.8(3) . .
C1 C2 C3 C4 178.8(2) . .
F1 C3 C4 F2 -0.4(3) . .
C2 C3 C4 F2 -178.3(2) . .
F1 C3 C4 C5 179.1(2) . .
C2 C3 C4 C5 1.2(4) . .
F2 C4 C5 F3 -1.2(4) . .
C3 C4 C5 F3 179.3(2) . .
F2 C4 C5 C6 178.8(3) . .
C3 C4 C5 C6 -0.7(4) . .
F3 C5 C6 F4 -0.4(4) . .
C4 C5 C6 F4 179.6(3) . .
F3 C5 C6 C7 179.9(2) . .
C4 C5 C6 C7 -0.1(4) . .
F4 C6 C7 F5 -0.8(4) . .
C5 C6 C7 F5 178.9(3) . .
F4 C6 C7 C2 -179.3(3) . .
C5 C6 C7 C2 0.4(4) . .
C3 C2 C7 F5 -178.4(2) . .
C1 C2 C7 F5 2.0(4) . .
C3 C2 C7 C6 0.0(4) . .
C1 C2 C7 C6 -179.6(2) . .
N1 C8 C9 C10 -0.5(3) . .
C8 C9 C10 C9 1.9(4) . 8_556
C9 C8 N1 C8 -1.0(4) . 8_556
C9 C8 N1 Fe1 172.05(15) . .
O3 C1 O2 Fe1 2.2(3) . .
C2 C1 O2 Fe1 -177.45(13) . .
O2 C1 O3 Fe1 -2.3(3) . 3
C2 C1 O3 Fe1 177.42(13) . 3
C11 Cl1 C11 Cl1 37.1(3) 4_565 8_556
C11 Cl1 C11 Cl1 -37.1(3) 3_665 8_556
