#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/03/7010325.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_7010325
loop_
_publ_author_name
'Sowrey, Frank E.'
'Tilford, Claire'
'Wocadlo, Sigrid'
'Anson, Christopher E.'
'Powell, Annie K.'
'Bennington, Stephen M.'
'Montfrooij, Wouter'
'Jayasooriya, Upali A.'
'Cannon, Roderick D.'
_publ_section_title
;
 Spin frustration and concealed asymmetry: structure and magnetic
 spectrum of [Fe3O(O2CPh)6(py)3]ClO4·py †
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              862
_journal_paper_doi               10.1039/b008121n
_journal_year                    2001
_chemical_formula_sum            'C62 H50 Cl Fe3 N4 O17'
_chemical_formula_weight         1326.06
_chemical_name_systematic
; 
Hexakis(O,O'-μ-benzoate)(μ3-oxo)tris(pyridine)triiron(III)
perchlorate pyridine solvate 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.541(3)
_cell_length_b                   13.541(3)
_cell_length_c                   19.136(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      12.34
_cell_measurement_theta_min      10.96
_cell_volume                     3038.7(12)
_computing_cell_refinement       'AFC7R Control Software (MSC, 1994)'
_computing_data_collection       'AFC7R Control Software (MSC, 1994)'
_computing_data_reduction        'TEXSAN 1.6 (MSC, 1996)'
_computing_molecular_graphics    'XP in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_publication_material  'XCIF in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_refinement  'XL in SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_solution    'XS in SHELXTL/PC 5.03 (Siemens, 1995)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1687
_diffrn_reflns_theta_full        23.16
_diffrn_reflns_theta_max         23.16
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1477
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0429
_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)+(0.0464P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                798
_reflns_number_total             1477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008121n.txt
_cod_data_source_block           clair1
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7010325
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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 0.21304(8) 0.51088(8) 0.2500 0.0481(4) Uani 1 2 d S . .
N1 N 0.0749(5) 0.3313(5) 0.2500 0.0536(16) Uani 1 2 d S . .
O1 O 0.3333 0.6667 0.2500 0.0414(19) Uani 1 6 d S . .
O2 O 0.2824(3) 0.4595(3) 0.17547(18) 0.0578(10) Uani 1 1 d . . .
O3 O 0.4691(3) 0.5874(3) 0.17622(18) 0.0624(10) Uani 1 1 d . . .
C1 C 0.3841(5) 0.4942(4) 0.1562(3) 0.0514(13) Uani 1 1 d . . .
C2 C 0.4056(4) 0.4239(4) 0.1053(3) 0.0508(12) Uani 1 1 d . . .
C3 C 0.5165(5) 0.4546(5) 0.0859(3) 0.0705(16) Uani 1 1 d . . .
H3 H 0.5787 0.5196 0.1056 0.085 Uiso 1 1 calc R . .
C4 C 0.5352(5) 0.3894(6) 0.0376(3) 0.082(2) Uani 1 1 d . . .
H4 H 0.6100 0.4087 0.0254 0.098 Uiso 1 1 calc R . .
C5 C 0.4437(6) 0.2963(5) 0.0074(3) 0.0806(18) Uani 1 1 d . . .
H5 H 0.4567 0.2540 -0.0266 0.097 Uiso 1 1 calc R . .
C6 C 0.3343(5) 0.2641(5) 0.0262(3) 0.0688(16) Uani 1 1 d . . .
H6 H 0.2725 0.1997 0.0057 0.083 Uiso 1 1 calc R . .
C7 C 0.3155(4) 0.3273(4) 0.0756(3) 0.0582(14) Uani 1 1 d . . .
H7 H 0.2404 0.3045 0.0893 0.070 Uiso 1 1 calc R . .
C8 C 0.0323(4) 0.2756(5) 0.1899(3) 0.0642(15) Uani 1 1 d . . .
H8 H 0.0609 0.3145 0.1474 0.077 Uiso 1 1 calc R . .
C9 C -0.0534(5) 0.1613(5) 0.1884(3) 0.086(2) Uani 1 1 d . . .
H9 H -0.0808 0.1234 0.1456 0.103 Uiso 1 1 calc R . .
C10 C -0.0973(9) 0.1049(8) 0.2500 0.096(3) Uani 1 2 d S . .
H10 H -0.1567 0.0286 0.2500 0.10(3) Uiso 1 2 calc SR . .
Cl1 Cl 0.0000 0.0000 0.0000 0.1040(16) Uani 1 6 d SD . .
O4 O 0.0945(12) 0.056(2) -0.0528(8) 0.092(8) Uiso 0.33 1 d PD . .
O5 O 0.105(3) 0.037(3) -0.040(3) 0.088(17) Uiso 0.17 1 d PD . .
O6 O 0.064(4) 0.114(2) -0.023(3) 0.165(15) Uiso 0.17 1 d PD . .
C11 C -0.228(3) 0.348(7) 0.2500 0.185(9) Uani 0.83 2 d SP . 1
H11 H -0.1540 0.3580 0.2500 0.222 Uiso 0.83 2 calc SPR . 1
C12 C -0.244(6) 0.436(3) 0.2500 0.215(11) Uani 0.83 2 d SP A 1
H12 H -0.1804 0.5104 0.2500 0.258 Uiso 0.83 2 calc SPR A 1
N3 N -0.228(3) 0.348(7) 0.2500 0.185(9) Uani 0.17 2 d SP . 2
N4 N -0.244(6) 0.436(3) 0.2500 0.215(11) Uani 0.17 2 d SP B 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
O1 Fe1 O2 95.39(10) . 10_556 ?
O1 Fe1 O2 95.39(10) . . ?
O2 Fe1 O2 90.2(2) 10_556 . ?
O1 Fe1 O3 95.73(10) . 3_565 ?
O2 Fe1 O3 168.87(14) 10_556 3_565 ?
O2 Fe1 O3 89.36(14) . 3_565 ?
O1 Fe1 O3 95.73(10) . 12_566 ?
O2 Fe1 O3 89.36(14) 10_556 12_566 ?
O2 Fe1 O3 168.87(14) . 12_566 ?
O3 Fe1 O3 89.0(2) 3_565 12_566 ?
O1 Fe1 N1 179.80(15) . . ?
O2 Fe1 N1 84.48(14) 10_556 . ?
O2 Fe1 N1 84.48(14) . . ?
O3 Fe1 N1 84.41(14) 3_565 . ?
O3 Fe1 N1 84.41(14) 12_566 . ?
C8 N1 C8 118.6(7) . 10_556 ?
C8 N1 Fe1 120.7(3) . . ?
C8 N1 Fe1 120.7(3) 10_556 . ?
Fe1 O1 Fe1 120.0 3_565 . ?
Fe1 O1 Fe1 120.0 3_565 2_665 ?
Fe1 O1 Fe1 120.0 . 2_665 ?
C1 O2 Fe1 133.3(3) . . ?
C1 O3 Fe1 133.1(3) . 2_665 ?
O2 C1 O3 123.9(5) . . ?
O2 C1 C2 118.5(5) . . ?
O3 C1 C2 117.6(5) . . ?
C7 C2 C3 118.7(5) . . ?
C7 C2 C1 120.7(5) . . ?
C3 C2 C1 120.6(5) . . ?
C4 C3 C2 120.0(5) . . ?
C5 C4 C3 119.7(6) . . ?
C6 C5 C4 121.2(6) . . ?
C5 C6 C7 119.2(5) . . ?
C6 C7 C2 121.1(5) . . ?
N1 C8 C9 121.8(6) . . ?
C10 C9 C8 119.4(7) . . ?
C9 C10 C9 119.0(9) 10_556 . ?
O6 Cl1 O6 180(4) 8 2 ?
O6 Cl1 O6 69(2) 8 . ?
O6 Cl1 O6 111(2) 2 . ?
O6 Cl1 O6 111(2) 8 9 ?
O6 Cl1 O6 69(2) 2 9 ?
O6 Cl1 O6 69(2) . 9 ?
O6 Cl1 O6 69(2) 8 3 ?
O6 Cl1 O6 111(2) 2 3 ?
O6 Cl1 O6 111(2) . 3 ?
O6 Cl1 O6 180(4) 9 3 ?
O6 Cl1 O6 111(2) 8 7 ?
O6 Cl1 O6 69(2) 2 7 ?
O6 Cl1 O6 180(4) . 7 ?
O6 Cl1 O6 111(2) 9 7 ?
O6 Cl1 O6 69(2) 3 7 ?
O6 Cl1 O5 129(2) 8 3 ?
O6 Cl1 O5 51(2) 2 3 ?
O6 Cl1 O5 130.6(17) . 3 ?
O6 Cl1 O5 120(3) 9 3 ?
O6 Cl1 O5 60(3) 3 3 ?
O6 Cl1 O5 49.4(17) 7 3 ?
O6 Cl1 O5 51(2) 8 9 ?
O6 Cl1 O5 129(2) 2 9 ?
O6 Cl1 O5 49.4(17) . 9 ?
O6 Cl1 O5 60(3) 9 9 ?
O6 Cl1 O5 120(3) 3 9 ?
O6 Cl1 O5 130.6(17) 7 9 ?
O5 Cl1 O5 180(2) 3 9 ?
O6 Cl1 O5 120(3) 8 2 ?
O6 Cl1 O5 60(3) 2 2 ?
O6 Cl1 O5 51(2) . 2 ?
O6 Cl1 O5 49.4(17) 9 2 ?
O6 Cl1 O5 130.6(17) 3 2 ?
O6 Cl1 O5 129(2) 7 2 ?
O5 Cl1 O5 96(3) 3 2 ?
O5 Cl1 O5 84(3) 9 2 ?
O6 Cl1 O5 49.4(17) 8 . ?
O6 Cl1 O5 130.6(17) 2 . ?
O6 Cl1 O5 60(3) . . ?
O6 Cl1 O5 129(2) 9 . ?
O6 Cl1 O5 51(2) 3 . ?
O6 Cl1 O5 120(3) 7 . ?
O5 Cl1 O5 96(3) 3 . ?
O5 Cl1 O5 84(3) 9 . ?
O5 Cl1 O5 96(3) 2 . ?
O6 Cl1 O5 60(3) 8 8 ?
O6 Cl1 O5 120(3) 2 8 ?
O6 Cl1 O5 129(2) . 8 ?
O6 Cl1 O5 130.6(17) 9 8 ?
O6 Cl1 O5 49.4(17) 3 8 ?
O6 Cl1 O5 51(2) 7 8 ?
O5 Cl1 O5 84(3) 3 8 ?
O5 Cl1 O5 96(3) 9 8 ?
O5 Cl1 O5 180(2) 2 8 ?
O5 Cl1 O5 84(3) . 8 ?
O6 Cl1 O5 130.6(17) 8 7 ?
O6 Cl1 O5 49.4(17) 2 7 ?
O6 Cl1 O5 120(3) . 7 ?
O6 Cl1 O5 51(2) 9 7 ?
O6 Cl1 O5 129(2) 3 7 ?
O6 Cl1 O5 60(3) 7 7 ?
O5 Cl1 O5 84(3) 3 7 ?
O5 Cl1 O5 96(3) 9 7 ?
O5 Cl1 O5 84(3) 2 7 ?
O5 Cl1 O5 180(2) . 7 ?
O5 Cl1 O5 96(3) 8 7 ?
O6 O4 O6 72.3(18) . 8 ?
O6 O4 Cl1 61.5(12) . . ?
O6 O4 Cl1 56.4(14) 8 . ?
O6 O4 O6 115(3) . 3 ?
O6 O4 O6 64(2) 8 3 ?
Cl1 O4 O6 55.1(13) . 3 ?
O6 O5 O6 82(4) 8 3 ?
O6 O5 O6 73(4) 8 . ?
O6 O5 O6 119.9(19) 3 . ?
O6 O5 Cl1 62.7(12) 8 . ?
O6 O5 Cl1 62.2(13) 3 . ?
O6 O5 Cl1 57.8(15) . . ?
O4 O6 O5 111(3) . 9 ?
O4 O6 O5 102(5) . 2 ?
O5 O6 O5 108(5) 9 2 ?
O4 O6 Cl1 69.9(16) . . ?
O5 O6 Cl1 67.8(14) 9 . ?
O5 O6 Cl1 67.2(16) 2 . ?
O4 O6 O5 16(2) . . ?
O5 O6 O5 96(3) 9 . ?
O5 O6 O5 108(6) 2 . ?
Cl1 O6 O5 61.8(16) . . ?
O4 O6 O4 119(3) . 9 ?
O5 O6 O4 15(2) 9 9 ?
O5 O6 O4 94(4) 2 9 ?
Cl1 O6 O4 62.8(16) . 9 ?
O5 O6 O4 104(4) . 9 ?
O4 O6 O4 89(3) . 2 ?
O5 O6 O4 113(3) 9 2 ?
O5 O6 O4 13(3) 2 2 ?
Cl1 O6 O4 61.2(16) . 2 ?
O5 O6 O4 95(4) . 2 ?
O4 O6 O4 100(2) 9 2 ?
O4 O6 O6 62(2) . 8 ?
O5 O6 O6 50(3) 9 8 ?
O5 O6 O6 123(2) 2 8 ?
Cl1 O6 O6 55.5(12) . 8 ?
O5 O6 O6 46.3(15) . 8 ?
O4 O6 O6 60(4) 9 8 ?
O4 O6 O6 115.9(13) 2 8 ?
O4 O6 O6 124.1(15) . 9 ?
O5 O6 O6 60(5) 9 9 ?
O5 O6 O6 48.3(18) 2 9 ?
Cl1 O6 O6 55.5(12) . 9 ?
O5 O6 O6 117.3(14) . 9 ?
O4 O6 O6 46(3) 9 9 ?
O4 O6 O6 56(2) 2 9 ?
O6 O6 O6 93(5) 8 9 ?
C12 C11 C12 118(4) . 3_455 ?
C11 C12 C11 122(4) . 2_565 ?
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 O1 1.9149(10) . ?
Fe1 O2 2.014(3) 10_556 ?
Fe1 O2 2.014(3) . ?
Fe1 O3 2.015(3) 3_565 ?
Fe1 O3 2.015(3) 12_566 ?
Fe1 N1 2.206(6) . ?
N1 C8 1.338(5) . ?
N1 C8 1.338(5) 10_556 ?
O1 Fe1 1.9149(10) 3_565 ?
O1 Fe1 1.9149(10) 2_665 ?
O2 C1 1.267(5) . ?
O3 C1 1.269(5) . ?
O3 Fe1 2.015(3) 2_665 ?
C1 C2 1.489(6) . ?
C2 C7 1.388(6) . ?
C2 C3 1.393(7) . ?
C3 C4 1.387(7) . ?
C4 C5 1.377(7) . ?
C5 C6 1.367(8) . ?
C6 C7 1.381(6) . ?
C8 C9 1.395(8) . ?
C9 C10 1.367(7) . ?
C10 C9 1.367(7) 10_556 ?
Cl1 O6 1.408(17) 8 ?
Cl1 O6 1.408(17) 2 ?
Cl1 O6 1.408(17) . ?
Cl1 O6 1.408(17) 9 ?
Cl1 O6 1.408(17) 3 ?
Cl1 O6 1.408(17) 7 ?
Cl1 O5 1.467(16) 3 ?
Cl1 O5 1.467(16) 9 ?
Cl1 O5 1.467(16) 2 ?
Cl1 O5 1.467(16) . ?
Cl1 O5 1.467(16) 8 ?
Cl1 O5 1.467(16) 7 ?
O4 O6 1.20(5) . ?
O4 O6 1.48(6) 8 ?
O4 O6 1.54(6) 3 ?
O5 O6 1.20(4) 8 ?
O5 O6 1.23(5) 3 ?
O5 O6 1.45(6) . ?
O6 O5 1.20(4) 9 ?
O6 O5 1.23(5) 2 ?
O6 O4 1.48(6) 9 ?
O6 O4 1.54(6) 2 ?
O6 O6 1.59(5) 8 ?
O6 O6 1.59(5) 9 ?
C11 C12 1.323(19) . ?
C11 C12 1.33(3) 3_455 ?
C12 C11 1.33(2) 2_565 ?
