#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:22:04 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233603 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/91/4349122.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_4349122
loop_
_publ_author_name
'Georgopoulou, Anastasia N.'
'Margiolaki, Irene'
'Psycharis, Vassilis'
'Boudalis, Athanassios K.'
_publ_section_title
;
 Dynamic versus Static Character of the Magnetic Jahn-Teller Effect:
 Magnetostructural Studies of
 [Fe₃O(O₂CPh)₆(py)₃]ClO₄·py.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              762
_journal_page_last               772
_journal_paper_doi               10.1021/acs.inorgchem.6b01912
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C62 H50 Cl Fe3 N4 O17'
_chemical_formula_weight         1326.06
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.36800(10)
_cell_length_b                   13.36800(10)
_cell_length_c                   19.0237(2)
_cell_measurement_reflns_used    15428
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.2377
_cell_measurement_theta_min      1.7324
_cell_volume                     2944.14(4)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2006)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'KM6 SNBL, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51699
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_min         3.002
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.34.32a (release 01-07-2010 CrysAlis171 .NET)
(compiled Jul  1 2010,18:57:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²+0.9427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2900
_reflns_number_total             3038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01912_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2944.14(5)
_cod_database_code               4349122
_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.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.21221(2) 0.50931(2) 0.2500 0.01908(7) Uani 1 2 d S T P . .
N1 N 0.07319(10) 0.32819(10) 0.2500 0.0235(2) Uani 1 2 d S T P . .
O1 O 0.3333 0.6667 0.2500 0.0201(3) Uani 1 6 d S T P . .
O2 O 0.28242(6) 0.45748(6) 0.17508(4) 0.02821(16) Uani 1 1 d . . . . .
O3 O 0.11606(7) 0.52912(7) 0.17629(5) 0.03513(19) Uani 1 1 d . . . . .
C1 C 0.38508(8) 0.49406(8) 0.15576(5) 0.02243(17) Uani 1 1 d . . . . .
C2 C 0.40649(9) 0.42301(8) 0.10418(5) 0.02476(18) Uani 1 1 d . . . . .
C3 C 0.51942(10) 0.45480(10) 0.08547(7) 0.0345(2) Uani 1 1 d . . . . .
C4 C 0.53855(11) 0.39141(12) 0.03473(8) 0.0407(3) Uani 1 1 d . . . . .
C5 C 0.44619(12) 0.29763(11) 0.00257(7) 0.0387(3) Uani 1 1 d . . . . .
C6 C 0.33388(11) 0.26389(10) 0.02255(7) 0.0348(2) Uani 1 1 d . . . . .
C7 C 0.31396(9) 0.32623(9) 0.07378(6) 0.02750(19) Uani 1 1 d . . . . .
C8 C 0.02963(9) 0.27129(9) 0.18936(6) 0.0296(2) Uani 1 1 d . . . . .
C9 C -0.05744(11) 0.15662(11) 0.18721(8) 0.0419(3) Uani 1 1 d . . . . .
C10 C -0.10196(18) 0.09884(15) 0.2500 0.0483(5) Uani 1 2 d S T P . .
Cl1 Cl 0.9913(18) 0.9863(14) 0.0054(12) 0.050(2) Uani 0.1667 1 d D . P A -1
O41 O 0.960(3) 0.9130(19) -0.0530(12) 0.071(6) Uani 0.1667 1 d D . P A -1
O42 O 1.0794(16) 0.982(2) 0.0464(13) 0.085(8) Uani 0.1667 1 d D . P A -1
O43 O 0.8959(7) 0.9543(12) 0.0527(7) 0.027(2) Uani 0.1667 1 d D . P A -1
O44 O 1.0290(19) 1.1023(8) -0.0146(12) 0.122(8) Uani 0.1667 1 d D . P A -1
C11 C 0.6536(5) 0.4290(4) 0.2500 0.1007(13) Uani 0.8333 2 d S T P . .
H11 H 0.6454 0.4942 0.2500 0.121 Uiso 0.8333 2 d S U P . .
C12 C 0.5599(5) 0.3205(6) 0.2500 0.1115(14) Uani 0.8333 2 d S T P . .
H12 H 0.4878 0.3127 0.2500 0.134 Uiso 0.8333 2 d S U P . .
N11 N 0.6536(5) 0.4290(4) 0.2500 0.1007(13) Uani 0.1667 2 d S T P . .
N12 N 0.5599(5) 0.3205(6) 0.2500 0.1115(14) Uani 0.1667 2 d S T P . .
H3 H 0.5815(16) 0.5253(16) 0.1045(10) 0.050(5) Uiso 1 1 d . . . . .
H4 H 0.6172(17) 0.4121(18) 0.0224(11) 0.053(5) Uiso 1 1 d . . . . .
H5 H 0.4613(17) 0.2565(16) -0.0351(10) 0.047(5) Uiso 1 1 d . . . . .
H6 H 0.2719(16) 0.2013(16) 0.0023(8) 0.041(4) Uiso 1 1 d . . . . .
H7 H 0.2388(14) 0.3040(13) 0.0881(8) 0.033(4) Uiso 1 1 d . . . . .
H8 H 0.0620(13) 0.3120(13) 0.1483(8) 0.031(4) Uiso 1 1 d . . . . .
H9 H -0.0839(16) 0.1187(16) 0.1447(10) 0.051(5) Uiso 1 1 d . . . . .
H10 H -0.163(3) 0.021(2) 0.2500 0.057(8) Uiso 1 2 d S . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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'
Cl Cl 0.1460 0.1544 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3470 0.8244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 '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
O1 Fe1 O3 95.80(2) . 10_556
O1 Fe1 O3 95.80(2) . .
O3 Fe1 O3 88.63(6) 10_556 .
O1 Fe1 O2 95.44(2) . .
O3 Fe1 O2 168.73(3) 10_556 .
O3 Fe1 O2 89.44(4) . .
O1 Fe1 O2 95.44(2) . 10_556
O3 Fe1 O2 89.44(4) 10_556 10_556
O3 Fe1 O2 168.73(3) . 10_556
O2 Fe1 O2 90.29(5) . 10_556
O1 Fe1 N1 179.87(3) . .
O3 Fe1 N1 84.30(3) 10_556 .
O3 Fe1 N1 84.30(3) . .
O2 Fe1 N1 84.46(3) . .
O2 Fe1 N1 84.46(3) 10_556 .
C8 N1 C8 118.31(13) . 10_556
C8 N1 Fe1 120.85(6) . .
C8 N1 Fe1 120.85(6) 10_556 .
Fe1 O1 Fe1 120.0 2_665 .
Fe1 O1 Fe1 120.0 2_665 3_565
Fe1 O1 Fe1 120.0 . 3_565
C1 O2 Fe1 132.75(6) . .
C1 O3 Fe1 132.97(7) 3_565 .
O3 C1 O2 124.81(9) 2_665 .
O3 C1 C2 117.54(9) 2_665 .
O2 C1 C2 117.65(8) . .
C7 C2 C3 120.04(9) . .
C7 C2 C1 120.10(9) . .
C3 C2 C1 119.85(9) . .
C4 C3 C2 119.51(11) . .
C4 C3 H3 121.7(11) . .
C2 C3 H3 118.4(11) . .
C5 C4 C3 120.37(11) . .
C5 C4 H4 119.8(12) . .
C3 C4 H4 119.8(12) . .
C4 C5 C6 120.19(11) . .
C4 C5 H5 119.2(12) . .
C6 C5 H5 120.6(12) . .
C5 C6 C7 119.80(11) . .
C5 C6 H6 121.2(11) . .
C7 C6 H6 119.0(11) . .
C6 C7 C2 120.02(10) . .
C6 C7 H7 120.7(10) . .
C2 C7 H7 119.3(10) . .
N1 C8 C9 122.54(12) . .
N1 C8 H8 116.7(9) . .
C9 C8 H8 120.8(9) . .
C10 C9 C8 118.71(13) . .
C10 C9 H9 120.5(11) . .
C8 C9 H9 120.7(11) . .
C9 C10 C9 119.20(16) 10_556 .
C9 C10 H10 120.39(8) 10_556 .
C9 C10 H10 120.39(8) . .
O41 Cl1 O44 111.7(18) . .
O41 Cl1 O42 111(2) . .
O44 Cl1 O42 109.7(19) . .
O41 Cl1 O43 112.3(18) . .
O44 Cl1 O43 105.7(16) . .
O42 Cl1 O43 105.7(14) . .
C12 C11 N12 118.1 . 3_665
C12 C11 C12 118.1(6) . 3_665
N12 C11 C12 0.0 3_665 3_665
C12 C11 H11 121.4(6) . .
N12 C11 H11 120.5(6) 3_665 .
C12 C11 H11 120.5(6) 3_665 .
C11 C12 N11 121.9 . 2_655
C11 C12 C11 121.9(6) . 2_655
N11 C12 C11 0.0 2_655 2_655
C11 C12 H12 118.4(7) . .
N11 C12 H12 119.7(7) 2_655 .
C11 C12 H12 119.7(7) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.90804(18) .
Fe1 O3 2.0071(8) 10_556
Fe1 O3 2.0072(8) .
Fe1 O2 2.0107(7) .
Fe1 O2 2.0108(7) 10_556
Fe1 N1 2.1946(12) .
N1 C8 1.3438(12) .
N1 C8 1.3438(12) 10_556
O1 Fe1 1.90799(18) 2_665
O1 Fe1 1.90809(18) 3_565
O2 C1 1.2595(12) .
O3 C1 1.2592(12) 3_565
C1 O3 1.2593(12) 2_665
C1 C2 1.4896(13) .
C2 C7 1.3921(14) .
C2 C3 1.3945(15) .
C3 C4 1.3899(16) .
C3 H3 0.962(19) .
C4 C5 1.3865(18) .
C4 H4 0.97(2) .
C5 C6 1.3873(18) .
C5 H5 0.983(18) .
C6 C7 1.3918(14) .
C6 H6 0.917(18) .
C7 H7 0.934(16) .
C8 C9 1.3864(15) .
C8 H8 0.927(15) .
C9 C10 1.3850(18) .
C9 H9 0.925(19) .
C10 C9 1.3849(18) 10_556
C10 H10 0.95(3) .
Cl1 O41 1.402(17) .
Cl1 O44 1.421(15) .
Cl1 O42 1.436(18) .
Cl1 O43 1.439(17) .
C11 C12 1.362(7) .
C11 N12 1.362(6) 3_665
C11 C12 1.362(6) 3_665
C11 H11 0.931(4) .
C12 N11 1.362(6) 2_655
C12 C11 1.362(6) 2_655
C12 H12 0.917(6) .
