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#$Date: 2023-05-05 05:15:11 +0300 (Fri, 05 May 2023) $
#$Revision: 283296 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712154.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_7712154
loop_
_publ_author_name
'Tzani, Sofia'
'Pissas, Michael'
'Psycharis, Vassilis'
'Pantazis, Dimitrios A.'
'Sanakis, Yiannis'
'Raptopoulou, Catherine P.'
_publ_section_title
;
 Synthesis and structural, magnetic and spectroscopic characterization of
 iron(III) complexes with in situ formed ligands from
 methyl-2-pyridyl ketone transformations.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1582
_journal_page_last               1594
_journal_paper_doi               10.1039/d2dt03944c
_journal_volume                  52
_journal_year                    2023
_chemical_formula_sum            'C31.8 H33.7 Cl6 Fe4 N4.7 O6.4'
_chemical_formula_weight         1020.23
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   34.0344(2)
_cell_length_b                   34.0344(2)
_cell_length_c                   21.8653(3)
_cell_measurement_reflns_used    23647
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      71.87
_cell_measurement_theta_min      6.61
_cell_volume                     21934.2(4)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32103
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_min         6.607
_exptl_absorpt_coefficient_mu    12.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9263
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0553
_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)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3032
_reflns_number_total             4124
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03944c2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7712154--7712155.cif.'
_cod_original_formula_sum        'C31.80 H33.70 Cl6 Fe4 N4.70 O6.40'
_cod_database_code               7712154
_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'
'y, x, -z+1/2'
'-x+y, -x, z'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x-y+2/3, x+1/3, -z+1/3'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x-y+1/3, x+2/3, -z+2/3'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
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 0.23430(2) 0.85980(2) 0.03687(4) 0.0282(2) Uani 1 1 d . . . . .
Fe2 Fe 0.17571(2) 0.75192(2) 0.01262(4) 0.0321(3) Uani 1 1 d . . . . .
Cl1 Cl 0.31023(4) 0.90778(4) 0.03261(6) 0.0407(4) Uani 1 1 d . . . . .
Cl2 Cl 0.17230(4) 0.70254(4) 0.08119(6) 0.0504(4) Uani 1 1 d . . . . .
Cl3 Cl 0.18419(5) 0.73271(5) -0.08065(7) 0.0549(4) Uani 1 1 d . . . . .
N1 N 0.22785(13) 0.87362(12) -0.05712(18) 0.0327(10) Uani 1 1 d . . . . .
N2 N 0.10404(13) 0.72659(12) 0.00727(18) 0.0347(10) Uani 1 1 d . . . . .
O1 O 0.20096(10) 0.89496(9) 0.04085(14) 0.0282(8) Uani 1 1 d . . . . .
O2 O 0.16912(9) 0.80574(9) 0.02085(13) 0.0301(8) Uani 1 1 d . . . . .
O3 O 0.23681(10) 0.80315(10) 0.02854(15) 0.0350(8) Uani 1 1 d . . . . .
C1 C 0.24972(18) 0.86740(18) -0.1050(3) 0.0421(14) Uani 1 1 d . . . . .
C2 C 0.24168(18) 0.87474(18) -0.1644(3) 0.0435(15) Uani 1 1 d . . . . .
C3 C 0.21048(19) 0.88882(18) -0.1751(3) 0.0475(15) Uani 1 1 d . . . . .
C4 C 0.18831(18) 0.89526(16) -0.1262(3) 0.0390(14) Uani 1 1 d . . . . .
C5 C 0.19759(15) 0.88706(14) -0.0673(2) 0.0288(11) Uani 1 1 d . . . . .
C6 C 0.17186(16) 0.88857(15) -0.0109(2) 0.0297(11) Uani 1 1 d . . . . .
C7 C 0.12917(15) 0.84267(15) -0.0074(2) 0.0289(12) Uani 1 1 d . . . . .
H7 H 0.1038(15) 0.8390(15) -0.013(2) 0.038 Uiso 1 1 d . U . . .
C8 C 0.12989(15) 0.80521(15) 0.0063(2) 0.0288(11) Uani 1 1 d . . . . .
C9 C 0.09109(15) 0.75830(15) 0.0043(2) 0.0284(11) Uani 1 1 d . . . . .
C10 C 0.04624(17) 0.74629(17) -0.0008(2) 0.0365(13) Uani 1 1 d . . . . .
C11 C 0.01337(17) 0.70139(17) -0.0039(2) 0.0437(14) Uani 1 1 d . . . . .
H11 H -0.0177 0.6928 -0.0078 0.057 Uiso 1 1 calc R U . . .
C12 C 0.02627(19) 0.66873(19) -0.0012(3) 0.0511(16) Uani 1 1 d . . . . .
C13 C 0.07172(18) 0.68242(18) 0.0045(3) 0.0462(15) Uani 1 1 d . . . . .
C14 C 0.16207(17) 0.92749(16) -0.0130(3) 0.0426(14) Uani 1 1 d . . . . .
H14A H 0.1907 0.9564 -0.0137 0.064 Uiso 1 1 calc R U . . .
H14B H 0.1445 0.9263 0.0232 0.064 Uiso 1 1 calc R U . . .
H14C H 0.1446 0.9249 -0.0500 0.064 Uiso 1 1 calc R U . . .
C15 C 0.27592(18) 0.79696(19) 0.0226(3) 0.0643(19) Uani 1 1 d . . . . .
H15A H 0.2693 0.7683 0.0419 0.096 Uiso 1 1 calc R U . . .
H15B H 0.3022 0.8222 0.0426 0.096 Uiso 1 1 calc R U . . .
H15C H 0.2826 0.7962 -0.0209 0.096 Uiso 1 1 calc R U . . .
H1 H 0.2729(14) 0.8584(14) -0.0909(18) 0.027(12) Uiso 1 1 d . . . . .
H2 H 0.2547(17) 0.8715(16) -0.202(2) 0.054(17) Uiso 1 1 d . . . . .
H3 H 0.2042(16) 0.8974(16) -0.218(2) 0.051(16) Uiso 1 1 d . . . . .
H4 H 0.1665(16) 0.9041(16) -0.129(2) 0.046(16) Uiso 1 1 d . . . . .
H10 H 0.0398(14) 0.7685(13) -0.0010(18) 0.024(12) Uiso 1 1 d . . . . .
H12 H 0.0030(18) 0.6377(18) -0.004(2) 0.062(17) Uiso 1 1 d . . . . .
H13 H 0.0823(16) 0.6602(17) 0.002(2) 0.051(16) Uiso 1 1 d . . . . .
N1S N 0.3953(7) 0.8510(7) 0.0508(9) 0.113(7) Uiso 0.35 1 d . . P A 1
C1S C 0.3997(7) 0.8238(8) 0.0312(11) 0.094(7) Uiso 0.35 1 d . . P A 1
C2S C 0.4062(8) 0.7868(9) 0.0114(12) 0.112(8) Uiso 0.35 1 d . . P A 1
O1M O 0.4189(17) 0.7655(18) -0.026(2) 0.095(16) Uiso 0.1 1 d . . P B 2
C1M C 0.376(2) 0.761(2) -0.031(3) 0.08(2) Uiso 0.1 1 d . . P B 2
O2M O 0.080(2) 0.994(3) 0.023(3) 0.16(3) Uiso 0.1 1 d . . P . .
C2M C 0.044(3) 0.955(3) 0.015(4) 0.09(2) Uiso 0.1 1 d . . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
O3 Fe1 O1 106.13(13) . 15_454 ?
O3 Fe1 O1 152.95(12) . . ?
O1 Fe1 O1 75.68(14) 15_454 . ?
O3 Fe1 O2 70.75(12) . . ?
O1 Fe1 O2 98.47(12) 15_454 . ?
O1 Fe1 O2 82.25(11) . . ?
O3 Fe1 N1 100.62(14) . . ?
O1 Fe1 N1 151.65(14) 15_454 . ?
O1 Fe1 N1 76.24(14) . . ?
O2 Fe1 N1 81.49(13) . . ?
O3 Fe1 Cl1 96.25(9) . . ?
O1 Fe1 Cl1 95.76(9) 15_454 . ?
O1 Fe1 Cl1 110.54(9) . . ?
O2 Fe1 Cl1 162.93(9) . . ?
N1 Fe1 Cl1 90.43(11) . . ?
O2 Fe2 O3 73.73(12) . . ?
O2 Fe2 N2 75.07(13) . . ?
O3 Fe2 N2 148.49(13) . . ?
O2 Fe2 Cl3 117.05(10) . . ?
O3 Fe2 Cl3 100.93(11) . . ?
N2 Fe2 Cl3 96.98(12) . . ?
O2 Fe2 Cl2 131.33(10) . . ?
O3 Fe2 Cl2 100.62(10) . . ?
N2 Fe2 Cl2 96.58(11) . . ?
Cl3 Fe2 Cl2 111.51(6) . . ?
C5 N1 C1 120.0(5) . . ?
C5 N1 Fe1 114.5(3) . . ?
C1 N1 Fe1 125.4(4) . . ?
C13 N2 C9 118.4(4) . . ?
C13 N2 Fe2 125.4(3) . . ?
C9 N2 Fe2 116.1(3) . . ?
C6 O1 Fe1 131.6(3) . 15_454 ?
C6 O1 Fe1 115.0(2) . . ?
Fe1 O1 Fe1 104.29(14) 15_454 . ?
C8 O2 Fe2 122.3(2) . . ?
C8 O2 Fe1 130.8(2) . . ?
Fe2 O2 Fe1 105.75(13) . . ?
C15 O3 Fe2 119.7(3) . . ?
C15 O3 Fe1 129.6(3) . . ?
Fe2 O3 Fe1 109.77(14) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 H1 112(2) . . ?
C2 C1 H1 126(2) . . ?
C1 C2 C3 118.6(6) . . ?
C1 C2 H2 130(3) . . ?
C3 C2 H2 111(3) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 124(3) . . ?
C4 C3 H3 117(3) . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 115(3) . . ?
C3 C4 H4 126(3) . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 115.4(4) . . ?
C4 C5 C6 123.4(5) . . ?
O1 C6 C7 110.4(4) . . ?
O1 C6 C14 109.0(4) . . ?
C7 C6 C14 112.7(4) . . ?
O1 C6 C5 106.0(4) . . ?
C7 C6 C5 106.1(4) . . ?
C14 C6 C5 112.5(4) . . ?
C8 C7 C6 122.4(4) . . ?
C8 C7 H7 114(3) . . ?
C6 C7 H7 123(3) . . ?
C7 C8 O2 122.0(4) . . ?
C7 C8 C9 126.7(4) . . ?
O2 C8 C9 111.2(4) . . ?
N2 C9 C10 121.5(4) . . ?
N2 C9 C8 112.8(4) . . ?
C10 C9 C8 125.7(4) . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10 123(3) . . ?
C9 C10 H10 117(3) . . ?
C10 C11 C12 118.9(5) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 119.0(5) . . ?
C13 C12 H12 123(3) . . ?
C11 C12 H12 118(3) . . ?
N2 C13 C12 122.1(5) . . ?
N2 C13 H13 117(3) . . ?
C12 C13 H13 121(3) . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1S C1S C2S 174(3) . . ?
C2M O2M C2M 123(7) . 22_665 ?
O2M C2M O2M 156(7) . 20_455 ?
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 O3 1.981(3) . ?
Fe1 O1 1.987(3) 15_454 ?
Fe1 O1 2.021(3) . ?
Fe1 O2 2.085(3) . ?
Fe1 N1 2.144(4) . ?
Fe1 Cl1 2.2656(13) . ?
Fe2 O2 1.962(3) . ?
Fe2 O3 1.965(3) . ?
Fe2 N2 2.146(4) . ?
Fe2 Cl3 2.2043(16) . ?
Fe2 Cl2 2.2116(15) . ?
N1 C5 1.338(5) . ?
N1 C1 1.361(6) . ?
N2 C13 1.349(6) . ?
N2 C9 1.356(5) . ?
O1 C6 1.446(5) . ?
O1 Fe1 1.987(3) 15_454 ?
O2 C8 1.364(5) . ?
O3 C15 1.454(6) . ?
C1 C2 1.376(8) . ?
C1 H1 1.02(4) . ?
C2 C3 1.386(8) . ?
C2 H2 0.97(5) . ?
C3 C4 1.388(8) . ?
C3 H3 1.03(5) . ?
C4 C5 1.387(7) . ?
C4 H4 0.93(5) . ?
C5 C6 1.529(6) . ?
C6 C7 1.512(6) . ?
C6 C14 1.520(6) . ?
C7 C8 1.322(6) . ?
C7 H7 0.82(4) . ?
C8 C9 1.478(6) . ?
C9 C10 1.373(6) . ?
C10 C11 1.372(6) . ?
C10 H10 0.89(4) . ?
C11 C12 1.385(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(7) . ?
C12 H12 0.95(5) . ?
C13 H13 0.99(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1S C1S 1.10(3) . ?
C1S C2S 1.45(3) . ?
O1M C1M 1.41(8) . ?
O2M C2M 1.28(9) . ?
O2M C2M 1.78(9) 22_665 ?
C2M O2M 1.78(9) 20_455 ?
