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#$Date: 2023-05-02 11:26:54 +0300 (Tue, 02 May 2023) $
#$Revision: 282938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/71/8107117.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_8107117
loop_
_publ_author_name
'Fuentealba, Mauricio'
'González, Deborah'
'Artigas, Vania'
_publ_section_title
;
 Crystal structure of
 dichloridobis{μ2-2,2′-((1E,1′E)-(ethane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(4-chlorophenolato)-κ5O,N,N′,O′:O′}diiron(III),
 C32H24Cl6Fe2N4O4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1115
_journal_page_last               1116
_journal_paper_doi               10.1515/ncrs-2016-0081
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C32 H24 Cl6 Fe2 N4 O4'
_chemical_formula_sum            'C32 H24 Cl6 Fe2 N4 O4'
_chemical_formula_weight         852.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                105.927(4)
_cell_angle_beta                 95.407(4)
_cell_angle_gamma                96.752(4)
_cell_formula_units_Z            1
_cell_length_a                   7.3325(10)
_cell_length_b                   9.1317(14)
_cell_length_c                   13.161(2)
_cell_measurement_reflns_used    5754
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.54
_cell_measurement_theta_min      2.35
_cell_volume                     834.1(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32140
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         2.346
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker, 2012) was used for absorption correction. wR2(int) was
 0.0609 before and 0.0569 after correction. The Ratio of minimum to maximum
 transmission is 0.8990. The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0323P)²+0.9891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2530
_reflns_number_total             3439
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2016-0081_suppl.cif
_cod_data_source_block           mf_df11morado_0m
_cod_database_code               8107117
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C13(H13), C15(H15), C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.53007(6) 0.39682(5) 0.08307(3) 0.02262(13) Uani 1 1 d . . . . .
Cl1 Cl 0.75085(11) 0.24620(10) 0.11124(7) 0.0391(2) Uani 1 1 d . . . . .
Cl2 Cl 0.2708(2) 0.72363(17) 0.61550(9) 0.0855(4) Uani 1 1 d . . . . .
Cl3 Cl 0.04111(18) 0.97578(15) 0.36323(11) 0.0859(5) Uani 1 1 d . . . . .
O1 O 0.5915(3) 0.5516(2) 0.21604(16) 0.0315(5) Uani 1 1 d . . . . .
O2 O 0.3466(2) 0.5380(2) 0.03063(15) 0.0222(4) Uani 1 1 d . . . . .
N1 N 0.3240(3) 0.2933(3) 0.1539(2) 0.0281(6) Uani 1 1 d . . . . .
N2 N 0.3788(3) 0.2196(3) -0.0481(2) 0.0262(6) Uani 1 1 d . . . . .
C1 C 0.5165(4) 0.5849(4) 0.3052(2) 0.0325(7) Uani 1 1 d . . . . .
C2 C 0.5883(5) 0.7208(5) 0.3858(3) 0.0485(10) Uani 1 1 d . . . . .
H2 H 0.6903 0.7840 0.3762 0.058 Uiso 1 1 calc R . . . .
C3 C 0.5110(6) 0.7625(5) 0.4786(3) 0.0576(11) Uani 1 1 d . . . . .
H3 H 0.5602 0.8540 0.5305 0.069 Uiso 1 1 calc R . . . .
C4 C 0.3620(6) 0.6705(5) 0.4954(3) 0.0539(11) Uani 1 1 d . . . . .
C5 C 0.2897(5) 0.5360(5) 0.4200(3) 0.0498(10) Uani 1 1 d . . . . .
H5 H 0.1899 0.4733 0.4324 0.060 Uiso 1 1 calc R . . . .
C6 C 0.3642(5) 0.4905(4) 0.3233(3) 0.0351(8) Uani 1 1 d . . . . .
C7 C 0.2791(4) 0.3481(4) 0.2468(3) 0.0358(8) Uani 1 1 d . . . . .
H7 H 0.1828 0.2907 0.2667 0.043 Uiso 1 1 calc R . . . .
C8 C 0.2258(4) 0.1454(4) 0.0851(3) 0.0362(8) Uani 1 1 d . . . . .
H8A H 0.1069 0.1221 0.1083 0.043 Uiso 1 1 calc R . . . .
H8B H 0.2976 0.0637 0.0883 0.043 Uiso 1 1 calc R . . . .
C9 C 0.1986(4) 0.1577(4) -0.0270(3) 0.0323(7) Uani 1 1 d . . . . .
H9A H 0.1543 0.0572 -0.0772 0.039 Uiso 1 1 calc R . . . .
H9B H 0.1089 0.2258 -0.0334 0.039 Uiso 1 1 calc R . . . .
C10 C 0.4443(4) 0.1561(4) -0.1319(3) 0.0337(7) Uani 1 1 d . . . . .
H10 H 0.3730 0.0699 -0.1804 0.040 Uiso 1 1 calc R . . . .
C11 C 0.2755(4) 0.6414(3) 0.1056(2) 0.0271(7) Uani 1 1 d . . . . .
C12 C 0.3759(4) 0.7904(4) 0.1572(2) 0.0305(7) Uani 1 1 d . . . . .
C13 C 0.3018(5) 0.8905(4) 0.2381(3) 0.0386(8) Uani 1 1 d . . . . .
H13 H 0.3672 0.9879 0.2729 0.046 Uiso 1 1 calc R . . . .
C14 C 0.1329(5) 0.8459(4) 0.2665(3) 0.0433(9) Uani 1 1 d . . . . .
C15 C 0.0357(5) 0.7010(4) 0.2173(3) 0.0402(8) Uani 1 1 d . . . . .
H15 H -0.0777 0.6710 0.2374 0.048 Uiso 1 1 calc R . . . .
C16 C 0.1085(4) 0.6000(4) 0.1375(3) 0.0330(7) Uani 1 1 d . . . . .
H16 H 0.0428 0.5022 0.1048 0.040 Uiso 1 1 calc R . . . .
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'
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'
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'
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 Cl1 96.91(7) . .
O1 Fe1 O2 89.12(8) . .
O1 Fe1 O2 110.63(8) . 2_665
O1 Fe1 N1 86.90(9) . .
O1 Fe1 N2 161.90(9) . .
O2 Fe1 Cl1 93.77(6) 2_665 .
O2 Fe1 Cl1 169.46(6) . .
O2 Fe1 O2 75.97(8) 2_665 .
O2 Fe1 N1 158.76(9) 2_665 .
O2 Fe1 N2 83.60(8) 2_665 .
N1 Fe1 Cl1 95.95(7) . .
N1 Fe1 O2 93.00(8) . .
N1 Fe1 N2 77.07(10) . .
N2 Fe1 Cl1 93.11(7) . .
N2 Fe1 O2 83.46(9) . .
C1 O1 Fe1 134.4(2) . .
Fe1 O2 Fe1 104.03(8) 2_665 .
C11 O2 Fe1 120.50(17) . 2_665
C11 O2 Fe1 118.26(17) . .
C7 N1 Fe1 126.6(2) . .
C7 N1 C8 119.6(3) . .
C8 N1 Fe1 113.83(19) . .
C9 N2 Fe1 113.71(19) . .
C10 N2 Fe1 124.6(2) . .
C10 N2 C9 121.0(3) . .
O1 C1 C2 119.3(3) . .
O1 C1 C6 122.9(3) . .
C2 C1 C6 117.8(3) . .
C1 C2 H2 119.4 . .
C3 C2 C1 121.3(4) . .
C3 C2 H2 119.4 . .
C2 C3 H3 119.7 . .
C4 C3 C2 120.6(4) . .
C4 C3 H3 119.7 . .
C3 C4 Cl2 119.6(3) . .
C5 C4 Cl2 120.3(3) . .
C5 C4 C3 120.1(3) . .
C4 C5 H5 119.6 . .
C4 C5 C6 120.8(4) . .
C6 C5 H5 119.6 . .
C1 C6 C5 119.4(3) . .
C1 C6 C7 122.9(3) . .
C5 C6 C7 117.7(3) . .
N1 C7 C6 125.8(3) . .
N1 C7 H7 117.1 . .
C6 C7 H7 117.1 . .
N1 C8 H8A 110.2 . .
N1 C8 H8B 110.2 . .
N1 C8 C9 107.6(2) . .
H8A C8 H8B 108.5 . .
C9 C8 H8A 110.2 . .
C9 C8 H8B 110.2 . .
N2 C9 C8 106.5(2) . .
N2 C9 H9A 110.4 . .
N2 C9 H9B 110.4 . .
C8 C9 H9A 110.4 . .
C8 C9 H9B 110.4 . .
H9A C9 H9B 108.6 . .
N2 C10 H10 118.0 . .
N2 C10 C12 124.0(3) . 2_665
C12 C10 H10 118.0 2_665 .
O2 C11 C12 121.1(3) . .
O2 C11 C16 120.2(3) . .
C16 C11 C12 118.7(3) . .
C11 C12 C10 123.1(3) . 2_665
C13 C12 C10 117.7(3) . 2_665
C13 C12 C11 119.2(3) . .
C12 C13 H13 119.8 . .
C14 C13 C12 120.4(3) . .
C14 C13 H13 119.8 . .
C13 C14 Cl3 119.1(3) . .
C13 C14 C15 120.7(3) . .
C15 C14 Cl3 120.2(3) . .
C14 C15 H15 120.3 . .
C14 C15 C16 119.5(3) . .
C16 C15 H15 120.3 . .
C11 C16 C15 121.6(3) . .
C11 C16 H16 119.2 . .
C15 C16 H16 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl1 2.3109(9) .
Fe1 O1 1.899(2) .
Fe1 O2 2.0071(19) 2_665
Fe1 O2 2.161(2) .
Fe1 N1 2.111(2) .
Fe1 N2 2.125(2) .
Cl2 C4 1.743(4) .
Cl3 C14 1.733(3) .
O1 C1 1.318(4) .
O2 Fe1 2.0070(19) 2_665
O2 C11 1.356(3) .
N1 C7 1.278(4) .
N1 C8 1.463(4) .
N2 C9 1.457(4) .
N2 C10 1.264(4) .
C1 C2 1.400(5) .
C1 C6 1.408(5) .
C2 H2 0.9300 .
C2 C3 1.372(5) .
C3 H3 0.9300 .
C3 C4 1.371(6) .
C4 C5 1.362(6) .
C5 H5 0.9300 .
C5 C6 1.408(5) .
C6 C7 1.438(5) .
C7 H7 0.9300 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C9 1.507(5) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10 0.9300 .
C10 C12 1.452(4) 2_665
C11 C12 1.421(4) .
C11 C16 1.376(4) .
C12 C10 1.452(4) 2_665
C12 C13 1.398(4) .
C13 H13 0.9300 .
C13 C14 1.376(5) .
C14 C15 1.378(5) .
C15 H15 0.9300 .
C15 C16 1.389(5) .
C16 H16 0.9300 .
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Fe1 O1 C1 C2 -172.8(2) . . . .
Fe1 O1 C1 C6 6.2(5) . . . .
Fe1 O2 C11 C12 85.1(3) . . . .
Fe1 O2 C11 C12 -44.4(3) 2_665 . . .
Fe1 O2 C11 C16 -91.1(3) . . . .
Fe1 O2 C11 C16 139.4(2) 2_665 . . .
Fe1 N1 C7 C6 -1.8(5) . . . .
Fe1 N1 C8 C9 -38.3(3) . . . .
Fe1 N2 C9 C8 -40.4(3) . . . .
Fe1 N2 C10 C12 -9.0(5) . . . 2_665
Cl1 Fe1 O1 C1 -103.7(3) . . . .
Cl2 C4 C5 C6 -178.9(3) . . . .
Cl3 C14 C15 C16 177.9(3) . . . .
O1 C1 C2 C3 177.9(3) . . . .
O1 C1 C6 C5 -178.6(3) . . . .
O1 C1 C6 C7 1.2(5) . . . .
O2 Fe1 O1 C1 159.6(3) 2_665 . . .
O2 Fe1 O1 C1 85.0(3) . . . .
O2 C11 C12 C10 1.9(5) . . . 2_665
O2 C11 C12 C13 -176.6(3) . . . .
O2 C11 C16 C15 177.2(3) . . . .
N1 Fe1 O1 C1 -8.0(3) . . . .
N1 C8 C9 N2 49.8(3) . . . .
N2 Fe1 O1 C1 19.4(5) . . . .
C1 C2 C3 C4 0.8(6) . . . .
C1 C6 C7 N1 -2.9(5) . . . .
C2 C1 C6 C5 0.4(5) . . . .
C2 C1 C6 C7 -179.8(3) . . . .
C2 C3 C4 Cl2 178.2(3) . . . .
C2 C3 C4 C5 0.4(7) . . . .
C3 C4 C5 C6 -1.1(6) . . . .
C4 C5 C6 C1 0.7(6) . . . .
C4 C5 C6 C7 -179.1(3) . . . .
C5 C6 C7 N1 176.9(3) . . . .
C6 C1 C2 C3 -1.2(6) . . . .
C7 N1 C8 C9 140.8(3) . . . .
C8 N1 C7 C6 179.2(3) . . . .
C9 N2 C10 C12 -178.8(3) . . . 2_665
C10 N2 C9 C8 130.4(3) . . . .
C10 C12 C13 C14 -179.3(3) 2_665 . . .
C11 C12 C13 C14 -0.7(5) . . . .
C12 C11 C16 C15 0.9(5) . . . .
C12 C13 C14 Cl3 -177.4(3) . . . .
C12 C13 C14 C15 1.3(6) . . . .
C13 C14 C15 C16 -0.8(6) . . . .
C14 C15 C16 C11 -0.4(5) . . . .
C16 C11 C12 C10 178.1(3) . . . 2_665
C16 C11 C12 C13 -0.4(5) . . . .
