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#$Date: 2024-09-06 01:48:15 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294398 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572068.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_1572068
loop_
_publ_author_name
'Körner, Lukas'
'Bockfeld, Dirk'
'Bannenberg, Thomas'
'Tamm, Matthias'
_publ_section_title
;
 2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as
 catalysts for reductive amination reactions
;
_journal_issue                   16
_journal_name_full               'Catalysis Science & Technology'
_journal_page_first              4522
_journal_page_last               4532
_journal_paper_doi               10.1039/D4CY00372A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C34 H38 Fe N2 O4'
_chemical_formula_sum            'C34 H38 Fe N2 O4'
_chemical_formula_weight         594.51
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                105.1650(10)
_cell_angle_beta                 92.6020(10)
_cell_angle_gamma                114.222(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9427(2)
_cell_length_b                   10.8687(2)
_cell_length_c                   16.2473(3)
_cell_measurement_reflns_used    130034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.9580
_cell_measurement_theta_min      2.2620
_cell_volume                     1521.98(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_publication_material
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            250909
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.910
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         24953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0491P)²+0.1343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21485
_reflns_number_total             24953
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cy00372a3.cif
_cod_data_source_block           lk40db
_cod_depositor_comments
'Adding full bibliography for 1572060--1572070.cif.'
_cod_database_code               1572068
_shelx_shelxl_version_number     2018/3
_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   0.846
_shelx_estimated_absorpt_t_max   0.911
_oxdiff_exptl_absorpt_empirical_full_min 0.932
_oxdiff_exptl_absorpt_empirical_full_max 1.166
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
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 0.38426(2) 0.59421(2) 0.79976(2) 0.01074(2) Uani 1 1 d . . . . .
O1 O 0.41113(4) 0.31669(4) 0.64747(3) 0.01431(6) Uani 1 1 d . . . . .
O4 O 0.09820(5) 0.61345(6) 0.78534(4) 0.02562(9) Uani 1 1 d . . . . .
O3 O 0.26623(7) 0.34378(5) 0.86097(4) 0.02792(10) Uani 1 1 d . . . . .
O2 O 0.51511(7) 0.81449(6) 0.96943(3) 0.03105(11) Uani 1 1 d . . . . .
N1 N 0.73246(4) 0.80340(4) 0.80585(3) 0.01191(5) Uani 1 1 d . . . . .
N2 N 0.65691(4) 0.50469(4) 0.80928(3) 0.01139(5) Uani 1 1 d . . . . .
C2 C 0.37748(5) 0.52987(5) 0.66465(3) 0.01096(6) Uani 1 1 d . . . . .
C1 C 0.44870(5) 0.44326(4) 0.68421(3) 0.01086(6) Uani 1 1 d . . . . .
C15 C 0.57746(5) 0.85402(5) 0.62252(3) 0.01239(6) Uani 1 1 d . . . . .
C11 C 0.28010(5) 0.53716(5) 0.52421(3) 0.01339(6) Uani 1 1 d . . . . .
H11 H 0.372734 0.617714 0.531591 0.016 Uiso 1 1 calc R U . . .
C31 C 0.70658(5) 0.58553(5) 0.90186(3) 0.01313(6) Uani 1 1 d . . . . .
H31A H 0.623114 0.550984 0.933601 0.016 Uiso 1 1 calc R U . . .
H31B H 0.735010 0.686960 0.909518 0.016 Uiso 1 1 calc R U . . .
C4 C 0.60252(5) 0.68510(4) 0.76061(3) 0.01023(6) Uani 1 1 d . . . . .
C3 C 0.47999(5) 0.67891(4) 0.70537(3) 0.01040(6) Uani 1 1 d . . . . .
C14 C 0.47991(5) 0.79994(4) 0.67799(3) 0.01085(6) Uani 1 1 d . . . . .
C6 C 0.25423(5) 0.47132(5) 0.58946(3) 0.01229(6) Uani 1 1 d . . . . .
C5 C 0.56938(5) 0.54223(4) 0.76122(3) 0.01019(6) Uani 1 1 d . . . . .
C17 C 0.47040(6) 1.02008(5) 0.62259(3) 0.01493(7) Uani 1 1 d . . . . .
H17 H 0.468496 1.094860 0.603419 0.018 Uiso 1 1 calc R U . . .
C26 C 0.74117(6) 0.94622(5) 0.82401(3) 0.01466(7) Uani 1 1 d . . . . .
H26A H 0.643438 0.943995 0.835609 0.018 Uiso 1 1 calc R U . . .
H26B H 0.764865 0.980030 0.773112 0.018 Uiso 1 1 calc R U . . .
C7 C 0.11884(5) 0.34866(5) 0.57730(3) 0.01491(7) Uani 1 1 d . . . . .
C16 C 0.57126(6) 0.96498(5) 0.59680(3) 0.01471(7) Uani 1 1 d . . . . .
H16 H 0.638006 1.004034 0.560554 0.018 Uiso 1 1 calc R U . . .
C30 C 0.84016(6) 0.56971(6) 0.93921(3) 0.01569(7) Uani 1 1 d . . . . .
H30A H 0.868780 0.621315 1.002016 0.019 Uiso 1 1 calc R U . . .
H30B H 0.926575 0.612350 0.911154 0.019 Uiso 1 1 calc R U . . .
C19 C 0.38004(5) 0.85704(5) 0.70398(3) 0.01309(6) Uani 1 1 d . . . . .
H19 H 0.315190 0.820523 0.741717 0.016 Uiso 1 1 calc R U . . .
C22 C 0.87427(5) 0.79623(5) 0.78972(3) 0.01360(6) Uani 1 1 d . . . . .
H22A H 0.900925 0.821582 0.736478 0.016 Uiso 1 1 calc R U . . .
H22B H 0.861541 0.698126 0.780687 0.016 Uiso 1 1 calc R U . . .
C23 C 1.00014(5) 0.89732(5) 0.86594(4) 0.01620(7) Uani 1 1 d . . . . .
H23A H 1.095980 0.897590 0.851651 0.019 Uiso 1 1 calc R U . . .
H23B H 0.980100 0.863998 0.917264 0.019 Uiso 1 1 calc R U . . .
C10 C 0.17608(6) 0.48972(6) 0.44912(3) 0.01496(7) Uani 1 1 d . . . . .
C27 C 0.61269(6) 0.35266(5) 0.79515(3) 0.01572(7) Uani 1 1 d . . . . .
H27A H 0.578856 0.300573 0.732532 0.019 Uiso 1 1 calc R U . . .
H27B H 0.528185 0.314332 0.825486 0.019 Uiso 1 1 calc R U . . .
C20 C 0.68459(6) 0.79543(6) 0.58815(3) 0.01734(8) Uani 1 1 d . . . . .
H20A H 0.787372 0.863780 0.616036 0.026 Uiso 1 1 calc R U . . .
H20B H 0.675092 0.778395 0.525416 0.026 Uiso 1 1 calc R U . . .
H20C H 0.660886 0.706065 0.600685 0.026 Uiso 1 1 calc R U . . .
C25 C 0.86265(6) 1.04688(5) 0.90258(4) 0.01738(8) Uani 1 1 d . . . . .
H25A H 0.834977 1.016605 0.954256 0.021 Uiso 1 1 calc R U . . .
H25B H 0.870834 1.143923 0.913721 0.021 Uiso 1 1 calc R U . . .
C32 C 0.46386(6) 0.72865(6) 0.90372(4) 0.01820(8) Uani 1 1 d . . . . .
C13 C 0.20863(7) 0.56981(7) 0.38403(3) 0.01952(9) Uani 1 1 d . . . . .
H13A H 0.140118 0.613660 0.383193 0.029 Uiso 1 1 calc R U . . .
H13B H 0.194797 0.504271 0.326467 0.029 Uiso 1 1 calc R U . . .
H13C H 0.312185 0.643666 0.400030 0.029 Uiso 1 1 calc R U . . .
C9 C 0.04276(6) 0.36853(6) 0.43784(3) 0.01783(8) Uani 1 1 d . . . . .
H9 H -0.030203 0.332976 0.387177 0.021 Uiso 1 1 calc R U . . .
C33 C 0.31207(6) 0.44056(6) 0.83656(4) 0.01681(8) Uani 1 1 d . . . . .
C18 C 0.37212(5) 0.96565(5) 0.67655(3) 0.01416(7) Uani 1 1 d . . . . .
C8 C 0.01651(6) 0.29977(6) 0.50056(4) 0.01763(8) Uani 1 1 d . . . . .
H8 H -0.074234 0.216405 0.491128 0.021 Uiso 1 1 calc R U . . .
C34 C 0.21119(6) 0.60844(6) 0.79049(4) 0.01683(8) Uani 1 1 d . . . . .
C28 C 0.74428(7) 0.33083(6) 0.82893(4) 0.01978(9) Uani 1 1 d . . . . .
H28A H 0.825769 0.362581 0.795458 0.024 Uiso 1 1 calc R U . . .
H28B H 0.712063 0.228635 0.820594 0.024 Uiso 1 1 calc R U . . .
C24 C 1.01341(6) 1.04767(6) 0.88716(4) 0.01852(8) Uani 1 1 d . . . . .
H24A H 1.045407 1.085660 0.838585 0.022 Uiso 1 1 calc R U . . .
H24B H 1.090034 1.109834 0.939589 0.022 Uiso 1 1 calc R U . . .
C21 C 0.25984(7) 1.02108(6) 0.70442(5) 0.02154(10) Uani 1 1 d . . . . .
H21A H 0.271845 1.098335 0.680632 0.032 Uiso 1 1 calc R U . . .
H21B H 0.276315 1.056508 0.767779 0.032 Uiso 1 1 calc R U . . .
H21C H 0.158312 0.944450 0.682974 0.032 Uiso 1 1 calc R U . . .
C29 C 0.80286(7) 0.41369(6) 0.92493(4) 0.02046(9) Uani 1 1 d . . . . .
H29A H 0.893694 0.405188 0.944197 0.025 Uiso 1 1 calc R U . . .
H29B H 0.726065 0.374033 0.959509 0.025 Uiso 1 1 calc R U . . .
C12 C 0.07684(6) 0.26904(6) 0.64256(4) 0.01992(9) Uani 1 1 d . . . . .
H12A H 0.156525 0.243375 0.657127 0.030 Uiso 1 1 calc R U . . .
H12B H -0.016901 0.182785 0.617974 0.030 Uiso 1 1 calc R U . . .
H12C H 0.063582 0.329179 0.695015 0.030 Uiso 1 1 calc R U . . .
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 12 -18 0.0698
-12 0 -3 0.0884
-5 -10 14 0.1159
-2 -11 17 0.1115
0 -1 -21 0.0972
-4 8 -21 0.0922
-6 14 2 0.1169
0 1 21 0.0954
6 -13 -7 0.1161
-7 14 -13 0.1013
6 -14 -3 0.1212
1 -14 0 0.0914
-1 -10 -10 0.1026
-4 15 -11 0.0815
-2 15 -3 0.0751
-1 -13 8 0.0994
-5 -10 -1 0.1004
-2 14 -14 0.0701
-1 14 -12 0.0631
4 11 -3 0.0914
9 7 -8 0.1034
12 1 2 0.1468
10 -8 15 0.1870
12 1 -11 0.1034
14 -3 -4 0.1360
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
C34 Fe1 C33 95.24(3) . . ?
C34 Fe1 C32 95.01(3) . . ?
C33 Fe1 C32 98.55(3) . . ?
C34 Fe1 C3 100.75(2) . . ?
C33 Fe1 C3 146.70(2) . . ?
C32 Fe1 C3 108.81(2) . . ?
C34 Fe1 C2 93.97(2) . . ?
C33 Fe1 C2 109.49(2) . . ?
C32 Fe1 C2 149.58(2) . . ?
C3 Fe1 C2 40.844(17) . . ?
C34 Fe1 C4 137.60(2) . . ?
C33 Fe1 C4 126.14(2) . . ?
C32 Fe1 C4 88.14(2) . . ?
C3 Fe1 C4 39.692(16) . . ?
C2 Fe1 C4 66.054(16) . . ?
C34 Fe1 C5 159.60(2) . . ?
C33 Fe1 C5 88.74(2) . . ?
C32 Fe1 C5 104.19(2) . . ?
C3 Fe1 C5 66.757(16) . . ?
C2 Fe1 C5 65.928(16) . . ?
C4 Fe1 C5 38.580(15) . . ?
C34 Fe1 C1 123.22(2) . . ?
C33 Fe1 C1 83.86(2) . . ?
C32 Fe1 C1 141.46(2) . . ?
C3 Fe1 C1 62.936(16) . . ?
C2 Fe1 C1 36.802(15) . . ?
C4 Fe1 C1 61.174(15) . . ?
C5 Fe1 C1 37.264(15) . . ?
C4 N1 C26 120.73(4) . . ?
C4 N1 C22 116.06(4) . . ?
C26 N1 C22 113.90(4) . . ?
C5 N2 C31 116.73(4) . . ?
C5 N2 C27 118.16(4) . . ?
C31 N2 C27 111.16(4) . . ?
C3 C2 C1 108.39(4) . . ?
C3 C2 C6 126.36(4) . . ?
C1 C2 C6 121.19(4) . . ?
C3 C2 Fe1 67.82(2) . . ?
C1 C2 Fe1 84.09(3) . . ?
C6 C2 Fe1 132.55(3) . . ?
O1 C1 C2 126.84(4) . . ?
O1 C1 C5 128.80(4) . . ?
C2 C1 C5 104.27(3) . . ?
O1 C1 Fe1 139.81(4) . . ?
C2 C1 Fe1 59.11(2) . . ?
C5 C1 Fe1 62.69(2) . . ?
C16 C15 C14 117.99(4) . . ?
C16 C15 C20 118.85(4) . . ?
C14 C15 C20 123.14(4) . . ?
C10 C11 C6 123.00(5) . . ?
N2 C31 C30 110.80(4) . . ?
N1 C4 C3 127.96(4) . . ?
N1 C4 C5 123.58(4) . . ?
C3 C4 C5 108.45(4) . . ?
N1 C4 Fe1 129.49(3) . . ?
C3 C4 Fe1 65.53(2) . . ?
C5 C4 Fe1 71.45(2) . . ?
C4 C3 C2 107.56(4) . . ?
C4 C3 C14 125.13(4) . . ?
C2 C3 C14 125.58(4) . . ?
C4 C3 Fe1 74.78(3) . . ?
C2 C3 Fe1 71.34(3) . . ?
C14 C3 Fe1 131.22(3) . . ?
C19 C14 C15 119.28(4) . . ?
C19 C14 C3 120.86(4) . . ?
C15 C14 C3 119.82(4) . . ?
C11 C6 C7 118.62(4) . . ?
C11 C6 C2 117.30(4) . . ?
C7 C6 C2 123.92(4) . . ?
N2 C5 C4 125.92(4) . . ?
N2 C5 C1 125.75(4) . . ?
C4 C5 C1 106.49(3) . . ?
N2 C5 Fe1 127.37(3) . . ?
C4 C5 Fe1 69.97(2) . . ?
C1 C5 Fe1 80.05(2) . . ?
C16 C17 C18 120.13(4) . . ?
N1 C26 C25 109.50(4) . . ?
C8 C7 C6 117.91(5) . . ?
C8 C7 C12 118.21(5) . . ?
C6 C7 C12 123.87(4) . . ?
C17 C16 C15 122.13(5) . . ?
C31 C30 C29 111.07(4) . . ?
C18 C19 C14 122.45(4) . . ?
N1 C22 C23 110.70(4) . . ?
C22 C23 C24 110.98(4) . . ?
C11 C10 C9 117.83(5) . . ?
C11 C10 C13 119.99(5) . . ?
C9 C10 C13 122.17(5) . . ?
N2 C27 C28 110.37(4) . . ?
C26 C25 C24 110.55(4) . . ?
O2 C32 Fe1 179.54(6) . . ?
C8 C9 C10 120.08(5) . . ?
O3 C33 Fe1 179.17(5) . . ?
C19 C18 C17 118.00(4) . . ?
C19 C18 C21 120.50(5) . . ?
C17 C18 C21 121.50(4) . . ?
C9 C8 C7 122.52(5) . . ?
O4 C34 Fe1 177.69(5) . . ?
C27 C28 C29 111.07(5) . . ?
C23 C24 C25 109.95(4) . . ?
C28 C29 C30 109.61(4) . . ?
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 C34 1.7929(5) . ?
Fe1 C33 1.7999(5) . ?
Fe1 C32 1.8035(6) . ?
Fe1 C3 2.0634(4) . ?
Fe1 C2 2.1111(5) . ?
Fe1 C4 2.1874(4) . ?
Fe1 C5 2.2073(4) . ?
Fe1 C1 2.4469(4) . ?
O1 C1 1.2315(6) . ?
O4 C34 1.1473(7) . ?
O3 C33 1.1457(7) . ?
O2 C32 1.1443(7) . ?
N1 C4 1.3852(6) . ?
N1 C26 1.4669(6) . ?
N1 C22 1.4751(6) . ?
N2 C5 1.3893(6) . ?
N2 C31 1.4709(6) . ?
N2 C27 1.4740(6) . ?
C2 C3 1.4573(6) . ?
C2 C1 1.4737(6) . ?
C2 C6 1.4888(6) . ?
C1 C5 1.5042(6) . ?
C15 C16 1.3983(7) . ?
C15 C14 1.4096(6) . ?
C15 C20 1.5087(7) . ?
C11 C10 1.3937(6) . ?
C11 C6 1.4046(7) . ?
C31 C30 1.5267(7) . ?
C4 C3 1.4478(6) . ?
C4 C5 1.4519(6) . ?
C3 C14 1.4951(6) . ?
C14 C19 1.3986(6) . ?
C6 C7 1.4121(7) . ?
C17 C16 1.3927(7) . ?
C17 C18 1.3959(7) . ?
C26 C25 1.5266(7) . ?
C7 C8 1.4023(7) . ?
C7 C12 1.5071(8) . ?
C30 C29 1.5287(8) . ?
C19 C18 1.3952(7) . ?
C22 C23 1.5251(7) . ?
C23 C24 1.5267(8) . ?
C10 C9 1.3945(8) . ?
C10 C13 1.5041(8) . ?
C27 C28 1.5255(7) . ?
C25 C24 1.5279(8) . ?
C9 C8 1.3884(9) . ?
C18 C21 1.5064(7) . ?
C28 C29 1.5281(8) . ?
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
_geom_torsion_publ_flag
C3 C2 C1 O1 -164.13(5) . . . . ?
C6 C2 C1 O1 -5.43(7) . . . . ?
Fe1 C2 C1 O1 131.62(5) . . . . ?
C3 C2 C1 C5 18.99(5) . . . . ?
C6 C2 C1 C5 177.69(4) . . . . ?
Fe1 C2 C1 C5 -45.26(3) . . . . ?
C3 C2 C1 Fe1 64.25(3) . . . . ?
C6 C2 C1 Fe1 -137.05(5) . . . . ?
C5 N2 C31 C30 -160.94(4) . . . . ?
C27 N2 C31 C30 59.46(5) . . . . ?
C26 N1 C4 C3 19.06(7) . . . . ?
C22 N1 C4 C3 -125.58(5) . . . . ?
C26 N1 C4 C5 -161.77(4) . . . . ?
C22 N1 C4 C5 53.59(6) . . . . ?
C26 N1 C4 Fe1 -68.77(6) . . . . ?
C22 N1 C4 Fe1 146.59(4) . . . . ?
N1 C4 C3 C2 173.64(4) . . . . ?
C5 C4 C3 C2 -5.64(5) . . . . ?
Fe1 C4 C3 C2 -64.28(3) . . . . ?
N1 C4 C3 C14 7.98(7) . . . . ?
C5 C4 C3 C14 -171.30(4) . . . . ?
Fe1 C4 C3 C14 130.06(4) . . . . ?
N1 C4 C3 Fe1 -122.08(5) . . . . ?
C5 C4 C3 Fe1 58.65(3) . . . . ?
C1 C2 C3 C4 -8.78(5) . . . . ?
C6 C2 C3 C4 -166.08(4) . . . . ?
Fe1 C2 C3 C4 66.57(3) . . . . ?
C1 C2 C3 C14 156.80(4) . . . . ?
C6 C2 C3 C14 -0.50(7) . . . . ?
Fe1 C2 C3 C14 -127.85(4) . . . . ?
C1 C2 C3 Fe1 -75.36(3) . . . . ?
C6 C2 C3 Fe1 127.35(5) . . . . ?
C16 C15 C14 C19 0.93(7) . . . . ?
C20 C15 C14 C19 -177.46(5) . . . . ?
C16 C15 C14 C3 178.48(4) . . . . ?
C20 C15 C14 C3 0.08(7) . . . . ?
C4 C3 C14 C19 -115.41(5) . . . . ?
C2 C3 C14 C19 81.46(6) . . . . ?
Fe1 C3 C14 C19 -14.49(6) . . . . ?
C4 C3 C14 C15 67.08(6) . . . . ?
C2 C3 C14 C15 -96.04(6) . . . . ?
Fe1 C3 C14 C15 168.01(3) . . . . ?
C10 C11 C6 C7 2.17(7) . . . . ?
C10 C11 C6 C2 177.71(4) . . . . ?
C3 C2 C6 C11 36.79(7) . . . . ?
C1 C2 C6 C11 -117.87(5) . . . . ?
Fe1 C2 C6 C11 129.04(4) . . . . ?
C3 C2 C6 C7 -147.93(5) . . . . ?
C1 C2 C6 C7 57.41(7) . . . . ?
Fe1 C2 C6 C7 -55.68(6) . . . . ?
C31 N2 C5 C4 49.11(6) . . . . ?
C27 N2 C5 C4 -174.17(4) . . . . ?
C31 N2 C5 C1 -148.47(4) . . . . ?
C27 N2 C5 C1 -11.75(7) . . . . ?
C31 N2 C5 Fe1 -42.09(5) . . . . ?
C27 N2 C5 Fe1 94.62(5) . . . . ?
N1 C4 C5 N2 3.36(7) . . . . ?
C3 C4 C5 N2 -177.32(4) . . . . ?
Fe1 C4 C5 N2 -122.25(4) . . . . ?
N1 C4 C5 C1 -161.83(4) . . . . ?
C3 C4 C5 C1 17.49(5) . . . . ?
Fe1 C4 C5 C1 72.56(3) . . . . ?
N1 C4 C5 Fe1 125.62(4) . . . . ?
C3 C4 C5 Fe1 -55.07(3) . . . . ?
O1 C1 C5 N2 -4.20(8) . . . . ?
C2 C1 C5 N2 172.59(4) . . . . ?
Fe1 C1 C5 N2 129.27(5) . . . . ?
O1 C1 C5 C4 161.02(5) . . . . ?
C2 C1 C5 C4 -22.19(5) . . . . ?
Fe1 C1 C5 C4 -65.51(3) . . . . ?
O1 C1 C5 Fe1 -133.48(5) . . . . ?
C2 C1 C5 Fe1 43.32(3) . . . . ?
C4 N1 C26 C25 156.62(5) . . . . ?
C22 N1 C26 C25 -58.04(6) . . . . ?
C11 C6 C7 C8 -0.52(7) . . . . ?
C2 C6 C7 C8 -175.74(4) . . . . ?
C11 C6 C7 C12 -179.36(5) . . . . ?
C2 C6 C7 C12 5.42(8) . . . . ?
C18 C17 C16 C15 0.65(8) . . . . ?
C14 C15 C16 C17 -1.50(7) . . . . ?
C20 C15 C16 C17 176.96(5) . . . . ?
N2 C31 C30 C29 -56.57(6) . . . . ?
C15 C14 C19 C18 0.47(7) . . . . ?
C3 C14 C19 C18 -177.04(4) . . . . ?
C4 N1 C22 C23 -156.41(4) . . . . ?
C26 N1 C22 C23 56.56(5) . . . . ?
N1 C22 C23 C24 -53.89(6) . . . . ?
C6 C11 C10 C9 -2.13(7) . . . . ?
C6 C11 C10 C13 177.08(5) . . . . ?
C5 N2 C27 C28 161.25(5) . . . . ?
C31 N2 C27 C28 -59.79(6) . . . . ?
N1 C26 C25 C24 57.38(6) . . . . ?
C11 C10 C9 C8 0.46(8) . . . . ?
C13 C10 C9 C8 -178.73(5) . . . . ?
C14 C19 C18 C17 -1.33(7) . . . . ?
C14 C19 C18 C21 178.37(5) . . . . ?
C16 C17 C18 C19 0.76(7) . . . . ?
C16 C17 C18 C21 -178.94(5) . . . . ?
C10 C9 C8 C7 1.13(8) . . . . ?
C6 C7 C8 C9 -1.09(8) . . . . ?
C12 C7 C8 C9 177.82(5) . . . . ?
N2 C27 C28 C29 57.42(6) . . . . ?
C22 C23 C24 C25 54.81(6) . . . . ?
C26 C25 C24 C23 -56.69(6) . . . . ?
C27 C28 C29 C30 -54.27(7) . . . . ?
C31 C30 C29 C28 53.70(7) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.5263 11.5104 -17.7217 0.2513 0.4118 0.8759
-12.0869 -0.3068 -2.6962 -0.5017 -0.8179 0.2817
-5.3345 -9.6878 13.6319 -0.4121 -0.6735 -0.6136
-1.5663 -11.2790 17.0897 -0.2893 -0.4738 -0.8318
-0.1990 -0.7849 -21.2733 -0.7227 0.2552 0.6424
-4.2852 8.3690 -21.0641 -0.2253 0.0786 0.9711
-6.4007 14.4243 1.8079 0.8311 -0.2950 0.4714
0.0379 1.1360 21.1152 0.7364 -0.2601 -0.6245
5.5748 -12.8728 -6.9315 -0.9119 0.3233 -0.2530
-6.6581 14.1315 -13.2162 0.3348 -0.1197 0.9347
6.1854 -14.0340 -3.3876 -0.8607 0.3054 -0.4073
1.3901 -13.8329 -0.2172 -0.9057 -0.0707 -0.4181
-1.1918 -9.6664 -9.5390 -0.9962 -0.0783 0.0369
-4.1091 14.8283 -11.1323 0.5309 0.0407 0.8465
-2.2573 14.6204 -3.1904 0.8248 0.0642 0.5617
-1.4836 -13.2109 8.2438 -0.6940 -0.3759 -0.6141
-5.1148 -9.8320 -0.8608 -0.8661 -0.4699 -0.1708
-1.8379 13.6706 -14.4145 0.4242 0.2290 0.8761
-0.5977 13.7634 -12.3273 0.5362 0.2900 0.7927
3.8748 11.4032 -2.5905 0.8251 0.4474 0.3449
8.9765 6.6387 -7.9249 0.5012 0.8169 0.2854
12.0095 0.7075 2.0367 0.5060 0.8261 -0.2483
9.9108 -8.2809 15.3875 0.2391 0.3923 -0.8882
11.6434 1.2448 -10.8645 0.1288 0.9761 0.1749
13.5815 -2.7615 -4.1447 0.1282 0.9746 -0.1835
