#------------------------------------------------------------------------------
#$Date: 2024-09-06 01:48:15 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294398 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572069.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_1572069
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         '(C31 H33 Fe N3 O3),0.5 (C7 H8)'
_chemical_formula_sum            'C34.5 H37 Fe N3 O3'
_chemical_formula_weight         597.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 117.667(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3890(5)
_cell_length_b                   28.6159(7)
_cell_length_c                   10.6867(5)
_cell_measurement_reflns_used    52831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.0000
_cell_measurement_theta_min      2.2480
_cell_volume                     3084.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            202323
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.567
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         17413
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0522
_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)+(0.0570P)²+1.3905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13594
_reflns_number_total             17413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cy00372a3.cif
_cod_data_source_block           lk31db
_cod_depositor_comments
'Adding full bibliography for 1572060--1572070.cif.'
_cod_original_cell_volume        3084.6(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C34.50 H37 Fe N3 O3'
_cod_database_code               1572069
_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   0.902
_shelx_estimated_absorpt_t_max   0.949
_oxdiff_exptl_absorpt_empirical_full_min 0.772
_oxdiff_exptl_absorpt_empirical_full_max 1.317
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 0.78364(2) 0.41760(2) 0.36422(2) 0.01520(4) Uani 1 1 d . . . . .
O1 O 0.50523(9) 0.48438(3) 0.21907(9) 0.02290(16) Uani 1 1 d . . . . .
O2 O 1.05343(9) 0.41702(4) 0.60117(10) 0.02669(18) Uani 1 1 d . . . . .
N2 N 0.77467(9) 0.39888(3) 0.65207(10) 0.01845(16) Uani 1 1 d . . . . .
N1 N 0.70849(9) 0.49703(3) 0.53467(10) 0.01767(15) Uani 1 1 d . . . . .
N3 N 0.78990(9) 0.47091(4) 0.25317(10) 0.01892(16) Uani 1 1 d . . . . .
O3 O 0.85163(15) 0.34828(5) 0.20684(15) 0.0446(3) Uani 1 1 d . . . . .
C4 C 0.57997(10) 0.40418(4) 0.26321(11) 0.01749(17) Uani 1 1 d . . . . .
C2 C 0.70402(10) 0.40926(4) 0.50771(11) 0.01631(16) Uani 1 1 d . . . . .
C22 C 0.49820(11) 0.38676(4) 0.11789(12) 0.02037(19) Uani 1 1 d . . . . .
C28 C 0.78558(10) 0.49927(4) 0.17559(11) 0.01778(17) Uani 1 1 d . . . . .
C6 C 0.84854(11) 0.50170(4) 0.63978(12) 0.02000(18) Uani 1 1 d . . . . .
H6A H 0.901442 0.510913 0.591922 0.024 Uiso 1 1 calc R U . . .
H6B H 0.882191 0.471230 0.686665 0.024 Uiso 1 1 calc R U . . .
C30 C 0.94828(11) 0.41900(4) 0.50665(12) 0.01893(17) Uani 1 1 d . . . . .
C1 C 0.67293(10) 0.45640(4) 0.45311(11) 0.01565(16) Uani 1 1 d . . . . .
C5 C 0.57217(10) 0.45302(4) 0.30099(11) 0.01761(17) Uani 1 1 d . . . . .
C10 C 0.65707(12) 0.54144(4) 0.46077(14) 0.0248(2) Uani 1 1 d . . . . .
H10A H 0.563226 0.537524 0.389314 0.030 Uiso 1 1 calc R U . . .
H10B H 0.708283 0.550784 0.411141 0.030 Uiso 1 1 calc R U . . .
C29 C 0.77910(12) 0.53350(4) 0.07229(12) 0.02142(19) Uani 1 1 d . . . . .
H29A H 0.696724 0.529217 -0.015719 0.032 Uiso 1 1 calc R U . . .
H29B H 0.855106 0.529352 0.053862 0.032 Uiso 1 1 calc R U . . .
H29C H 0.781114 0.565035 0.108997 0.032 Uiso 1 1 calc R U . . .
C11 C 0.84804(12) 0.35480(4) 0.69807(13) 0.0231(2) Uani 1 1 d . . . . .
H11A H 0.887240 0.346776 0.635308 0.028 Uiso 1 1 calc R U . . .
H11B H 0.786974 0.329318 0.692434 0.028 Uiso 1 1 calc R U . . .
C3 C 0.64820(10) 0.37696(4) 0.39111(12) 0.01731(17) Uani 1 1 d . . . . .
C16 C 0.63260(12) 0.32584(4) 0.40416(13) 0.0219(2) Uani 1 1 d . . . . .
C31 C 0.82571(13) 0.37554(5) 0.26858(14) 0.0248(2) Uani 1 1 d . . . . .
C23 C 0.39969(13) 0.35301(5) 0.08753(15) 0.0282(2) Uani 1 1 d . . . . .
H23 H 0.386864 0.339893 0.161941 0.034 Uiso 1 1 calc R U . . .
C9 C 0.66750(14) 0.57937(5) 0.56507(18) 0.0312(3) Uani 1 1 d . . . . .
H9A H 0.609790 0.571196 0.608187 0.037 Uiso 1 1 calc R U . . .
H9B H 0.635573 0.609312 0.513991 0.037 Uiso 1 1 calc R U . . .
C7 C 0.86451(17) 0.53820(5) 0.74989(15) 0.0330(3) Uani 1 1 d . . . . .
H7A H 0.959637 0.541520 0.817976 0.040 Uiso 1 1 calc R U . . .
H7B H 0.817274 0.527709 0.802704 0.040 Uiso 1 1 calc R U . . .
C15 C 0.71335(13) 0.41411(5) 0.73904(14) 0.0250(2) Uani 1 1 d . . . . .
H15A H 0.645156 0.391164 0.731082 0.030 Uiso 1 1 calc R U . . .
H15B H 0.669165 0.444628 0.704396 0.030 Uiso 1 1 calc R U . . .
C27 C 0.51267(13) 0.40623(5) 0.00611(13) 0.0272(2) Uani 1 1 d . . . . .
H27 H 0.577622 0.429726 0.024656 0.033 Uiso 1 1 calc R U . . .
C8 C 0.80967(15) 0.58545(5) 0.68149(16) 0.0298(3) Uani 1 1 d . . . . .
H8A H 0.865294 0.598405 0.641033 0.036 Uiso 1 1 calc R U . . .
H8B H 0.811537 0.607596 0.753557 0.036 Uiso 1 1 calc R U . . .
C12 C 0.95721(15) 0.35979(6) 0.84931(15) 0.0335(3) Uani 1 1 d . . . . .
H12A H 1.004995 0.329750 0.881657 0.040 Uiso 1 1 calc R U . . .
H12B H 1.021541 0.383778 0.853395 0.040 Uiso 1 1 calc R U . . .
C26 C 0.43318(15) 0.39164(6) -0.13207(15) 0.0348(3) Uani 1 1 d . . . . .
H26 H 0.444767 0.404940 -0.207051 0.042 Uiso 1 1 calc R U . . .
C25 C 0.33689(16) 0.35769(6) -0.16079(16) 0.0382(4) Uani 1 1 d . . . . .
H25 H 0.282698 0.347675 -0.255188 0.046 Uiso 1 1 calc R U . . .
C14 C 0.81734(18) 0.41862(6) 0.89305(15) 0.0343(3) Uani 1 1 d . . . . .
H14A H 0.772999 0.425397 0.951742 0.041 Uiso 1 1 calc R U . . .
H14B H 0.877064 0.445082 0.903021 0.041 Uiso 1 1 calc R U . . .
C24 C 0.32030(15) 0.33853(5) -0.05122(17) 0.0361(3) Uani 1 1 d . . . . .
H24 H 0.254355 0.315351 -0.070652 0.043 Uiso 1 1 calc R U . . .
C13 C 0.89896(19) 0.37380(6) 0.94583(15) 0.0398(4) Uani 1 1 d . . . . .
H13A H 0.971434 0.378780 1.042725 0.048 Uiso 1 1 calc R U . . .
H13B H 0.841777 0.348312 0.949306 0.048 Uiso 1 1 calc R U . . .
C19 C 0.5960(2) 0.23046(5) 0.4377(2) 0.0439(4) Uani 1 1 d . . . . .
H19 H 0.594125 0.198119 0.456661 0.053 Uiso 0.587(10) 1 calc R U P A 1
H19A H 0.581624 0.198308 0.447951 0.053 Uiso 0.413(10) 1 calc R U P A 2
C21 C 0.5750(4) 0.31133(15) 0.4929(5) 0.0261(6) Uani 0.587(10) 1 d . . P A 1
H21 H 0.550115 0.334136 0.540775 0.031 Uiso 0.587(10) 1 calc R U P A 1
C17 C 0.6568(4) 0.29184(9) 0.3271(5) 0.0282(6) Uani 0.587(10) 1 d . . P A 1
H17 H 0.687647 0.300849 0.261958 0.034 Uiso 0.587(10) 1 calc R U P A 1
C20 C 0.5558(5) 0.26412(15) 0.5089(7) 0.0355(9) Uani 0.587(10) 1 d . . P A 1
H20 H 0.516639 0.254451 0.566155 0.043 Uiso 0.587(10) 1 calc R U P A 1
C18 C 0.6369(4) 0.24448(11) 0.3432(6) 0.0373(8) Uani 0.587(10) 1 d . . P A 1
H18 H 0.652109 0.221900 0.287153 0.045 Uiso 0.587(10) 1 calc R U P A 1
C17A C 0.7159(10) 0.29313(14) 0.3839(9) 0.0390(17) Uani 0.413(10) 1 d . . P A 2
H17A H 0.781953 0.303274 0.359304 0.047 Uiso 0.413(10) 1 calc R U P A 2
C18A C 0.6986(12) 0.24575(15) 0.4010(9) 0.050(2) Uani 0.413(10) 1 d . . P A 2
H18A H 0.753768 0.223281 0.388764 0.060 Uiso 0.413(10) 1 calc R U P A 2
C21A C 0.5449(7) 0.3099(2) 0.4417(9) 0.0326(11) Uani 0.413(10) 1 d . . P A 2
H21A H 0.491951 0.331691 0.460248 0.039 Uiso 0.413(10) 1 calc R U P A 2
C20A C 0.5270(9) 0.2622(3) 0.4551(9) 0.0441(15) Uani 0.413(10) 1 d . . P A 2
H20A H 0.459485 0.253030 0.478617 0.053 Uiso 0.413(10) 1 calc R U P A 2
C97 C 0.9885(5) 0.24553(16) 0.6296(6) 0.0657(14) Uani 0.5 1 d . U P B -1
H97 H 0.898405 0.244999 0.610979 0.079 Uiso 0.5 1 calc R U P B -1
C94 C 1.2390(5) 0.24441(19) 0.6750(8) 0.0754(17) Uani 0.5 1 d . U P B -1
H94 H 1.328144 0.244661 0.690287 0.091 Uiso 0.5 1 calc R U P B -1
C95 C 1.2111(5) 0.22146(17) 0.7710(9) 0.086(2) Uani 0.5 1 d . U P B -1
H95 H 1.278335 0.204777 0.847637 0.103 Uiso 0.5 1 calc R U P B -1
C98 C 1.0192(5) 0.26759(16) 0.5364(7) 0.0666(15) Uani 0.5 1 d . U P B -1
H98 H 0.952715 0.283289 0.456668 0.080 Uiso 0.5 1 calc R U P B -1
C96 C 1.0845(6) 0.2231(2) 0.7539(10) 0.098(2) Uani 0.5 1 d . U P B -1
H96 H 1.061846 0.210015 0.821550 0.118 Uiso 0.5 1 calc R U P B -1
C93 C 1.1455(6) 0.2668(2) 0.5590(7) 0.0744(16) Uani 0.5 1 d . U P B -1
C99 C 1.1805(10) 0.2921(3) 0.4468(12) 0.143(4) Uani 0.5 1 d . U P B -1
H99A H 1.276240 0.290190 0.479224 0.215 Uiso 0.5 1 calc R U P B -1
H99B H 1.153635 0.324962 0.437623 0.215 Uiso 0.5 1 calc R U P B -1
H99C H 1.133176 0.276578 0.354924 0.215 Uiso 0.5 1 calc R U P B -1
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
12 15 -13 0.0915
-8 -11 14 0.1101
-14 -17 7 0.0712
12 18 1 0.0779
10 3 7 0.1047
-8 -34 6 0.0646
3 39 -4 0.0558
6 38 -2 0.0632
-1 -38 5 0.0564
0 40 0 0.0604
13 -13 1 0.0743
-11 -12 -4 0.0798
-15 13 7 0.0852
15 6 -1 0.0676
-16 -9 7 0.0726
10 26 -10 0.0763
6 33 -8 0.0675
-6 -33 8 0.0626
0 -37 5 0.0561
7 -37 -4 0.0864
-7 37 4 0.0779
9 -31 -8 0.0998
-3 33 9 0.1045
12 -11 -13 0.1131
-16 2 8 0.0798
1 -1 -2 0.0029
-1 -2 0 0.0404
1 2 0 0.0680
2 40 -2 0.0469
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
C31 Fe1 C30 92.78(6) . . ?
C31 Fe1 N3 94.79(5) . . ?
C30 Fe1 N3 100.39(5) . . ?
C31 Fe1 C3 96.73(5) . . ?
C30 Fe1 C3 116.94(5) . . ?
N3 Fe1 C3 140.15(4) . . ?
C31 Fe1 C4 96.27(5) . . ?
C30 Fe1 C4 156.84(5) . . ?
N3 Fe1 C4 100.05(4) . . ?
C3 Fe1 C4 40.83(4) . . ?
C31 Fe1 C2 130.99(5) . . ?
C30 Fe1 C2 91.06(4) . . ?
N3 Fe1 C2 132.34(4) . . ?
C3 Fe1 C2 40.25(4) . . ?
C4 Fe1 C2 66.99(4) . . ?
C31 Fe1 C1 161.65(5) . . ?
C30 Fe1 C1 101.91(5) . . ?
N3 Fe1 C1 93.33(4) . . ?
C3 Fe1 C1 66.88(4) . . ?
C4 Fe1 C1 66.07(4) . . ?
C2 Fe1 C1 39.04(4) . . ?
C31 Fe1 C5 128.66(5) . . ?
C30 Fe1 C5 138.55(5) . . ?
N3 Fe1 C5 79.30(4) . . ?
C3 Fe1 C5 63.81(4) . . ?
C4 Fe1 C5 37.35(4) . . ?
C2 Fe1 C5 62.79(4) . . ?
C1 Fe1 C5 37.60(4) . . ?
C2 N2 C15 115.88(9) . . ?
C2 N2 C11 119.88(10) . . ?
C15 N2 C11 114.12(9) . . ?
C1 N1 C10 117.25(9) . . ?
C1 N1 C6 116.77(9) . . ?
C10 N1 C6 110.66(9) . . ?
C28 N3 Fe1 172.64(10) . . ?
C3 C4 C5 109.09(9) . . ?
C3 C4 C22 127.68(10) . . ?
C5 C4 C22 121.38(9) . . ?
C3 C4 Fe1 68.31(6) . . ?
C5 C4 Fe1 82.96(6) . . ?
C22 C4 Fe1 127.69(8) . . ?
N2 C2 C3 127.85(9) . . ?
N2 C2 C1 123.34(10) . . ?
C3 C2 C1 108.80(9) . . ?
N2 C2 Fe1 126.77(7) . . ?
C3 C2 Fe1 67.22(6) . . ?
C1 C2 Fe1 73.20(6) . . ?
C27 C22 C23 118.53(12) . . ?
C27 C22 C4 119.85(11) . . ?
C23 C22 C4 121.49(11) . . ?
N3 C28 C29 177.26(12) . . ?
N1 C6 C7 110.58(10) . . ?
O2 C30 Fe1 175.53(11) . . ?
N1 C1 C2 125.38(9) . . ?
N1 C1 C5 125.92(9) . . ?
C2 C1 C5 107.37(9) . . ?
N1 C1 Fe1 129.20(7) . . ?
C2 C1 Fe1 67.76(6) . . ?
C5 C1 Fe1 78.59(6) . . ?
O1 C5 C4 126.25(10) . . ?
O1 C5 C1 129.15(10) . . ?
C4 C5 C1 104.28(8) . . ?
O1 C5 Fe1 135.41(8) . . ?
C4 C5 Fe1 59.69(5) . . ?
C1 C5 Fe1 63.81(5) . . ?
N1 C10 C9 110.36(11) . . ?
N2 C11 C12 109.45(11) . . ?
C2 C3 C4 107.43(9) . . ?
C2 C3 C16 125.00(10) . . ?
C4 C3 C16 125.65(10) . . ?
C2 C3 Fe1 72.52(6) . . ?
C4 C3 Fe1 70.86(6) . . ?
C16 C3 Fe1 134.37(8) . . ?
C21A C16 C17A 118.2(4) . . ?
C17 C16 C21 117.8(2) . . ?
C21A C16 C3 120.6(3) . . ?
C17 C16 C3 124.80(16) . . ?
C17A C16 C3 121.1(2) . . ?
C21 C16 C3 117.1(2) . . ?
O3 C31 Fe1 179.33(13) . . ?
C24 C23 C22 120.39(14) . . ?
C10 C9 C8 111.78(11) . . ?
C6 C7 C8 111.27(11) . . ?
N2 C15 C14 110.52(11) . . ?
C26 C27 C22 120.79(14) . . ?
C7 C8 C9 109.44(12) . . ?
C13 C12 C11 110.35(13) . . ?
C25 C26 C27 120.18(15) . . ?
C24 C25 C26 119.64(13) . . ?
C15 C14 C13 111.22(13) . . ?
C25 C24 C23 120.45(14) . . ?
C12 C13 C14 110.71(12) . . ?
C18 C19 C20 120.3(3) . . ?
C20A C19 C18A 116.8(4) . . ?
C20 C21 C16 120.4(4) . . ?
C16 C17 C18 121.4(3) . . ?
C21 C20 C19 118.7(4) . . ?
C19 C18 C17 120.7(3) . . ?
C18A C17A C16 118.4(4) . . ?
C17A C18A C19 120.4(4) . . ?
C16 C21A C20A 122.4(6) . . ?
C19 C20A C21A 123.6(7) . . ?
C98 C97 C96 123.2(5) . . ?
C93 C94 C95 123.4(5) . . ?
C96 C95 C94 118.6(6) . . ?
C93 C98 C97 118.8(6) . . ?
C95 C96 C97 116.5(8) . . ?
C98 C93 C94 119.3(7) . . ?
C98 C93 C99 118.5(7) . . ?
C94 C93 C99 122.2(6) . . ?
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 C31 1.7825(13) . ?
Fe1 C30 1.7843(11) . ?
Fe1 N3 1.9542(10) . ?
Fe1 C3 2.0557(11) . ?
Fe1 C4 2.0900(10) . ?
Fe1 C2 2.1266(11) . ?
Fe1 C1 2.1995(11) . ?
Fe1 C5 2.4027(11) . ?
O1 C5 1.2383(13) . ?
O2 C30 1.1552(14) . ?
N2 C2 1.4010(14) . ?
N2 C15 1.4643(15) . ?
N2 C11 1.4661(15) . ?
N1 C1 1.3955(14) . ?
N1 C10 1.4672(15) . ?
N1 C6 1.4697(14) . ?
N3 C28 1.1450(14) . ?
O3 C31 1.1454(17) . ?
C4 C3 1.4464(15) . ?
C4 C5 1.4688(16) . ?
C4 C22 1.4780(16) . ?
C2 C3 1.4406(16) . ?
C2 C1 1.4470(14) . ?
C22 C27 1.3953(18) . ?
C22 C23 1.3996(17) . ?
C28 C29 1.4518(15) . ?
C6 C7 1.5197(18) . ?
C1 C5 1.4955(15) . ?
C10 C9 1.520(2) . ?
C11 C12 1.5206(19) . ?
C3 C16 1.4880(15) . ?
C16 C21A 1.318(6) . ?
C16 C17 1.382(3) . ?
C16 C17A 1.419(5) . ?
C16 C21 1.442(4) . ?
C23 C24 1.394(2) . ?
C9 C8 1.526(2) . ?
C7 C8 1.526(2) . ?
C15 C14 1.522(2) . ?
C27 C26 1.3903(19) . ?
C12 C13 1.517(2) . ?
C26 C25 1.389(3) . ?
C25 C24 1.383(3) . ?
C14 C13 1.530(2) . ?
C19 C20A 1.271(10) . ?
C19 C18 1.354(5) . ?
C19 C20 1.429(6) . ?
C19 C18A 1.461(9) . ?
C21 C20 1.392(6) . ?
C17 C18 1.398(4) . ?
C17A C18A 1.394(6) . ?
C21A C20A 1.398(9) . ?
C97 C98 1.355(9) . ?
C97 C96 1.422(9) . ?
C94 C93 1.363(9) . ?
C94 C95 1.374(10) . ?
C95 C96 1.368(8) . ?
C98 C93 1.344(8) . ?
C93 C99 1.601(12) . ?
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
C15 N2 C2 C3 -117.05(13) . . . . ?
C11 N2 C2 C3 26.32(16) . . . . ?
C15 N2 C2 C1 61.32(14) . . . . ?
C11 N2 C2 C1 -155.31(10) . . . . ?
C15 N2 C2 Fe1 154.74(9) . . . . ?
C11 N2 C2 Fe1 -61.89(13) . . . . ?
C3 C4 C22 C27 -136.07(13) . . . . ?
C5 C4 C22 C27 61.15(15) . . . . ?
Fe1 C4 C22 C27 -45.70(15) . . . . ?
C3 C4 C22 C23 48.09(17) . . . . ?
C5 C4 C22 C23 -114.69(13) . . . . ?
Fe1 C4 C22 C23 138.47(10) . . . . ?
C1 N1 C6 C7 -161.67(11) . . . . ?
C10 N1 C6 C7 60.75(13) . . . . ?
C10 N1 C1 C2 -174.39(10) . . . . ?
C6 N1 C1 C2 50.84(14) . . . . ?
C10 N1 C1 C5 -9.25(15) . . . . ?
C6 N1 C1 C5 -144.02(10) . . . . ?
C10 N1 C1 Fe1 96.75(11) . . . . ?
C6 N1 C1 Fe1 -38.02(13) . . . . ?
N2 C2 C1 N1 0.19(16) . . . . ?
C3 C2 C1 N1 178.83(9) . . . . ?
Fe1 C2 C1 N1 -123.17(10) . . . . ?
N2 C2 C1 C5 -167.24(9) . . . . ?
C3 C2 C1 C5 11.40(11) . . . . ?
Fe1 C2 C1 C5 69.40(7) . . . . ?
N2 C2 C1 Fe1 123.36(10) . . . . ?
C3 C2 C1 Fe1 -58.00(7) . . . . ?
C3 C4 C5 O1 -169.43(11) . . . . ?
C22 C4 C5 O1 -3.79(17) . . . . ?
Fe1 C4 C5 O1 126.46(11) . . . . ?
C3 C4 C5 C1 16.66(11) . . . . ?
C22 C4 C5 C1 -177.70(10) . . . . ?
Fe1 C4 C5 C1 -47.44(7) . . . . ?
C3 C4 C5 Fe1 64.10(7) . . . . ?
C22 C4 C5 Fe1 -130.26(11) . . . . ?
N1 C1 C5 O1 2.00(18) . . . . ?
C2 C1 C5 O1 169.35(11) . . . . ?
Fe1 C1 C5 O1 -128.54(12) . . . . ?
N1 C1 C5 C4 175.67(10) . . . . ?
C2 C1 C5 C4 -16.99(11) . . . . ?
Fe1 C1 C5 C4 45.12(7) . . . . ?
N1 C1 C5 Fe1 130.54(11) . . . . ?
C2 C1 C5 Fe1 -62.12(7) . . . . ?
C1 N1 C10 C9 162.41(10) . . . . ?
C6 N1 C10 C9 -60.23(13) . . . . ?
C2 N2 C11 C12 157.01(11) . . . . ?
C15 N2 C11 C12 -59.02(14) . . . . ?
N2 C2 C3 C4 177.60(10) . . . . ?
C1 C2 C3 C4 -0.96(12) . . . . ?
Fe1 C2 C3 C4 -62.67(7) . . . . ?
N2 C2 C3 C16 12.68(17) . . . . ?
C1 C2 C3 C16 -165.88(10) . . . . ?
Fe1 C2 C3 C16 132.41(11) . . . . ?
N2 C2 C3 Fe1 -119.73(11) . . . . ?
C1 C2 C3 Fe1 61.71(7) . . . . ?
C5 C4 C3 C2 -10.15(12) . . . . ?
C22 C4 C3 C2 -174.64(11) . . . . ?
Fe1 C4 C3 C2 63.75(7) . . . . ?
C5 C4 C3 C16 154.64(11) . . . . ?
C22 C4 C3 C16 -9.84(18) . . . . ?
Fe1 C4 C3 C16 -131.45(11) . . . . ?
C5 C4 C3 Fe1 -73.91(7) . . . . ?
C22 C4 C3 Fe1 121.61(12) . . . . ?
C2 C3 C16 C21A 70.0(5) . . . . ?
C4 C3 C16 C21A -92.2(5) . . . . ?
Fe1 C3 C16 C21A 169.9(4) . . . . ?
C2 C3 C16 C17 -139.2(2) . . . . ?
C4 C3 C16 C17 58.6(3) . . . . ?
Fe1 C3 C16 C17 -39.3(3) . . . . ?
C2 C3 C16 C17A -106.6(5) . . . . ?
C4 C3 C16 C17A 91.1(5) . . . . ?
Fe1 C3 C16 C17A -6.7(5) . . . . ?
C2 C3 C16 C21 47.5(2) . . . . ?
C4 C3 C16 C21 -114.7(2) . . . . ?
Fe1 C3 C16 C21 147.4(2) . . . . ?
C27 C22 C23 C24 1.5(2) . . . . ?
C4 C22 C23 C24 177.40(12) . . . . ?
N1 C10 C9 C8 56.82(16) . . . . ?
N1 C6 C7 C8 -57.36(16) . . . . ?
C2 N2 C15 C14 -157.79(11) . . . . ?
C11 N2 C15 C14 56.74(14) . . . . ?
C23 C22 C27 C26 -1.5(2) . . . . ?
C4 C22 C27 C26 -177.47(12) . . . . ?
C6 C7 C8 C9 52.87(18) . . . . ?
C10 C9 C8 C7 -52.79(17) . . . . ?
N2 C11 C12 C13 57.40(15) . . . . ?
C22 C27 C26 C25 0.7(2) . . . . ?
C27 C26 C25 C24 0.1(2) . . . . ?
N2 C15 C14 C13 -52.66(16) . . . . ?
C26 C25 C24 C23 -0.1(2) . . . . ?
C22 C23 C24 C25 -0.7(2) . . . . ?
C11 C12 C13 C14 -55.79(19) . . . . ?
C15 C14 C13 C12 53.44(19) . . . . ?
C17 C16 C21 C20 5.4(4) . . . . ?
C3 C16 C21 C20 179.2(3) . . . . ?
C21 C16 C17 C18 -5.3(4) . . . . ?
C3 C16 C17 C18 -178.5(2) . . . . ?
C16 C21 C20 C19 1.0(5) . . . . ?
C18 C19 C20 C21 -8.0(5) . . . . ?
C20 C19 C18 C17 8.4(5) . . . . ?
C16 C17 C18 C19 -1.6(5) . . . . ?
C21A C16 C17A C18A 1.7(7) . . . . ?
C3 C16 C17A C18A 178.4(4) . . . . ?
C16 C17A C18A C19 0.5(8) . . . . ?
C20A C19 C18A C17A -1.2(8) . . . . ?
C17A C16 C21A C20A -3.3(7) . . . . ?
C3 C16 C21A C20A 180.0(4) . . . . ?
C18A C19 C20A C21A -0.3(8) . . . . ?
C16 C21A C20A C19 2.6(9) . . . . ?
C93 C94 C95 C96 -3.5(9) . . . . ?
C96 C97 C98 C93 2.7(8) . . . . ?
C94 C95 C96 C97 5.2(10) . . . . ?
C98 C97 C96 C95 -5.1(10) . . . . ?
C97 C98 C93 C94 -0.6(7) . . . . ?
C97 C98 C93 C99 178.8(6) . . . . ?
C95 C94 C93 C98 1.1(8) . . . . ?
C95 C94 C93 C99 -178.3(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
11.6855 14.9183 -12.8040 0.7091 -0.6734 0.2092
-8.1253 -11.1490 14.4452 -0.7193 0.6825 0.1298
-14.4718 -17.2691 7.2397 -0.5265 0.5008 -0.6871
12.4142 17.6663 0.7167 0.2495 -0.1203 0.9609
9.5188 2.8668 6.5567 -0.2615 0.0333 0.9646
-8.1057 -33.6644 6.4947 -0.8935 0.1182 -0.4331
2.6136 38.6806 -4.2528 0.9570 0.1770 0.2297
5.9047 37.5127 -2.2750 0.8320 0.1535 0.5331
-1.2987 -38.0403 4.8803 -0.9775 -0.1809 -0.1088
-0.4164 40.3306 0.2373 0.8453 0.4585 0.2743
12.7946 -13.3882 1.1608 -0.4255 -0.4497 0.7853
-10.8307 -12.0187 -4.2953 -0.0071 -0.0057 -1.0000
-15.2260 12.6714 7.2479 0.1109 0.8466 -0.5206
14.6911 6.3161 -1.4346 0.0738 -0.3923 0.9169
-15.6440 -9.1174 6.8005 -0.3287 0.6037 -0.7263
9.9248 25.8174 -10.4234 0.8626 -0.4112 0.2948
5.6296 33.3265 -8.3461 0.9757 -0.1283 0.1778
-5.6082 -33.3138 8.3586 -0.9760 0.1284 -0.1756
-0.2110 -37.0942 5.3376 -0.9832 -0.1821 -0.0089
6.7513 -36.5506 -3.5707 -0.6884 -0.7253 -0.0089
-6.7513 36.5506 3.5707 0.6884 0.7253 0.0089
9.3886 -30.8217 -7.7266 -0.4306 -0.9025 -0.0090
-3.3828 32.6228 8.8027 0.3813 0.8005 0.4624
11.7102 -11.1988 -13.4475 0.1821 -0.9832 -0.0090
-15.9980 1.6596 7.9850 -0.1434 0.7779 -0.6118
1.5000 -1.0004 -1.9999 0.0430 -0.1324 -0.0121
-0.5000 -2.0002 0.0000 -0.0383 -0.0080 -0.0465
0.5000 2.0002 -0.0000 0.0383 0.0080 0.0465
2.3318 39.6983 -2.4046 0.9107 0.2700 0.3125
