#------------------------------------------------------------------------------
#$Date: 2024-09-06 01:48:15 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294398 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572066.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_1572066
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         'C38 H46 Fe N2 O4, C H Cl3'
_chemical_formula_sum            'C39 H47 Cl3 Fe N2 O4'
_chemical_formula_weight         769.98
_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                99.388(2)
_cell_angle_beta                 97.450(2)
_cell_angle_gamma                109.190(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3708(3)
_cell_length_b                   12.4378(2)
_cell_length_c                   13.3652(3)
_cell_measurement_reflns_used    56141
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.3580
_cell_measurement_theta_min      3.4110
_cell_volume                     1878.73(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (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 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            81045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.751
_diffrn_reflns_theta_min         3.419
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.516
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (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    1.361
_exptl_crystal_description       'fragment of block'
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0322
_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)+(0.0443P)²+1.0640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7775
_reflns_number_total             7933
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cy00372a3.cif
_cod_data_source_block           lk34db
_cod_depositor_comments
'Adding full bibliography for 1572060--1572070.cif.'
_cod_original_cell_volume        1878.73(7)
_cod_database_code               1572066
_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   0.298
_shelx_estimated_absorpt_t_max   0.637
_oxdiff_exptl_absorpt_empirical_full_min 0.820
_oxdiff_exptl_absorpt_empirical_full_max 1.354
_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 0.66098(2) 0.26069(2) 0.50313(2) 0.01410(7) Uani 1 1 d . . . . .
Cl1 Cl 0.28519(5) 0.03690(4) 0.15482(4) 0.04908(14) Uani 1 1 d . . . . .
Cl2 Cl 0.49419(6) 0.13079(6) 0.07130(5) 0.05682(16) Uani 1 1 d . . . . .
Cl3 Cl 0.31132(4) 0.22652(5) 0.05008(4) 0.04170(12) Uani 1 1 d . . . . .
O1 O 0.47477(9) 0.33395(9) 0.34104(8) 0.0184(2) Uani 1 1 d . . . . .
O2 O 0.54807(11) 0.07750(10) 0.31319(9) 0.0278(3) Uani 1 1 d . . . . .
O3 O 0.66727(10) 0.12284(10) 0.66164(9) 0.0259(2) Uani 1 1 d . . . . .
O4 O 0.89592(10) 0.27852(10) 0.46996(9) 0.0254(2) Uani 1 1 d . . . . .
N1 N 0.39128(10) 0.22331(11) 0.52100(10) 0.0168(2) Uani 1 1 d . . . . .
N2 N 0.58139(11) 0.36428(11) 0.70806(9) 0.0173(2) Uani 1 1 d . . . . .
C1 C 0.53559(12) 0.34972(12) 0.42706(11) 0.0158(3) Uani 1 1 d . . . . .
C2 C 0.50081(12) 0.30044(12) 0.51778(11) 0.0151(3) Uani 1 1 d . . . . .
C3 C 0.59299(12) 0.36661(12) 0.60663(11) 0.0153(3) Uani 1 1 d . . . . .
C4 C 0.69410(12) 0.43300(12) 0.57042(11) 0.0147(3) Uani 1 1 d . . . . .
C5 C 0.66193(12) 0.41540(12) 0.45915(11) 0.0150(3) Uani 1 1 d . . . . .
C6 C 0.30861(13) 0.16492(13) 0.42207(12) 0.0214(3) Uani 1 1 d . . . . .
H6A H 0.332770 0.103908 0.384588 0.026 Uiso 1 1 calc R U . . .
H6B H 0.309999 0.222521 0.378667 0.026 Uiso 1 1 calc R U . . .
C7 C 0.18484(13) 0.10947(14) 0.43999(14) 0.0250(3) Uani 1 1 d . . . . .
H7A H 0.157857 0.171638 0.470776 0.030 Uiso 1 1 calc R U . . .
H7B H 0.131861 0.067459 0.372701 0.030 Uiso 1 1 calc R U . . .
C8 C 0.17846(14) 0.02467(14) 0.51130(15) 0.0267(3) Uani 1 1 d . . . . .
H8A H 0.099599 -0.002232 0.528038 0.032 Uiso 1 1 calc R U . . .
H8B H 0.192892 -0.044351 0.476187 0.032 Uiso 1 1 calc R U . . .
C9 C 0.26951(14) 0.08496(15) 0.61038(14) 0.0271(3) Uani 1 1 d . . . . .
H9A H 0.270797 0.027566 0.653434 0.033 Uiso 1 1 calc R U . . .
H9B H 0.248230 0.146765 0.650253 0.033 Uiso 1 1 calc R U . . .
C10 C 0.39033(13) 0.13874(13) 0.58636(12) 0.0202(3) Uani 1 1 d . . . . .
H10A H 0.447702 0.178398 0.651795 0.024 Uiso 1 1 calc R U . . .
H10B H 0.413691 0.076290 0.550351 0.024 Uiso 1 1 calc R U . . .
C11 C 0.48705(13) 0.40079(14) 0.74217(12) 0.0205(3) Uani 1 1 d . . . . .
H11A H 0.418707 0.373143 0.684528 0.025 Uiso 1 1 calc R U . . .
H11B H 0.514388 0.487041 0.761249 0.025 Uiso 1 1 calc R U . . .
C12 C 0.45109(14) 0.35095(16) 0.83482(13) 0.0261(3) Uani 1 1 d . . . . .
H12A H 0.412101 0.265178 0.812684 0.031 Uiso 1 1 calc R U . . .
H12B H 0.394534 0.383412 0.861215 0.031 Uiso 1 1 calc R U . . .
C13 C 0.55668(15) 0.38007(17) 0.92129(13) 0.0282(4) Uani 1 1 d . . . . .
H13A H 0.591137 0.465507 0.948794 0.034 Uiso 1 1 calc R U . . .
H13B H 0.531963 0.342439 0.978484 0.034 Uiso 1 1 calc R U . . .
C14 C 0.64746(14) 0.33663(15) 0.87920(13) 0.0248(3) Uani 1 1 d . . . . .
H14A H 0.716463 0.356414 0.934847 0.030 Uiso 1 1 calc R U . . .
H14B H 0.614130 0.250724 0.854733 0.030 Uiso 1 1 calc R U . . .
C15 C 0.68419(13) 0.39327(14) 0.78994(11) 0.0196(3) Uani 1 1 d . . . . .
H15A H 0.720363 0.478997 0.814942 0.024 Uiso 1 1 calc R U . . .
H15B H 0.742548 0.364656 0.762250 0.024 Uiso 1 1 calc R U . . .
C16 C 0.79672(12) 0.52734(12) 0.64011(11) 0.0153(3) Uani 1 1 d . . . . .
C17 C 0.77631(13) 0.62119(13) 0.69599(12) 0.0189(3) Uani 1 1 d . . . . .
H17 H 0.699044 0.621556 0.689385 0.023 Uiso 1 1 calc R U . . .
C18 C 0.86770(14) 0.71438(13) 0.76133(12) 0.0202(3) Uani 1 1 d . . . . .
H18 H 0.851786 0.777837 0.797966 0.024 Uiso 1 1 calc R U . . .
C19 C 0.98176(13) 0.71659(13) 0.77413(11) 0.0188(3) Uani 1 1 d . . . . .
C20 C 1.00137(13) 0.62248(14) 0.71759(12) 0.0204(3) Uani 1 1 d . . . . .
H20 H 1.078603 0.621997 0.724435 0.024 Uiso 1 1 calc R U . . .
C21 C 0.91089(13) 0.52939(13) 0.65153(11) 0.0182(3) Uani 1 1 d . . . . .
H21 H 0.927071 0.466679 0.613867 0.022 Uiso 1 1 calc R U . . .
C22 C 1.08397(14) 0.81806(14) 0.84620(12) 0.0245(3) Uani 1 1 d . . . . .
C23 C 1.15178(16) 0.76999(17) 0.92190(14) 0.0324(4) Uani 1 1 d . . . . .
H23A H 1.099058 0.727259 0.962508 0.049 Uiso 1 1 calc R U . . .
H23B H 1.216269 0.834948 0.968497 0.049 Uiso 1 1 calc R U . . .
H23C H 1.182983 0.717287 0.882657 0.049 Uiso 1 1 calc R U . . .
C24 C 1.04225(17) 0.90425(16) 0.91046(16) 0.0361(4) Uani 1 1 d . . . . .
H24A H 1.002035 0.938857 0.864340 0.054 Uiso 1 1 calc R U . . .
H24B H 1.109523 0.965984 0.957138 0.054 Uiso 1 1 calc R U . . .
H24C H 0.988408 0.863237 0.951133 0.054 Uiso 1 1 calc R U . . .
C25 C 1.1656(2) 0.8816(2) 0.78143(17) 0.0492(6) Uani 1 1 d . . . . .
H25A H 1.197112 0.827932 0.744064 0.074 Uiso 1 1 calc R U . . .
H25B H 1.229890 0.947887 0.826805 0.074 Uiso 1 1 calc R U . . .
H25C H 1.122320 0.909994 0.731744 0.074 Uiso 1 1 calc R U . . .
C26 C 0.72920(12) 0.47853(12) 0.38895(11) 0.0155(3) Uani 1 1 d . . . . .
C27 C 0.81181(14) 0.59154(13) 0.42314(12) 0.0203(3) Uani 1 1 d . . . . .
H27 H 0.829174 0.628252 0.494409 0.024 Uiso 1 1 calc R U . . .
C28 C 0.86898(14) 0.65109(14) 0.35467(12) 0.0225(3) Uani 1 1 d . . . . .
H28 H 0.925596 0.727276 0.380727 0.027 Uiso 1 1 calc R U . . .
C29 C 0.84604(13) 0.60280(13) 0.24911(12) 0.0193(3) Uani 1 1 d . . . . .
C30 C 0.76283(13) 0.49021(13) 0.21507(12) 0.0198(3) Uani 1 1 d . . . . .
H30 H 0.744341 0.454379 0.143523 0.024 Uiso 1 1 calc R U . . .
C31 C 0.70632(13) 0.42917(13) 0.28317(12) 0.0187(3) Uani 1 1 d . . . . .
H31 H 0.651002 0.352312 0.257247 0.022 Uiso 1 1 calc R U . . .
C32 C 0.91332(14) 0.67191(15) 0.17708(12) 0.0237(3) Uani 1 1 d . . . . .
C33 C 0.86688(17) 0.61048(17) 0.06355(14) 0.0331(4) Uani 1 1 d . . . . .
H33A H 0.878345 0.535467 0.051624 0.050 Uiso 1 1 calc R U . . .
H33B H 0.908988 0.659329 0.020244 0.050 Uiso 1 1 calc R U . . .
H33C H 0.783437 0.597149 0.045792 0.050 Uiso 1 1 calc R U . . .
C34 C 0.90233(18) 0.79355(16) 0.19079(15) 0.0335(4) Uani 1 1 d . . . . .
H34A H 0.819781 0.784308 0.174462 0.050 Uiso 1 1 calc R U . . .
H34B H 0.944608 0.836721 0.144108 0.050 Uiso 1 1 calc R U . . .
H34C H 0.935624 0.836704 0.262483 0.050 Uiso 1 1 calc R U . . .
C35 C 1.04203(16) 0.6878(2) 0.20550(17) 0.0386(5) Uani 1 1 d . . . . .
H35A H 1.072368 0.727835 0.278314 0.058 Uiso 1 1 calc R U . . .
H35B H 1.086134 0.734431 0.161821 0.058 Uiso 1 1 calc R U . . .
H35C H 1.050207 0.611188 0.194611 0.058 Uiso 1 1 calc R U . . .
C36 C 0.58926(13) 0.14708(13) 0.38769(12) 0.0192(3) Uani 1 1 d . . . . .
C37 C 0.66323(13) 0.17445(13) 0.59893(12) 0.0192(3) Uani 1 1 d . . . . .
C38 C 0.80578(14) 0.27447(13) 0.48428(11) 0.0192(3) Uani 1 1 d . . . . .
C39 C 0.38537(17) 0.16257(16) 0.12949(14) 0.0319(4) Uani 1 1 d . . . . .
H39 H 0.423924 0.219949 0.196720 0.038 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 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -3 0 0.0836
0 -1 -8 0.0590
0 1 8 0.0305
8 -5 1 0.0715
0 8 -2 0.0615
0 -8 2 0.0344
-8 1 1 0.1802
0 4 -8 0.0466
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
C38 Fe1 C37 93.59(7) . . ?
C38 Fe1 C36 94.34(7) . . ?
C37 Fe1 C36 100.71(7) . . ?
C38 Fe1 C4 98.40(6) . . ?
C37 Fe1 C4 111.63(6) . . ?
C36 Fe1 C4 144.21(6) . . ?
C38 Fe1 C5 96.12(6) . . ?
C37 Fe1 C5 151.82(6) . . ?
C36 Fe1 C5 104.84(6) . . ?
C4 Fe1 C5 40.73(5) . . ?
C38 Fe1 C3 133.15(6) . . ?
C37 Fe1 C3 88.15(6) . . ?
C36 Fe1 C3 131.31(6) . . ?
C4 Fe1 C3 39.58(5) . . ?
C5 Fe1 C3 66.05(5) . . ?
C38 Fe1 C2 161.82(6) . . ?
C37 Fe1 C2 101.23(6) . . ?
C36 Fe1 C2 93.19(6) . . ?
C4 Fe1 C2 66.43(5) . . ?
C5 Fe1 C2 65.93(5) . . ?
C3 Fe1 C2 38.39(5) . . ?
C38 Fe1 C1 127.72(6) . . ?
C37 Fe1 C1 138.49(6) . . ?
C36 Fe1 C1 82.06(6) . . ?
C4 Fe1 C1 63.72(5) . . ?
C5 Fe1 C1 37.46(5) . . ?
C3 Fe1 C1 61.93(5) . . ?
C2 Fe1 C1 37.53(5) . . ?
C2 N1 C10 115.74(12) . . ?
C2 N1 C6 117.69(12) . . ?
C10 N1 C6 110.11(12) . . ?
C3 N2 C15 120.83(12) . . ?
C3 N2 C11 115.94(12) . . ?
C15 N2 C11 114.18(12) . . ?
O1 C1 C5 126.55(13) . . ?
O1 C1 C2 128.48(13) . . ?
C5 C1 C2 104.83(12) . . ?
O1 C1 Fe1 136.06(10) . . ?
C5 C1 Fe1 60.14(7) . . ?
C2 C1 Fe1 64.69(7) . . ?
N1 C2 C3 125.68(13) . . ?
N1 C2 C1 126.08(13) . . ?
C3 C2 C1 107.00(12) . . ?
N1 C2 Fe1 127.73(10) . . ?
C3 C2 Fe1 69.70(8) . . ?
C1 C2 Fe1 77.78(8) . . ?
N2 C3 C4 127.62(13) . . ?
N2 C3 C2 123.80(13) . . ?
C4 C3 C2 108.58(12) . . ?
N2 C3 Fe1 128.80(10) . . ?
C4 C3 Fe1 65.61(8) . . ?
C2 C3 Fe1 71.90(8) . . ?
C3 C4 C5 107.74(12) . . ?
C3 C4 C16 123.12(12) . . ?
C5 C4 C16 126.79(12) . . ?
C3 C4 Fe1 74.81(8) . . ?
C5 C4 Fe1 70.85(8) . . ?
C16 C4 Fe1 133.74(10) . . ?
C4 C5 C1 108.65(12) . . ?
C4 C5 C26 127.98(13) . . ?
C1 C5 C26 121.05(12) . . ?
C4 C5 Fe1 68.42(8) . . ?
C1 C5 Fe1 82.39(8) . . ?
C26 C5 Fe1 129.42(10) . . ?
N1 C6 C7 110.88(13) . . ?
C8 C7 C6 111.91(13) . . ?
C9 C8 C7 109.59(13) . . ?
C8 C9 C10 110.94(14) . . ?
N1 C10 C9 110.98(13) . . ?
N2 C11 C12 110.70(13) . . ?
C11 C12 C13 111.26(13) . . ?
C14 C13 C12 109.56(14) . . ?
C15 C14 C13 109.75(14) . . ?
N2 C15 C14 109.43(12) . . ?
C21 C16 C17 118.20(13) . . ?
C21 C16 C4 124.76(13) . . ?
C17 C16 C4 117.03(13) . . ?
C18 C17 C16 120.82(14) . . ?
C19 C18 C17 121.40(14) . . ?
C18 C19 C20 117.35(14) . . ?
C18 C19 C22 122.38(14) . . ?
C20 C19 C22 120.27(14) . . ?
C21 C20 C19 121.73(14) . . ?
C20 C21 C16 120.50(14) . . ?
C25 C22 C24 109.29(17) . . ?
C25 C22 C19 109.04(14) . . ?
C24 C22 C19 111.91(14) . . ?
C25 C22 C23 109.19(17) . . ?
C24 C22 C23 107.78(14) . . ?
C19 C22 C23 109.59(14) . . ?
C27 C26 C31 117.01(13) . . ?
C27 C26 C5 122.31(13) . . ?
C31 C26 C5 120.56(13) . . ?
C28 C27 C26 121.12(14) . . ?
C27 C28 C29 122.18(14) . . ?
C28 C29 C30 116.55(14) . . ?
C28 C29 C32 119.99(14) . . ?
C30 C29 C32 123.44(14) . . ?
C31 C30 C29 121.73(14) . . ?
C30 C31 C26 121.39(14) . . ?
C33 C32 C35 109.24(15) . . ?
C33 C32 C29 112.10(14) . . ?
C35 C32 C29 108.90(13) . . ?
C33 C32 C34 107.78(14) . . ?
C35 C32 C34 108.84(15) . . ?
C29 C32 C34 109.92(14) . . ?
O2 C36 Fe1 177.11(14) . . ?
O3 C37 Fe1 177.85(14) . . ?
O4 C38 Fe1 177.13(14) . . ?
Cl2 C39 Cl3 110.17(10) . . ?
Cl2 C39 Cl1 111.66(11) . . ?
Cl3 C39 Cl1 109.96(10) . . ?
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 C38 1.7975(16) . ?
Fe1 C37 1.8025(16) . ?
Fe1 C36 1.8094(16) . ?
Fe1 C4 2.0659(14) . ?
Fe1 C5 2.0986(14) . ?
Fe1 C3 2.1890(14) . ?
Fe1 C2 2.2185(14) . ?
Fe1 C1 2.3985(14) . ?
Cl1 C39 1.761(2) . ?
Cl2 C39 1.759(2) . ?
Cl3 C39 1.7608(19) . ?
O1 C1 1.2376(18) . ?
O2 C36 1.139(2) . ?
O3 C37 1.141(2) . ?
O4 C38 1.142(2) . ?
N1 C2 1.3900(18) . ?
N1 C10 1.4711(18) . ?
N1 C6 1.4728(19) . ?
N2 C3 1.3855(19) . ?
N2 C15 1.4676(19) . ?
N2 C11 1.4815(19) . ?
C1 C5 1.4719(19) . ?
C1 C2 1.4951(19) . ?
C2 C3 1.449(2) . ?
C3 C4 1.4453(19) . ?
C4 C5 1.450(2) . ?
C4 C16 1.4878(19) . ?
C5 C26 1.4842(19) . ?
C6 C7 1.527(2) . ?
C7 C8 1.523(2) . ?
C8 C9 1.523(3) . ?
C9 C10 1.524(2) . ?
C11 C12 1.526(2) . ?
C12 C13 1.528(2) . ?
C13 C14 1.527(2) . ?
C14 C15 1.526(2) . ?
C16 C21 1.392(2) . ?
C16 C17 1.394(2) . ?
C17 C18 1.392(2) . ?
C18 C19 1.390(2) . ?
C19 C20 1.395(2) . ?
C19 C22 1.536(2) . ?
C20 C21 1.390(2) . ?
C22 C25 1.523(2) . ?
C22 C24 1.527(3) . ?
C22 C23 1.547(3) . ?
C26 C27 1.398(2) . ?
C26 C31 1.398(2) . ?
C27 C28 1.390(2) . ?
C28 C29 1.393(2) . ?
C29 C30 1.397(2) . ?
C29 C32 1.538(2) . ?
C30 C31 1.391(2) . ?
C32 C33 1.524(2) . ?
C32 C35 1.527(2) . ?
C32 C34 1.547(2) . ?
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
C10 N1 C2 C3 -47.5(2) . . . . ?
C6 N1 C2 C3 179.39(13) . . . . ?
C10 N1 C2 C1 146.89(14) . . . . ?
C6 N1 C2 C1 13.7(2) . . . . ?
C10 N1 C2 Fe1 43.44(18) . . . . ?
C6 N1 C2 Fe1 -89.72(15) . . . . ?
O1 C1 C2 N1 1.8(2) . . . . ?
C5 C1 C2 N1 -174.06(13) . . . . ?
Fe1 C1 C2 N1 -128.09(15) . . . . ?
O1 C1 C2 C3 -166.02(14) . . . . ?
C5 C1 C2 C3 18.09(15) . . . . ?
Fe1 C1 C2 C3 64.06(9) . . . . ?
O1 C1 C2 Fe1 129.91(15) . . . . ?
C5 C1 C2 Fe1 -45.97(9) . . . . ?
C15 N2 C3 C4 -24.6(2) . . . . ?
C11 N2 C3 C4 120.60(15) . . . . ?
C15 N2 C3 C2 155.98(14) . . . . ?
C11 N2 C3 C2 -58.86(19) . . . . ?
C15 N2 C3 Fe1 62.62(18) . . . . ?
C11 N2 C3 Fe1 -152.23(11) . . . . ?
N1 C2 C3 N2 -2.6(2) . . . . ?
C1 C2 C3 N2 165.36(13) . . . . ?
Fe1 C2 C3 N2 -125.07(14) . . . . ?
N1 C2 C3 C4 177.90(13) . . . . ?
C1 C2 C3 C4 -14.19(15) . . . . ?
Fe1 C2 C3 C4 55.38(9) . . . . ?
N1 C2 C3 Fe1 122.52(14) . . . . ?
C1 C2 C3 Fe1 -69.57(9) . . . . ?
N2 C3 C4 C5 -175.07(13) . . . . ?
C2 C3 C4 C5 4.46(15) . . . . ?
Fe1 C3 C4 C5 63.65(9) . . . . ?
N2 C3 C4 C16 -11.4(2) . . . . ?
C2 C3 C4 C16 168.10(12) . . . . ?
Fe1 C3 C4 C16 -132.71(14) . . . . ?
N2 C3 C4 Fe1 121.28(14) . . . . ?
C2 C3 C4 Fe1 -59.19(10) . . . . ?
C3 C4 C5 C1 7.24(15) . . . . ?
C16 C4 C5 C1 -155.62(13) . . . . ?
Fe1 C4 C5 C1 73.52(10) . . . . ?
C3 C4 C5 C26 169.84(13) . . . . ?
C16 C4 C5 C26 7.0(2) . . . . ?
Fe1 C4 C5 C26 -123.88(15) . . . . ?
C3 C4 C5 Fe1 -66.27(9) . . . . ?
C16 C4 C5 Fe1 130.86(14) . . . . ?
O1 C1 C5 C4 168.45(14) . . . . ?
C2 C1 C5 C4 -15.56(15) . . . . ?
Fe1 C1 C5 C4 -64.11(9) . . . . ?
O1 C1 C5 C26 4.4(2) . . . . ?
C2 C1 C5 C26 -179.59(12) . . . . ?
Fe1 C1 C5 C26 131.86(14) . . . . ?
O1 C1 C5 Fe1 -127.45(14) . . . . ?
C2 C1 C5 Fe1 48.55(10) . . . . ?
C2 N1 C6 C7 -165.20(13) . . . . ?
C10 N1 C6 C7 59.21(16) . . . . ?
N1 C6 C7 C8 -56.02(18) . . . . ?
C6 C7 C8 C9 52.57(19) . . . . ?
C7 C8 C9 C10 -53.34(19) . . . . ?
C2 N1 C10 C9 162.82(13) . . . . ?
C6 N1 C10 C9 -60.65(17) . . . . ?
C8 C9 C10 N1 58.23(18) . . . . ?
C3 N2 C11 C12 157.63(13) . . . . ?
C15 N2 C11 C12 -54.90(17) . . . . ?
N2 C11 C12 C13 52.76(18) . . . . ?
C11 C12 C13 C14 -55.63(19) . . . . ?
C12 C13 C14 C15 58.56(18) . . . . ?
C3 N2 C15 C14 -156.29(13) . . . . ?
C11 N2 C15 C14 57.99(17) . . . . ?
C13 C14 C15 N2 -58.98(17) . . . . ?
C3 C4 C16 C21 122.24(16) . . . . ?
C5 C4 C16 C21 -77.3(2) . . . . ?
Fe1 C4 C16 C21 21.2(2) . . . . ?
C3 C4 C16 C17 -59.16(19) . . . . ?
C5 C4 C16 C17 101.27(17) . . . . ?
Fe1 C4 C16 C17 -160.18(12) . . . . ?
C21 C16 C17 C18 0.0(2) . . . . ?
C4 C16 C17 C18 -178.65(13) . . . . ?
C16 C17 C18 C19 -0.8(2) . . . . ?
C17 C18 C19 C20 1.0(2) . . . . ?
C17 C18 C19 C22 -179.66(14) . . . . ?
C18 C19 C20 C21 -0.5(2) . . . . ?
C22 C19 C20 C21 -179.86(14) . . . . ?
C19 C20 C21 C16 -0.2(2) . . . . ?
C17 C16 C21 C20 0.4(2) . . . . ?
C4 C16 C21 C20 179.03(14) . . . . ?
C18 C19 C22 C25 -113.39(19) . . . . ?
C20 C19 C22 C25 66.0(2) . . . . ?
C18 C19 C22 C24 7.6(2) . . . . ?
C20 C19 C22 C24 -173.01(15) . . . . ?
C18 C19 C22 C23 127.15(16) . . . . ?
C20 C19 C22 C23 -53.51(19) . . . . ?
C4 C5 C26 C27 -24.8(2) . . . . ?
C1 C5 C26 C27 135.86(15) . . . . ?
Fe1 C5 C26 C27 -116.99(15) . . . . ?
C4 C5 C26 C31 159.44(14) . . . . ?
C1 C5 C26 C31 -39.9(2) . . . . ?
Fe1 C5 C26 C31 67.28(18) . . . . ?
C31 C26 C27 C28 -0.6(2) . . . . ?
C5 C26 C27 C28 -176.44(14) . . . . ?
C26 C27 C28 C29 1.1(3) . . . . ?
C27 C28 C29 C30 -0.6(2) . . . . ?
C27 C28 C29 C32 -179.05(15) . . . . ?
C28 C29 C30 C31 -0.4(2) . . . . ?
C32 C29 C30 C31 178.04(14) . . . . ?
C29 C30 C31 C26 0.9(2) . . . . ?
C27 C26 C31 C30 -0.4(2) . . . . ?
C5 C26 C31 C30 175.58(14) . . . . ?
C28 C29 C32 C33 -173.77(15) . . . . ?
C30 C29 C32 C33 7.9(2) . . . . ?
C28 C29 C32 C35 65.2(2) . . . . ?
C30 C29 C32 C35 -113.15(18) . . . . ?
C28 C29 C32 C34 -53.9(2) . . . . ?
C30 C29 C32 C34 127.71(17) . . . . ?
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
7.9492 -3.4409 -0.1325 -0.0188 -0.0255 0.9995
0.3031 -1.0326 -8.1345 -0.6068 -0.7914 -0.0733
-0.3191 1.0396 8.1354 0.6069 0.7916 0.0713
7.6494 -4.6425 0.5022 -0.1505 0.0927 0.9843
-0.4589 7.7598 -2.1038 0.8413 -0.5152 -0.1635
0.1058 -7.6562 2.1113 -0.8467 0.5184 0.1197
-7.7697 0.8476 0.5620 -0.2774 0.1693 -0.9457
-0.2967 3.7988 -8.2066 -0.0252 -0.9805 -0.1950
