# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk29db
_database_code_depnum_ccdc_archive 'CCDC 2338289'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H30 N2 O'
_chemical_formula_sum            'C27 H30 N2 O'
_chemical_formula_weight         398.53

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   19.5712(6)
_cell_length_b                   5.91540(10)
_cell_length_c                   20.8266(6)
_cell_angle_alpha                90
_cell_angle_beta                 115.442(4)
_cell_angle_gamma                90
_cell_volume                     2177.30(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16544
_cell_measurement_theta_min      2.4970
_cell_measurement_theta_max      76.4760

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.569
_shelx_estimated_absorpt_T_min   0.749
_shelx_estimated_absorpt_T_max   0.983
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0781
0 1 0 0.4534
-6 0 13 0.0228
6 0 -14 0.0229
-11 0 0 0.0171
11 0 0 0.0114
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
-0.0024 -1.0004 0.0004 0.0238 0.0101 0.2593
0.0024 1.0004 -0.0004 -0.0238 -0.0101 -0.2593
-5.7903 0.2689 13.4772 -0.9724 0.2330 0.0093
5.8601 0.0495 -13.5076 0.9683 -0.2321 -0.0923
-11.2675 0.1944 -0.4615 -0.2330 -0.9724 0.0091
11.2675 -0.1944 0.4615 0.2330 0.9724 -0.0091
_exptl_absorpt_correction_T_min  0.65030
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.682
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            34754
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.500
_diffrn_reflns_theta_max         77.378
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4537
_reflns_number_gt                3919
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+0.8745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00069(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4537
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O1 O 0.30640(5) 0.24896(14) 0.61183(4) 0.02044(19) Uani 1 1 d . . . . .
N1 N 0.18984(5) 0.62022(17) 0.57525(5) 0.0174(2) Uani 1 1 d . . . . .
N2 N 0.19989(5) 0.75569(17) 0.72271(5) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.29348(6) 0.35229(19) 0.65635(6) 0.0162(2) Uani 1 1 d . . . . .
C2 C 0.24097(6) 0.54115(19) 0.64398(6) 0.0168(2) Uani 1 1 d . . . . .
C3 C 0.23959(6) 0.59231(19) 0.70746(6) 0.0159(2) Uani 1 1 d . . . . .
C4 C 0.29621(6) 0.44353(19) 0.76548(6) 0.0165(2) Uani 1 1 d . . . . .
C5 C 0.32868(6) 0.30157(19) 0.73617(6) 0.0162(2) Uani 1 1 d . . . . .
C6 C 0.22771(7) 0.7105(2) 0.53302(6) 0.0216(2) Uani 1 1 d . . . . .
H6A H 0.256370 0.588114 0.523163 0.026 Uiso 1 1 calc R U . . .
H6B H 0.264045 0.829659 0.560496 0.026 Uiso 1 1 calc R U . . .
C7 C 0.17011(7) 0.8088(2) 0.46314(6) 0.0264(3) Uani 1 1 d . . . . .
H7A H 0.144919 0.940605 0.472994 0.032 Uiso 1 1 calc R U . . .
H7B H 0.196391 0.861622 0.434552 0.032 Uiso 1 1 calc R U . . .
C8 C 0.11088(7) 0.6333(2) 0.42104(6) 0.0284(3) Uani 1 1 d . . . . .
H8A H 0.135004 0.508577 0.406582 0.034 Uiso 1 1 calc R U . . .
H8B H 0.071928 0.703222 0.377522 0.034 Uiso 1 1 calc R U . . .
C9 C 0.07408(7) 0.5408(3) 0.46693(6) 0.0292(3) Uani 1 1 d . . . . .
H9A H 0.045616 0.662913 0.477176 0.035 Uiso 1 1 calc R U . . .
H9B H 0.037863 0.419706 0.440773 0.035 Uiso 1 1 calc R U . . .
C10 C 0.13361(7) 0.4469(2) 0.53634(6) 0.0232(3) Uani 1 1 d . . . . .
H10A H 0.108876 0.392586 0.566119 0.028 Uiso 1 1 calc R U . . .
H10B H 0.159222 0.316648 0.526203 0.028 Uiso 1 1 calc R U . . .
C11 C 0.16694(6) 0.9489(2) 0.67526(6) 0.0204(2) Uani 1 1 d . . . . .
H11A H 0.190937 0.961869 0.642155 0.025 Uiso 1 1 calc R U . . .
H11B H 0.178162 1.089079 0.703934 0.025 Uiso 1 1 calc R U . . .
C12 C 0.08161(7) 0.9272(2) 0.63240(7) 0.0241(3) Uani 1 1 d . . . . .
H12A H 0.070354 0.801279 0.598048 0.029 Uiso 1 1 calc R U . . .
H12B H 0.061295 1.068153 0.605214 0.029 Uiso 1 1 calc R U . . .
C13 C 0.04323(7) 0.8832(2) 0.68146(7) 0.0281(3) Uani 1 1 d . . . . .
H13A H 0.048411 1.017989 0.711368 0.034 Uiso 1 1 calc R U . . .
H13B H -0.011373 0.854473 0.652636 0.034 Uiso 1 1 calc R U . . .
C14 C 0.07930(7) 0.6796(2) 0.72877(7) 0.0271(3) Uani 1 1 d . . . . .
H14A H 0.069985 0.542281 0.698995 0.033 Uiso 1 1 calc R U . . .
H14B H 0.055847 0.656854 0.761978 0.033 Uiso 1 1 calc R U . . .
C15 C 0.16452(7) 0.7146(2) 0.77109(6) 0.0234(3) Uani 1 1 d . . . . .
H15A H 0.173899 0.845125 0.803533 0.028 Uiso 1 1 calc R U . . .
H15B H 0.187271 0.578804 0.800270 0.028 Uiso 1 1 calc R U . . .
C16 C 0.31805(6) 0.4737(2) 0.84252(6) 0.0173(2) Uani 1 1 d . . . . .
C17 C 0.30930(7) 0.2992(2) 0.88358(6) 0.0215(2) Uani 1 1 d . . . . .
H17 H 0.287287 0.159907 0.861771 0.026 Uiso 1 1 calc R U . . .
C18 C 0.33268(7) 0.3285(2) 0.95624(6) 0.0257(3) Uani 1 1 d . . . . .
H18 H 0.325786 0.210148 0.983740 0.031 Uiso 1 1 calc R U . . .
C19 C 0.36599(8) 0.5298(2) 0.98864(6) 0.0271(3) Uani 1 1 d . . . . .
H19 H 0.382662 0.548764 1.038398 0.033 Uiso 1 1 calc R U . . .
C20 C 0.37488(8) 0.7030(2) 0.94823(6) 0.0268(3) Uani 1 1 d . . . . .
H20 H 0.397820 0.840937 0.970412 0.032 Uiso 1 1 calc R U . . .
C21 C 0.35047(7) 0.6764(2) 0.87540(6) 0.0211(2) Uani 1 1 d . . . . .
H21 H 0.355934 0.797280 0.847927 0.025 Uiso 1 1 calc R U . . .
C22 C 0.39087(6) 0.13939(19) 0.77034(6) 0.0164(2) Uani 1 1 d . . . . .
C23 C 0.45009(6) 0.1807(2) 0.83774(6) 0.0196(2) Uani 1 1 d . . . . .
H23 H 0.450931 0.317305 0.862065 0.023 Uiso 1 1 calc R U . . .
C24 C 0.50730(7) 0.0228(2) 0.86883(6) 0.0229(3) Uani 1 1 d . . . . .
H24 H 0.547036 0.052197 0.914437 0.027 Uiso 1 1 calc R U . . .
C25 C 0.50726(7) -0.1778(2) 0.83419(6) 0.0218(2) Uani 1 1 d . . . . .
H25 H 0.546385 -0.285815 0.856145 0.026 Uiso 1 1 calc R U . . .
C26 C 0.44960(7) -0.2193(2) 0.76721(6) 0.0200(2) Uani 1 1 d . . . . .
H26 H 0.449365 -0.355787 0.743068 0.024 Uiso 1 1 calc R U . . .
C27 C 0.39224(6) -0.06163(19) 0.73540(6) 0.0179(2) Uani 1 1 d . . . . .
H27 H 0.353382 -0.090608 0.689290 0.021 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O1 C1 1.2241(14) . ?
N1 C2 1.4278(14) . ?
N1 C10 1.4674(15) . ?
N1 C6 1.4725(14) . ?
N2 C3 1.3604(14) . ?
N2 C11 1.4665(15) . ?
N2 C15 1.4673(14) . ?
C1 C2 1.4639(16) . ?
C1 C5 1.5311(14) . ?
C2 C3 1.3677(15) . ?
C3 C4 1.5205(15) . ?
C4 C5 1.3471(16) . ?
C4 C16 1.4832(15) . ?
C5 C22 1.4711(15) . ?
C6 C7 1.5222(16) . ?
C7 C8 1.5221(18) . ?
C8 C9 1.5241(18) . ?
C9 C10 1.5193(16) . ?
C11 C12 1.5237(16) . ?
C12 C13 1.5282(17) . ?
C13 C14 1.5236(19) . ?
C14 C15 1.5292(17) . ?
C16 C21 1.3915(17) . ?
C16 C17 1.3973(16) . ?
C17 C18 1.3909(17) . ?
C18 C19 1.3858(19) . ?
C19 C20 1.3836(19) . ?
C20 C21 1.3896(16) . ?
C22 C27 1.4003(16) . ?
C22 C23 1.4057(15) . ?
C23 C24 1.3867(17) . ?
C24 C25 1.3887(18) . ?
C25 C26 1.3882(17) . ?
C26 C27 1.3893(16) . ?

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
C2 N1 C10 111.17(9) . . ?
C2 N1 C6 113.69(9) . . ?
C10 N1 C6 111.97(9) . . ?
C3 N2 C11 121.75(9) . . ?
C3 N2 C15 121.86(10) . . ?
C11 N2 C15 113.03(9) . . ?
O1 C1 C2 127.27(10) . . ?
O1 C1 C5 125.56(10) . . ?
C2 C1 C5 107.15(9) . . ?
C3 C2 N1 126.88(10) . . ?
C3 C2 C1 107.62(9) . . ?
N1 C2 C1 124.27(10) . . ?
N2 C3 C2 129.29(10) . . ?
N2 C3 C4 121.33(9) . . ?
C2 C3 C4 109.26(10) . . ?
C5 C4 C16 126.33(10) . . ?
C5 C4 C3 108.98(9) . . ?
C16 C4 C3 124.26(10) . . ?
C4 C5 C22 129.84(10) . . ?
C4 C5 C1 106.86(9) . . ?
C22 C5 C1 123.08(9) . . ?
N1 C6 C7 110.70(10) . . ?
C8 C7 C6 111.00(11) . . ?
C7 C8 C9 109.38(10) . . ?
C10 C9 C8 110.61(10) . . ?
N1 C10 C9 110.89(10) . . ?
N2 C11 C12 112.54(10) . . ?
C11 C12 C13 110.63(10) . . ?
C14 C13 C12 110.05(10) . . ?
C13 C14 C15 110.69(11) . . ?
N2 C15 C14 110.25(10) . . ?
C21 C16 C17 119.04(10) . . ?
C21 C16 C4 119.66(10) . . ?
C17 C16 C4 121.26(10) . . ?
C18 C17 C16 120.28(11) . . ?
C19 C18 C17 120.19(11) . . ?
C20 C19 C18 119.74(11) . . ?
C19 C20 C21 120.40(12) . . ?
C20 C21 C16 120.33(11) . . ?
C27 C22 C23 118.36(10) . . ?
C27 C22 C5 119.94(10) . . ?
C23 C22 C5 121.71(10) . . ?
C24 C23 C22 120.21(11) . . ?
C23 C24 C25 120.87(11) . . ?
C26 C25 C24 119.46(11) . . ?
C25 C26 C27 120.13(11) . . ?
C26 C27 C22 120.95(10) . . ?

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 -101.61(13) . . . . ?
C6 N1 C2 C3 130.93(12) . . . . ?
C10 N1 C2 C1 64.13(14) . . . . ?
C6 N1 C2 C1 -63.32(14) . . . . ?
O1 C1 C2 C3 174.95(11) . . . . ?
C5 C1 C2 C3 -3.60(12) . . . . ?
O1 C1 C2 N1 6.87(18) . . . . ?
C5 C1 C2 N1 -171.68(10) . . . . ?
C11 N2 C3 C2 -17.82(18) . . . . ?
C15 N2 C3 C2 140.04(12) . . . . ?
C11 N2 C3 C4 157.75(10) . . . . ?
C15 N2 C3 C4 -44.39(15) . . . . ?
N1 C2 C3 N2 -12.91(19) . . . . ?
C1 C2 C3 N2 179.42(11) . . . . ?
N1 C2 C3 C4 171.11(10) . . . . ?
C1 C2 C3 C4 3.43(12) . . . . ?
N2 C3 C4 C5 -178.34(10) . . . . ?
C2 C3 C4 C5 -1.98(13) . . . . ?
N2 C3 C4 C16 -5.46(16) . . . . ?
C2 C3 C4 C16 170.91(10) . . . . ?
C16 C4 C5 C22 1.63(19) . . . . ?
C3 C4 C5 C22 174.33(11) . . . . ?
C16 C4 C5 C1 -173.04(10) . . . . ?
C3 C4 C5 C1 -0.34(12) . . . . ?
O1 C1 C5 C4 -176.21(11) . . . . ?
C2 C1 C5 C4 2.38(12) . . . . ?
O1 C1 C5 C22 8.67(17) . . . . ?
C2 C1 C5 C22 -172.74(10) . . . . ?
C2 N1 C6 C7 -175.39(10) . . . . ?
C10 N1 C6 C7 57.57(13) . . . . ?
N1 C6 C7 C8 -56.33(14) . . . . ?
C6 C7 C8 C9 55.40(15) . . . . ?
C7 C8 C9 C10 -55.62(15) . . . . ?
C2 N1 C10 C9 173.48(10) . . . . ?
C6 N1 C10 C9 -58.14(13) . . . . ?
C8 C9 C10 N1 57.13(15) . . . . ?
C3 N2 C11 C12 104.31(12) . . . . ?
C15 N2 C11 C12 -55.34(13) . . . . ?
N2 C11 C12 C13 53.14(14) . . . . ?
C11 C12 C13 C14 -53.73(14) . . . . ?
C12 C13 C14 C15 56.39(14) . . . . ?
C3 N2 C15 C14 -102.87(13) . . . . ?
C11 N2 C15 C14 56.75(13) . . . . ?
C13 C14 C15 N2 -57.38(14) . . . . ?
C5 C4 C16 C21 112.06(14) . . . . ?
C3 C4 C16 C21 -59.58(15) . . . . ?
C5 C4 C16 C17 -65.54(16) . . . . ?
C3 C4 C16 C17 122.81(12) . . . . ?
C21 C16 C17 C18 0.06(17) . . . . ?
C4 C16 C17 C18 177.68(11) . . . . ?
C16 C17 C18 C19 -1.09(18) . . . . ?
C17 C18 C19 C20 0.99(19) . . . . ?
C18 C19 C20 C21 0.1(2) . . . . ?
C19 C20 C21 C16 -1.18(19) . . . . ?
C17 C16 C21 C20 1.07(17) . . . . ?
C4 C16 C21 C20 -176.59(11) . . . . ?
C4 C5 C22 C27 147.81(12) . . . . ?
C1 C5 C22 C27 -38.28(15) . . . . ?
C4 C5 C22 C23 -32.56(18) . . . . ?
C1 C5 C22 C23 141.35(11) . . . . ?
C27 C22 C23 C24 -1.25(17) . . . . ?
C5 C22 C23 C24 179.11(11) . . . . ?
C22 C23 C24 C25 0.10(18) . . . . ?
C23 C24 C25 C26 0.73(18) . . . . ?
C24 C25 C26 C27 -0.36(17) . . . . ?
C25 C26 C27 C22 -0.83(17) . . . . ?
C23 C22 C27 C26 1.62(16) . . . . ?
C5 C22 C27 C26 -178.74(10) . . . . ?

_refine_diff_density_max         0.266
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.036


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk28db3
_database_code_depnum_ccdc_archive 'CCDC 2338291'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 Fe N2 O4'
_chemical_formula_sum            'C30 H30 Fe N2 O4'
_chemical_formula_weight         538.41

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.5244(5)
_cell_length_b                   27.7280(10)
_cell_length_c                   10.4699(5)
_cell_angle_alpha                90
_cell_angle_beta                 114.029(7)
_cell_angle_gamma                90
_cell_volume                     2525.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9625
_cell_measurement_theta_min      2.4440
_cell_measurement_theta_max      30.5600

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.637
_shelx_estimated_absorpt_T_min   0.817
_shelx_estimated_absorpt_T_max   0.883
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 7 2 0.1361
-11 19 10 0.1500
9 -25 -9 0.1369
-1 9 -13 0.1456
4 -17 10 0.1327
6 -34 -5 0.1205
-5 34 -3 0.1065
2 -26 9 0.1152
-3 -37 4 0.1082
-1 -38 -3 0.1099
-5 10 14 0.1508
-10 -27 3 0.1213
10 12 -12 0.1391
-7 -20 -6 0.1374
11 18 0 0.1191
-11 -2 13 0.1439
-13 -6 1 0.1328
-3 -12 -11 0.1500
12 -6 0 0.1442
-11 17 -1 0.1328
8 -27 2 0.1344
-6 35 3 0.1227
4 8 -14 0.1473
1 -37 4 0.1016
-2 -28 10 0.1188
-1 38 -2 0.0923
3 37 -4 0.0918
-6 -16 13 0.1387
-6 -35 1 0.1127
-7 -29 -3 0.1212
9 28 -2 0.1135
-12 -16 4 0.1256
12 -3 -11 0.1344
10 9 4 0.1368
0 19 12 0.1180
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
-12.7015 7.2222 2.0963 0.4246 0.8933 -0.1476
-10.5171 18.7730 10.0366 0.0825 0.6462 -0.7587
8.9074 -25.4573 -8.9607 0.1258 -0.6652 0.7360
-1.1957 8.7026 -12.5524 -0.1123 0.6129 0.7822
3.9851 -16.6698 9.7335 0.1516 -0.8207 -0.5509
6.4422 -33.6059 -5.2525 0.4003 -0.7328 0.5502
-4.5129 33.5194 -3.2317 -0.4780 0.8783 0.0091
2.1154 -26.2500 8.8143 0.4327 -0.7972 -0.4210
-3.2196 -37.2458 3.9592 0.9030 -0.4296 -0.0092
-0.7498 -37.9433 -2.8194 0.8118 -0.3850 0.4390
-4.7337 10.2924 14.2273 -0.0094 -0.0012 -1.0000
-9.7391 -26.7107 3.2240 0.9830 0.1832 -0.0092
10.2193 11.6701 -12.3453 -0.6890 -0.1267 0.7136
-6.7578 -19.8359 -6.4004 0.7166 0.3916 0.5772
10.9602 18.3958 -0.3932 -0.8709 -0.4743 -0.1285
-10.8235 -2.3092 12.7905 0.5247 0.2834 -0.8028
-12.5554 -5.9381 1.3070 0.6876 0.7260 -0.0092
-3.0895 -11.6058 -11.1091 0.3870 0.4114 0.8252
12.1674 -5.8832 -0.1234 -0.4296 -0.9030 0.0091
-10.5927 17.1375 -1.0596 0.1295 0.9915 -0.0091
7.9854 -26.7233 2.1262 0.1832 -0.9830 0.0091
-6.1038 34.8196 2.7975 -0.4382 0.8070 -0.3958
3.9592 8.4464 -14.3231 -0.3384 0.3177 0.8858
0.7700 -37.3908 3.5140 0.7260 -0.6876 0.0091
-1.5923 -28.4829 9.8092 0.6450 -0.6094 -0.4611
-1.2817 38.2084 -1.9713 -0.7210 0.6832 -0.1155
3.1317 37.4285 -3.6995 -0.9030 0.4296 -0.0091
-5.7645 -15.8724 13.4604 0.5725 -0.2704 -0.7740
-5.9372 -34.8714 1.3939 0.9796 -0.1283 0.1544
-6.9446 -28.5997 -2.8753 0.9009 0.1669 0.4006
9.1881 27.6451 -1.7160 -0.9786 -0.1822 -0.0956
-12.1755 -15.9057 3.9593 0.8717 0.4748 -0.1215
12.3062 -2.7852 -10.8237 -0.4894 -0.5192 0.7007
10.2012 9.0451 3.6207 -0.6492 -0.6843 -0.3320
0.2769 19.4194 11.5721 -0.4199 -0.1271 -0.8986
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.910
_oxdiff_exptl_absorpt_empirical_full_max 1.105
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      110(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            58781
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.253
_diffrn_reflns_theta_max         30.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8034
_reflns_number_gt                6088
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0376P)²+0.9907P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8034
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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 0.59750(3) 0.58416(2) 0.57183(2) 0.01177(6) Uani 1 1 d . . . . .
O1 O 0.84156(14) 0.65292(4) 0.46741(12) 0.0165(2) Uani 1 1 d . . . . .
O2 O 0.72238(17) 0.52634(5) 0.40641(15) 0.0286(3) Uani 1 1 d . . . . .
O3 O 0.60074(15) 0.51104(4) 0.77693(14) 0.0233(3) Uani 1 1 d . . . . .
O4 O 0.27061(16) 0.56889(5) 0.39229(15) 0.0272(3) Uani 1 1 d . . . . .
N1 N 0.96852(16) 0.59621(5) 0.74552(14) 0.0128(3) Uani 1 1 d . . . . .
N2 N 0.75676(16) 0.62684(5) 0.88481(14) 0.0137(3) Uani 1 1 d . . . . .
C1 C 0.77220(19) 0.64410(5) 0.54108(16) 0.0120(3) Uani 1 1 d . . . . .
C2 C 0.82678(18) 0.61835(5) 0.67938(16) 0.0115(3) Uani 1 1 d . . . . .
C3 C 0.72475(18) 0.63288(5) 0.74425(16) 0.0119(3) Uani 1 1 d . . . . .
C4 C 0.58878(18) 0.65400(5) 0.63827(16) 0.0118(3) Uani 1 1 d . . . . .
C5 C 0.60984(19) 0.65428(5) 0.50865(16) 0.0120(3) Uani 1 1 d . . . . .
C6 C 1.06064(19) 0.58708(6) 0.66391(18) 0.0157(3) Uani 1 1 d . . . . .
H6A H 1.052908 0.614996 0.602461 0.019 Uiso 1 1 calc R U . . .
H6B H 1.020633 0.558274 0.604167 0.019 Uiso 1 1 calc R U . . .
C7 C 1.2283(2) 0.57896(6) 0.76308(19) 0.0187(3) Uani 1 1 d . . . . .
H7A H 1.289294 0.572153 0.707909 0.022 Uiso 1 1 calc R U . . .
H7B H 1.269647 0.608662 0.818052 0.022 Uiso 1 1 calc R U . . .
C8 C 1.2447(2) 0.53708(7) 0.86239(19) 0.0210(4) Uani 1 1 d . . . . .
H8A H 1.352765 0.534691 0.931446 0.025 Uiso 1 1 calc R U . . .
H8B H 1.217317 0.506516 0.808977 0.025 Uiso 1 1 calc R U . . .
C9 C 1.1396(2) 0.54482(7) 0.93822(19) 0.0196(4) Uani 1 1 d . . . . .
H9A H 1.141996 0.515850 0.994324 0.023 Uiso 1 1 calc R U . . .
H9B H 1.177276 0.572547 1.002863 0.023 Uiso 1 1 calc R U . . .
C10 C 0.9755(2) 0.55439(6) 0.83452(18) 0.0153(3) Uani 1 1 d . . . . .
H10A H 0.934825 0.525552 0.775090 0.018 Uiso 1 1 calc R U . . .
H10B H 0.910110 0.560531 0.886007 0.018 Uiso 1 1 calc R U . . .
C11 C 0.8998(2) 0.64702(6) 0.98898(17) 0.0173(3) Uani 1 1 d . . . . .
H11A H 0.882735 0.680994 1.007970 0.021 Uiso 1 1 calc R U . . .
H11B H 0.980038 0.646485 0.951619 0.021 Uiso 1 1 calc R U . . .
C12 C 0.9549(2) 0.61813(7) 1.12501(19) 0.0235(4) Uani 1 1 d . . . . .
H12A H 0.990477 0.585988 1.109632 0.028 Uiso 1 1 calc R U . . .
H12B H 1.043087 0.634926 1.197557 0.028 Uiso 1 1 calc R U . . .
C13 C 0.8275(2) 0.61190(7) 1.17668(18) 0.0244(4) Uani 1 1 d . . . . .
H13A H 0.862306 0.589430 1.257126 0.029 Uiso 1 1 calc R U . . .
H13B H 0.805003 0.643395 1.208796 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6825(2) 0.59233(6) 1.06120(19) 0.0211(4) Uani 1 1 d . . . . .
H14A H 0.599534 0.590502 1.094970 0.025 Uiso 1 1 calc R U . . .
H14B H 0.702030 0.559317 1.036236 0.025 Uiso 1 1 calc R U . . .
C15 C 0.6315(2) 0.62442(6) 0.93237(18) 0.0178(3) Uani 1 1 d . . . . .
H15A H 0.537887 0.610975 0.857417 0.021 Uiso 1 1 calc R U . . .
H15B H 0.607382 0.657153 0.955455 0.021 Uiso 1 1 calc R U . . .
C16 C 0.47578(19) 0.68464(6) 0.66577(16) 0.0125(3) Uani 1 1 d . . . . .
C17 C 0.31799(19) 0.67770(6) 0.60264(18) 0.0168(3) Uani 1 1 d . . . . .
H17 H 0.277074 0.651348 0.540512 0.020 Uiso 1 1 calc R U . . .
C18 C 0.2189(2) 0.70909(6) 0.62963(19) 0.0202(4) Uani 1 1 d . . . . .
H18 H 0.111087 0.703652 0.587313 0.024 Uiso 1 1 calc R U . . .
C19 C 0.2770(2) 0.74812(6) 0.71779(19) 0.0198(4) Uani 1 1 d . . . . .
H19 H 0.209391 0.769495 0.736031 0.024 Uiso 1 1 calc R U . . .
C20 C 0.4338(2) 0.75585(6) 0.77915(19) 0.0196(4) Uani 1 1 d . . . . .
H20 H 0.473791 0.782867 0.838792 0.023 Uiso 1 1 calc R U . . .
C21 C 0.5329(2) 0.72453(6) 0.75436(18) 0.0172(3) Uani 1 1 d . . . . .
H21 H 0.640550 0.730072 0.797698 0.021 Uiso 1 1 calc R U . . .
C22 C 0.51349(18) 0.67921(6) 0.37617(17) 0.0133(3) Uani 1 1 d . . . . .
C23 C 0.4607(2) 0.65493(6) 0.24851(18) 0.0205(4) Uani 1 1 d . . . . .
H23 H 0.475993 0.621115 0.247041 0.025 Uiso 1 1 calc R U . . .
C24 C 0.3861(2) 0.67963(7) 0.12345(19) 0.0238(4) Uani 1 1 d . . . . .
H24 H 0.349260 0.662573 0.037300 0.029 Uiso 1 1 calc R U . . .
C25 C 0.3653(2) 0.72907(7) 0.12409(19) 0.0212(4) Uani 1 1 d . . . . .
H25 H 0.316457 0.746150 0.038622 0.025 Uiso 1 1 calc R U . . .
C26 C 0.4163(2) 0.75329(6) 0.25037(19) 0.0213(4) Uani 1 1 d . . . . .
H26 H 0.401444 0.787151 0.251301 0.026 Uiso 1 1 calc R U . . .
C27 C 0.4888(2) 0.72872(6) 0.37578(18) 0.0173(3) Uani 1 1 d . . . . .
H27 H 0.521880 0.745771 0.461779 0.021 Uiso 1 1 calc R U . . .
C28 C 0.6736(2) 0.54863(6) 0.47017(18) 0.0173(3) Uani 1 1 d . . . . .
C29 C 0.60060(19) 0.53918(6) 0.69684(18) 0.0162(3) Uani 1 1 d . . . . .
C30 C 0.3970(2) 0.57566(6) 0.46330(19) 0.0180(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C30 1.7964(19) . ?
Fe1 C29 1.7994(17) . ?
Fe1 C28 1.8045(18) . ?
Fe1 C4 2.0707(15) . ?
Fe1 C5 2.0724(15) . ?
Fe1 C3 2.1843(16) . ?
Fe1 C2 2.2210(16) . ?
Fe1 C1 2.4639(16) . ?
O1 C1 1.2273(19) . ?
O2 C28 1.139(2) . ?
O3 C29 1.145(2) . ?
O4 C30 1.144(2) . ?
N1 C2 1.385(2) . ?
N1 C10 1.472(2) . ?
N1 C6 1.475(2) . ?
N2 C3 1.386(2) . ?
N2 C11 1.466(2) . ?
N2 C15 1.469(2) . ?
C1 C5 1.469(2) . ?
C1 C2 1.504(2) . ?
C2 C3 1.451(2) . ?
C3 C4 1.442(2) . ?
C4 C5 1.451(2) . ?
C4 C16 1.489(2) . ?
C5 C22 1.486(2) . ?
C6 C7 1.526(2) . ?
C7 C8 1.524(2) . ?
C8 C9 1.525(3) . ?
C9 C10 1.520(2) . ?
C11 C12 1.529(2) . ?
C12 C13 1.526(3) . ?
C13 C14 1.518(3) . ?
C14 C15 1.521(2) . ?
C16 C17 1.387(2) . ?
C16 C21 1.403(2) . ?
C17 C18 1.395(2) . ?
C18 C19 1.383(3) . ?
C19 C20 1.381(3) . ?
C20 C21 1.383(2) . ?
C22 C27 1.392(2) . ?
C22 C23 1.395(2) . ?
C23 C24 1.389(2) . ?
C24 C25 1.385(3) . ?
C25 C26 1.383(3) . ?
C26 C27 1.388(2) . ?

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
C30 Fe1 C29 93.87(8) . . ?
C30 Fe1 C28 97.71(8) . . ?
C29 Fe1 C28 99.15(8) . . ?
C30 Fe1 C4 99.06(7) . . ?
C29 Fe1 C4 113.26(7) . . ?
C28 Fe1 C4 142.13(7) . . ?
C30 Fe1 C5 96.03(7) . . ?
C29 Fe1 C5 153.66(7) . . ?
C28 Fe1 C5 103.61(7) . . ?
C4 Fe1 C5 40.99(6) . . ?
C30 Fe1 C3 133.88(7) . . ?
C29 Fe1 C3 89.33(7) . . ?
C28 Fe1 C3 127.17(7) . . ?
C4 Fe1 C3 39.52(6) . . ?
C5 Fe1 C3 66.36(6) . . ?
C30 Fe1 C2 161.68(7) . . ?
C29 Fe1 C2 101.86(7) . . ?
C28 Fe1 C2 89.09(7) . . ?
C4 Fe1 C2 66.18(6) . . ?
C5 Fe1 C2 65.76(6) . . ?
C3 Fe1 C2 38.45(6) . . ?
C30 Fe1 C1 127.34(7) . . ?
C29 Fe1 C1 138.64(7) . . ?
C28 Fe1 C1 80.59(7) . . ?
C4 Fe1 C1 62.27(6) . . ?
C5 Fe1 C1 36.52(6) . . ?
C3 Fe1 C1 60.91(6) . . ?
C2 Fe1 C1 37.00(5) . . ?
C2 N1 C10 116.69(13) . . ?
C2 N1 C6 118.38(13) . . ?
C10 N1 C6 110.34(13) . . ?
C3 N2 C11 118.67(13) . . ?
C3 N2 C15 120.49(14) . . ?
C11 N2 C15 113.72(13) . . ?
O1 C1 C5 126.99(15) . . ?
O1 C1 C2 129.49(15) . . ?
C5 C1 C2 103.43(13) . . ?
O1 C1 Fe1 141.39(12) . . ?
C5 C1 Fe1 57.08(8) . . ?
C2 C1 Fe1 62.69(8) . . ?
N1 C2 C3 126.25(14) . . ?
N1 C2 C1 125.18(14) . . ?
C3 C2 C1 106.49(13) . . ?
N1 C2 Fe1 128.41(11) . . ?
C3 C2 Fe1 69.40(9) . . ?
C1 C2 Fe1 80.30(9) . . ?
N2 C3 C4 127.31(14) . . ?
N2 C3 C2 124.31(14) . . ?
C4 C3 C2 108.37(13) . . ?
N2 C3 Fe1 127.65(11) . . ?
C4 C3 Fe1 65.99(8) . . ?
C2 C3 Fe1 72.14(9) . . ?
C3 C4 C5 107.40(14) . . ?
C3 C4 C16 125.19(14) . . ?
C5 C4 C16 124.35(14) . . ?
C3 C4 Fe1 74.49(9) . . ?
C5 C4 Fe1 69.57(9) . . ?
C16 C4 Fe1 136.88(12) . . ?
C4 C5 C1 108.43(14) . . ?
C4 C5 C22 127.43(14) . . ?
C1 C5 C22 119.81(14) . . ?
C4 C5 Fe1 69.45(9) . . ?
C1 C5 Fe1 86.40(9) . . ?
C22 C5 Fe1 129.85(11) . . ?
N1 C6 C7 109.62(14) . . ?
C8 C7 C6 111.41(14) . . ?
C7 C8 C9 109.95(14) . . ?
C10 C9 C8 110.80(14) . . ?
N1 C10 C9 110.94(14) . . ?
N2 C11 C12 110.82(14) . . ?
C13 C12 C11 111.67(16) . . ?
C14 C13 C12 110.77(15) . . ?
C13 C14 C15 110.84(15) . . ?
N2 C15 C14 108.48(14) . . ?
C17 C16 C21 118.52(15) . . ?
C17 C16 C4 123.86(15) . . ?
C21 C16 C4 117.50(15) . . ?
C16 C17 C18 120.54(16) . . ?
C19 C18 C17 120.22(17) . . ?
C20 C19 C18 119.67(16) . . ?
C19 C20 C21 120.43(16) . . ?
C20 C21 C16 120.59(17) . . ?
C27 C22 C23 118.59(16) . . ?
C27 C22 C5 120.05(15) . . ?
C23 C22 C5 120.97(15) . . ?
C24 C23 C22 120.78(17) . . ?
C25 C24 C23 120.15(17) . . ?
C26 C25 C24 119.35(17) . . ?
C25 C26 C27 120.77(17) . . ?
C26 C27 C22 120.34(16) . . ?
O2 C28 Fe1 179.60(18) . . ?
O3 C29 Fe1 178.78(16) . . ?
O4 C30 Fe1 177.66(16) . . ?

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 48.5(2) . . . . ?
C6 N1 C2 C3 -175.94(15) . . . . ?
C10 N1 C2 C1 -150.10(15) . . . . ?
C6 N1 C2 C1 -14.6(2) . . . . ?
C10 N1 C2 Fe1 -42.89(19) . . . . ?
C6 N1 C2 Fe1 92.64(16) . . . . ?
O1 C1 C2 N1 -5.0(3) . . . . ?
C5 C1 C2 N1 171.82(14) . . . . ?
Fe1 C1 C2 N1 130.59(16) . . . . ?
O1 C1 C2 C3 159.44(16) . . . . ?
C5 C1 C2 C3 -23.76(16) . . . . ?
Fe1 C1 C2 C3 -64.99(10) . . . . ?
O1 C1 C2 Fe1 -135.57(17) . . . . ?
C5 C1 C2 Fe1 41.23(10) . . . . ?
C11 N2 C3 C4 -124.77(17) . . . . ?
C15 N2 C3 C4 23.9(2) . . . . ?
C11 N2 C3 C2 55.3(2) . . . . ?
C15 N2 C3 C2 -156.10(15) . . . . ?
C11 N2 C3 Fe1 148.56(13) . . . . ?
C15 N2 C3 Fe1 -62.79(19) . . . . ?
N1 C2 C3 N2 0.7(2) . . . . ?
C1 C2 C3 N2 -163.54(14) . . . . ?
Fe1 C2 C3 N2 123.86(15) . . . . ?
N1 C2 C3 C4 -179.31(14) . . . . ?
C1 C2 C3 C4 16.48(17) . . . . ?
Fe1 C2 C3 C4 -56.12(10) . . . . ?
N1 C2 C3 Fe1 -123.19(16) . . . . ?
C1 C2 C3 Fe1 72.61(10) . . . . ?
N2 C3 C4 C5 177.73(15) . . . . ?
C2 C3 C4 C5 -2.29(17) . . . . ?
Fe1 C3 C4 C5 -62.19(10) . . . . ?
N2 C3 C4 C16 16.9(3) . . . . ?
C2 C3 C4 C16 -163.13(14) . . . . ?
Fe1 C3 C4 C16 136.98(16) . . . . ?
N2 C3 C4 Fe1 -120.09(16) . . . . ?
C2 C3 C4 Fe1 59.89(11) . . . . ?
C3 C4 C5 C1 -13.28(17) . . . . ?
C16 C4 C5 C1 147.75(15) . . . . ?
Fe1 C4 C5 C1 -78.71(11) . . . . ?
C3 C4 C5 C22 -169.48(15) . . . . ?
C16 C4 C5 C22 -8.5(3) . . . . ?
Fe1 C4 C5 C22 125.08(16) . . . . ?
C3 C4 C5 Fe1 65.43(11) . . . . ?
C16 C4 C5 Fe1 -133.54(16) . . . . ?
O1 C1 C5 C4 -160.40(15) . . . . ?
C2 C1 C5 C4 22.70(16) . . . . ?
Fe1 C1 C5 C4 66.93(10) . . . . ?
O1 C1 C5 C22 -2.1(2) . . . . ?
C2 C1 C5 C22 -178.97(13) . . . . ?
Fe1 C1 C5 C22 -134.74(15) . . . . ?
O1 C1 C5 Fe1 132.67(16) . . . . ?
C2 C1 C5 Fe1 -44.23(11) . . . . ?
C2 N1 C6 C7 160.89(14) . . . . ?
C10 N1 C6 C7 -60.99(17) . . . . ?
N1 C6 C7 C8 57.82(18) . . . . ?
C6 C7 C8 C9 -53.7(2) . . . . ?
C7 C8 C9 C10 52.8(2) . . . . ?
C2 N1 C10 C9 -159.90(14) . . . . ?
C6 N1 C10 C9 61.19(18) . . . . ?
C8 C9 C10 N1 -56.98(19) . . . . ?
C3 N2 C11 C12 -152.25(15) . . . . ?
C15 N2 C11 C12 57.08(19) . . . . ?
N2 C11 C12 C13 -51.3(2) . . . . ?
C11 C12 C13 C14 51.5(2) . . . . ?
C12 C13 C14 C15 -55.6(2) . . . . ?
C3 N2 C15 C14 149.48(15) . . . . ?
C11 N2 C15 C14 -60.43(18) . . . . ?
C13 C14 C15 N2 58.75(19) . . . . ?
C3 C4 C16 C17 -131.35(18) . . . . ?
C5 C4 C16 C17 71.0(2) . . . . ?
Fe1 C4 C16 C17 -25.4(3) . . . . ?
C3 C4 C16 C21 52.7(2) . . . . ?
C5 C4 C16 C21 -105.02(19) . . . . ?
Fe1 C4 C16 C21 158.59(14) . . . . ?
C21 C16 C17 C18 -1.6(2) . . . . ?
C4 C16 C17 C18 -177.49(16) . . . . ?
C16 C17 C18 C19 1.3(3) . . . . ?
C17 C18 C19 C20 -0.1(3) . . . . ?
C18 C19 C20 C21 -0.8(3) . . . . ?
C19 C20 C21 C16 0.5(3) . . . . ?
C17 C16 C21 C20 0.7(2) . . . . ?
C4 C16 C21 C20 176.90(15) . . . . ?
C4 C5 C22 C27 56.1(2) . . . . ?
C1 C5 C22 C27 -97.76(19) . . . . ?
Fe1 C5 C22 C27 149.67(14) . . . . ?
C4 C5 C22 C23 -131.17(18) . . . . ?
C1 C5 C22 C23 75.0(2) . . . . ?
Fe1 C5 C22 C23 -37.6(2) . . . . ?
C27 C22 C23 C24 0.4(3) . . . . ?
C5 C22 C23 C24 -172.43(17) . . . . ?
C22 C23 C24 C25 1.0(3) . . . . ?
C23 C24 C25 C26 -1.5(3) . . . . ?
C24 C25 C26 C27 0.5(3) . . . . ?
C25 C26 C27 C22 0.9(3) . . . . ?
C23 C22 C27 C26 -1.4(3) . . . . ?
C5 C22 C27 C26 171.53(16) . . . . ?

_refine_diff_density_max         0.494
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.077


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk43db
_database_code_depnum_ccdc_archive 'CCDC 2338297'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H41 Fe N3 O3, 0.705(C7 H8), 0.295(C6 H14)'
_chemical_formula_sum            'C41.71 H50.77 Fe N3 O3'
_chemical_formula_weight         697.93

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1925(5)
_cell_length_b                   28.2554(8)
_cell_length_c                   12.9763(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.551(6)
_cell_angle_gamma                90
_cell_volume                     3761.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    36595
_cell_measurement_theta_min      2.1060
_cell_measurement_theta_max      35.9520

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.442
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.978
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-15 6 5 0.0800
-8 34 8 0.0627
15 -6 -5 0.0889
13 -23 -7 0.0992
13 0 -16 0.0309
-12 -4 16 0.0190
11 7 -17 0.0358
-14 11 12 0.0460
-12 -2 16 0.0202
8 -11 -17 0.0519
-3 5 -15 0.1108
12 -17 -14 0.0593
7 -11 11 0.1087
-2 2 18 0.0912
-7 9 18 0.0655
-11 16 15 0.0369
5 34 5 0.1206
3 -37 -7 0.0834
-7 -31 -4 0.0608
-10 -31 6 0.0451
-15 -11 8 0.0443
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
-15.4373 5.8424 4.6887 -0.0092 -0.3955 0.9184
-7.6384 33.5485 7.5454 0.0151 0.5374 0.8432
15.4248 -6.1903 -4.7449 0.0090 0.3868 -0.9221
12.9314 -22.7282 -6.9673 -0.0037 -0.0951 -0.9955
12.8985 0.3909 -15.6385 -0.6816 0.1629 -0.7133
-11.8664 -4.4565 16.3922 0.7728 -0.1849 0.6071
11.1333 6.8515 -16.6863 -0.8201 0.1963 -0.5375
-14.3693 10.9764 11.8370 0.3533 -0.0838 0.9317
-12.4454 -2.3042 16.0323 0.7262 -0.1736 0.6652
7.7188 -10.9161 -17.4685 -0.7559 -0.3137 -0.5746
-3.4440 5.3831 -14.6095 -0.8970 -0.3712 0.2400
11.5828 -16.6520 -14.3546 -0.4810 -0.2001 -0.8536
7.0923 -10.6490 11.0036 0.7959 0.3291 -0.5082
-1.9475 2.4545 17.5128 0.9127 0.3782 0.1546
-6.7008 9.4169 17.7659 0.7995 0.3317 0.5007
-11.2412 16.1403 14.8293 0.5163 0.2147 0.8290
4.6396 34.3826 4.7433 0.0256 0.9829 0.1822
2.6114 -36.9084 -6.8915 -0.0202 -0.7915 -0.6108
-7.3435 -31.1538 -3.5536 -0.0262 -0.9996 0.0066
-9.6215 -31.3259 6.0829 0.4724 -0.8705 0.1383
-15.1542 -10.6358 8.3607 0.3399 -0.6274 0.7006
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_T_max  1.000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.839
_oxdiff_exptl_absorpt_empirical_full_max 1.325
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            133590
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.112
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13691
_reflns_number_gt                10581
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to 
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Solvent molecules were found disordered and refined with a disorder model 
 comprising of 0.705 molecules of toluene and 0.295 molecules of n-hexane per
 asymmetric unit. C-C distances have been restrained in the hexane molecule.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+4.2590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13691
_refine_ls_number_parameters     547
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0675
_refine_ls_wR_factor_ref         0.1516
_refine_ls_wR_factor_gt          0.1425
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.36174(3) 0.36542(2) 0.31199(2) 0.01937(7) Uani 1 1 d . . . . .
O1 O 0.61798(15) 0.40762(5) 0.53132(13) 0.0263(3) Uani 1 1 d . . . . .
O2 O 0.31054(17) 0.33820(6) 0.08044(13) 0.0332(3) Uani 1 1 d . . . . .
O3 O 0.08047(16) 0.37964(6) 0.24091(16) 0.0360(4) Uani 1 1 d . . . . .
N1 N 0.67269(16) 0.35096(6) 0.35669(15) 0.0224(3) Uani 1 1 d . . . . .
N2 N 0.49123(15) 0.26603(5) 0.30117(14) 0.0191(3) Uani 1 1 d . . . . .
N3 N 0.40178(18) 0.43241(6) 0.31179(16) 0.0258(3) Uani 1 1 d . . . . .
C1 C 0.55416(19) 0.37271(6) 0.48110(16) 0.0207(3) Uani 1 1 d . . . . .
C2 C 0.57198(18) 0.34457(6) 0.39162(16) 0.0196(3) Uani 1 1 d . . . . .
C3 C 0.48652(17) 0.30379(6) 0.36769(15) 0.0174(3) Uani 1 1 d . . . . .
C4 C 0.40019(18) 0.31027(6) 0.42457(16) 0.0184(3) Uani 1 1 d . . . . .
C5 C 0.43449(19) 0.35432(6) 0.48629(17) 0.0202(3) Uani 1 1 d . . . . .
C6 C 0.6473(2) 0.34679(7) 0.23762(18) 0.0258(4) Uani 1 1 d . . . . .
H6A H 0.571297 0.325814 0.200349 0.031 Uiso 1 1 calc R U . . .
H6B H 0.723644 0.332186 0.229789 0.031 Uiso 1 1 calc R U . . .
C7 C 0.6201(2) 0.39534(8) 0.1793(2) 0.0309(5) Uani 1 1 d . . . . .
H7A H 0.607872 0.391626 0.099893 0.037 Uiso 1 1 calc R U . . .
H7B H 0.538836 0.408693 0.180513 0.037 Uiso 1 1 calc R U . . .
C8 C 0.7336(3) 0.42922(9) 0.2392(2) 0.0380(5) Uani 1 1 d . . . . .
H8A H 0.812371 0.417883 0.229767 0.046 Uiso 1 1 calc R U . . .
H8B H 0.711825 0.461066 0.204930 0.046 Uiso 1 1 calc R U . . .
C9 C 0.7615(2) 0.43226(8) 0.3639(2) 0.0331(5) Uani 1 1 d . . . . .
H9A H 0.687617 0.447967 0.373568 0.040 Uiso 1 1 calc R U . . .
H9B H 0.840590 0.451619 0.402666 0.040 Uiso 1 1 calc R U . . .
C10 C 0.7817(2) 0.38302(7) 0.4164(2) 0.0264(4) Uani 1 1 d . . . . .
H10A H 0.862931 0.369305 0.416112 0.032 Uiso 1 1 calc R U . . .
H10B H 0.792304 0.385799 0.495688 0.032 Uiso 1 1 calc R U . . .
C11 C 0.37803(18) 0.23481(7) 0.25168(17) 0.0215(4) Uani 1 1 d . . . . .
H11A H 0.296935 0.253243 0.233623 0.026 Uiso 1 1 calc R U . . .
H11B H 0.381284 0.209836 0.306242 0.026 Uiso 1 1 calc R U . . .
C12 C 0.3779(2) 0.21219(7) 0.14488(18) 0.0255(4) Uani 1 1 d . . . . .
H12A H 0.367143 0.237077 0.088137 0.031 Uiso 1 1 calc R U . . .
H12B H 0.303493 0.190054 0.113478 0.031 Uiso 1 1 calc R U . . .
C13 C 0.5049(2) 0.18547(7) 0.1695(2) 0.0280(4) Uani 1 1 d . . . . .
H13A H 0.505809 0.173084 0.098491 0.034 Uiso 1 1 calc R U . . .
H13B H 0.510809 0.158248 0.219372 0.034 Uiso 1 1 calc R U . . .
C14 C 0.6221(2) 0.21812(7) 0.22612(19) 0.0261(4) Uani 1 1 d . . . . .
H14A H 0.703525 0.199542 0.248050 0.031 Uiso 1 1 calc R U . . .
H14B H 0.622806 0.242770 0.172162 0.031 Uiso 1 1 calc R U . . .
C15 C 0.61696(19) 0.24158(7) 0.32978(18) 0.0230(4) Uani 1 1 d . . . . .
H15A H 0.628290 0.217326 0.388003 0.028 Uiso 1 1 calc R U . . .
H15B H 0.689107 0.264673 0.360841 0.028 Uiso 1 1 calc R U . . .
C16 C 0.31912(18) 0.27322(6) 0.44818(16) 0.0189(3) Uani 1 1 d . . . . .
C17 C 0.37947(19) 0.23398(7) 0.51566(17) 0.0216(4) Uani 1 1 d . . . . .
C18 C 0.3013(2) 0.20168(7) 0.54186(17) 0.0249(4) Uani 1 1 d . . . . .
H18 H 0.340831 0.175179 0.587919 0.030 Uiso 1 1 calc R U . . .
C19 C 0.1671(2) 0.20739(8) 0.50215(18) 0.0257(4) Uani 1 1 d . . . . .
H19 H 0.116457 0.184724 0.521049 0.031 Uiso 1 1 calc R U . . .
C20 C 0.10591(19) 0.24591(7) 0.43506(17) 0.0233(4) Uani 1 1 d . . . . .
C21 C 0.18409(19) 0.27852(7) 0.41049(17) 0.0211(3) Uani 1 1 d . . . . .
H21 H 0.144074 0.305444 0.366355 0.025 Uiso 1 1 calc R U . . .
C22 C 0.5241(2) 0.22454(8) 0.56099(19) 0.0277(4) Uani 1 1 d . . . . .
H22A H 0.540574 0.196875 0.523025 0.042 Uiso 1 1 calc R U . . .
H22B H 0.556901 0.218431 0.641966 0.042 Uiso 1 1 calc R U . . .
H22C H 0.568692 0.252175 0.547420 0.042 Uiso 1 1 calc R U . . .
C23 C -0.0397(2) 0.25169(9) 0.3882(2) 0.0333(5) Uani 1 1 d . . . . .
H23A H -0.075898 0.246222 0.306863 0.050 Uiso 1 1 calc R U . . .
H23B H -0.061231 0.283849 0.403365 0.050 Uiso 1 1 calc R U . . .
H23C H -0.076870 0.228763 0.423847 0.050 Uiso 1 1 calc R U . . .
C24 C 0.3887(2) 0.37005(7) 0.57419(18) 0.0231(4) Uani 1 1 d . . . . .
C25 C 0.4669(2) 0.36099(7) 0.68763(19) 0.0271(4) Uani 1 1 d . . . . .
C26 C 0.4225(3) 0.37620(8) 0.7685(2) 0.0328(5) Uani 1 1 d . . . . .
H26 H 0.473865 0.369751 0.845512 0.039 Uiso 1 1 calc R U . . .
C27 C 0.3062(2) 0.40034(8) 0.7402(2) 0.0330(5) Uani 1 1 d . . . . .
H27 H 0.278862 0.410131 0.797459 0.040 Uiso 1 1 calc R U . . .
C28 C 0.2295(2) 0.41027(8) 0.6288(2) 0.0308(5) Uani 1 1 d . . . . .
C29 C 0.2723(2) 0.39480(7) 0.5470(2) 0.0262(4) Uani 1 1 d . . . . .
H29 H 0.220320 0.401391 0.470244 0.031 Uiso 1 1 calc R U . . .
C30 C 0.5953(3) 0.33571(10) 0.7234(2) 0.0375(5) Uani 1 1 d . . . . .
H30A H 0.580186 0.302558 0.699490 0.056 Uiso 1 1 calc R U . . .
H30B H 0.640870 0.337183 0.805391 0.056 Uiso 1 1 calc R U . . .
H30C H 0.648689 0.350911 0.688596 0.056 Uiso 1 1 calc R U . . .
C31 C 0.1040(2) 0.43744(9) 0.5964(3) 0.0392(6) Uani 1 1 d . . . . .
H31A H 0.034124 0.415804 0.592955 0.059 Uiso 1 1 calc R U . . .
H31B H 0.081820 0.452101 0.522553 0.059 Uiso 1 1 calc R U . . .
H31C H 0.114524 0.462094 0.652431 0.059 Uiso 1 1 calc R U . . .
C32 C 0.3316(2) 0.35030(7) 0.17029(18) 0.0242(4) Uani 1 1 d . . . . .
C33 C 0.1913(2) 0.37370(7) 0.27295(19) 0.0260(4) Uani 1 1 d . . . . .
C34 C 0.4317(3) 0.47106(8) 0.3184(2) 0.0358(5) Uani 1 1 d . . . . .
C35 C 0.4702(4) 0.52067(10) 0.3246(4) 0.0797(14) Uani 1 1 d . . . . .
H35A H 0.432975 0.534607 0.249135 0.120 Uiso 1 1 calc R U . . .
H35B H 0.565421 0.522900 0.354721 0.120 Uiso 1 1 calc R U . . .
H35C H 0.437898 0.537838 0.373897 0.120 Uiso 1 1 calc R U . . .
C36A C 0.0901(6) 0.4750(2) 0.9223(5) 0.0434(17) Uani 0.404(3) 1 d G U P A 1
C37A C 0.0528(8) 0.4287(2) 0.9303(6) 0.057(2) Uani 0.404(3) 1 d G U P A 1
H37C H 0.103115 0.409832 0.993252 0.069 Uiso 0.404(3) 1 calc R U P A 1
C38A C -0.0583(8) 0.4101(2) 0.8460(8) 0.083(3) Uani 0.404(3) 1 d G U P A 1
H38C H -0.083836 0.378400 0.851470 0.100 Uiso 0.404(3) 1 calc R U P A 1
C39A C -0.1320(6) 0.4377(3) 0.7539(7) 0.072(3) Uani 0.404(3) 1 d G U P A 1
H39C H -0.207890 0.424928 0.696321 0.086 Uiso 0.404(3) 1 calc R U P A 1
C40A C -0.0946(7) 0.4840(3) 0.7459(5) 0.069(3) Uani 0.404(3) 1 d G U P A 1
H40C H -0.144993 0.502888 0.682952 0.082 Uiso 0.404(3) 1 calc R U P A 1
C41A C 0.0164(7) 0.5027(2) 0.8302(6) 0.0482(18) Uani 0.404(3) 1 d G U P A 1
H41D H 0.041959 0.534321 0.824733 0.058 Uiso 0.404(3) 1 calc R U P A 1
C42A C 0.2068(9) 0.4934(5) 1.0139(8) 0.081(3) Uani 0.404(3) 1 d . U P A 1
H42A H 0.206259 0.483740 1.086274 0.121 Uiso 0.404(3) 1 calc R U P A 1
H42B H 0.207475 0.528039 1.009853 0.121 Uiso 0.404(3) 1 calc R U P A 1
H42C H 0.284762 0.480749 1.006961 0.121 Uiso 0.404(3) 1 calc R U P A 1
C42B C -0.1404(14) 0.4953(4) 0.6594(12) 0.067(3) Uani 0.301(3) 1 d . U P B 2
H42D H -0.210961 0.478057 0.600619 0.100 Uiso 0.301(3) 1 calc R U P B 2
H42E H -0.072525 0.503111 0.632456 0.100 Uiso 0.301(3) 1 calc R U P B 2
H42F H -0.174994 0.524502 0.677612 0.100 Uiso 0.301(3) 1 calc R U P B 2
C36B C -0.0865(10) 0.4666(3) 0.7571(7) 0.046(2) Uani 0.301(3) 1 d G U P B 2
C41B C -0.1424(8) 0.4264(3) 0.7812(7) 0.050(3) Uani 0.301(3) 1 d G U P B 2
H41E H -0.222733 0.414673 0.727603 0.061 Uiso 0.301(3) 1 calc R U P B 2
C40B C -0.0809(9) 0.4035(3) 0.8838(7) 0.048(2) Uani 0.301(3) 1 d G U P B 2
H40D H -0.119165 0.376107 0.900264 0.057 Uiso 0.301(3) 1 calc R U P B 2
C39B C 0.0366(9) 0.4207(4) 0.9622(6) 0.060(3) Uani 0.301(3) 1 d G U P B 2
H39D H 0.078604 0.405087 1.032326 0.073 Uiso 0.301(3) 1 calc R U P B 2
C38B C 0.0925(9) 0.4609(4) 0.9381(9) 0.081(5) Uani 0.301(3) 1 d G U P B 2
H38D H 0.172806 0.472632 0.991729 0.097 Uiso 0.301(3) 1 calc R U P B 2
C37B C 0.0310(11) 0.4838(3) 0.8355(10) 0.071(4) Uani 0.301(3) 1 d G U P B 2
H37D H 0.069240 0.511199 0.819067 0.085 Uiso 0.301(3) 1 calc R U P B 2
C41C C 0.445(2) 0.5031(7) 1.0355(19) 0.138(7) Uani 0.295(3) 1 d D U P C -3
H41A H 0.506516 0.501747 1.114439 0.207 Uiso 0.295(3) 1 calc R U P C -3
H41B H 0.472487 0.527763 0.996520 0.207 Uiso 0.295(3) 1 calc R U P C -3
H41C H 0.443609 0.472431 0.999695 0.207 Uiso 0.295(3) 1 calc R U P C -3
C40C C 0.308(2) 0.5146(9) 1.029(3) 0.171(9) Uani 0.295(3) 1 d D U P C -3
H40A H 0.310420 0.528394 1.099988 0.205 Uiso 0.295(3) 1 calc R U P C -3
H40B H 0.259491 0.535876 0.965458 0.205 Uiso 0.295(3) 1 calc R U P C -3
C39C C 0.253(3) 0.4652(10) 1.010(3) 0.184(10) Uani 0.295(3) 1 d D U P C -3
H39A H 0.281577 0.450202 0.954790 0.221 Uiso 0.295(3) 1 calc R U P C -3
H39B H 0.297108 0.447906 1.081757 0.221 Uiso 0.295(3) 1 calc R U P C -3
C36C C -0.115(3) 0.4261(14) 0.918(3) 0.215(14) Uani 0.295(3) 1 d D U P C -3
H36A H -0.181700 0.405489 0.865649 0.322 Uiso 0.295(3) 1 calc R U P C -3
H36B H -0.150250 0.458074 0.914967 0.322 Uiso 0.295(3) 1 calc R U P C -3
H36C H -0.087394 0.413643 0.994765 0.322 Uiso 0.295(3) 1 calc R U P C -3
C38C C 0.113(3) 0.4556(15) 0.972(4) 0.230(12) Uani 0.295(3) 1 d D U P C -3
H38A H 0.077022 0.488024 0.960254 0.275 Uiso 0.295(3) 1 calc R U P C -3
H38B H 0.108025 0.445003 1.043017 0.275 Uiso 0.295(3) 1 calc R U P C -3
C37C C 0.004(3) 0.4281(15) 0.886(3) 0.212(12) Uani 0.295(3) 1 d D U P C -3
H37A H 0.033205 0.395502 0.880845 0.255 Uiso 0.295(3) 1 calc R U P C -3
H37B H -0.022203 0.443269 0.811583 0.255 Uiso 0.295(3) 1 calc R U P C -3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C33 1.782(2) . ?
Fe1 C32 1.784(2) . ?
Fe1 N3 1.9456(17) . ?
Fe1 C4 2.0602(18) . ?
Fe1 C5 2.099(2) . ?
Fe1 C3 2.1675(18) . ?
Fe1 C2 2.2381(19) . ?
Fe1 C1 2.392(2) . ?
O1 C1 1.239(2) . ?
O2 C32 1.146(3) . ?
O3 C33 1.153(3) . ?
N1 C2 1.385(2) . ?
N1 C6 1.460(3) . ?
N1 C10 1.468(3) . ?
N2 C3 1.387(2) . ?
N2 C11 1.465(2) . ?
N2 C15 1.476(2) . ?
N3 C34 1.136(3) . ?
C1 C5 1.463(3) . ?
C1 C2 1.485(3) . ?
C2 C3 1.450(2) . ?
C3 C4 1.443(3) . ?
C4 C5 1.446(3) . ?
C4 C16 1.495(3) . ?
C5 C24 1.493(3) . ?
C6 C7 1.537(3) . ?
C7 C8 1.532(3) . ?
C8 C9 1.523(4) . ?
C9 C10 1.526(3) . ?
C11 C12 1.526(3) . ?
C12 C13 1.526(3) . ?
C13 C14 1.530(3) . ?
C14 C15 1.521(3) . ?
C16 C21 1.398(3) . ?
C16 C17 1.407(3) . ?
C17 C18 1.397(3) . ?
C17 C22 1.509(3) . ?
C18 C19 1.389(3) . ?
C19 C20 1.391(3) . ?
C20 C21 1.393(3) . ?
C20 C23 1.503(3) . ?
C24 C29 1.394(3) . ?
C24 C25 1.403(3) . ?
C25 C26 1.397(3) . ?
C25 C30 1.503(3) . ?
C26 C27 1.383(4) . ?
C27 C28 1.384(4) . ?
C28 C29 1.398(3) . ?
C28 C31 1.505(3) . ?
C34 C35 1.459(3) . ?
C36A C37A 1.3900 . ?
C36A C41A 1.3900 . ?
C36A C42A 1.466(10) . ?
C37A C38A 1.3900 . ?
C38A C39A 1.3900 . ?
C39A C40A 1.3900 . ?
C40A C41A 1.3900 . ?
C42B C36B 1.421(14) . ?
C36B C41B 1.3900 . ?
C36B C37B 1.3900 . ?
C41B C40B 1.3900 . ?
C40B C39B 1.3900 . ?
C39B C38B 1.3900 . ?
C38B C37B 1.3900 . ?
C41C C40C 1.538(18) . ?
C40C C39C 1.504(18) . ?
C39C C38C 1.464(18) . ?
C36C C37C 1.540(19) . ?
C38C C37C 1.506(18) . ?

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
C33 Fe1 C32 89.91(10) . . ?
C33 Fe1 N3 95.32(8) . . ?
C32 Fe1 N3 100.39(9) . . ?
C33 Fe1 C4 101.39(8) . . ?
C32 Fe1 C4 116.73(8) . . ?
N3 Fe1 C4 138.92(8) . . ?
C33 Fe1 C5 103.67(9) . . ?
C32 Fe1 C5 155.13(8) . . ?
N3 Fe1 C5 99.00(7) . . ?
C4 Fe1 C5 40.69(7) . . ?
C33 Fe1 C3 132.38(8) . . ?
C32 Fe1 C3 89.00(8) . . ?
N3 Fe1 C3 131.60(7) . . ?
C4 Fe1 C3 39.81(7) . . ?
C5 Fe1 C3 66.41(7) . . ?
C33 Fe1 C2 166.93(8) . . ?
C32 Fe1 C2 98.26(8) . . ?
N3 Fe1 C2 93.23(7) . . ?
C4 Fe1 C2 65.82(7) . . ?
C5 Fe1 C2 65.14(7) . . ?
C3 Fe1 C2 38.38(6) . . ?
C33 Fe1 C1 135.94(9) . . ?
C32 Fe1 C1 134.14(8) . . ?
N3 Fe1 C1 78.10(7) . . ?
C4 Fe1 C1 63.78(7) . . ?
C5 Fe1 C1 37.32(7) . . ?
C3 Fe1 C1 62.56(7) . . ?
C2 Fe1 C1 37.23(7) . . ?
C2 N1 C6 119.76(17) . . ?
C2 N1 C10 121.41(17) . . ?
C6 N1 C10 112.22(16) . . ?
C3 N2 C11 119.67(15) . . ?
C3 N2 C15 118.25(15) . . ?
C11 N2 C15 113.52(15) . . ?
C34 N3 Fe1 175.4(2) . . ?
O1 C1 C5 127.18(18) . . ?
O1 C1 C2 127.46(18) . . ?
C5 C1 C2 104.91(15) . . ?
O1 C1 Fe1 132.04(14) . . ?
C5 C1 Fe1 60.41(10) . . ?
C2 C1 Fe1 65.76(10) . . ?
N1 C2 C3 125.97(17) . . ?
N1 C2 C1 124.57(16) . . ?
C3 C2 C1 108.05(16) . . ?
N1 C2 Fe1 131.14(14) . . ?
C3 C2 Fe1 68.17(10) . . ?
C1 C2 Fe1 77.01(11) . . ?
N2 C3 C4 128.02(16) . . ?
N2 C3 C2 123.98(16) . . ?
C4 C3 C2 108.00(15) . . ?
N2 C3 Fe1 126.17(13) . . ?
C4 C3 Fe1 66.09(10) . . ?
C2 C3 Fe1 73.45(10) . . ?
C3 C4 C5 107.98(15) . . ?
C3 C4 C16 126.96(16) . . ?
C5 C4 C16 122.52(17) . . ?
C3 C4 Fe1 74.10(10) . . ?
C5 C4 Fe1 71.09(11) . . ?
C16 C4 Fe1 134.66(13) . . ?
C4 C5 C1 108.99(16) . . ?
C4 C5 C24 125.66(17) . . ?
C1 C5 C24 121.98(17) . . ?
C4 C5 Fe1 68.22(11) . . ?
C1 C5 Fe1 82.27(12) . . ?
C24 C5 Fe1 132.46(14) . . ?
N1 C6 C7 111.42(17) . . ?
C8 C7 C6 110.3(2) . . ?
C9 C8 C7 110.49(19) . . ?
C8 C9 C10 110.76(19) . . ?
N1 C10 C9 112.53(18) . . ?
N2 C11 C12 109.71(16) . . ?
C11 C12 C13 110.74(18) . . ?
C12 C13 C14 110.51(16) . . ?
C15 C14 C13 111.06(17) . . ?
N2 C15 C14 110.53(17) . . ?
C21 C16 C17 119.02(17) . . ?
C21 C16 C4 120.87(17) . . ?
C17 C16 C4 119.97(16) . . ?
C18 C17 C16 118.33(18) . . ?
C18 C17 C22 117.93(18) . . ?
C16 C17 C22 123.74(17) . . ?
C19 C18 C17 121.57(19) . . ?
C18 C19 C20 120.80(18) . . ?
C19 C20 C21 117.63(18) . . ?
C19 C20 C23 121.40(19) . . ?
C21 C20 C23 120.95(19) . . ?
C20 C21 C16 122.64(18) . . ?
C29 C24 C25 119.00(19) . . ?
C29 C24 C5 121.84(19) . . ?
C25 C24 C5 119.12(18) . . ?
C26 C25 C24 118.2(2) . . ?
C26 C25 C30 119.9(2) . . ?
C24 C25 C30 121.95(19) . . ?
C27 C26 C25 122.1(2) . . ?
C26 C27 C28 120.2(2) . . ?
C27 C28 C29 118.2(2) . . ?
C27 C28 C31 121.0(2) . . ?
C29 C28 C31 120.8(2) . . ?
C24 C29 C28 122.3(2) . . ?
O2 C32 Fe1 176.32(19) . . ?
O3 C33 Fe1 175.7(2) . . ?
N3 C34 C35 178.8(3) . . ?
C37A C36A C41A 120.0 . . ?
C37A C36A C42A 118.1(7) . . ?
C41A C36A C42A 121.9(7) . . ?
C36A C37A C38A 120.0 . . ?
C37A C38A C39A 120.0 . . ?
C40A C39A C38A 120.0 . . ?
C39A C40A C41A 120.0 . . ?
C40A C41A C36A 120.0 . . ?
C41B C36B C37B 120.0 . . ?
C41B C36B C42B 126.7(9) . . ?
C37B C36B C42B 113.2(9) . . ?
C36B C41B C40B 120.0 . . ?
C41B C40B C39B 120.0 . . ?
C38B C39B C40B 120.0 . . ?
C39B C38B C37B 120.0 . . ?
C38B C37B C36B 120.0 . . ?
C39C C40C C41C 98.4(18) . . ?
C38C C39C C40C 123(3) . . ?
C39C C38C C37C 142(3) . . ?
C38C C37C C36C 111(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
C6 N1 C2 C3 53.8(3) . . . . ?
C10 N1 C2 C3 -156.96(19) . . . . ?
C6 N1 C2 C1 -141.43(19) . . . . ?
C10 N1 C2 C1 7.8(3) . . . . ?
C6 N1 C2 Fe1 -37.6(3) . . . . ?
C10 N1 C2 Fe1 111.7(2) . . . . ?
O1 C1 C2 N1 5.9(3) . . . . ?
C5 C1 C2 N1 178.52(18) . . . . ?
Fe1 C1 C2 N1 131.37(19) . . . . ?
O1 C1 C2 C3 172.99(19) . . . . ?
C5 C1 C2 C3 -14.4(2) . . . . ?
Fe1 C1 C2 C3 -61.54(12) . . . . ?
O1 C1 C2 Fe1 -125.5(2) . . . . ?
C5 C1 C2 Fe1 47.15(13) . . . . ?
C11 N2 C3 C4 20.1(3) . . . . ?
C15 N2 C3 C4 -125.7(2) . . . . ?
C11 N2 C3 C2 -159.99(18) . . . . ?
C15 N2 C3 C2 54.2(3) . . . . ?
C11 N2 C3 Fe1 -66.1(2) . . . . ?
C15 N2 C3 Fe1 148.02(14) . . . . ?
N1 C2 C3 N2 -3.0(3) . . . . ?
C1 C2 C3 N2 -169.83(17) . . . . ?
Fe1 C2 C3 N2 122.83(18) . . . . ?
N1 C2 C3 C4 176.96(18) . . . . ?
C1 C2 C3 C4 10.1(2) . . . . ?
Fe1 C2 C3 C4 -57.24(12) . . . . ?
N1 C2 C3 Fe1 -125.8(2) . . . . ?
C1 C2 C3 Fe1 67.34(13) . . . . ?
N2 C3 C4 C5 178.31(18) . . . . ?
C2 C3 C4 C5 -1.6(2) . . . . ?
Fe1 C3 C4 C5 -63.47(13) . . . . ?
N2 C3 C4 C16 16.2(3) . . . . ?
C2 C3 C4 C16 -163.70(18) . . . . ?
Fe1 C3 C4 C16 134.45(19) . . . . ?
N2 C3 C4 Fe1 -118.22(19) . . . . ?
C2 C3 C4 Fe1 61.85(13) . . . . ?
C3 C4 C5 C1 -7.6(2) . . . . ?
C16 C4 C5 C1 155.40(17) . . . . ?
Fe1 C4 C5 C1 -73.10(14) . . . . ?
C3 C4 C5 C24 -167.11(18) . . . . ?
C16 C4 C5 C24 -4.1(3) . . . . ?
Fe1 C4 C5 C24 127.4(2) . . . . ?
C3 C4 C5 Fe1 65.45(13) . . . . ?
C16 C4 C5 Fe1 -131.51(18) . . . . ?
O1 C1 C5 C4 -173.87(19) . . . . ?
C2 C1 C5 C4 13.5(2) . . . . ?
Fe1 C1 C5 C4 63.72(13) . . . . ?
O1 C1 C5 C24 -13.5(3) . . . . ?
C2 C1 C5 C24 173.84(17) . . . . ?
Fe1 C1 C5 C24 -135.92(19) . . . . ?
O1 C1 C5 Fe1 122.4(2) . . . . ?
C2 C1 C5 Fe1 -50.24(13) . . . . ?
C2 N1 C6 C7 94.9(2) . . . . ?
C10 N1 C6 C7 -57.0(2) . . . . ?
N1 C6 C7 C8 56.3(2) . . . . ?
C6 C7 C8 C9 -54.5(3) . . . . ?
C7 C8 C9 C10 53.4(3) . . . . ?
C2 N1 C10 C9 -95.2(2) . . . . ?
C6 N1 C10 C9 56.2(2) . . . . ?
C8 C9 C10 N1 -54.1(3) . . . . ?
C3 N2 C11 C12 153.88(17) . . . . ?
C15 N2 C11 C12 -58.8(2) . . . . ?
N2 C11 C12 C13 56.7(2) . . . . ?
C11 C12 C13 C14 -55.0(2) . . . . ?
C12 C13 C14 C15 53.7(2) . . . . ?
C3 N2 C15 C14 -154.43(17) . . . . ?
C11 N2 C15 C14 57.7(2) . . . . ?
C13 C14 C15 N2 -54.1(2) . . . . ?
C3 C4 C16 C21 -123.4(2) . . . . ?
C5 C4 C16 C21 76.9(2) . . . . ?
Fe1 C4 C16 C21 -18.2(3) . . . . ?
C3 C4 C16 C17 61.0(3) . . . . ?
C5 C4 C16 C17 -98.6(2) . . . . ?
Fe1 C4 C16 C17 166.22(15) . . . . ?
C21 C16 C17 C18 0.3(3) . . . . ?
C4 C16 C17 C18 175.93(18) . . . . ?
C21 C16 C17 C22 179.90(19) . . . . ?
C4 C16 C17 C22 -4.5(3) . . . . ?
C16 C17 C18 C19 0.6(3) . . . . ?
C22 C17 C18 C19 -179.1(2) . . . . ?
C17 C18 C19 C20 -0.4(3) . . . . ?
C18 C19 C20 C21 -0.7(3) . . . . ?
C18 C19 C20 C23 177.9(2) . . . . ?
C19 C20 C21 C16 1.6(3) . . . . ?
C23 C20 C21 C16 -176.99(19) . . . . ?
C17 C16 C21 C20 -1.4(3) . . . . ?
C4 C16 C21 C20 -177.00(18) . . . . ?
C4 C5 C24 C29 -87.5(3) . . . . ?
C1 C5 C24 C29 115.5(2) . . . . ?
Fe1 C5 C24 C29 4.7(3) . . . . ?
C4 C5 C24 C25 94.6(2) . . . . ?
C1 C5 C24 C25 -62.4(3) . . . . ?
Fe1 C5 C24 C25 -173.28(15) . . . . ?
C29 C24 C25 C26 1.7(3) . . . . ?
C5 C24 C25 C26 179.70(19) . . . . ?
C29 C24 C25 C30 -178.3(2) . . . . ?
C5 C24 C25 C30 -0.2(3) . . . . ?
C24 C25 C26 C27 -1.1(3) . . . . ?
C30 C25 C26 C27 178.8(2) . . . . ?
C25 C26 C27 C28 -0.1(4) . . . . ?
C26 C27 C28 C29 0.7(3) . . . . ?
C26 C27 C28 C31 -178.6(2) . . . . ?
C25 C24 C29 C28 -1.1(3) . . . . ?
C5 C24 C29 C28 -179.08(18) . . . . ?
C27 C28 C29 C24 -0.1(3) . . . . ?
C31 C28 C29 C24 179.2(2) . . . . ?
C41A C36A C37A C38A 0.0 . . . . ?
C42A C36A C37A C38A 179.1(7) . . . . ?
C36A C37A C38A C39A 0.0 . . . . ?
C37A C38A C39A C40A 0.0 . . . . ?
C38A C39A C40A C41A 0.0 . . . . ?
C39A C40A C41A C36A 0.0 . . . . ?
C37A C36A C41A C40A 0.0 . . . . ?
C42A C36A C41A C40A -179.1(7) . . . . ?
C37B C36B C41B C40B 0.0 . . . . ?
C42B C36B C41B C40B -176.3(10) . . . . ?
C36B C41B C40B C39B 0.0 . . . . ?
C41B C40B C39B C38B 0.0 . . . . ?
C40B C39B C38B C37B 0.0 . . . . ?
C39B C38B C37B C36B 0.0 . . . . ?
C41B C36B C37B C38B 0.0 . . . . ?
C42B C36B C37B C38B 176.7(9) . . . . ?
C41C C40C C39C C38C -166(3) . . . . ?
C40C C39C C38C C37C 130(6) . . . . ?
C39C C38C C37C C36C 165(5) . . . . ?

_refine_diff_density_max         0.833
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.072


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk39db
_database_code_depnum_ccdc_archive 'CCDC 2338294'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 F6 Fe N2 O4, C6 H12'
_chemical_formula_sum            'C38 H40 F6 Fe N2 O4'
_chemical_formula_weight         758.57

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.59054(12)
_cell_length_b                   15.4277(2)
_cell_length_c                   23.2167(3)
_cell_angle_alpha                101.0985(12)
_cell_angle_beta                 99.2340(10)
_cell_angle_gamma                103.2907(8)
_cell_volume                     3538.46(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    144939
_cell_measurement_theta_min      2.1100
_cell_measurement_theta_max      45.0640

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.017
_exptl_absorpt_coefficient_mu    0.501
_shelx_estimated_absorpt_T_min   0.825
_shelx_estimated_absorpt_T_max   0.992
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -9 -26 0.0761
-10 0 -17 0.1933
-14 5 -5 0.1876
-14 9 11 0.2027
0 7 27 0.0897
0 -20 19 0.0910
-13 -2 -3 0.1860
1 19 -18 0.0675
12 -11 15 0.1650
-5 19 -20 0.1162
6 -16 -16 0.0979
10 3 14 0.1380
6 9 18 0.1041
2 12 19 0.0851
0 14 18 0.0845
-3 16 18 0.0953
-9 17 13 0.1425
12 3 -23 0.1336
4 6 -32 0.0745
3 19 0 0.0625
11 6 7 0.1300
0 21 -1 0.0559
-2 22 -3 0.0732
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
5.5910 -9.1145 -26.3653 0.0262 0.9979 -0.0589
-10.4649 0.2292 -16.9697 0.0076 0.3356 -0.9420
-14.1059 4.7600 -5.3356 -0.0047 -0.1304 -0.9915
-14.2588 8.8667 10.5852 -0.0184 -0.6627 -0.7487
-0.1581 6.9678 27.1855 -0.0233 -0.9067 0.4212
-0.1164 -19.5998 18.9039 0.9929 -0.0262 0.1163
-13.3002 -2.1681 -3.2485 0.2875 -0.0064 -0.9578
1.4285 19.3836 -18.1676 -0.9995 0.0263 -0.0191
11.5047 -11.1685 15.4219 0.4111 -0.0119 0.9115
-5.1014 18.5678 -20.0029 -0.8709 0.0235 -0.4909
5.5496 -16.4905 -16.0621 0.4304 0.9021 0.0298
10.4505 2.8822 14.3107 -0.1614 -0.3410 0.9261
6.1892 8.6657 17.6123 -0.2949 -0.6202 0.7269
2.2152 12.4239 18.5439 -0.3726 -0.7823 0.4992
0.1356 13.9280 18.4241 -0.3999 -0.8393 0.3682
-2.8252 15.5568 17.5804 -0.4243 -0.8897 0.1685
-8.5912 16.7439 13.3312 -0.4148 -0.8685 -0.2713
11.6835 3.4678 -22.9844 -0.5657 0.6634 0.4899
4.3544 6.3449 -32.0670 -0.6455 0.7557 -0.1109
2.7246 19.0771 0.3456 -0.8310 -0.4507 0.3260
11.3329 6.0423 6.7332 -0.3799 -0.2051 0.9020
0.4437 20.5511 -1.2038 -0.8675 -0.4707 0.1611
-2.3761 21.5470 -3.0597 -0.8778 -0.4766 -0.0479
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_T_max  1.000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_oxdiff_exptl_absorpt_empirical_full_max 1.379
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            78215
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.020
_diffrn_reflns_theta_max         40.327
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             78215
_reflns_number_gt                55547
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Refined as a 2-component twin. Component 2 rotated by -179.9521°
 around [0.00 0.71 -0.71] (reciprocal) or [0.21 0.93 -0.30] (direct).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1217P)²+3.4697P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         78215
_refine_ls_number_parameters     976
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2484
_refine_ls_wR_factor_gt          0.2310
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.92366(3) 1.02387(2) 0.16775(2) 0.01347(5) Uani 1 1 d . . . . .
F7 F 1.0890(3) 0.53299(13) 0.06081(11) 0.0487(5) Uani 1 1 d . . . . .
F8 F 0.9039(3) 0.50046(15) 0.08675(19) 0.0778(10) Uani 1 1 d . . . . .
F9 F 1.0830(4) 0.55530(16) 0.15371(11) 0.0646(8) Uani 1 1 d . . . . .
O1 O 0.84438(16) 1.07875(11) 0.03101(7) 0.0210(3) Uani 1 1 d . . . . .
O2 O 0.7180(2) 0.90329(14) 0.20907(11) 0.0351(4) Uani 1 1 d . . . . .
O3 O 0.79099(18) 1.17183(12) 0.18722(9) 0.0265(3) Uani 1 1 d . . . . .
O4 O 1.11407(18) 1.07983(13) 0.28442(7) 0.0261(3) Uani 1 1 d . . . . .
N1 N 1.21958(15) 1.01854(11) 0.14757(7) 0.0155(2) Uani 1 1 d . . . . .
N2 N 1.11497(16) 1.17722(11) 0.11890(7) 0.0154(2) Uani 1 1 d . . . . .
C1 C 0.90749(18) 1.04483(12) 0.06548(8) 0.0155(3) Uani 1 1 d . . . . .
C2 C 0.86285(17) 0.95332(12) 0.07763(8) 0.0144(2) Uani 1 1 d . . . . .
C3 C 0.97717(17) 0.93016(11) 0.10780(8) 0.0134(2) Uani 1 1 d . . . . .
C4 C 1.08847(17) 1.01089(12) 0.12253(8) 0.0135(2) Uani 1 1 d . . . . .
C5 C 1.04084(17) 1.08654(12) 0.10756(8) 0.0141(2) Uani 1 1 d . . . . .
C6 C 0.73144(17) 0.89126(12) 0.04568(8) 0.0149(2) Uani 1 1 d . . . . .
C7 C 0.71731(19) 0.80118(13) 0.01451(9) 0.0185(3) Uani 1 1 d . . . . .
H7 H 0.792834 0.777650 0.015744 0.022 Uiso 1 1 calc R U . . .
C8 C 0.59369(19) 0.74569(14) -0.01830(10) 0.0197(3) Uani 1 1 d . . . . .
H8 H 0.585156 0.684415 -0.038846 0.024 Uiso 1 1 calc R U . . .
C9 C 0.48314(18) 0.77964(14) -0.02105(9) 0.0178(3) Uani 1 1 d . . . . .
C10 C 0.49472(19) 0.86952(15) 0.00973(10) 0.0206(3) Uani 1 1 d . . . . .
H10 H 0.418876 0.892730 0.008093 0.025 Uiso 1 1 calc R U . . .
C11 C 0.6180(2) 0.92446(14) 0.04268(9) 0.0197(3) Uani 1 1 d . . . . .
H11 H 0.625892 0.985455 0.063530 0.024 Uiso 1 1 calc R U . . .
C12 C 0.3507(2) 0.72050(16) -0.05698(10) 0.0213(3) Uani 1 1 d . . . . .
C13 C 0.98810(17) 0.83569(12) 0.10744(8) 0.0143(2) Uani 1 1 d . . . . .
C14 C 0.9367(2) 0.78599(14) 0.14671(10) 0.0206(3) Uani 1 1 d . . . . .
H14 H 0.894027 0.813062 0.175516 0.025 Uiso 1 1 calc R U . . .
C15 C 0.9476(2) 0.69687(15) 0.14400(11) 0.0244(4) Uani 1 1 d . . . . .
H15 H 0.912967 0.663631 0.171023 0.029 Uiso 1 1 calc R U . . .
C16 C 1.0091(2) 0.65708(14) 0.10175(11) 0.0223(3) Uani 1 1 d . . . . .
C17 C 1.0611(2) 0.70548(14) 0.06241(10) 0.0210(3) Uani 1 1 d . . . . .
H17 H 1.103051 0.677762 0.033538 0.025 Uiso 1 1 calc R U . . .
C18 C 1.0515(2) 0.79489(13) 0.06537(9) 0.0179(3) Uani 1 1 d . . . . .
H18 H 1.088047 0.828265 0.038805 0.021 Uiso 1 1 calc R U . . .
C19 C 1.0212(3) 0.56185(17) 0.10088(14) 0.0323(5) Uani 1 1 d . . . . .
C20 C 1.25435(19) 0.95140(14) 0.17985(9) 0.0188(3) Uani 1 1 d . . . . .
H20A H 1.261555 0.897460 0.150915 0.023 Uiso 1 1 calc R U . . .
H20B H 1.183953 0.930336 0.201316 0.023 Uiso 1 1 calc R U . . .
C21 C 1.3864(2) 0.99555(17) 0.22473(10) 0.0228(4) Uani 1 1 d . . . . .
H21A H 1.411330 0.949811 0.245660 0.027 Uiso 1 1 calc R U . . .
H21B H 1.377056 1.046821 0.255227 0.027 Uiso 1 1 calc R U . . .
C22 C 1.4955(2) 1.03149(19) 0.19273(11) 0.0265(4) Uani 1 1 d . . . . .
H22A H 1.511009 0.979495 0.165005 0.032 Uiso 1 1 calc R U . . .
H22B H 1.579323 1.062925 0.222677 0.032 Uiso 1 1 calc R U . . .
C23 C 1.4553(2) 1.09852(19) 0.15732(12) 0.0262(4) Uani 1 1 d . . . . .
H23A H 1.451966 1.154371 0.185671 0.031 Uiso 1 1 calc R U . . .
H23B H 1.522894 1.116898 0.133881 0.031 Uiso 1 1 calc R U . . .
C24 C 1.31996(19) 1.05536(15) 0.11474(9) 0.0197(3) Uani 1 1 d . . . . .
H24A H 1.292102 1.102036 0.095676 0.024 Uiso 1 1 calc R U . . .
H24B H 1.326616 1.005226 0.082582 0.024 Uiso 1 1 calc R U . . .
C25 C 1.1989(2) 1.21574(13) 0.17978(9) 0.0188(3) Uani 1 1 d . . . . .
H25A H 1.245288 1.170713 0.191180 0.023 Uiso 1 1 calc R U . . .
H25B H 1.141959 1.227075 0.208766 0.023 Uiso 1 1 calc R U . . .
C26 C 1.3009(2) 1.30497(15) 0.18333(11) 0.0242(4) Uani 1 1 d . . . . .
H26A H 1.361304 1.293229 0.156105 0.029 Uiso 1 1 calc R U . . .
H26B H 1.354843 1.329323 0.224802 0.029 Uiso 1 1 calc R U . . .
C27 C 1.2322(2) 1.37561(14) 0.16555(11) 0.0249(4) Uani 1 1 d . . . . .
H27A H 1.299481 1.431199 0.164211 0.030 Uiso 1 1 calc R U . . .
H27B H 1.180755 1.393523 0.195677 0.030 Uiso 1 1 calc R U . . .
C28 C 1.1391(2) 1.33403(14) 0.10359(10) 0.0226(3) Uani 1 1 d . . . . .
H28A H 1.087925 1.377439 0.093753 0.027 Uiso 1 1 calc R U . . .
H28B H 1.192582 1.324627 0.072825 0.027 Uiso 1 1 calc R U . . .
C29 C 1.0436(2) 1.24324(13) 0.10167(10) 0.0200(3) Uani 1 1 d . . . . .
H29A H 0.983718 1.253607 0.129423 0.024 Uiso 1 1 calc R U . . .
H29B H 0.988256 1.217143 0.060569 0.024 Uiso 1 1 calc R U . . .
C30 C 0.7999(2) 0.94834(15) 0.19288(10) 0.0220(3) Uani 1 1 d . . . . .
C31 C 0.84435(19) 1.11566(14) 0.17840(9) 0.0180(3) Uani 1 1 d . . . . .
C32 C 1.0400(2) 1.05845(14) 0.23917(8) 0.0184(3) Uani 1 1 d . . . . .
F1 F 0.3036(3) 0.7553(2) -0.10248(13) 0.0468(8) Uani 0.753(5) 1 d . U P A 1
F2 F 0.2570(2) 0.7130(2) -0.02538(12) 0.0459(8) Uani 0.753(5) 1 d . U P A 1
F3 F 0.3518(3) 0.63589(19) -0.08253(16) 0.0495(8) Uani 0.753(5) 1 d . U P A 1
F4 F 0.3603(9) 0.6817(7) -0.1091(4) 0.049(2) Uani 0.247(5) 1 d . U P A 2
F5 F 0.2579(10) 0.7627(7) -0.0575(5) 0.056(3) Uani 0.247(5) 1 d . U P A 2
F6 F 0.3071(10) 0.6519(7) -0.0307(5) 0.051(2) Uani 0.247(5) 1 d . U P A 2
Fe1A Fe 1.02648(3) 0.26003(2) 0.40157(2) 0.01543(5) Uani 1 1 d . . . . .
F7A F 0.8020(3) 0.20128(19) 0.71752(10) 0.0636(8) Uani 1 1 d . . . . .
F8A F 0.9531(3) 0.1309(2) 0.70711(11) 0.0603(7) Uani 1 1 d . . . . .
F9A F 0.7534(3) 0.06545(18) 0.65938(11) 0.0565(6) Uani 1 1 d . . . . .
O1A O 1.17370(17) 0.49524(12) 0.44516(7) 0.0242(3) Uani 1 1 d . . . . .
O2A O 1.1576(3) 0.1211(2) 0.43128(10) 0.0455(6) Uani 1 1 d . . . . .
O3A O 1.2072(2) 0.30804(18) 0.32158(9) 0.0355(5) Uani 1 1 d . . . . .
O4A O 0.81243(19) 0.11687(12) 0.31317(8) 0.0262(3) Uani 1 1 d . . . . .
N1A N 0.73845(16) 0.28993(12) 0.41649(8) 0.0179(3) Uani 1 1 d . . . . .
N2A N 0.90475(17) 0.41347(11) 0.35251(7) 0.0162(2) Uani 1 1 d . . . . .
C1A C 1.08685(19) 0.42575(13) 0.44405(8) 0.0170(3) Uani 1 1 d . . . . .
C2A C 1.09778(18) 0.35998(13) 0.48194(8) 0.0159(3) Uani 1 1 d . . . . .
C3A C 0.96503(18) 0.30431(13) 0.47914(8) 0.0150(3) Uani 1 1 d . . . . .
C4A C 0.87490(17) 0.32337(13) 0.43232(8) 0.0151(3) Uani 1 1 d . . . . .
C5A C 0.95300(18) 0.38386(12) 0.40251(8) 0.0153(3) Uani 1 1 d . . . . .
C6A C 1.21909(19) 0.37691(14) 0.52855(8) 0.0173(3) Uani 1 1 d . . . . .
C7A C 1.21496(19) 0.38422(16) 0.58929(8) 0.0201(3) Uani 1 1 d . . . . .
H7A H 1.131750 0.374704 0.600890 0.024 Uiso 1 1 calc R U . . .
C8A C 1.3315(2) 0.40529(17) 0.63284(9) 0.0217(3) Uani 1 1 d . . . . .
H8A H 1.327303 0.409746 0.673840 0.026 Uiso 1 1 calc R U . . .
C9A C 1.4532(2) 0.41973(16) 0.61658(9) 0.0212(3) Uani 1 1 d . . . . .
C10A C 1.4605(2) 0.4152(2) 0.55660(10) 0.0285(5) Uani 1 1 d . . . . .
H10A H 1.544300 0.427255 0.545619 0.034 Uiso 1 1 calc R U . . .
C11A C 1.3437(2) 0.3929(2) 0.51297(9) 0.0262(4) Uani 1 1 d . . . . .
H11A H 1.348425 0.388537 0.472031 0.031 Uiso 1 1 calc R U . . .
C12A C 1.5778(2) 0.4438(2) 0.66433(11) 0.0282(4) Uani 1 1 d . . . . .
C13A C 0.92752(19) 0.25855(13) 0.52723(8) 0.0165(3) Uani 1 1 d . . . . .
C14A C 0.9737(3) 0.18500(19) 0.53948(12) 0.0305(5) Uani 1 1 d . . . . .
H14A H 1.023808 0.158617 0.514064 0.037 Uiso 1 1 calc R U . . .
C15A C 0.9474(3) 0.1497(2) 0.58854(13) 0.0346(6) Uani 1 1 d . . . . .
H15A H 0.979907 0.099754 0.596594 0.042 Uiso 1 1 calc R U . . .
C16A C 0.8738(3) 0.18755(17) 0.62546(10) 0.0267(4) Uani 1 1 d . . . . .
C17A C 0.8275(2) 0.26127(16) 0.61418(10) 0.0232(3) Uani 1 1 d . . . . .
H17A H 0.777477 0.287413 0.639759 0.028 Uiso 1 1 calc R U . . .
C18A C 0.8544(2) 0.29669(14) 0.56533(8) 0.0186(3) Uani 1 1 d . . . . .
H18A H 0.822946 0.347211 0.557795 0.022 Uiso 1 1 calc R U . . .
C19A C 0.8450(4) 0.1470(2) 0.67729(14) 0.0409(7) Uani 1 1 d . . . . .
C20A C 0.6706(2) 0.20646(16) 0.43201(10) 0.0225(3) Uani 1 1 d . . . . .
H20C H 0.652506 0.222025 0.472733 0.027 Uiso 1 1 calc R U . . .
H20D H 0.727982 0.164054 0.432131 0.027 Uiso 1 1 calc R U . . .
C21A C 0.5399(2) 0.15997(17) 0.38611(11) 0.0258(4) Uani 1 1 d . . . . .
H21C H 0.558775 0.140757 0.345903 0.031 Uiso 1 1 calc R U . . .
H21D H 0.492809 0.104433 0.397262 0.031 Uiso 1 1 calc R U . . .
C22A C 0.4518(2) 0.2250(2) 0.38373(13) 0.0321(5) Uani 1 1 d . . . . .
H22C H 0.425586 0.239529 0.422770 0.039 Uiso 1 1 calc R U . . .
H22D H 0.370106 0.195211 0.352222 0.039 Uiso 1 1 calc R U . . .
C23A C 0.5260(2) 0.3134(2) 0.37002(13) 0.0293(5) Uani 1 1 d . . . . .
H23C H 0.471050 0.357413 0.372620 0.035 Uiso 1 1 calc R U . . .
H23D H 0.539959 0.299756 0.328439 0.035 Uiso 1 1 calc R U . . .
C24A C 0.6603(2) 0.35719(16) 0.41356(10) 0.0228(3) Uani 1 1 d . . . . .
H24C H 0.710121 0.409504 0.400173 0.027 Uiso 1 1 calc R U . . .
H24D H 0.646107 0.380947 0.454089 0.027 Uiso 1 1 calc R U . . .
C25A C 0.8154(2) 0.33970(14) 0.30241(8) 0.0188(3) Uani 1 1 d . . . . .
H25C H 0.749513 0.299694 0.318438 0.023 Uiso 1 1 calc R U . . .
H25D H 0.868007 0.301756 0.283252 0.023 Uiso 1 1 calc R U . . .
C26A C 0.7429(2) 0.37799(17) 0.25546(10) 0.0239(4) Uani 1 1 d . . . . .
H26C H 0.687115 0.413811 0.273967 0.029 Uiso 1 1 calc R U . . .
H26D H 0.684106 0.326885 0.222675 0.029 Uiso 1 1 calc R U . . .
C27A C 0.8430(3) 0.43951(17) 0.22979(9) 0.0256(4) Uani 1 1 d . . . . .
H27C H 0.795913 0.467891 0.201441 0.031 Uiso 1 1 calc R U . . .
H27D H 0.892959 0.402603 0.207681 0.031 Uiso 1 1 calc R U . . .
C28A C 0.9389(3) 0.51417(16) 0.28157(10) 0.0239(4) Uani 1 1 d . . . . .
H28C H 1.008431 0.551149 0.265618 0.029 Uiso 1 1 calc R U . . .
H28D H 0.889857 0.555462 0.300122 0.029 Uiso 1 1 calc R U . . .
C29A C 1.0047(2) 0.47352(15) 0.32950(9) 0.0212(3) Uani 1 1 d . . . . .
H29C H 1.061815 0.437682 0.312111 0.025 Uiso 1 1 calc R U . . .
H29D H 1.061988 0.523859 0.363195 0.025 Uiso 1 1 calc R U . . .
C30A C 1.1066(3) 0.17599(19) 0.42179(10) 0.0271(4) Uani 1 1 d . . . . .
C31A C 1.1358(2) 0.29111(17) 0.35244(9) 0.0223(3) Uani 1 1 d . . . . .
C32A C 0.8954(2) 0.17306(14) 0.34699(9) 0.0193(3) Uani 1 1 d . . . . .
F1A F 1.6455(5) 0.5359(4) 0.6746(3) 0.0557(14) Uani 0.472(5) 1 d . U P B 3
F2A F 1.6724(4) 0.4079(3) 0.64447(19) 0.0361(9) Uani 0.472(5) 1 d . U P B 3
F3A F 1.5635(5) 0.4291(5) 0.7143(2) 0.0530(13) Uani 0.472(5) 1 d . U P B 3
F4A F 1.5780(5) 0.5078(4) 0.7098(2) 0.0624(14) Uani 0.528(5) 1 d . U P B 4
F5A F 1.6843(5) 0.4620(5) 0.6456(2) 0.0585(13) Uani 0.528(5) 1 d . U P B 4
F6A F 1.5813(4) 0.3715(3) 0.6915(2) 0.0539(12) Uani 0.528(5) 1 d . U P B 4
C94 C 0.6033(4) 0.6690(3) 0.1969(2) 0.0541(6) Uani 1 1 d . . . . .
H94A H 0.622084 0.667171 0.239713 0.065 Uiso 1 1 calc R U . . .
H94B H 0.676832 0.716303 0.190341 0.065 Uiso 1 1 calc R U . . .
C95 C 0.5953(5) 0.5752(3) 0.1573(3) 0.0613(7) Uani 1 1 d . . . . .
H95A H 0.682969 0.562428 0.165450 0.074 Uiso 1 1 calc R U . . .
H95B H 0.530174 0.527271 0.168158 0.074 Uiso 1 1 calc R U . . .
C96 C 0.5547(5) 0.5697(4) 0.0906(3) 0.0679(8) Uani 1 1 d . . . . .
H96A H 0.624612 0.612553 0.078356 0.081 Uiso 1 1 calc R U . . .
H96B H 0.545755 0.506827 0.067367 0.081 Uiso 1 1 calc R U . . .
C97 C 0.4248(5) 0.5937(4) 0.0766(3) 0.0683(9) Uani 1 1 d . . . . .
H97A H 0.352839 0.546743 0.084469 0.082 Uiso 1 1 calc R U . . .
H97B H 0.403271 0.593998 0.033557 0.082 Uiso 1 1 calc R U . . .
C98 C 0.4331(5) 0.6875(4) 0.1150(2) 0.0580(7) Uani 1 1 d . . . . .
H98A H 0.498730 0.734797 0.103859 0.070 Uiso 1 1 calc R U . . .
H98B H 0.345651 0.700532 0.106385 0.070 Uiso 1 1 calc R U . . .
C99 C 0.4728(4) 0.6941(4) 0.1817(2) 0.0553(7) Uani 1 1 d . . . . .
H99A H 0.402019 0.652240 0.194094 0.066 Uiso 1 1 calc R U . . .
H99B H 0.482449 0.757436 0.204358 0.066 Uiso 1 1 calc R U . . .
C94A C 0.4210(6) 0.1128(5) 0.5405(4) 0.0858(12) Uani 1 1 d . . . . .
H94C H 0.376388 0.149290 0.517653 0.103 Uiso 1 1 calc R U . . .
H94D H 0.499138 0.105425 0.523702 0.103 Uiso 1 1 calc R U . . .
C95A C 0.3350(6) 0.0275(5) 0.5317(3) 0.0766(10) Uani 1 1 d . . . . .
H95C H 0.386211 -0.013971 0.544908 0.092 Uiso 1 1 calc R U . . .
H95D H 0.297420 0.003355 0.488099 0.092 Uiso 1 1 calc R U . . .
C96A C 0.2244(5) 0.0243(4) 0.5631(3) 0.0675(9) Uani 1 1 d . . . . .
H96C H 0.163127 0.056039 0.544712 0.081 Uiso 1 1 calc R U . . .
H96D H 0.174469 -0.040467 0.557364 0.081 Uiso 1 1 calc R U . . .
C97A C 0.2672(6) 0.0666(4) 0.6274(3) 0.0754(10) Uani 1 1 d . . . . .
H97C H 0.187109 0.067559 0.644119 0.090 Uiso 1 1 calc R U . . .
H97D H 0.313103 0.027092 0.646684 0.090 Uiso 1 1 calc R U . . .
C98A C 0.3541(8) 0.1586(5) 0.6440(4) 0.0947(15) Uani 1 1 d . . . . .
H98C H 0.395898 0.174639 0.687351 0.114 Uiso 1 1 calc R U . . .
H98D H 0.301969 0.202583 0.636763 0.114 Uiso 1 1 calc R U . . .
C99A C 0.4687(8) 0.1656(6) 0.6046(4) 0.1070(18) Uani 1 1 d . . . . .
H99C H 0.506676 0.230883 0.605574 0.128 Uiso 1 1 calc R U . . .
H99D H 0.540972 0.142895 0.623838 0.128 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C30 1.795(2) . ?
Fe1 C31 1.803(2) . ?
Fe1 C32 1.804(2) . ?
Fe1 C3 2.0503(17) . ?
Fe1 C2 2.0847(17) . ?
Fe1 C4 2.2039(17) . ?
Fe1 C5 2.2255(18) . ?
Fe1 C1 2.4418(18) . ?
F7 C19 1.334(3) . ?
F8 C19 1.325(4) . ?
F9 C19 1.328(4) . ?
O1 C1 1.229(2) . ?
O2 C30 1.142(3) . ?
O3 C31 1.143(3) . ?
O4 C32 1.145(2) . ?
N1 C4 1.385(2) . ?
N1 C20 1.468(2) . ?
N1 C24 1.478(2) . ?
N2 C5 1.389(2) . ?
N2 C25 1.474(2) . ?
N2 C29 1.478(3) . ?
C1 C2 1.478(3) . ?
C1 C5 1.503(2) . ?
C2 C3 1.452(2) . ?
C2 C6 1.479(2) . ?
C3 C4 1.445(2) . ?
C3 C13 1.487(2) . ?
C4 C5 1.452(2) . ?
C6 C7 1.400(3) . ?
C6 C11 1.407(3) . ?
C7 C8 1.393(3) . ?
C8 C9 1.386(3) . ?
C9 C10 1.400(3) . ?
C9 C12 1.497(3) . ?
C10 C11 1.389(3) . ?
C12 F4 1.272(9) . ?
C12 F5 1.298(10) . ?
C12 F2 1.322(3) . ?
C12 F3 1.329(3) . ?
C12 F6 1.349(9) . ?
C12 F1 1.351(3) . ?
C13 C14 1.397(3) . ?
C13 C18 1.403(3) . ?
C14 C15 1.396(3) . ?
C15 C16 1.386(3) . ?
C16 C17 1.389(3) . ?
C16 C19 1.501(3) . ?
C17 C18 1.396(3) . ?
C20 C21 1.526(3) . ?
C21 C22 1.528(3) . ?
C22 C23 1.531(4) . ?
C23 C24 1.526(3) . ?
C25 C26 1.521(3) . ?
C26 C27 1.526(3) . ?
C27 C28 1.534(3) . ?
C28 C29 1.516(3) . ?
Fe1A C30A 1.798(2) . ?
Fe1A C31A 1.803(2) . ?
Fe1A C32A 1.805(2) . ?
Fe1A C3A 2.0591(17) . ?
Fe1A C2A 2.0819(18) . ?
Fe1A C4A 2.2051(18) . ?
Fe1A C5A 2.2201(18) . ?
Fe1A C1A 2.448(2) . ?
F7A C19A 1.338(4) . ?
F8A C19A 1.340(4) . ?
F9A C19A 1.344(5) . ?
O1A C1A 1.235(2) . ?
O2A C30A 1.141(3) . ?
O3A C31A 1.144(3) . ?
O4A C32A 1.143(3) . ?
N1A C4A 1.380(2) . ?
N1A C20A 1.463(3) . ?
N1A C24A 1.473(3) . ?
N2A C5A 1.392(2) . ?
N2A C25A 1.478(3) . ?
N2A C29A 1.479(3) . ?
C1A C2A 1.477(3) . ?
C1A C5A 1.502(3) . ?
C2A C3A 1.453(3) . ?
C2A C6A 1.477(3) . ?
C3A C4A 1.448(2) . ?
C3A C13A 1.490(2) . ?
C4A C5A 1.453(3) . ?
C6A C7A 1.402(3) . ?
C6A C11A 1.404(3) . ?
C7A C8A 1.393(3) . ?
C8A C9A 1.382(3) . ?
C9A C10A 1.396(3) . ?
C9A C12A 1.502(3) . ?
C10A C11A 1.394(3) . ?
C12A F3A 1.250(5) . ?
C12A F5A 1.264(5) . ?
C12A F4A 1.299(5) . ?
C12A F2A 1.352(4) . ?
C12A F6A 1.387(5) . ?
C12A F1A 1.391(6) . ?
C13A C14A 1.394(3) . ?
C13A C18A 1.399(3) . ?
C14A C15A 1.394(3) . ?
C15A C16A 1.384(4) . ?
C16A C17A 1.390(3) . ?
C16A C19A 1.501(3) . ?
C17A C18A 1.392(3) . ?
C20A C21A 1.531(3) . ?
C21A C22A 1.522(4) . ?
C22A C23A 1.527(4) . ?
C23A C24A 1.528(3) . ?
C25A C26A 1.521(3) . ?
C26A C27A 1.529(3) . ?
C27A C28A 1.530(3) . ?
C28A C29A 1.529(3) . ?
C94 C99 1.526(5) . ?
C94 C95 1.534(7) . ?
C95 C96 1.519(8) . ?
C96 C97 1.508(7) . ?
C97 C98 1.522(8) . ?
C98 C99 1.515(6) . ?
C94A C95A 1.374(9) . ?
C94A C99A 1.495(11) . ?
C95A C96A 1.472(8) . ?
C96A C97A 1.459(8) . ?
C97A C98A 1.444(9) . ?
C98A C99A 1.630(11) . ?

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
C30 Fe1 C31 93.12(9) . . ?
C30 Fe1 C32 94.15(10) . . ?
C31 Fe1 C32 98.33(9) . . ?
C30 Fe1 C3 100.17(8) . . ?
C31 Fe1 C3 146.79(8) . . ?
C32 Fe1 C3 110.77(8) . . ?
C30 Fe1 C2 95.14(9) . . ?
C31 Fe1 C2 107.85(8) . . ?
C32 Fe1 C2 151.63(8) . . ?
C3 Fe1 C2 41.09(7) . . ?
C30 Fe1 C4 136.25(8) . . ?
C31 Fe1 C4 129.57(8) . . ?
C32 Fe1 C4 89.12(8) . . ?
C3 Fe1 C4 39.52(6) . . ?
C2 Fe1 C4 65.92(7) . . ?
C30 Fe1 C5 161.01(9) . . ?
C31 Fe1 C5 91.98(8) . . ?
C32 Fe1 C5 103.20(8) . . ?
C3 Fe1 C5 66.61(6) . . ?
C2 Fe1 C5 65.89(7) . . ?
C4 Fe1 C5 38.27(6) . . ?
C30 Fe1 C1 125.39(9) . . ?
C31 Fe1 C1 84.11(8) . . ?
C32 Fe1 C1 140.33(8) . . ?
C3 Fe1 C1 63.36(6) . . ?
C2 Fe1 C1 37.07(6) . . ?
C4 Fe1 C1 61.09(6) . . ?
C5 Fe1 C1 37.22(6) . . ?
C4 N1 C20 120.85(15) . . ?
C4 N1 C24 116.53(15) . . ?
C20 N1 C24 113.92(15) . . ?
C5 N2 C25 115.52(15) . . ?
C5 N2 C29 116.74(15) . . ?
C25 N2 C29 109.86(15) . . ?
O1 C1 C2 126.65(17) . . ?
O1 C1 C5 129.40(17) . . ?
C2 C1 C5 103.84(14) . . ?
O1 C1 Fe1 139.02(15) . . ?
C2 C1 Fe1 58.22(9) . . ?
C5 C1 Fe1 63.56(9) . . ?
C3 C2 C1 108.81(15) . . ?
C3 C2 C6 128.34(15) . . ?
C1 C2 C6 120.27(15) . . ?
C3 C2 Fe1 68.18(9) . . ?
C1 C2 Fe1 84.70(10) . . ?
C6 C2 Fe1 128.41(13) . . ?
C4 C3 C2 107.43(14) . . ?
C4 C3 C13 124.80(15) . . ?
C2 C3 C13 125.55(15) . . ?
C4 C3 Fe1 75.98(10) . . ?
C2 C3 Fe1 70.72(10) . . ?
C13 C3 Fe1 132.17(12) . . ?
N1 C4 C3 127.52(16) . . ?
N1 C4 C5 123.90(15) . . ?
C3 C4 C5 108.57(15) . . ?
N1 C4 Fe1 129.05(12) . . ?
C3 C4 Fe1 64.50(9) . . ?
C5 C4 Fe1 71.68(10) . . ?
N2 C5 C4 126.38(16) . . ?
N2 C5 C1 125.66(15) . . ?
C4 C5 C1 106.61(14) . . ?
N2 C5 Fe1 126.44(12) . . ?
C4 C5 Fe1 70.06(9) . . ?
C1 C5 Fe1 79.23(10) . . ?
C7 C6 C11 118.38(17) . . ?
C7 C6 C2 121.66(16) . . ?
C11 C6 C2 119.81(16) . . ?
C8 C7 C6 120.70(17) . . ?
C9 C8 C7 120.16(18) . . ?
C8 C9 C10 120.21(17) . . ?
C8 C9 C12 120.19(18) . . ?
C10 C9 C12 119.60(18) . . ?
C11 C10 C9 119.45(18) . . ?
C10 C11 C6 121.10(18) . . ?
F4 C12 F5 113.8(7) . . ?
F2 C12 F3 107.1(3) . . ?
F4 C12 F6 105.8(7) . . ?
F5 C12 F6 103.1(7) . . ?
F2 C12 F1 104.3(2) . . ?
F3 C12 F1 105.6(3) . . ?
F4 C12 C9 110.7(4) . . ?
F5 C12 C9 113.2(5) . . ?
F2 C12 C9 113.3(2) . . ?
F3 C12 C9 113.87(19) . . ?
F6 C12 C9 109.6(4) . . ?
F1 C12 C9 111.9(2) . . ?
C14 C13 C18 119.01(16) . . ?
C14 C13 C3 122.69(16) . . ?
C18 C13 C3 118.29(15) . . ?
C15 C14 C13 120.57(18) . . ?
C16 C15 C14 119.77(19) . . ?
C15 C16 C17 120.51(18) . . ?
C15 C16 C19 118.3(2) . . ?
C17 C16 C19 121.2(2) . . ?
C16 C17 C18 119.88(18) . . ?
C17 C18 C13 120.25(17) . . ?
F8 C19 F9 106.8(3) . . ?
F8 C19 F7 105.8(3) . . ?
F9 C19 F7 106.4(3) . . ?
F8 C19 C16 112.2(2) . . ?
F9 C19 C16 112.3(2) . . ?
F7 C19 C16 112.9(2) . . ?
N1 C20 C21 109.44(17) . . ?
C20 C21 C22 110.62(18) . . ?
C21 C22 C23 110.22(18) . . ?
C24 C23 C22 111.2(2) . . ?
N1 C24 C23 110.64(17) . . ?
N2 C25 C26 111.60(17) . . ?
C25 C26 C27 110.51(19) . . ?
C26 C27 C28 109.20(17) . . ?
C29 C28 C27 111.71(18) . . ?
N2 C29 C28 111.47(17) . . ?
O2 C30 Fe1 176.9(2) . . ?
O3 C31 Fe1 176.46(19) . . ?
O4 C32 Fe1 179.5(2) . . ?
C30A Fe1A C31A 93.24(11) . . ?
C30A Fe1A C32A 91.81(11) . . ?
C31A Fe1A C32A 98.68(10) . . ?
C30A Fe1A C3A 101.34(9) . . ?
C31A Fe1A C3A 145.51(9) . . ?
C32A Fe1A C3A 111.76(8) . . ?
C30A Fe1A C2A 98.34(10) . . ?
C31A Fe1A C2A 106.25(9) . . ?
C32A Fe1A C2A 152.38(8) . . ?
C3A Fe1A C2A 41.09(7) . . ?
C30A Fe1A C4A 135.94(9) . . ?
C31A Fe1A C4A 130.19(9) . . ?
C32A Fe1A C4A 88.78(8) . . ?
C3A Fe1A C4A 39.53(7) . . ?
C2A Fe1A C4A 66.13(7) . . ?
C30A Fe1A C5A 164.30(9) . . ?
C31A Fe1A C5A 92.31(9) . . ?
C32A Fe1A C5A 101.85(8) . . ?
C3A Fe1A C5A 66.53(7) . . ?
C2A Fe1A C5A 65.99(7) . . ?
C4A Fe1A C5A 38.34(7) . . ?
C30A Fe1A C1A 129.25(10) . . ?
C31A Fe1A C1A 83.57(9) . . ?
C32A Fe1A C1A 138.84(8) . . ?
C3A Fe1A C1A 62.97(7) . . ?
C2A Fe1A C1A 36.96(7) . . ?
C4A Fe1A C1A 60.97(7) . . ?
C5A Fe1A C1A 37.14(6) . . ?
C4A N1A C20A 121.11(16) . . ?
C4A N1A C24A 117.38(17) . . ?
C20A N1A C24A 114.34(17) . . ?
C5A N2A C25A 114.57(15) . . ?
C5A N2A C29A 116.16(16) . . ?
C25A N2A C29A 110.06(15) . . ?
O1A C1A C2A 126.29(18) . . ?
O1A C1A C5A 129.71(17) . . ?
C2A C1A C5A 103.85(15) . . ?
O1A C1A Fe1A 139.31(16) . . ?
C2A C1A Fe1A 57.92(10) . . ?
C5A C1A Fe1A 63.16(10) . . ?
C3A C2A C6A 128.06(16) . . ?
C3A C2A C1A 108.43(15) . . ?
C6A C2A C1A 120.10(17) . . ?
C3A C2A Fe1A 68.62(10) . . ?
C6A C2A Fe1A 129.62(14) . . ?
C1A C2A Fe1A 85.12(11) . . ?
C4A C3A C2A 107.57(15) . . ?
C4A C3A C13A 126.35(16) . . ?
C2A C3A C13A 123.94(16) . . ?
C4A C3A Fe1A 75.68(10) . . ?
C2A C3A Fe1A 70.29(10) . . ?
C13A C3A Fe1A 132.51(13) . . ?
N1A C4A C3A 127.50(17) . . ?
N1A C4A C5A 124.26(16) . . ?
C3A C4A C5A 108.24(15) . . ?
N1A C4A Fe1A 128.61(13) . . ?
C3A C4A Fe1A 64.80(10) . . ?
C5A C4A Fe1A 71.39(10) . . ?
N2A C5A C4A 126.27(16) . . ?
N2A C5A C1A 125.64(16) . . ?
C4A C5A C1A 106.59(15) . . ?
N2A C5A Fe1A 126.37(13) . . ?
C4A C5A Fe1A 70.27(10) . . ?
C1A C5A Fe1A 79.70(11) . . ?
C7A C6A C11A 118.28(17) . . ?
C7A C6A C2A 121.82(17) . . ?
C11A C6A C2A 119.73(17) . . ?
C8A C7A C6A 120.73(18) . . ?
C9A C8A C7A 120.19(18) . . ?
C8A C9A C10A 120.30(19) . . ?
C8A C9A C12A 119.37(19) . . ?
C10A C9A C12A 120.3(2) . . ?
C11A C10A C9A 119.4(2) . . ?
C10A C11A C6A 121.05(19) . . ?
F5A C12A F4A 111.5(5) . . ?
F3A C12A F2A 111.7(4) . . ?
F5A C12A F6A 106.5(4) . . ?
F4A C12A F6A 100.9(4) . . ?
F3A C12A F1A 106.7(4) . . ?
F2A C12A F1A 97.6(4) . . ?
F3A C12A C9A 116.3(3) . . ?
F5A C12A C9A 114.6(3) . . ?
F4A C12A C9A 111.9(3) . . ?
F2A C12A C9A 111.9(3) . . ?
F6A C12A C9A 110.3(3) . . ?
F1A C12A C9A 110.9(3) . . ?
C14A C13A C18A 118.70(18) . . ?
C14A C13A C3A 122.41(18) . . ?
C18A C13A C3A 118.56(17) . . ?
C13A C14A C15A 120.9(2) . . ?
C16A C15A C14A 119.7(2) . . ?
C15A C16A C17A 120.3(2) . . ?
C15A C16A C19A 118.6(2) . . ?
C17A C16A C19A 121.2(2) . . ?
C16A C17A C18A 119.9(2) . . ?
C17A C18A C13A 120.56(19) . . ?
F7A C19A F8A 106.8(3) . . ?
F7A C19A F9A 107.4(3) . . ?
F8A C19A F9A 105.4(3) . . ?
F7A C19A C16A 113.0(3) . . ?
F8A C19A C16A 111.6(3) . . ?
F9A C19A C16A 112.2(3) . . ?
N1A C20A C21A 109.53(18) . . ?
C22A C21A C20A 110.7(2) . . ?
C21A C22A C23A 110.1(2) . . ?
C22A C23A C24A 111.9(2) . . ?
N1A C24A C23A 110.80(19) . . ?
N2A C25A C26A 111.78(17) . . ?
C25A C26A C27A 110.10(18) . . ?
C26A C27A C28A 108.86(18) . . ?
C29A C28A C27A 111.78(18) . . ?
N2A C29A C28A 111.42(18) . . ?
O2A C30A Fe1A 176.1(2) . . ?
O3A C31A Fe1A 177.3(2) . . ?
O4A C32A Fe1A 178.7(2) . . ?
C99 C94 C95 110.2(4) . . ?
C96 C95 C94 112.9(4) . . ?
C97 C96 C95 110.8(5) . . ?
C96 C97 C98 110.5(5) . . ?
C99 C98 C97 112.8(4) . . ?
C98 C99 C94 111.1(4) . . ?
C95A C94A C99A 115.0(7) . . ?
C94A C95A C96A 115.4(6) . . ?
C97A C96A C95A 113.5(5) . . ?
C98A C97A C96A 116.2(6) . . ?
C97A C98A C99A 109.9(6) . . ?
C94A C99A C98A 114.3(6) . . ?

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
O1 C1 C2 C3 164.96(19) . . . . ?
C5 C1 C2 C3 -18.59(19) . . . . ?
Fe1 C1 C2 C3 -64.79(11) . . . . ?
O1 C1 C2 C6 1.7(3) . . . . ?
C5 C1 C2 C6 178.15(15) . . . . ?
Fe1 C1 C2 C6 131.94(17) . . . . ?
O1 C1 C2 Fe1 -130.2(2) . . . . ?
C5 C1 C2 Fe1 46.20(12) . . . . ?
C1 C2 C3 C4 8.29(19) . . . . ?
C6 C2 C3 C4 169.80(17) . . . . ?
Fe1 C2 C3 C4 -67.74(12) . . . . ?
C1 C2 C3 C13 -155.35(16) . . . . ?
C6 C2 C3 C13 6.2(3) . . . . ?
Fe1 C2 C3 C13 128.62(17) . . . . ?
C1 C2 C3 Fe1 76.03(12) . . . . ?
C6 C2 C3 Fe1 -122.46(18) . . . . ?
C20 N1 C4 C3 -19.7(3) . . . . ?
C24 N1 C4 C3 126.05(19) . . . . ?
C20 N1 C4 C5 159.29(17) . . . . ?
C24 N1 C4 C5 -55.0(2) . . . . ?
C20 N1 C4 Fe1 66.0(2) . . . . ?
C24 N1 C4 Fe1 -148.30(14) . . . . ?
C2 C3 C4 N1 -174.87(17) . . . . ?
C13 C3 C4 N1 -11.1(3) . . . . ?
Fe1 C3 C4 N1 120.92(18) . . . . ?
C2 C3 C4 C5 6.06(19) . . . . ?
C13 C3 C4 C5 169.85(16) . . . . ?
Fe1 C3 C4 C5 -58.16(12) . . . . ?
C2 C3 C4 Fe1 64.21(11) . . . . ?
C13 C3 C4 Fe1 -131.99(17) . . . . ?
C25 N2 C5 C4 -46.2(2) . . . . ?
C29 N2 C5 C4 -177.65(17) . . . . ?
C25 N2 C5 C1 148.90(18) . . . . ?
C29 N2 C5 C1 17.5(3) . . . . ?
C25 N2 C5 Fe1 44.8(2) . . . . ?
C29 N2 C5 Fe1 -86.65(19) . . . . ?
N1 C4 C5 N2 -4.1(3) . . . . ?
C3 C4 C5 N2 175.04(16) . . . . ?
Fe1 C4 C5 N2 121.16(18) . . . . ?
N1 C4 C5 C1 163.16(16) . . . . ?
C3 C4 C5 C1 -17.72(19) . . . . ?
Fe1 C4 C5 C1 -71.60(12) . . . . ?
N1 C4 C5 Fe1 -125.24(17) . . . . ?
C3 C4 C5 Fe1 53.87(11) . . . . ?
O1 C1 C5 N2 5.6(3) . . . . ?
C2 C1 C5 N2 -170.68(17) . . . . ?
Fe1 C1 C5 N2 -127.41(18) . . . . ?
O1 C1 C5 C4 -161.7(2) . . . . ?
C2 C1 C5 C4 21.97(18) . . . . ?
Fe1 C1 C5 C4 65.23(11) . . . . ?
O1 C1 C5 Fe1 133.1(2) . . . . ?
C2 C1 C5 Fe1 -43.26(12) . . . . ?
C3 C2 C6 C7 -32.8(3) . . . . ?
C1 C2 C6 C7 126.8(2) . . . . ?
Fe1 C2 C6 C7 -124.12(18) . . . . ?
C3 C2 C6 C11 151.60(19) . . . . ?
C1 C2 C6 C11 -48.7(3) . . . . ?
Fe1 C2 C6 C11 60.3(2) . . . . ?
C11 C6 C7 C8 -0.5(3) . . . . ?
C2 C6 C7 C8 -176.08(19) . . . . ?
C6 C7 C8 C9 0.8(3) . . . . ?
C7 C8 C9 C10 -0.8(3) . . . . ?
C7 C8 C9 C12 179.1(2) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C12 C9 C10 C11 -179.5(2) . . . . ?
C9 C10 C11 C6 -0.1(3) . . . . ?
C7 C6 C11 C10 0.1(3) . . . . ?
C2 C6 C11 C10 175.79(19) . . . . ?
C8 C9 C12 F4 -48.0(6) . . . . ?
C10 C9 C12 F4 131.9(6) . . . . ?
C8 C9 C12 F5 -177.2(6) . . . . ?
C10 C9 C12 F5 2.7(7) . . . . ?
C8 C9 C12 F2 124.8(3) . . . . ?
C10 C9 C12 F2 -55.3(3) . . . . ?
C8 C9 C12 F3 2.0(3) . . . . ?
C10 C9 C12 F3 -178.0(3) . . . . ?
C8 C9 C12 F6 68.3(6) . . . . ?
C10 C9 C12 F6 -111.7(6) . . . . ?
C8 C9 C12 F1 -117.6(3) . . . . ?
C10 C9 C12 F1 62.4(3) . . . . ?
C4 C3 C13 C14 115.9(2) . . . . ?
C2 C3 C13 C14 -83.2(2) . . . . ?
Fe1 C3 C13 C14 12.5(3) . . . . ?
C4 C3 C13 C18 -64.8(2) . . . . ?
C2 C3 C13 C18 96.1(2) . . . . ?
Fe1 C3 C13 C18 -168.20(14) . . . . ?
C18 C13 C14 C15 -0.3(3) . . . . ?
C3 C13 C14 C15 179.0(2) . . . . ?
C13 C14 C15 C16 -0.4(4) . . . . ?
C14 C15 C16 C17 0.6(4) . . . . ?
C14 C15 C16 C19 178.9(2) . . . . ?
C15 C16 C17 C18 0.0(4) . . . . ?
C19 C16 C17 C18 -178.2(2) . . . . ?
C16 C17 C18 C13 -0.8(3) . . . . ?
C14 C13 C18 C17 0.9(3) . . . . ?
C3 C13 C18 C17 -178.39(18) . . . . ?
C15 C16 C19 F8 64.3(4) . . . . ?
C17 C16 C19 F8 -117.4(3) . . . . ?
C15 C16 C19 F9 -56.0(4) . . . . ?
C17 C16 C19 F9 122.3(3) . . . . ?
C15 C16 C19 F7 -176.2(3) . . . . ?
C17 C16 C19 F7 2.1(4) . . . . ?
C4 N1 C20 C21 -154.95(17) . . . . ?
C24 N1 C20 C21 58.5(2) . . . . ?
N1 C20 C21 C22 -57.5(2) . . . . ?
C20 C21 C22 C23 56.2(3) . . . . ?
C21 C22 C23 C24 -53.9(3) . . . . ?
C4 N1 C24 C23 155.33(18) . . . . ?
C20 N1 C24 C23 -56.6(2) . . . . ?
C22 C23 C24 N1 53.2(3) . . . . ?
C5 N2 C25 C26 165.56(17) . . . . ?
C29 N2 C25 C26 -59.8(2) . . . . ?
N2 C25 C26 C27 58.6(2) . . . . ?
C25 C26 C27 C28 -54.1(3) . . . . ?
C26 C27 C28 C29 53.4(3) . . . . ?
C5 N2 C29 C28 -167.63(17) . . . . ?
C25 N2 C29 C28 58.4(2) . . . . ?
C27 C28 C29 N2 -56.2(2) . . . . ?
O1A C1A C2A C3A 163.9(2) . . . . ?
C5A C1A C2A C3A -20.23(19) . . . . ?
Fe1A C1A C2A C3A -65.53(12) . . . . ?
O1A C1A C2A C6A 3.1(3) . . . . ?
C5A C1A C2A C6A 178.96(16) . . . . ?
Fe1A C1A C2A C6A 133.66(18) . . . . ?
O1A C1A C2A Fe1A -130.5(2) . . . . ?
C5A C1A C2A Fe1A 45.31(13) . . . . ?
C6A C2A C3A C4A 168.62(18) . . . . ?
C1A C2A C3A C4A 9.8(2) . . . . ?
Fe1A C2A C3A C4A -67.10(12) . . . . ?
C6A C2A C3A C13A 4.3(3) . . . . ?
C1A C2A C3A C13A -154.49(17) . . . . ?
Fe1A C2A C3A C13A 128.62(18) . . . . ?
C6A C2A C3A Fe1A -124.3(2) . . . . ?
C1A C2A C3A Fe1A 76.89(13) . . . . ?
C20A N1A C4A C3A -20.9(3) . . . . ?
C24A N1A C4A C3A 127.8(2) . . . . ?
C20A N1A C4A C5A 157.70(19) . . . . ?
C24A N1A C4A C5A -53.6(3) . . . . ?
C20A N1A C4A Fe1A 64.8(2) . . . . ?
C24A N1A C4A Fe1A -146.45(15) . . . . ?
C2A C3A C4A N1A -175.94(18) . . . . ?
C13A C3A C4A N1A -12.1(3) . . . . ?
Fe1A C3A C4A N1A 120.54(19) . . . . ?
C2A C3A C4A C5A 5.3(2) . . . . ?
C13A C3A C4A C5A 169.08(17) . . . . ?
Fe1A C3A C4A C5A -58.24(13) . . . . ?
C2A C3A C4A Fe1A 63.52(12) . . . . ?
C13A C3A C4A Fe1A -132.69(19) . . . . ?
C25A N2A C5A C4A -48.6(3) . . . . ?
C29A N2A C5A C4A -178.72(18) . . . . ?
C25A N2A C5A C1A 147.33(18) . . . . ?
C29A N2A C5A C1A 17.2(3) . . . . ?
C25A N2A C5A Fe1A 42.6(2) . . . . ?
C29A N2A C5A Fe1A -87.6(2) . . . . ?
N1A C4A C5A N2A -3.4(3) . . . . ?
C3A C4A C5A N2A 175.47(17) . . . . ?
Fe1A C4A C5A N2A 121.21(18) . . . . ?
N1A C4A C5A C1A 163.20(18) . . . . ?
C3A C4A C5A C1A -18.0(2) . . . . ?
Fe1A C4A C5A C1A -72.24(13) . . . . ?
N1A C4A C5A Fe1A -124.57(18) . . . . ?
C3A C4A C5A Fe1A 54.26(12) . . . . ?
O1A C1A C5A N2A 5.5(3) . . . . ?
C2A C1A C5A N2A -170.14(17) . . . . ?
Fe1A C1A C5A N2A -127.68(19) . . . . ?
O1A C1A C5A C4A -161.2(2) . . . . ?
C2A C1A C5A C4A 23.20(19) . . . . ?
Fe1A C1A C5A C4A 65.66(12) . . . . ?
O1A C1A C5A Fe1A 133.2(2) . . . . ?
C2A C1A C5A Fe1A -42.46(12) . . . . ?
C3A C2A C6A C7A -35.1(3) . . . . ?
C1A C2A C6A C7A 121.6(2) . . . . ?
Fe1A C2A C6A C7A -127.79(19) . . . . ?
C3A C2A C6A C11A 149.7(2) . . . . ?
C1A C2A C6A C11A -53.6(3) . . . . ?
Fe1A C2A C6A C11A 57.0(3) . . . . ?
C11A C6A C7A C8A -1.1(3) . . . . ?
C2A C6A C7A C8A -176.4(2) . . . . ?
C6A C7A C8A C9A 0.3(4) . . . . ?
C7A C8A C9A C10A 1.4(4) . . . . ?
C7A C8A C9A C12A 179.1(2) . . . . ?
C8A C9A C10A C11A -2.2(4) . . . . ?
C12A C9A C10A C11A -179.9(3) . . . . ?
C9A C10A C11A C6A 1.4(4) . . . . ?
C7A C6A C11A C10A 0.2(4) . . . . ?
C2A C6A C11A C10A 175.6(2) . . . . ?
C8A C9A C12A F3A 15.7(5) . . . . ?
C10A C9A C12A F3A -166.5(5) . . . . ?
C8A C9A C12A F5A -175.2(4) . . . . ?
C10A C9A C12A F5A 2.5(5) . . . . ?
C8A C9A C12A F4A -47.0(5) . . . . ?
C10A C9A C12A F4A 130.8(4) . . . . ?
C8A C9A C12A F2A 145.7(3) . . . . ?
C10A C9A C12A F2A -36.5(4) . . . . ?
C8A C9A C12A F6A 64.6(4) . . . . ?
C10A C9A C12A F6A -117.7(4) . . . . ?
C8A C9A C12A F1A -106.4(4) . . . . ?
C10A C9A C12A F1A 71.3(4) . . . . ?
C4A C3A C13A C14A 129.6(2) . . . . ?
C2A C3A C13A C14A -69.1(3) . . . . ?
Fe1A C3A C13A C14A 24.7(3) . . . . ?
C4A C3A C13A C18A -57.0(3) . . . . ?
C2A C3A C13A C18A 104.3(2) . . . . ?
Fe1A C3A C13A C18A -161.98(15) . . . . ?
C18A C13A C14A C15A 0.3(4) . . . . ?
C3A C13A C14A C15A 173.6(3) . . . . ?
C13A C14A C15A C16A 0.4(5) . . . . ?
C14A C15A C16A C17A -0.7(5) . . . . ?
C14A C15A C16A C19A 178.9(3) . . . . ?
C15A C16A C17A C18A 0.4(4) . . . . ?
C19A C16A C17A C18A -179.2(3) . . . . ?
C16A C17A C18A C13A 0.2(3) . . . . ?
C14A C13A C18A C17A -0.6(3) . . . . ?
C3A C13A C18A C17A -174.18(19) . . . . ?
C15A C16A C19A F7A 165.0(3) . . . . ?
C17A C16A C19A F7A -15.3(5) . . . . ?
C15A C16A C19A F8A 44.6(4) . . . . ?
C17A C16A C19A F8A -135.7(3) . . . . ?
C15A C16A C19A F9A -73.4(4) . . . . ?
C17A C16A C19A F9A 106.3(3) . . . . ?
C4A N1A C20A C21A -152.40(19) . . . . ?
C24A N1A C20A C21A 58.0(2) . . . . ?
N1A C20A C21A C22A -57.6(3) . . . . ?
C20A C21A C22A C23A 56.0(3) . . . . ?
C21A C22A C23A C24A -53.3(3) . . . . ?
C4A N1A C24A C23A 153.91(19) . . . . ?
C20A N1A C24A C23A -55.3(3) . . . . ?
C22A C23A C24A N1A 51.9(3) . . . . ?
C5A N2A C25A C26A 167.48(17) . . . . ?
C29A N2A C25A C26A -59.4(2) . . . . ?
N2A C25A C26A C27A 59.3(2) . . . . ?
C25A C26A C27A C28A -55.5(3) . . . . ?
C26A C27A C28A C29A 54.4(3) . . . . ?
C5A N2A C29A C28A -170.68(17) . . . . ?
C25A N2A C29A C28A 57.1(2) . . . . ?
C27A C28A C29A N2A -55.9(3) . . . . ?
C99 C94 C95 C96 54.2(5) . . . . ?
C94 C95 C96 C97 -55.7(6) . . . . ?
C95 C96 C97 C98 55.2(6) . . . . ?
C96 C97 C98 C99 -56.2(6) . . . . ?
C97 C98 C99 C94 55.4(5) . . . . ?
C95 C94 C99 C98 -53.0(5) . . . . ?
C99A C94A C95A C96A 48.3(9) . . . . ?
C94A C95A C96A C97A -52.6(8) . . . . ?
C95A C96A C97A C98A 52.0(8) . . . . ?
C96A C97A C98A C99A -44.5(9) . . . . ?
C95A C94A C99A C98A -41.6(10) . . . . ?
C97A C98A C99A C94A 38.8(10) . . . . ?

_refine_diff_density_max         2.068
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.138


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk42db
_database_code_depnum_ccdc_archive 'CCDC 2338298'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H31 F6 Fe N3 O3 [0.5 (C2 H3 N1)]'
_chemical_formula_sum            'C34 H32.50 F6 Fe N3.50 O3'
_chemical_formula_weight         707.98

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'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7552(4)
_cell_length_b                   11.5325(3)
_cell_length_c                   14.6781(6)
_cell_angle_alpha                106.515(3)
_cell_angle_beta                 110.781(4)
_cell_angle_gamma                94.220(3)
_cell_volume                     1600.72(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31930
_cell_measurement_theta_min      3.3540
_cell_measurement_theta_max      78.3480

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             730
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    4.446
_shelx_estimated_absorpt_T_min   0.470
_shelx_estimated_absorpt_T_max   0.776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -2 2 0.0554
1 -7 3 0.0877
7 1 -1 0.0779
1 7 -3 0.0637
0 1 8 0.0343
-1 -1 -7 0.0255
1 -1 -8 0.0332
-7 -1 4 0.0674
-1 -5 -3 0.0528
2 -5 -4 0.0821
0 2 -9 0.0403
1 -2 9 0.0553
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
-6.4191 -1.6544 1.7315 -0.0208 0.1100 0.9937
0.6140 -7.4678 3.2212 -0.1822 0.9802 0.0776
6.5454 1.0765 -1.4944 0.0065 -0.0328 -0.9994
0.8275 7.3476 -3.3917 0.1750 -0.9410 -0.2896
0.2200 0.7022 7.9643 -0.9301 -0.1731 -0.3239
-1.0723 -0.7762 -7.3824 0.8834 0.1645 0.4388
0.5249 -0.6289 -8.3708 0.9591 0.1784 0.2199
-6.8730 -0.6147 4.4792 -0.3518 -0.0648 0.9338
-1.3047 -5.0220 -3.2356 0.5281 0.6894 0.4958
1.7011 -5.3592 -4.3883 0.6062 0.7909 0.0834
0.3836 2.4497 -9.0802 0.9614 -0.2304 0.1502
0.5338 -2.2629 8.6174 -0.9326 0.2236 -0.2832
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_T_max  1.000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.574
_oxdiff_exptl_absorpt_empirical_full_max 1.782
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            6848
_diffrn_reflns_av_unetI/netI     0.0042
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.415
_diffrn_reflns_theta_max         80.574
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6848
_reflns_number_gt                6677
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Refined as a 2-component twin. Component 2 rotated by 0.8956°
 around [0.28 -0.94 0.21] (reciprocal) or [0.25 -0.97 -0.01] (direct).

 One CF3 group was refined with a 3-component disorder model. Chemically
 equivalent C-F and F-F distances were restrained to be equal.

 0.5 molecules of acetonitrile per Asymmetric unit have been identified
 but could not be refined satisfactorily. Therefore, a solvent mask, the Olex2
 implementation of the program SQUEEZE (Spek, A. L. (2015). Acta Cryst.
 C71, 9-18.) has been used to mathematically remove the electron density of
 these molecules. 21 electrons were found in a volume of 129Å³ in 1 void
 per unit cell. This is consistent with the presence of 0.5[C2H3N] per
 Asymmetric Unit which account for 22 electrons per unit cell. The sum
 formula and derived parameters are based on 0.5 molecules of C2H3N per
 Asymmetric unit.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 128.7 20.0 '1 MeCN'

_smtbx_masks_special_details     
;
 0.5 molecules of acetonitrile per Asymmetric unit have been identified
 but could not be refined satisfactorily. Therefore, a solvent mask, the Olex2
 implementation of the program SQUEEZE (Spek, A. L. (2015). Acta Cryst.
 C71, 9-18.) has been used to mathematically remove the electron density of
 these molecules. 21 electrons were found in a volume of 129Å³ in 1 void
 per unit cell. This is consistent with the presence of 0.5[C2H3N] per
 Asymmetric Unit which account for 22 electrons per unit cell. The sum
 formula and derived parameters are based on 0.5 molecules of C2H3N per
 Asymmetric unit.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1010P)²+2.0608P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6848
_refine_ls_number_parameters     474
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1675
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.42780(4) 0.36758(3) 0.15287(3) 0.02468(14) Uani 1 1 d . . . . .
F1 F -0.0705(2) 0.0272(2) 0.34347(19) 0.0586(6) Uani 1 1 d . . . . .
F2 F -0.0779(3) -0.0851(2) 0.1984(3) 0.0770(9) Uani 1 1 d . . . . .
F3 F -0.20393(19) 0.0509(2) 0.20562(19) 0.0519(5) Uani 1 1 d . . . . .
O1 O 0.2017(2) 0.5305(2) 0.20934(18) 0.0356(5) Uani 1 1 d . . . . .
O2 O 0.6713(2) 0.3865(2) 0.10798(18) 0.0389(5) Uani 1 1 d . . . . .
O3 O 0.3635(3) 0.0969(2) 0.06602(19) 0.0474(6) Uani 1 1 d . . . . .
N1 N 0.6858(2) 0.5556(2) 0.34431(18) 0.0258(4) Uani 1 1 d . . . . .
N2 N 0.4671(2) 0.6656(2) 0.22400(18) 0.0273(5) Uani 1 1 d . . . . .
N3 N 0.2845(2) 0.3886(2) 0.03561(19) 0.0317(5) Uani 1 1 d . . . . .
C1 C 0.3121(3) 0.4980(2) 0.2392(2) 0.0273(5) Uani 1 1 d . . . . .
C2 C 0.3391(3) 0.3847(2) 0.2627(2) 0.0269(5) Uani 1 1 d . . . . .
C3 C 0.4843(3) 0.3909(2) 0.3052(2) 0.0248(5) Uani 1 1 d . . . . .
C4 C 0.5491(3) 0.5036(2) 0.30251(19) 0.0237(5) Uani 1 1 d . . . . .
C5 C 0.4444(3) 0.5587(2) 0.2473(2) 0.0250(5) Uani 1 1 d . . . . .
C6 C 0.2339(3) 0.2936(3) 0.2618(2) 0.0289(5) Uani 1 1 d . . . . .
C7 C 0.1102(3) 0.3242(3) 0.2600(3) 0.0353(6) Uani 1 1 d . . . . .
H7 H 0.095301 0.404661 0.261199 0.042 Uiso 1 1 calc R U . . .
C8 C 0.0086(3) 0.2400(3) 0.2566(3) 0.0398(7) Uani 1 1 d . . . . .
H8 H -0.075491 0.262392 0.254053 0.048 Uiso 1 1 calc R U . . .
C9 C 0.0298(3) 0.1223(3) 0.2570(2) 0.0351(6) Uani 1 1 d . . . . .
C10 C 0.1527(3) 0.0904(3) 0.2613(2) 0.0346(6) Uani 1 1 d . . . . .
H10 H 0.168125 0.010865 0.262991 0.042 Uiso 1 1 calc R U . . .
C11 C 0.2538(3) 0.1748(3) 0.2633(2) 0.0341(6) Uani 1 1 d . . . . .
H11 H 0.337661 0.151818 0.265738 0.041 Uiso 1 1 calc R U . . .
C12 C -0.0795(3) 0.0299(3) 0.2513(3) 0.0420(7) Uani 1 1 d . . . . .
C13 C 0.5499(3) 0.3132(2) 0.3672(2) 0.0242(5) Uani 1 1 d . . . . .
C14 C 0.6093(3) 0.2166(2) 0.3298(2) 0.0267(5) Uani 1 1 d . . . . .
H14 H 0.612629 0.201460 0.263697 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6633(3) 0.1426(2) 0.3877(2) 0.0291(5) Uani 1 1 d . . . . .
H15 H 0.703918 0.077655 0.361657 0.035 Uiso 1 1 calc R U . . .
C16 C 0.6578(3) 0.1640(3) 0.4836(2) 0.0311(6) Uani 1 1 d . . . . .
C17 C 0.5988(3) 0.2585(3) 0.5223(2) 0.0331(6) Uani 1 1 d . . . . .
H17 H 0.594868 0.272454 0.588141 0.040 Uiso 1 1 calc R U . . .
C18 C 0.5454(3) 0.3329(3) 0.4641(2) 0.0304(6) Uani 1 1 d . . . . .
H18 H 0.505304 0.397984 0.490807 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7169(3) 0.0848(3) 0.5465(3) 0.0392(7) Uani 1 1 d D . . . .
C20 C 0.7878(3) 0.4811(2) 0.3733(2) 0.0276(5) Uani 1 1 d . . . . .
H20A H 0.757731 0.397203 0.321458 0.033 Uiso 1 1 calc R U . . .
H20B H 0.798683 0.473776 0.441140 0.033 Uiso 1 1 calc R U . . .
C21 C 0.9226(3) 0.5407(3) 0.3792(2) 0.0313(6) Uani 1 1 d . . . . .
H21A H 0.991922 0.491896 0.402435 0.038 Uiso 1 1 calc R U . . .
H21B H 0.913289 0.539753 0.309403 0.038 Uiso 1 1 calc R U . . .
C22 C 0.9700(3) 0.6730(3) 0.4530(3) 0.0368(6) Uani 1 1 d . . . . .
H22A H 1.053846 0.710835 0.450404 0.044 Uiso 1 1 calc R U . . .
H22B H 0.990464 0.674079 0.524528 0.044 Uiso 1 1 calc R U . . .
C23 C 0.8589(3) 0.7465(3) 0.4220(3) 0.0376(7) Uani 1 1 d . . . . .
H23A H 0.886577 0.830750 0.473060 0.045 Uiso 1 1 calc R U . . .
H23B H 0.846469 0.753487 0.353728 0.045 Uiso 1 1 calc R U . . .
C24 C 0.7253(3) 0.6839(2) 0.4166(2) 0.0320(6) Uani 1 1 d . . . . .
H24A H 0.735206 0.683773 0.486215 0.038 Uiso 1 1 calc R U . . .
H24B H 0.653589 0.730406 0.392914 0.038 Uiso 1 1 calc R U . . .
C25 C 0.5605(3) 0.6668(2) 0.1713(2) 0.0291(5) Uani 1 1 d . . . . .
H25A H 0.513006 0.615852 0.097524 0.035 Uiso 1 1 calc R U . . .
H25B H 0.638134 0.629794 0.202410 0.035 Uiso 1 1 calc R U . . .
C26 C 0.6128(3) 0.7968(3) 0.1794(2) 0.0332(6) Uani 1 1 d . . . . .
H26A H 0.669720 0.793420 0.138783 0.040 Uiso 1 1 calc R U . . .
H26B H 0.670277 0.844783 0.252442 0.040 Uiso 1 1 calc R U . . .
C27 C 0.4970(3) 0.8617(3) 0.1397(3) 0.0350(6) Uani 1 1 d . . . . .
H27A H 0.533615 0.949069 0.153410 0.042 Uiso 1 1 calc R U . . .
H27B H 0.447530 0.821823 0.064131 0.042 Uiso 1 1 calc R U . . .
C28 C 0.4010(3) 0.8548(3) 0.1936(3) 0.0343(6) Uani 1 1 d . . . . .
H28A H 0.322633 0.891908 0.164273 0.041 Uiso 1 1 calc R U . . .
H28B H 0.448347 0.903070 0.267986 0.041 Uiso 1 1 calc R U . . .
C29 C 0.3503(3) 0.7217(3) 0.1813(2) 0.0315(6) Uani 1 1 d . . . . .
H29A H 0.289315 0.720144 0.218274 0.038 Uiso 1 1 calc R U . . .
H29B H 0.298330 0.673927 0.107282 0.038 Uiso 1 1 calc R U . . .
C30 C 0.5717(3) 0.3790(3) 0.1203(2) 0.0301(6) Uani 1 1 d . . . . .
C31 C 0.3887(3) 0.2023(3) 0.1002(2) 0.0337(6) Uani 1 1 d . . . . .
C32 C 0.1926(3) 0.3996(3) -0.0277(3) 0.0418(7) Uani 1 1 d . . . . .
C33 C 0.0741(4) 0.4122(6) -0.1096(4) 0.0738(14) Uani 1 1 d . . . . .
H33A H 0.079410 0.374512 -0.176608 0.111 Uiso 1 1 calc R U . . .
H33B H 0.071625 0.499784 -0.098135 0.111 Uiso 1 1 calc R U . . .
H33C H -0.008332 0.370684 -0.108987 0.111 Uiso 1 1 calc R U . . .
F4 F 0.8271(6) 0.1522(5) 0.6350(4) 0.0401(13) Uani 0.387(3) 1 d D U P A 1
F5 F 0.7541(8) -0.0092(6) 0.4999(5) 0.0503(14) Uani 0.387(3) 1 d D U P A 1
F6 F 0.6298(5) 0.0446(5) 0.5846(5) 0.0314(10) Uani 0.387(3) 1 d D U P A 1
F4A F 0.8251(6) 0.0429(6) 0.5265(5) 0.0331(13) Uani 0.304(3) 1 d D U P A 2
F5A F 0.6353(8) -0.0058(8) 0.5371(8) 0.066(2) Uani 0.304(3) 1 d D U P A 2
F6A F 0.7823(9) 0.1518(8) 0.6497(5) 0.052(2) Uani 0.304(3) 1 d D U P A 2
F4B F 0.6727(9) 0.0876(8) 0.6203(6) 0.0485(19) Uani 0.309(3) 1 d D U P A 3
F5B F 0.8438(7) 0.0968(9) 0.5806(8) 0.063(2) Uani 0.309(3) 1 d D U P A 3
F6B F 0.6702(8) -0.0400(5) 0.4823(5) 0.0406(14) Uani 0.309(3) 1 d D U P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C30 1.781(3) . ?
Fe1 C31 1.795(3) . ?
Fe1 N3 1.951(2) . ?
Fe1 C3 2.027(3) . ?
Fe1 C2 2.118(3) . ?
Fe1 C4 2.166(3) . ?
Fe1 C5 2.200(3) . ?
Fe1 C1 2.393(3) . ?
F1 C12 1.330(4) . ?
F2 C12 1.338(4) . ?
F3 C12 1.343(4) . ?
O1 C1 1.238(3) . ?
O2 C30 1.149(4) . ?
O3 C31 1.145(4) . ?
N1 C4 1.386(3) . ?
N1 C20 1.461(3) . ?
N1 C24 1.480(3) . ?
N2 C5 1.396(3) . ?
N2 C25 1.471(4) . ?
N2 C29 1.477(3) . ?
N3 C32 1.136(4) . ?
C1 C2 1.467(3) . ?
C1 C5 1.488(4) . ?
C2 C3 1.449(4) . ?
C2 C6 1.480(4) . ?
C3 C4 1.446(3) . ?
C3 C13 1.493(3) . ?
C4 C5 1.442(3) . ?
C6 C7 1.395(4) . ?
C6 C11 1.407(4) . ?
C7 C8 1.384(4) . ?
C8 C9 1.393(4) . ?
C9 C10 1.383(4) . ?
C9 C12 1.491(4) . ?
C10 C11 1.391(4) . ?
C13 C18 1.395(4) . ?
C13 C14 1.399(4) . ?
C14 C15 1.387(4) . ?
C15 C16 1.381(4) . ?
C16 C17 1.386(4) . ?
C16 C19 1.497(4) . ?
C17 C18 1.391(4) . ?
C19 F5B 1.257(7) . ?
C19 F5A 1.257(7) . ?
C19 F5 1.281(6) . ?
C19 F4B 1.322(7) . ?
C19 F6 1.364(5) . ?
C19 F6A 1.372(7) . ?
C19 F4 1.376(6) . ?
C19 F4A 1.384(6) . ?
C19 F6B 1.414(6) . ?
C20 C21 1.521(4) . ?
C21 C22 1.521(4) . ?
C22 C23 1.529(4) . ?
C23 C24 1.525(4) . ?
C25 C26 1.519(4) . ?
C26 C27 1.524(4) . ?
C27 C28 1.516(4) . ?
C28 C29 1.528(4) . ?
C32 C33 1.459(5) . ?

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
C30 Fe1 C31 93.35(13) . . ?
C30 Fe1 N3 102.66(12) . . ?
C31 Fe1 N3 94.12(12) . . ?
C30 Fe1 C3 111.11(12) . . ?
C31 Fe1 C3 100.02(12) . . ?
N3 Fe1 C3 142.29(10) . . ?
C30 Fe1 C2 151.49(12) . . ?
C31 Fe1 C2 96.86(12) . . ?
N3 Fe1 C2 103.06(10) . . ?
C3 Fe1 C2 40.85(10) . . ?
C30 Fe1 C4 88.08(11) . . ?
C31 Fe1 C4 135.74(11) . . ?
N3 Fe1 C4 128.67(10) . . ?
C3 Fe1 C4 40.16(10) . . ?
C2 Fe1 C4 66.18(10) . . ?
C30 Fe1 C5 102.27(11) . . ?
C31 Fe1 C5 162.38(12) . . ?
N3 Fe1 C5 90.39(10) . . ?
C3 Fe1 C5 66.89(10) . . ?
C2 Fe1 C5 65.52(10) . . ?
C4 Fe1 C5 38.55(9) . . ?
C30 Fe1 C1 139.53(11) . . ?
C31 Fe1 C1 127.05(12) . . ?
N3 Fe1 C1 79.18(10) . . ?
C3 Fe1 C1 64.37(10) . . ?
C2 Fe1 C1 37.34(9) . . ?
C4 Fe1 C1 62.45(9) . . ?
C5 Fe1 C1 37.50(9) . . ?
C4 N1 C20 120.3(2) . . ?
C4 N1 C24 116.0(2) . . ?
C20 N1 C24 113.0(2) . . ?
C5 N2 C25 115.9(2) . . ?
C5 N2 C29 118.7(2) . . ?
C25 N2 C29 111.4(2) . . ?
C32 N3 Fe1 173.0(3) . . ?
O1 C1 C2 127.9(2) . . ?
O1 C1 C5 127.2(2) . . ?
C2 C1 C5 104.6(2) . . ?
O1 C1 Fe1 133.7(2) . . ?
C2 C1 Fe1 61.09(14) . . ?
C5 C1 Fe1 64.21(14) . . ?
C3 C2 C1 109.0(2) . . ?
C3 C2 C6 126.6(2) . . ?
C1 C2 C6 123.3(2) . . ?
C3 C2 Fe1 66.22(14) . . ?
C1 C2 Fe1 81.57(16) . . ?
C6 C2 Fe1 127.7(2) . . ?
C4 C3 C2 107.8(2) . . ?
C4 C3 C13 126.8(2) . . ?
C2 C3 C13 123.2(2) . . ?
C4 C3 Fe1 75.10(15) . . ?
C2 C3 Fe1 72.93(15) . . ?
C13 C3 Fe1 131.17(19) . . ?
N1 C4 C5 123.3(2) . . ?
N1 C4 C3 128.8(2) . . ?
C5 C4 C3 107.9(2) . . ?
N1 C4 Fe1 129.28(18) . . ?
C5 C4 Fe1 72.00(15) . . ?
C3 C4 Fe1 64.73(14) . . ?
N2 C5 C4 125.0(2) . . ?
N2 C5 C1 125.8(2) . . ?
C4 C5 C1 108.1(2) . . ?
N2 C5 Fe1 127.27(19) . . ?
C4 C5 Fe1 69.45(14) . . ?
C1 C5 Fe1 78.29(15) . . ?
C7 C6 C11 117.6(3) . . ?
C7 C6 C2 120.2(2) . . ?
C11 C6 C2 122.2(2) . . ?
C8 C7 C6 121.5(3) . . ?
C7 C8 C9 120.0(3) . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 C12 119.7(3) . . ?
C8 C9 C12 120.6(3) . . ?
C9 C10 C11 120.1(3) . . ?
C10 C11 C6 121.1(3) . . ?
F1 C12 F2 105.6(3) . . ?
F1 C12 F3 105.7(3) . . ?
F2 C12 F3 106.8(3) . . ?
F1 C12 C9 113.4(3) . . ?
F2 C12 C9 112.2(3) . . ?
F3 C12 C9 112.6(3) . . ?
C18 C13 C14 118.3(2) . . ?
C18 C13 C3 118.9(2) . . ?
C14 C13 C3 122.7(2) . . ?
C15 C14 C13 121.0(3) . . ?
C16 C15 C14 119.6(2) . . ?
C15 C16 C17 120.7(2) . . ?
C15 C16 C19 119.7(2) . . ?
C17 C16 C19 119.6(3) . . ?
C16 C17 C18 119.5(3) . . ?
C17 C18 C13 120.9(3) . . ?
F5B C19 F4B 110.7(6) . . ?
F5 C19 F6 108.0(4) . . ?
F5A C19 F6A 108.4(6) . . ?
F5 C19 F4 107.5(5) . . ?
F6 C19 F4 102.5(4) . . ?
F5A C19 F4A 108.7(6) . . ?
F6A C19 F4A 99.7(5) . . ?
F5B C19 F6B 103.6(5) . . ?
F4B C19 F6B 102.1(5) . . ?
F5B C19 C16 116.0(4) . . ?
F5A C19 C16 115.7(5) . . ?
F5 C19 C16 115.3(4) . . ?
F4B C19 C16 114.4(4) . . ?
F6 C19 C16 111.6(3) . . ?
F6A C19 C16 112.0(4) . . ?
F4 C19 C16 111.1(3) . . ?
F4A C19 C16 111.1(3) . . ?
F6B C19 C16 108.4(3) . . ?
N1 C20 C21 109.9(2) . . ?
C22 C21 C20 112.2(2) . . ?
C21 C22 C23 109.4(2) . . ?
C24 C23 C22 110.8(2) . . ?
N1 C24 C23 110.2(2) . . ?
N2 C25 C26 111.6(2) . . ?
C25 C26 C27 111.6(2) . . ?
C28 C27 C26 109.4(2) . . ?
C27 C28 C29 111.6(2) . . ?
N2 C29 C28 109.5(2) . . ?
O2 C30 Fe1 173.9(3) . . ?
O3 C31 Fe1 179.6(3) . . ?
N3 C32 C33 179.4(5) . . ?

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
O1 C1 C2 C3 -174.1(3) . . . . ?
C5 C1 C2 C3 12.2(3) . . . . ?
Fe1 C1 C2 C3 61.16(18) . . . . ?
O1 C1 C2 C6 -5.3(5) . . . . ?
C5 C1 C2 C6 -178.9(2) . . . . ?
Fe1 C1 C2 C6 -130.0(3) . . . . ?
O1 C1 C2 Fe1 124.7(3) . . . . ?
C5 C1 C2 Fe1 -48.93(19) . . . . ?
C1 C2 C3 C4 -3.6(3) . . . . ?
C6 C2 C3 C4 -172.0(3) . . . . ?
Fe1 C2 C3 C4 67.60(18) . . . . ?
C1 C2 C3 C13 160.3(2) . . . . ?
C6 C2 C3 C13 -8.1(4) . . . . ?
Fe1 C2 C3 C13 -128.5(3) . . . . ?
C1 C2 C3 Fe1 -71.2(2) . . . . ?
C6 C2 C3 Fe1 120.4(3) . . . . ?
C20 N1 C4 C5 -162.9(2) . . . . ?
C24 N1 C4 C5 55.3(3) . . . . ?
C20 N1 C4 C3 17.7(4) . . . . ?
C24 N1 C4 C3 -124.2(3) . . . . ?
C20 N1 C4 Fe1 -69.5(3) . . . . ?
C24 N1 C4 Fe1 148.7(2) . . . . ?
C2 C3 C4 N1 172.6(3) . . . . ?
C13 C3 C4 N1 9.4(4) . . . . ?
Fe1 C3 C4 N1 -121.3(3) . . . . ?
C2 C3 C4 C5 -6.9(3) . . . . ?
C13 C3 C4 C5 -170.1(2) . . . . ?
Fe1 C3 C4 C5 59.25(18) . . . . ?
C2 C3 C4 Fe1 -66.14(18) . . . . ?
C13 C3 C4 Fe1 130.7(3) . . . . ?
C25 N2 C5 C4 52.6(4) . . . . ?
C29 N2 C5 C4 -170.7(3) . . . . ?
C25 N2 C5 C1 -140.7(3) . . . . ?
C29 N2 C5 C1 -4.0(4) . . . . ?
C25 N2 C5 Fe1 -37.2(3) . . . . ?
C29 N2 C5 Fe1 99.6(3) . . . . ?
N1 C4 C5 N2 3.9(4) . . . . ?
C3 C4 C5 N2 -176.6(2) . . . . ?
Fe1 C4 C5 N2 -121.8(3) . . . . ?
N1 C4 C5 C1 -164.8(2) . . . . ?
C3 C4 C5 C1 14.7(3) . . . . ?
Fe1 C4 C5 C1 69.49(18) . . . . ?
N1 C4 C5 Fe1 125.7(2) . . . . ?
C3 C4 C5 Fe1 -54.80(17) . . . . ?
O1 C1 C5 N2 1.2(5) . . . . ?
C2 C1 C5 N2 174.9(3) . . . . ?
Fe1 C1 C5 N2 127.8(3) . . . . ?
O1 C1 C5 C4 169.8(3) . . . . ?
C2 C1 C5 C4 -16.5(3) . . . . ?
Fe1 C1 C5 C4 -63.59(17) . . . . ?
O1 C1 C5 Fe1 -126.6(3) . . . . ?
C2 C1 C5 Fe1 47.14(19) . . . . ?
C3 C2 C6 C7 153.0(3) . . . . ?
C1 C2 C6 C7 -13.8(4) . . . . ?
Fe1 C2 C6 C7 -120.5(3) . . . . ?
C3 C2 C6 C11 -26.6(4) . . . . ?
C1 C2 C6 C11 166.5(3) . . . . ?
Fe1 C2 C6 C11 59.9(4) . . . . ?
C11 C6 C7 C8 -2.0(5) . . . . ?
C2 C6 C7 C8 178.4(3) . . . . ?
C6 C7 C8 C9 1.3(5) . . . . ?
C7 C8 C9 C10 0.4(5) . . . . ?
C7 C8 C9 C12 -178.8(3) . . . . ?
C8 C9 C10 C11 -1.3(5) . . . . ?
C12 C9 C10 C11 178.0(3) . . . . ?
C9 C10 C11 C6 0.5(5) . . . . ?
C7 C6 C11 C10 1.1(5) . . . . ?
C2 C6 C11 C10 -179.3(3) . . . . ?
C10 C9 C12 F1 86.1(4) . . . . ?
C8 C9 C12 F1 -94.6(4) . . . . ?
C10 C9 C12 F2 -33.4(5) . . . . ?
C8 C9 C12 F2 145.8(4) . . . . ?
C10 C9 C12 F3 -153.9(3) . . . . ?
C8 C9 C12 F3 25.3(5) . . . . ?
C4 C3 C13 C18 93.8(3) . . . . ?
C2 C3 C13 C18 -67.0(4) . . . . ?
Fe1 C3 C13 C18 -163.1(2) . . . . ?
C4 C3 C13 C14 -89.9(3) . . . . ?
C2 C3 C13 C14 109.3(3) . . . . ?
Fe1 C3 C13 C14 13.3(4) . . . . ?
C18 C13 C14 C15 -0.5(4) . . . . ?
C3 C13 C14 C15 -176.8(2) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
C14 C15 C16 C17 0.0(4) . . . . ?
C14 C15 C16 C19 -179.6(3) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C19 C16 C17 C18 179.2(3) . . . . ?
C16 C17 C18 C13 0.3(5) . . . . ?
C14 C13 C18 C17 0.1(4) . . . . ?
C3 C13 C18 C17 176.6(3) . . . . ?
C15 C16 C19 F5B 68.2(7) . . . . ?
C17 C16 C19 F5B -111.4(6) . . . . ?
C15 C16 C19 F5A -94.3(7) . . . . ?
C17 C16 C19 F5A 86.2(7) . . . . ?
C15 C16 C19 F5 -8.7(6) . . . . ?
C17 C16 C19 F5 171.8(5) . . . . ?
C15 C16 C19 F4B -161.0(5) . . . . ?
C17 C16 C19 F4B 19.4(6) . . . . ?
C15 C16 C19 F6 -132.3(4) . . . . ?
C17 C16 C19 F6 48.1(5) . . . . ?
C15 C16 C19 F6A 140.8(5) . . . . ?
C17 C16 C19 F6A -38.8(6) . . . . ?
C15 C16 C19 F4 114.0(4) . . . . ?
C17 C16 C19 F4 -65.6(5) . . . . ?
C15 C16 C19 F4A 30.2(5) . . . . ?
C17 C16 C19 F4A -149.3(4) . . . . ?
C15 C16 C19 F6B -47.8(5) . . . . ?
C17 C16 C19 F6B 132.6(4) . . . . ?
C4 N1 C20 C21 159.4(2) . . . . ?
C24 N1 C20 C21 -57.6(3) . . . . ?
N1 C20 C21 C22 55.9(3) . . . . ?
C20 C21 C22 C23 -54.8(3) . . . . ?
C21 C22 C23 C24 54.7(4) . . . . ?
C4 N1 C24 C23 -156.9(2) . . . . ?
C20 N1 C24 C23 58.5(3) . . . . ?
C22 C23 C24 N1 -56.4(3) . . . . ?
C5 N2 C25 C26 -162.1(2) . . . . ?
C29 N2 C25 C26 58.1(3) . . . . ?
N2 C25 C26 C27 -54.8(3) . . . . ?
C25 C26 C27 C28 52.8(3) . . . . ?
C26 C27 C28 C29 -55.1(3) . . . . ?
C5 N2 C29 C28 162.3(2) . . . . ?
C25 N2 C29 C28 -59.1(3) . . . . ?
C27 C28 C29 N2 58.4(3) . . . . ?

_refine_diff_density_max         1.052
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.084



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk44db
_database_code_depnum_ccdc_archive 'CCDC 2338290'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 F6 N2 O'
_chemical_formula_sum            'C29 H28 F6 N2 O'
_chemical_formula_weight         534.53

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'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.6211(6)
_cell_length_b                   16.9942(4)
_cell_length_c                   32.0027(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10127.3(5)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13841
_cell_measurement_theta_min      2.7510
_cell_measurement_theta_max      73.8480

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_F_000             4448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.990
_shelx_estimated_absorpt_T_min   0.908
_shelx_estimated_absorpt_T_max   0.971
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -10 -7 0.0196
-12 1 -1 0.0472
-2 10 6 0.0289
12 0 2 0.0427
0 -5 18 0.0175
-1 6 -17 0.0120
5 -2 -18 0.0163
-1 -3 -20 0.0102
2 -6 -17 0.0107
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
1.1405 -10.3710 -6.8218 -0.2360 0.4334 0.8698
-11.9602 1.4235 -1.4900 -0.3623 0.6670 -0.6510
-2.3552 10.2583 6.4954 0.1924 -0.3531 -0.9156
12.0085 -0.0094 2.4620 0.4013 -0.7387 0.5416
0.1233 -5.4419 18.0481 0.8593 0.4673 0.2078
-0.8448 6.2136 -17.0821 -0.8360 -0.4547 -0.3073
5.1379 -2.1515 -18.3521 -0.7102 -0.3858 0.5888
-0.9997 -2.7981 -20.0282 -0.9314 0.0237 0.3632
2.1523 -5.8349 -17.2454 -0.7131 0.0178 0.7008
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_T_max  1.000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.729
_oxdiff_exptl_absorpt_empirical_full_max 1.485
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            26477
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.761
_diffrn_reflns_theta_max         76.274
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             26477
_reflns_number_gt                16008
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to 
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Refined as a 2-component twin. Component 2 rotated by -179.2780° 
 around [0.00 -0.01 1.00] (reciprocal) or [0.01 -0.04 1.00] (direct).

 Two disordered CF3 groups were refined accordingly.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0925P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26477
_refine_ls_number_parameters     742
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0622
_refine_ls_wR_factor_ref         0.1727
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
F1 F 0.31817(14) 0.19286(17) 0.25630(7) 0.0805(8) Uani 1 1 d . . . . .
F2 F 0.34865(18) 0.07909(13) 0.27605(7) 0.0928(9) Uani 1 1 d . . . . .
F3 F 0.42734(12) 0.16021(15) 0.25530(6) 0.0676(6) Uani 1 1 d . . . . .
F4 F 0.35778(13) 0.63325(14) 0.34055(9) 0.0858(9) Uani 1 1 d . . . . .
F5 F 0.46098(16) 0.59374(14) 0.32409(7) 0.0813(8) Uani 1 1 d . . . . .
F6 F 0.44901(14) 0.67352(11) 0.37384(6) 0.0679(7) Uani 1 1 d . . . . .
O1 O 0.40492(12) 0.39151(12) 0.53110(6) 0.0416(5) Uani 1 1 d . . . . .
N1 N 0.38799(14) 0.22094(14) 0.56201(7) 0.0361(6) Uani 1 1 d . . . . .
N2 N 0.38369(14) 0.12772(13) 0.47814(7) 0.0362(6) Uani 1 1 d . . . . .
C1 C 0.39908(16) 0.33367(16) 0.50832(9) 0.0335(6) Uani 1 1 d . . . . .
C2 C 0.38911(16) 0.25018(16) 0.52066(9) 0.0344(6) Uani 1 1 d . . . . .
C3 C 0.39041(16) 0.20743(16) 0.48477(9) 0.0334(6) Uani 1 1 d . . . . .
C4 C 0.39583(16) 0.26196(17) 0.44753(9) 0.0342(6) Uani 1 1 d . . . . .
C5 C 0.40144(16) 0.33662(16) 0.46128(9) 0.0336(6) Uani 1 1 d . . . . .
C6 C 0.36574(18) 0.27551(17) 0.59492(9) 0.0389(7) Uani 1 1 d . . . . .
H6A H 0.323012 0.305391 0.585590 0.047 Uiso 1 1 calc R U . . .
H6B H 0.404860 0.313526 0.600520 0.047 Uiso 1 1 calc R U . . .
C7 C 0.34808(19) 0.23077(19) 0.63457(9) 0.0435(7) Uani 1 1 d . . . . .
H7A H 0.335179 0.268527 0.656893 0.052 Uiso 1 1 calc R U . . .
H7B H 0.306087 0.196327 0.629528 0.052 Uiso 1 1 calc R U . . .
C8 C 0.4107(2) 0.1815(2) 0.64871(10) 0.0510(9) Uani 1 1 d . . . . .
H8A H 0.395924 0.148420 0.672692 0.061 Uiso 1 1 calc R U . . .
H8B H 0.450168 0.216266 0.658083 0.061 Uiso 1 1 calc R U . . .
C9 C 0.4373(2) 0.12885(19) 0.61326(10) 0.0474(8) Uani 1 1 d . . . . .
H9A H 0.481651 0.101376 0.622130 0.057 Uiso 1 1 calc R U . . .
H9B H 0.400521 0.088560 0.606863 0.057 Uiso 1 1 calc R U . . .
C10 C 0.45257(17) 0.17717(18) 0.57438(10) 0.0403(7) Uani 1 1 d . . . . .
H10C H 0.492266 0.214436 0.580014 0.048 Uiso 1 1 calc R U . . .
H10D H 0.467573 0.141947 0.551335 0.048 Uiso 1 1 calc R U . . .
C11 C 0.34529(19) 0.07783(17) 0.50821(9) 0.0415(7) Uani 1 1 d . . . . .
H11C H 0.308354 0.109118 0.523007 0.050 Uiso 1 1 calc R U . . .
H11D H 0.379309 0.056721 0.529169 0.050 Uiso 1 1 calc R U . . .
C12 C 0.3099(2) 0.01046(19) 0.48451(11) 0.0504(8) Uani 1 1 d . . . . .
H12C H 0.273813 0.031785 0.464836 0.060 Uiso 1 1 calc R U . . .
H12D H 0.284911 -0.024628 0.504460 0.060 Uiso 1 1 calc R U . . .
C13 C 0.3662(2) -0.03645(19) 0.46034(11) 0.0563(10) Uani 1 1 d . . . . .
H13C H 0.399455 -0.062115 0.480270 0.068 Uiso 1 1 calc R U . . .
H13D H 0.342175 -0.078173 0.443897 0.068 Uiso 1 1 calc R U . . .
C14 C 0.4088(2) 0.01685(18) 0.43101(11) 0.0544(9) Uani 1 1 d . . . . .
H14C H 0.448354 -0.013532 0.418091 0.065 Uiso 1 1 calc R U . . .
H14D H 0.377008 0.035927 0.408371 0.065 Uiso 1 1 calc R U . . .
C15 C 0.43955(18) 0.08654(18) 0.45456(10) 0.0423(7) Uani 1 1 d . . . . .
H15C H 0.477262 0.067998 0.474017 0.051 Uiso 1 1 calc R U . . .
H15D H 0.462040 0.123422 0.434507 0.051 Uiso 1 1 calc R U . . .
C16 C 0.38843(16) 0.23564(16) 0.40378(9) 0.0339(6) Uani 1 1 d . . . . .
C17 C 0.33025(17) 0.18986(18) 0.39147(10) 0.0405(7) Uani 1 1 d . . . . .
H17 H 0.294670 0.175821 0.411395 0.049 Uiso 1 1 calc R U . . .
C18 C 0.32350(18) 0.16445(19) 0.35046(10) 0.0428(7) Uani 1 1 d . . . . .
H18 H 0.283050 0.134002 0.342351 0.051 Uiso 1 1 calc R U . . .
C19 C 0.37526(17) 0.18327(18) 0.32160(9) 0.0376(7) Uani 1 1 d . . . . .
C20 C 0.43339(17) 0.22930(17) 0.33332(9) 0.0381(7) Uani 1 1 d . . . . .
H20 H 0.468972 0.242942 0.313312 0.046 Uiso 1 1 calc R U . . .
C21 C 0.43959(16) 0.25532(17) 0.37406(9) 0.0350(6) Uani 1 1 d . . . . .
H21 H 0.479390 0.287086 0.381823 0.042 Uiso 1 1 calc R U . . .
C22 C 0.36760(19) 0.15472(19) 0.27745(10) 0.0452(8) Uani 1 1 d . . . . .
C23 C 0.40371(16) 0.40982(16) 0.43655(9) 0.0335(6) Uani 1 1 d . . . . .
C24 C 0.35169(17) 0.42490(17) 0.40653(10) 0.0397(7) Uani 1 1 d . . . . .
H24 H 0.312966 0.389097 0.403064 0.048 Uiso 1 1 calc R U . . .
C25 C 0.35537(17) 0.49127(18) 0.38160(10) 0.0409(7) Uani 1 1 d . . . . .
H25 H 0.319003 0.501325 0.361472 0.049 Uiso 1 1 calc R U . . .
C26 C 0.41236(17) 0.54301(16) 0.38612(9) 0.0356(6) Uani 1 1 d . . . . .
C27 C 0.46352(17) 0.52990(16) 0.41670(9) 0.0365(7) Uani 1 1 d . . . . .
H27 H 0.502090 0.565904 0.420163 0.044 Uiso 1 1 calc R U . . .
C28 C 0.45860(16) 0.46441(16) 0.44227(9) 0.0348(6) Uani 1 1 d . . . . .
H28 H 0.492900 0.456666 0.463852 0.042 Uiso 1 1 calc R U . . .
C29 C 0.41994(18) 0.61047(18) 0.35663(10) 0.0411(7) Uani 1 1 d . . . . .
O1A O 0.61022(12) 0.10869(12) 0.41178(6) 0.0413(5) Uani 1 1 d . . . . .
N1A N 0.65578(14) 0.26498(14) 0.44961(7) 0.0361(5) Uani 1 1 d . . . . .
N2A N 0.66837(14) 0.37240(13) 0.37130(7) 0.0350(5) Uani 1 1 d . . . . .
C1A C 0.62776(16) 0.16643(16) 0.39114(9) 0.0342(6) Uani 1 1 d . . . . .
C2A C 0.65149(16) 0.24384(17) 0.40668(9) 0.0347(6) Uani 1 1 d . . . . .
C3A C 0.65399(16) 0.29337(16) 0.37314(9) 0.0336(6) Uani 1 1 d . . . . .
C4A C 0.64074(15) 0.24655(16) 0.33333(9) 0.0329(6) Uani 1 1 d . . . . .
C5A C 0.62544(16) 0.17166(16) 0.34414(9) 0.0329(6) Uani 1 1 d . . . . .
C6A C 0.69261(18) 0.2083(2) 0.47653(9) 0.0427(7) Uani 1 1 d . . . . .
H6AA H 0.738385 0.192045 0.463372 0.051 Uiso 1 1 calc R U . . .
H6AB H 0.662345 0.160860 0.480073 0.051 Uiso 1 1 calc R U . . .
C7A C 0.70752(18) 0.2449(2) 0.51877(9) 0.0451(8) Uani 1 1 d . . . . .
H7AA H 0.731429 0.205749 0.536989 0.054 Uiso 1 1 calc R U . . .
H7AB H 0.740428 0.290149 0.515302 0.054 Uiso 1 1 calc R U . . .
C8A C 0.63927(19) 0.2721(2) 0.53910(10) 0.0484(8) Uani 1 1 d . . . . .
H8AA H 0.650647 0.300121 0.565405 0.058 Uiso 1 1 calc R U . . .
H8AB H 0.608963 0.226076 0.546025 0.058 Uiso 1 1 calc R U . . .
C9A C 0.5985(2) 0.3268(2) 0.50991(10) 0.0532(9) Uani 1 1 d . . . . .
H9AA H 0.551326 0.339933 0.522338 0.064 Uiso 1 1 calc R U . . .
H9AB H 0.625815 0.376290 0.506308 0.064 Uiso 1 1 calc R U . . .
C10A C 0.58736(18) 0.2882(2) 0.46768(10) 0.0450(8) Uani 1 1 d . . . . .
H10A H 0.556390 0.241205 0.470945 0.054 Uiso 1 1 calc R U . . .
H10B H 0.562765 0.325386 0.448671 0.054 Uiso 1 1 calc R U . . .
C11A C 0.70422(19) 0.41104(17) 0.40651(9) 0.0418(7) Uani 1 1 d . . . . .
H11A H 0.738352 0.374099 0.419850 0.050 Uiso 1 1 calc R U . . .
H11B H 0.668243 0.427022 0.427644 0.050 Uiso 1 1 calc R U . . .
C12A C 0.7443(2) 0.48314(18) 0.39056(10) 0.0471(8) Uani 1 1 d . . . . .
H12A H 0.767708 0.510262 0.414318 0.056 Uiso 1 1 calc R U . . .
H12B H 0.782287 0.466406 0.370817 0.056 Uiso 1 1 calc R U . . .
C13A C 0.6937(2) 0.53948(18) 0.36880(10) 0.0484(8) Uani 1 1 d . . . . .
H13A H 0.721127 0.584702 0.357632 0.058 Uiso 1 1 calc R U . . .
H13B H 0.658137 0.559835 0.389120 0.058 Uiso 1 1 calc R U . . .
C14A C 0.6548(2) 0.49805(17) 0.33325(10) 0.0460(8) Uani 1 1 d . . . . .
H14A H 0.689667 0.484133 0.311103 0.055 Uiso 1 1 calc R U . . .
H14B H 0.618635 0.534005 0.321009 0.055 Uiso 1 1 calc R U . . .
C15A C 0.61772(17) 0.42364(17) 0.34890(10) 0.0396(7) Uani 1 1 d . . . . .
H15A H 0.577812 0.438264 0.367807 0.047 Uiso 1 1 calc R U . . .
H15B H 0.597165 0.394667 0.324876 0.047 Uiso 1 1 calc R U . . .
C16A C 0.64869(16) 0.27723(16) 0.29039(9) 0.0330(6) Uani 1 1 d . . . . .
C17A C 0.70682(17) 0.32474(17) 0.27938(10) 0.0376(7) Uani 1 1 d . . . . .
H17A H 0.742017 0.337550 0.299763 0.045 Uiso 1 1 calc R U . . .
C18A C 0.71375(17) 0.35334(18) 0.23920(10) 0.0409(7) Uani 1 1 d . . . . .
H18A H 0.753838 0.385171 0.232025 0.049 Uiso 1 1 calc R U . . .
C19A C 0.66246(17) 0.33575(17) 0.20936(9) 0.0378(7) Uani 1 1 d . . . . .
C20A C 0.60483(17) 0.28783(18) 0.21954(9) 0.0387(7) Uani 1 1 d . . . . .
H20A H 0.569816 0.275067 0.199034 0.046 Uiso 1 1 calc R U . . .
C21A C 0.59862(16) 0.25879(17) 0.25961(9) 0.0352(6) Uani 1 1 d . . . . .
H21A H 0.559332 0.225469 0.266354 0.042 Uiso 1 1 calc R U . . .
C22A C 0.6691(2) 0.3672(2) 0.16619(11) 0.0480(8) Uani 1 1 d . . . . .
C23A C 0.61417(16) 0.10331(16) 0.31666(9) 0.0335(6) Uani 1 1 d . . . . .
C24A C 0.66184(16) 0.08706(16) 0.28415(9) 0.0364(6) Uani 1 1 d . . . . .
H24A H 0.703514 0.118624 0.280678 0.044 Uiso 1 1 calc R U . . .
C25A C 0.64899(17) 0.02535(17) 0.25691(9) 0.0376(7) Uani 1 1 d . . . . .
H25A H 0.681664 0.014676 0.234827 0.045 Uiso 1 1 calc R U . . .
C26A C 0.58817(17) -0.02080(17) 0.26200(9) 0.0365(7) Uani 1 1 d . . . . .
C27A C 0.54098(17) -0.00621(17) 0.29463(9) 0.0385(7) Uani 1 1 d . . . . .
H27A H 0.499501 -0.038099 0.298091 0.046 Uiso 1 1 calc R U . . .
C28A C 0.55442(16) 0.05493(17) 0.32217(9) 0.0369(7) Uani 1 1 d . . . . .
H28A H 0.522749 0.063955 0.344941 0.044 Uiso 1 1 calc R U . . .
C29A C 0.5716(2) -0.08580(18) 0.23216(10) 0.0436(8) Uani 1 1 d . . . . .
F1A F 0.7074(3) 0.31973(18) 0.14100(9) 0.0813(14) Uani 0.808(7) 1 d . . P A 1
F2A F 0.7018(2) 0.43591(19) 0.16385(9) 0.0746(12) Uani 0.808(7) 1 d . . P A 1
F3A F 0.60752(18) 0.3730(3) 0.14608(11) 0.0886(13) Uani 0.808(7) 1 d . U P A 1
F1B F 0.6495(10) 0.3249(8) 0.1378(4) 0.070(4) Uani 0.192(7) 1 d . U P A 2
F2B F 0.7272(9) 0.4000(12) 0.1591(5) 0.083(5) Uani 0.192(7) 1 d . U P A 2
F3B F 0.6189(6) 0.4282(7) 0.1614(4) 0.055(4) Uani 0.192(7) 1 d . U P A 2
F4A F 0.62060(17) -0.09355(17) 0.20168(8) 0.0737(10) Uani 0.897(5) 1 d . . P B
3
F5A F 0.51057(17) -0.07731(19) 0.21287(11) 0.0945(14) Uani 0.897(5) 1 d . . P B
3
F6A F 0.5707(2) -0.15574(13) 0.25021(7) 0.0866(14) Uani 0.897(5) 1 d . . P B 3
F4B F 0.5644(14) -0.0679(12) 0.1975(6) 0.051(6) Uani 0.103(5) 1 d . U P B 4
F5B F 0.5126(11) -0.1233(12) 0.2446(6) 0.050(6) Uani 0.103(5) 1 d . U P B 4
F6B F 0.6188(14) -0.1367(16) 0.2363(8) 0.067(7) Uani 0.103(5) 1 d . U P B 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
F1 C22 1.313(4) . ?
F2 C22 1.334(4) . ?
F3 C22 1.322(4) . ?
F4 C29 1.325(4) . ?
F5 C29 1.323(4) . ?
F6 C29 1.321(4) . ?
O1 C1 1.229(3) . ?
N1 C2 1.414(4) . ?
N1 C6 1.463(4) . ?
N1 C10 1.468(4) . ?
N2 C3 1.377(3) . ?
N2 C15 1.463(4) . ?
N2 C11 1.468(4) . ?
C1 C2 1.484(4) . ?
C1 C5 1.507(4) . ?
C2 C3 1.359(4) . ?
C3 C4 1.513(4) . ?
C4 C5 1.347(4) . ?
C4 C16 1.476(4) . ?
C5 C23 1.475(4) . ?
C6 C7 1.515(4) . ?
C7 C8 1.505(5) . ?
C8 C9 1.527(5) . ?
C9 C10 1.518(4) . ?
C11 C12 1.523(4) . ?
C12 C13 1.527(5) . ?
C13 C14 1.527(5) . ?
C14 C15 1.516(5) . ?
C16 C21 1.387(4) . ?
C16 C17 1.391(4) . ?
C17 C18 1.387(4) . ?
C18 C19 1.373(5) . ?
C19 C20 1.387(4) . ?
C19 C22 1.501(4) . ?
C20 C21 1.382(4) . ?
C23 C24 1.388(4) . ?
C23 C28 1.392(4) . ?
C24 C25 1.383(4) . ?
C25 C26 1.386(4) . ?
C26 C27 1.384(4) . ?
C26 C29 1.491(4) . ?
C27 C28 1.384(4) . ?
O1A C1A 1.227(3) . ?
N1A C2A 1.422(4) . ?
N1A C10A 1.453(4) . ?
N1A C6A 1.463(4) . ?
N2A C3A 1.371(3) . ?
N2A C11A 1.465(4) . ?
N2A C15A 1.470(4) . ?
C1A C2A 1.474(4) . ?
C1A C5A 1.507(4) . ?
C2A C3A 1.365(4) . ?
C3A C4A 1.522(4) . ?
C4A C5A 1.349(4) . ?
C4A C16A 1.477(4) . ?
C5A C23A 1.472(4) . ?
C6A C7A 1.513(4) . ?
C7A C8A 1.501(5) . ?
C8A C9A 1.520(5) . ?
C9A C10A 1.517(4) . ?
C11A C12A 1.523(4) . ?
C12A C13A 1.514(5) . ?
C13A C14A 1.521(5) . ?
C14A C15A 1.525(4) . ?
C16A C21A 1.392(4) . ?
C16A C17A 1.396(4) . ?
C17A C18A 1.381(4) . ?
C18A C19A 1.383(4) . ?
C19A C20A 1.386(4) . ?
C19A C22A 1.486(4) . ?
C20A C21A 1.379(4) . ?
C22A F1B 1.214(14) . ?
C22A F2B 1.237(17) . ?
C22A F3A 1.319(5) . ?
C22A F2A 1.319(5) . ?
C22A F1A 1.345(5) . ?
C22A F3B 1.404(12) . ?
C23A C28A 1.395(4) . ?
C23A C24A 1.395(4) . ?
C24A C25A 1.385(4) . ?
C25A C26A 1.387(4) . ?
C26A C27A 1.387(4) . ?
C26A C29A 1.493(4) . ?
C27A C28A 1.385(4) . ?
C29A F4B 1.157(19) . ?
C29A F6B 1.24(2) . ?
C29A F5A 1.301(4) . ?
C29A F6A 1.322(4) . ?
C29A F5B 1.330(19) . ?
C29A F4A 1.342(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
C2 N1 C6 117.1(2) . . ?
C2 N1 C10 114.7(2) . . ?
C6 N1 C10 111.0(2) . . ?
C3 N2 C15 119.0(2) . . ?
C3 N2 C11 120.8(2) . . ?
C15 N2 C11 114.1(2) . . ?
O1 C1 C2 128.2(3) . . ?
O1 C1 C5 124.3(2) . . ?
C2 C1 C5 107.5(2) . . ?
C3 C2 N1 127.1(3) . . ?
C3 C2 C1 106.5(2) . . ?
N1 C2 C1 125.9(2) . . ?
C2 C3 N2 130.9(3) . . ?
C2 C3 C4 109.8(2) . . ?
N2 C3 C4 119.2(2) . . ?
C5 C4 C16 127.0(3) . . ?
C5 C4 C3 109.0(2) . . ?
C16 C4 C3 123.7(3) . . ?
C4 C5 C23 128.4(3) . . ?
C4 C5 C1 107.0(2) . . ?
C23 C5 C1 124.4(2) . . ?
N1 C6 C7 110.2(2) . . ?
C8 C7 C6 111.3(3) . . ?
C7 C8 C9 110.7(3) . . ?
C10 C9 C8 110.7(3) . . ?
N1 C10 C9 110.0(3) . . ?
N2 C11 C12 108.6(2) . . ?
C11 C12 C13 110.4(3) . . ?
C14 C13 C12 111.0(3) . . ?
C15 C14 C13 110.7(3) . . ?
N2 C15 C14 111.2(3) . . ?
C21 C16 C17 118.4(3) . . ?
C21 C16 C4 120.9(3) . . ?
C17 C16 C4 120.7(3) . . ?
C18 C17 C16 120.8(3) . . ?
C19 C18 C17 120.0(3) . . ?
C18 C19 C20 119.8(3) . . ?
C18 C19 C22 119.4(3) . . ?
C20 C19 C22 120.7(3) . . ?
C21 C20 C19 120.0(3) . . ?
C20 C21 C16 120.8(3) . . ?
F1 C22 F3 106.2(3) . . ?
F1 C22 F2 105.8(3) . . ?
F3 C22 F2 105.8(3) . . ?
F1 C22 C19 113.1(3) . . ?
F3 C22 C19 113.7(3) . . ?
F2 C22 C19 111.6(3) . . ?
C24 C23 C28 118.7(3) . . ?
C24 C23 C5 120.5(3) . . ?
C28 C23 C5 120.8(3) . . ?
C25 C24 C23 121.0(3) . . ?
C24 C25 C26 119.7(3) . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 C29 120.4(3) . . ?
C25 C26 C29 119.6(3) . . ?
C26 C27 C28 120.1(3) . . ?
C27 C28 C23 120.4(3) . . ?
F6 C29 F5 105.4(3) . . ?
F6 C29 F4 106.4(3) . . ?
F5 C29 F4 105.2(3) . . ?
F6 C29 C26 113.5(3) . . ?
F5 C29 C26 112.8(3) . . ?
F4 C29 C26 112.8(3) . . ?
C2A N1A C10A 113.8(2) . . ?
C2A N1A C6A 115.4(2) . . ?
C10A N1A C6A 110.8(2) . . ?
C3A N2A C11A 119.7(2) . . ?
C3A N2A C15A 118.4(2) . . ?
C11A N2A C15A 113.7(2) . . ?
O1A C1A C2A 127.7(3) . . ?
O1A C1A C5A 125.2(3) . . ?
C2A C1A C5A 107.0(2) . . ?
C3A C2A N1A 127.0(3) . . ?
C3A C2A C1A 107.2(2) . . ?
N1A C2A C1A 124.6(3) . . ?
C2A C3A N2A 130.1(3) . . ?
C2A C3A C4A 109.3(2) . . ?
N2A C3A C4A 120.5(2) . . ?
C5A C4A C16A 126.3(3) . . ?
C5A C4A C3A 108.2(2) . . ?
C16A C4A C3A 125.3(3) . . ?
C4A C5A C23A 128.4(3) . . ?
C4A C5A C1A 107.8(2) . . ?
C23A C5A C1A 123.6(2) . . ?
N1A C6A C7A 110.0(3) . . ?
C8A C7A C6A 111.0(3) . . ?
C7A C8A C9A 110.2(3) . . ?
C10A C9A C8A 110.6(3) . . ?
N1A C10A C9A 110.6(3) . . ?
N2A C11A C12A 109.0(2) . . ?
C13A C12A C11A 110.9(3) . . ?
C12A C13A C14A 110.4(3) . . ?
C13A C14A C15A 110.7(3) . . ?
N2A C15A C14A 111.2(3) . . ?
C21A C16A C17A 118.1(3) . . ?
C21A C16A C4A 120.8(3) . . ?
C17A C16A C4A 121.1(3) . . ?
C18A C17A C16A 120.7(3) . . ?
C17A C18A C19A 120.2(3) . . ?
C18A C19A C20A 120.0(3) . . ?
C18A C19A C22A 120.4(3) . . ?
C20A C19A C22A 119.6(3) . . ?
C21A C20A C19A 119.6(3) . . ?
C20A C21A C16A 121.4(3) . . ?
F1B C22A F2B 113.1(11) . . ?
F3A C22A F2A 107.8(4) . . ?
F3A C22A F1A 102.4(4) . . ?
F2A C22A F1A 104.6(3) . . ?
F1B C22A F3B 98.9(9) . . ?
F2B C22A F3B 103.2(10) . . ?
F1B C22A C19A 117.2(7) . . ?
F2B C22A C19A 113.9(8) . . ?
F3A C22A C19A 114.1(3) . . ?
F2A C22A C19A 114.2(3) . . ?
F1A C22A C19A 112.7(3) . . ?
F3B C22A C19A 108.2(5) . . ?
C28A C23A C24A 119.0(3) . . ?
C28A C23A C5A 120.2(3) . . ?
C24A C23A C5A 120.7(3) . . ?
C25A C24A C23A 120.6(3) . . ?
C24A C25A C26A 119.7(3) . . ?
C27A C26A C25A 120.3(3) . . ?
C27A C26A C29A 118.9(3) . . ?
C25A C26A C29A 120.8(3) . . ?
C28A C27A C26A 119.9(3) . . ?
C27A C28A C23A 120.4(3) . . ?
F4B C29A F6B 111.6(17) . . ?
F5A C29A F6A 107.3(3) . . ?
F4B C29A F5B 108.5(15) . . ?
F6B C29A F5B 102.7(16) . . ?
F5A C29A F4A 105.1(3) . . ?
F6A C29A F4A 103.7(3) . . ?
F4B C29A C26A 116.2(10) . . ?
F6B C29A C26A 107.5(11) . . ?
F5A C29A C26A 113.7(3) . . ?
F6A C29A C26A 112.8(3) . . ?
F5B C29A C26A 109.5(9) . . ?
F4A C29A C26A 113.4(3) . . ?

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
C6 N1 C2 C3 -162.6(3) . . . . ?
C10 N1 C2 C3 64.7(4) . . . . ?
C6 N1 C2 C1 26.4(4) . . . . ?
C10 N1 C2 C1 -106.4(3) . . . . ?
O1 C1 C2 C3 -176.0(3) . . . . ?
C5 C1 C2 C3 3.7(3) . . . . ?
O1 C1 C2 N1 -3.4(5) . . . . ?
C5 C1 C2 N1 176.3(3) . . . . ?
N1 C2 C3 N2 7.5(5) . . . . ?
C1 C2 C3 N2 180.0(3) . . . . ?
N1 C2 C3 C4 -176.6(3) . . . . ?
C1 C2 C3 C4 -4.1(3) . . . . ?
C15 N2 C3 C2 -125.8(4) . . . . ?
C11 N2 C3 C2 25.1(5) . . . . ?
C15 N2 C3 C4 58.7(4) . . . . ?
C11 N2 C3 C4 -150.5(3) . . . . ?
C2 C3 C4 C5 3.1(4) . . . . ?
N2 C3 C4 C5 179.6(3) . . . . ?
C2 C3 C4 C16 -171.3(3) . . . . ?
N2 C3 C4 C16 5.2(4) . . . . ?
C16 C4 C5 C23 -1.9(5) . . . . ?
C3 C4 C5 C23 -176.0(3) . . . . ?
C16 C4 C5 C1 173.5(3) . . . . ?
C3 C4 C5 C1 -0.6(3) . . . . ?
O1 C1 C5 C4 177.9(3) . . . . ?
C2 C1 C5 C4 -1.8(3) . . . . ?
O1 C1 C5 C23 -6.5(5) . . . . ?
C2 C1 C5 C23 173.8(3) . . . . ?
C2 N1 C6 C7 164.7(3) . . . . ?
C10 N1 C6 C7 -60.9(3) . . . . ?
N1 C6 C7 C8 56.6(4) . . . . ?
C6 C7 C8 C9 -52.8(4) . . . . ?
C7 C8 C9 C10 52.9(4) . . . . ?
C2 N1 C10 C9 -163.3(3) . . . . ?
C6 N1 C10 C9 61.2(3) . . . . ?
C8 C9 C10 N1 -56.7(4) . . . . ?
C3 N2 C11 C12 148.3(3) . . . . ?
C15 N2 C11 C12 -59.5(4) . . . . ?
N2 C11 C12 C13 57.7(4) . . . . ?
C11 C12 C13 C14 -56.0(4) . . . . ?
C12 C13 C14 C15 52.9(4) . . . . ?
C3 N2 C15 C14 -149.7(3) . . . . ?
C11 N2 C15 C14 57.6(4) . . . . ?
C13 C14 C15 N2 -52.5(4) . . . . ?
C5 C4 C16 C21 57.8(4) . . . . ?
C3 C4 C16 C21 -128.9(3) . . . . ?
C5 C4 C16 C17 -122.8(4) . . . . ?
C3 C4 C16 C17 50.5(4) . . . . ?
C21 C16 C17 C18 0.0(5) . . . . ?
C4 C16 C17 C18 -179.4(3) . . . . ?
C16 C17 C18 C19 1.1(5) . . . . ?
C17 C18 C19 C20 -1.5(5) . . . . ?
C17 C18 C19 C22 179.4(3) . . . . ?
C18 C19 C20 C21 0.8(5) . . . . ?
C22 C19 C20 C21 179.8(3) . . . . ?
C19 C20 C21 C16 0.4(4) . . . . ?
C17 C16 C21 C20 -0.8(4) . . . . ?
C4 C16 C21 C20 178.6(3) . . . . ?
C18 C19 C22 F1 73.8(4) . . . . ?
C20 C19 C22 F1 -105.2(4) . . . . ?
C18 C19 C22 F3 -165.0(3) . . . . ?
C20 C19 C22 F3 16.0(4) . . . . ?
C18 C19 C22 F2 -45.4(4) . . . . ?
C20 C19 C22 F2 135.6(3) . . . . ?
C4 C5 C23 C24 51.4(4) . . . . ?
C1 C5 C23 C24 -123.3(3) . . . . ?
C4 C5 C23 C28 -127.4(3) . . . . ?
C1 C5 C23 C28 57.8(4) . . . . ?
C28 C23 C24 C25 2.4(4) . . . . ?
C5 C23 C24 C25 -176.5(3) . . . . ?
C23 C24 C25 C26 1.0(5) . . . . ?
C24 C25 C26 C27 -2.8(5) . . . . ?
C24 C25 C26 C29 174.4(3) . . . . ?
C25 C26 C27 C28 1.2(4) . . . . ?
C29 C26 C27 C28 -175.9(3) . . . . ?
C26 C27 C28 C23 2.2(4) . . . . ?
C24 C23 C28 C27 -4.0(4) . . . . ?
C5 C23 C28 C27 174.9(3) . . . . ?
C27 C26 C29 F6 -35.0(4) . . . . ?
C25 C26 C29 F6 147.9(3) . . . . ?
C27 C26 C29 F5 84.8(4) . . . . ?
C25 C26 C29 F5 -92.3(4) . . . . ?
C27 C26 C29 F4 -156.2(3) . . . . ?
C25 C26 C29 F4 26.7(4) . . . . ?
C10A N1A C2A C3A 84.7(4) . . . . ?
C6A N1A C2A C3A -145.6(3) . . . . ?
C10A N1A C2A C1A -81.1(4) . . . . ?
C6A N1A C2A C1A 48.6(4) . . . . ?
O1A C1A C2A C3A -170.3(3) . . . . ?
C5A C1A C2A C3A 7.1(3) . . . . ?
O1A C1A C2A N1A -2.1(5) . . . . ?
C5A C1A C2A N1A 175.4(3) . . . . ?
N1A C2A C3A N2A 7.6(5) . . . . ?
C1A C2A C3A N2A 175.4(3) . . . . ?
N1A C2A C3A C4A -174.9(3) . . . . ?
C1A C2A C3A C4A -7.1(3) . . . . ?
C11A N2A C3A C2A 17.9(5) . . . . ?
C15A N2A C3A C2A -128.7(3) . . . . ?
C11A N2A C3A C4A -159.4(3) . . . . ?
C15A N2A C3A C4A 54.1(4) . . . . ?
C2A C3A C4A C5A 4.4(3) . . . . ?
N2A C3A C4A C5A -177.8(3) . . . . ?
C2A C3A C4A C16A -171.5(3) . . . . ?
N2A C3A C4A C16A 6.3(4) . . . . ?
C16A C4A C5A C23A 1.0(5) . . . . ?
C3A C4A C5A C23A -174.9(3) . . . . ?
C16A C4A C5A C1A 176.1(3) . . . . ?
C3A C4A C5A C1A 0.2(3) . . . . ?
O1A C1A C5A C4A 173.1(3) . . . . ?
C2A C1A C5A C4A -4.4(3) . . . . ?
O1A C1A C5A C23A -11.5(4) . . . . ?
C2A C1A C5A C23A 171.0(3) . . . . ?
C2A N1A C6A C7A 167.9(3) . . . . ?
C10A N1A C6A C7A -60.9(3) . . . . ?
N1A C6A C7A C8A 57.8(4) . . . . ?
C6A C7A C8A C9A -54.1(4) . . . . ?
C7A C8A C9A C10A 53.3(4) . . . . ?
C2A N1A C10A C9A -167.4(3) . . . . ?
C6A N1A C10A C9A 60.7(4) . . . . ?
C8A C9A C10A N1A -56.6(4) . . . . ?
C3A N2A C11A C12A 153.8(3) . . . . ?
C15A N2A C11A C12A -58.2(4) . . . . ?
N2A C11A C12A C13A 57.8(3) . . . . ?
C11A C12A C13A C14A -56.8(4) . . . . ?
C12A C13A C14A C15A 53.9(4) . . . . ?
C3A N2A C15A C14A -154.9(3) . . . . ?
C11A N2A C15A C14A 56.6(3) . . . . ?
C13A C14A C15A N2A -53.1(4) . . . . ?
C5A C4A C16A C21A 46.6(4) . . . . ?
C3A C4A C16A C21A -138.2(3) . . . . ?
C5A C4A C16A C17A -132.7(3) . . . . ?
C3A C4A C16A C17A 42.5(4) . . . . ?
C21A C16A C17A C18A 0.8(4) . . . . ?
C4A C16A C17A C18A -179.8(3) . . . . ?
C16A C17A C18A C19A 0.7(5) . . . . ?
C17A C18A C19A C20A -1.5(5) . . . . ?
C17A C18A C19A C22A 179.2(3) . . . . ?
C18A C19A C20A C21A 0.8(5) . . . . ?
C22A C19A C20A C21A -179.9(3) . . . . ?
C19A C20A C21A C16A 0.7(4) . . . . ?
C17A C16A C21A C20A -1.5(4) . . . . ?
C4A C16A C21A C20A 179.1(3) . . . . ?
C18A C19A C22A F1B 144.0(11) . . . . ?
C20A C19A C22A F1B -35.2(11) . . . . ?
C18A C19A C22A F2B 8.7(12) . . . . ?
C20A C19A C22A F2B -170.6(11) . . . . ?
C18A C19A C22A F3A -155.1(4) . . . . ?
C20A C19A C22A F3A 25.6(5) . . . . ?
C18A C19A C22A F2A -30.5(5) . . . . ?
C20A C19A C22A F2A 150.2(4) . . . . ?
C18A C19A C22A F1A 88.7(4) . . . . ?
C20A C19A C22A F1A -90.6(4) . . . . ?
C18A C19A C22A F3B -105.4(7) . . . . ?
C20A C19A C22A F3B 75.3(7) . . . . ?
C4A C5A C23A C28A -131.0(3) . . . . ?
C1A C5A C23A C28A 54.6(4) . . . . ?
C4A C5A C23A C24A 47.4(5) . . . . ?
C1A C5A C23A C24A -127.0(3) . . . . ?
C28A C23A C24A C25A 2.0(4) . . . . ?
C5A C23A C24A C25A -176.4(3) . . . . ?
C23A C24A C25A C26A -0.1(4) . . . . ?
C24A C25A C26A C27A -1.1(4) . . . . ?
C24A C25A C26A C29A 177.7(3) . . . . ?
C25A C26A C27A C28A 0.3(4) . . . . ?
C29A C26A C27A C28A -178.6(3) . . . . ?
C26A C27A C28A C23A 1.7(4) . . . . ?
C24A C23A C28A C27A -2.8(4) . . . . ?
C5A C23A C28A C27A 175.6(3) . . . . ?
C27A C26A C29A F4B 119.5(15) . . . . ?
C25A C26A C29A F4B -59.3(15) . . . . ?
C27A C26A C29A F6B -114.6(15) . . . . ?
C25A C26A C29A F6B 66.6(15) . . . . ?
C27A C26A C29A F5A 59.2(4) . . . . ?
C25A C26A C29A F5A -119.6(4) . . . . ?
C27A C26A C29A F6A -63.2(4) . . . . ?
C25A C26A C29A F6A 117.9(4) . . . . ?
C27A C26A C29A F5B -3.8(12) . . . . ?
C25A C26A C29A F5B 177.4(11) . . . . ?
C27A C26A C29A F4A 179.2(3) . . . . ?
C25A C26A C29A F4A 0.4(4) . . . . ?

_refine_diff_density_max         0.385
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.055


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk34db
_database_code_depnum_ccdc_archive 'CCDC 2338292'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_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

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3708(3)
_cell_length_b                   12.4378(2)
_cell_length_c                   13.3652(3)
_cell_angle_alpha                99.388(2)
_cell_angle_beta                 97.450(2)
_cell_angle_gamma                109.190(2)
_cell_volume                     1878.73(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56141
_cell_measurement_theta_min      3.4110
_cell_measurement_theta_max      77.3580

_exptl_crystal_description       'fragment of block'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    5.516
_shelx_estimated_absorpt_T_min   0.298
_shelx_estimated_absorpt_T_max   0.637
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_
_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
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_T_max  1.000
_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.
;
_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
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            81045
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.419
_diffrn_reflns_theta_max         77.751
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7933
_reflns_number_gt                7775
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0443P)²+1.0640P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7933
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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_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_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) . . . . ?

_refine_diff_density_max         0.801
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.050


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lk38db
_database_code_depnum_ccdc_archive 'CCDC 2338296'
loop_
_audit_author_name
_audit_author_address
'Dirk Bockfeld'
;TU Braunschweig
Germany
;
_audit_update_record             
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H49 Fe N3 O3, 0.5(C6 H14)'
_chemical_formula_sum            'C42 H56 Fe N3 O3'
_chemical_formula_weight         706.74

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1854(5)
_cell_length_b                   12.6987(5)
_cell_length_c                   14.8312(7)
_cell_angle_alpha                86.447(4)
_cell_angle_beta                 71.724(4)
_cell_angle_gamma                71.449(4)
_cell_volume                     1894.75(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    34943
_cell_measurement_theta_min      2.0300
_cell_measurement_theta_max      34.0940

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_F_000             758
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.440
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.987
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 17 0 0.0143
0 -17 0 0.0152
-15 -5 -10 0.0644
-1 0 19 0.0733
-4 -2 -21 0.0601
14 4 16 0.0729
15 5 12 0.0867
-8 -16 5 0.0543
-10 0 10 0.0859
9 -5 -10 0.1242
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
0.3130 17.0842 -0.3842 0.0263 0.9980 0.0575
-0.3572 -17.0999 0.4266 -0.0263 -0.9982 -0.0534
-15.4687 -4.7011 -10.2058 -0.8512 0.0218 0.5244
-1.4504 0.0009 19.1071 0.6029 -0.0168 0.7976
-3.6613 -1.5174 -20.8005 -0.8270 0.0224 -0.5617
13.6608 4.2966 15.5971 0.9757 -0.0254 -0.2175
15.0361 4.6199 12.2052 0.9051 -0.0233 -0.4245
-8.0808 -15.7376 5.3739 -0.1036 -0.7920 0.6016
-10.0160 0.4897 10.1790 0.0255 0.1841 0.9826
8.8187 -4.5511 -9.6870 -0.0542 -0.4022 -0.9139
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_T_max  1.000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.699
_oxdiff_exptl_absorpt_empirical_full_max 1.272
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      101(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            25609
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.020
_diffrn_reflns_theta_max         32.037
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             25609
_reflns_number_gt                18980
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'

_computing_structure_solution    
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_computing_structure_refinement  
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_molecular_graphics    ?
_computing_publication_material  
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'

_refine_special_details          
;
 All H atoms were placed in idealised positions and refined using a riding
 model, with a common U restrained to be 1.2 (1.5 for methyl groups) times
 the equivalent isotropic displacement parameter of the parent atom.
 Ordered methyl groups were treated as rigid bodies and allowed to
 rotate around the E-CH3 bond.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 One ter-butyl group was found disordered and refined accordingly.

 Refined as a 2-component twin. Component 2 rotated by 0.8207°
 around [0.13 0.08 -0.99] (reciprocal) or [0.52 -0.01 -0.85] (direct)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0341P)²+4.3963P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         25609
_refine_ls_number_parameters     482
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0847
_refine_ls_wR_factor_ref         0.1632
_refine_ls_wR_factor_gt          0.1506
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.74755(4) 0.60356(3) 0.18021(3) 0.01627(9) Uani 1 1 d . . . . .
O1 O 0.55726(19) 0.45028(15) 0.16627(14) 0.0231(4) Uani 1 1 d . . . . .
O2 O 1.0248(2) 0.59237(17) 0.14016(15) 0.0273(4) Uani 1 1 d . . . . .
O3 O 0.6741(2) 0.84649(17) 0.17474(16) 0.0349(5) Uani 1 1 d . . . . .
N1 N 0.8462(2) 0.33391(17) 0.16043(16) 0.0188(4) Uani 1 1 d . . . . .
N2 N 0.8812(2) 0.43982(18) 0.32113(16) 0.0197(4) Uani 1 1 d . . . . .
N3 N 0.7313(2) 0.58044(18) 0.05632(16) 0.0208(4) Uani 1 1 d . . . . .
C1 C 0.6154(3) 0.4814(2) 0.21292(18) 0.0176(5) Uani 1 1 d . . . . .
C2 C 0.7553(3) 0.4303(2) 0.21203(18) 0.0171(5) Uani 1 1 d . . . . .
C3 C 0.7728(2) 0.4841(2) 0.28751(18) 0.0176(5) Uani 1 1 d . . . . .
C4 C 0.6604(3) 0.5832(2) 0.32082(18) 0.0174(5) Uani 1 1 d . . . . .
C5 C 0.5661(3) 0.5849(2) 0.27161(18) 0.0183(5) Uani 1 1 d . . . . .
C6 C 0.8052(3) 0.2804(2) 0.0945(2) 0.0223(5) Uani 1 1 d . . . . .
H6A H 0.807074 0.323820 0.036550 0.027 Uiso 1 1 calc R U . . .
H6B H 0.713271 0.279293 0.125236 0.027 Uiso 1 1 calc R U . . .
C7 C 0.8982(3) 0.1618(2) 0.0674(2) 0.0269(6) Uani 1 1 d . . . . .
H7A H 0.891680 0.117358 0.124979 0.032 Uiso 1 1 calc R U . . .
H7B H 0.870709 0.127506 0.022410 0.032 Uiso 1 1 calc R U . . .
C8 C 1.0415(3) 0.1597(2) 0.0218(2) 0.0279(6) Uani 1 1 d . . . . .
H8A H 1.100681 0.081853 0.009202 0.033 Uiso 1 1 calc R U . . .
H8B H 1.050696 0.196939 -0.039540 0.033 Uiso 1 1 calc R U . . .
C9 C 1.0810(3) 0.2193(2) 0.0882(2) 0.0260(6) Uani 1 1 d . . . . .
H9A H 1.170972 0.224327 0.055887 0.031 Uiso 1 1 calc R U . . .
H9B H 1.084083 0.175656 0.145545 0.031 Uiso 1 1 calc R U . . .
C10 C 0.9838(3) 0.3359(2) 0.11778(19) 0.0209(5) Uani 1 1 d . . . . .
H10A H 1.008992 0.369981 0.164323 0.025 Uiso 1 1 calc R U . . .
H10B H 0.989025 0.382348 0.061439 0.025 Uiso 1 1 calc R U . . .
C11 C 0.8891(3) 0.3297(2) 0.3621(2) 0.0271(6) Uani 1 1 d . . . . .
H11A H 0.863737 0.284864 0.323380 0.033 Uiso 1 1 calc R U . . .
H11B H 0.826309 0.338970 0.427386 0.033 Uiso 1 1 calc R U . . .
C12 C 1.0290(3) 0.2695(2) 0.3645(2) 0.0321(7) Uani 1 1 d . . . . .
H12A H 1.090068 0.252078 0.298713 0.039 Uiso 1 1 calc R U . . .
H12B H 1.031358 0.198586 0.396699 0.039 Uiso 1 1 calc R U . . .
C13 C 1.0753(3) 0.3405(2) 0.4168(2) 0.0298(6) Uani 1 1 d . . . . .
H13A H 1.168875 0.302382 0.413506 0.036 Uiso 1 1 calc R U . . .
H13B H 1.020760 0.350986 0.484587 0.036 Uiso 1 1 calc R U . . .
C14 C 1.0628(3) 0.4537(2) 0.3720(2) 0.0253(6) Uani 1 1 d . . . . .
H14A H 1.089268 0.500714 0.408027 0.030 Uiso 1 1 calc R U . . .
H14B H 1.123150 0.443555 0.305807 0.030 Uiso 1 1 calc R U . . .
C15 C 0.9203(3) 0.5114(2) 0.37245(19) 0.0214(5) Uani 1 1 d . . . . .
H15A H 0.860366 0.525903 0.438711 0.026 Uiso 1 1 calc R U . . .
H15B H 0.913659 0.583470 0.341522 0.026 Uiso 1 1 calc R U . . .
C16 C 0.6288(2) 0.6509(2) 0.40915(18) 0.0178(5) Uani 1 1 d . . . . .
C17 C 0.5856(3) 0.6060(2) 0.4971(2) 0.0297(6) Uani 1 1 d . . . . .
H17 H 0.579567 0.532863 0.499368 0.036 Uiso 1 1 calc R U . . .
C18 C 0.5513(3) 0.6664(3) 0.5816(2) 0.0315(7) Uani 1 1 d . . . . .
H18 H 0.520657 0.634184 0.640342 0.038 Uiso 1 1 calc R U . . .
C19 C 0.5609(3) 0.7734(2) 0.58203(18) 0.0196(5) Uani 1 1 d . . . . .
C20 C 0.6103(3) 0.8149(2) 0.49441(19) 0.0230(5) Uani 1 1 d . . . . .
H20 H 0.621298 0.886290 0.492054 0.028 Uiso 1 1 calc R U . . .
C21 C 0.6442(3) 0.7548(2) 0.40973(19) 0.0224(5) Uani 1 1 d . . . . .
H21 H 0.678615 0.785701 0.351109 0.027 Uiso 1 1 calc R U . . .
C22 C 0.5180(3) 0.8410(2) 0.67559(19) 0.0234(5) Uani 1 1 d . . . . .
C23 C 0.5624(3) 0.7672(3) 0.7524(2) 0.0300(6) Uani 1 1 d . . . . .
H23A H 0.524620 0.706030 0.762601 0.045 Uiso 1 1 calc R U . . .
H23B H 0.531656 0.811581 0.811860 0.045 Uiso 1 1 calc R U . . .
H23C H 0.659481 0.736954 0.731956 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5767(3) 0.9370(2) 0.6636(2) 0.0301(6) Uani 1 1 d . . . . .
H24A H 0.673635 0.907467 0.638555 0.045 Uiso 1 1 calc R U . . .
H24B H 0.550974 0.975424 0.725360 0.045 Uiso 1 1 calc R U . . .
H24C H 0.542911 0.989450 0.619240 0.045 Uiso 1 1 calc R U . . .
C25 C 0.3659(3) 0.8885(3) 0.7084(2) 0.0380(8) Uani 1 1 d . . . . .
H25A H 0.336976 0.936306 0.659802 0.057 Uiso 1 1 calc R U . . .
H25B H 0.335746 0.932263 0.768143 0.057 Uiso 1 1 calc R U . . .
H25C H 0.327969 0.827422 0.718357 0.057 Uiso 1 1 calc R U . . .
C26 C 0.4290(3) 0.6618(2) 0.29037(18) 0.0190(5) Uani 1 1 d . . . . .
C27 C 0.3275(3) 0.6218(2) 0.2864(2) 0.0234(5) Uani 1 1 d . . . . .
H27 H 0.345944 0.544249 0.276538 0.028 Uiso 1 1 calc R U . . .
C28 C 0.2001(3) 0.6934(2) 0.2965(2) 0.0248(6) Uani 1 1 d . . . . .
H28 H 0.133686 0.663638 0.293008 0.030 Uiso 1 1 calc R U . . .
C29 C 0.1676(3) 0.8075(2) 0.3116(2) 0.0227(5) Uani 1 1 d . . . . .
C30 C 0.2666(3) 0.8462(2) 0.3214(2) 0.0281(6) Uani 1 1 d . . . . .
H30 H 0.246110 0.922985 0.335747 0.034 Uiso 1 1 calc R U . . .
C31 C 0.3940(3) 0.7757(2) 0.3108(2) 0.0269(6) Uani 1 1 d . . . . .
H31 H 0.458823 0.805428 0.317490 0.032 Uiso 1 1 calc R U . . .
C32 C 0.0301(3) 0.8868(2) 0.3150(2) 0.0268(6) Uani 1 1 d . . . . .
C36 C 0.9167(3) 0.5954(2) 0.15165(18) 0.0209(5) Uani 1 1 d . . . . .
C37 C 0.7000(3) 0.7516(2) 0.17796(19) 0.0225(5) Uani 1 1 d . . . . .
C38 C 0.7068(3) 0.5598(2) -0.00787(19) 0.0226(5) Uani 1 1 d . . . . .
C39 C 0.6719(3) 0.5313(3) -0.0881(2) 0.0358(7) Uani 1 1 d . . . . .
H39A H 0.714341 0.565022 -0.145345 0.054 Uiso 1 1 calc R U . . .
H39B H 0.575419 0.559482 -0.074431 0.054 Uiso 1 1 calc R U . . .
H39C H 0.702656 0.450354 -0.098368 0.054 Uiso 1 1 calc R U . . .
C33 C 0.0089(6) 0.8713(5) 0.2127(4) 0.0349(14) Uani 0.563(6) 1 d . . P A 1
H33A H -0.080143 0.917838 0.213519 0.052 Uiso 0.563(6) 1 calc R U P A 1
H33B H 0.018859 0.793159 0.201841 0.052 Uiso 0.563(6) 1 calc R U P A 1
H33C H 0.075348 0.893509 0.161578 0.052 Uiso 0.563(6) 1 calc R U P A 1
C34 C 0.0175(6) 1.0075(4) 0.3205(5) 0.0326(14) Uani 0.563(6) 1 d . . P A 1
H34A H 0.088464 1.023087 0.268599 0.049 Uiso 0.563(6) 1 calc R U P A 1
H34B H 0.024486 1.025432 0.381574 0.049 Uiso 0.563(6) 1 calc R U P A 1
H34C H -0.068820 1.052814 0.314917 0.049 Uiso 0.563(6) 1 calc R U P A 1
C35 C -0.0752(5) 0.8566(5) 0.3896(5) 0.0375(15) Uani 0.563(6) 1 d . . P A 1
H35A H -0.066431 0.866212 0.452005 0.056 Uiso 0.563(6) 1 calc R U P A 1
H35B H -0.067004 0.778831 0.379011 0.056 Uiso 0.563(6) 1 calc R U P A 1
H35C H -0.162208 0.904636 0.387295 0.056 Uiso 0.563(6) 1 calc R U P A 1
C33A C 0.0443(7) 0.9793(6) 0.2521(6) 0.0319(17) Uani 0.437(6) 1 d . . P A 2
H33D H -0.043816 1.030241 0.255350 0.048 Uiso 0.437(6) 1 calc R U P A 2
H33E H 0.092182 0.949956 0.186669 0.048 Uiso 0.437(6) 1 calc R U P A 2
H33F H 0.093861 1.019250 0.272540 0.048 Uiso 0.437(6) 1 calc R U P A 2
C34A C -0.0386(8) 0.9445(7) 0.4240(5) 0.039(2) Uani 0.437(6) 1 d . . P A 2
H34D H 0.017175 0.984185 0.436458 0.058 Uiso 0.437(6) 1 calc R U P A 2
H34E H -0.046591 0.886465 0.470143 0.058 Uiso 0.437(6) 1 calc R U P A 2
H34F H -0.126802 0.996903 0.429832 0.058 Uiso 0.437(6) 1 calc R U P A 2
C35A C -0.0620(8) 0.8315(6) 0.3036(8) 0.047(3) Uani 0.437(6) 1 d . . P A 2
H35D H -0.148809 0.886925 0.310416 0.071 Uiso 0.437(6) 1 calc R U P A 2
H35E H -0.071566 0.776331 0.352298 0.071 Uiso 0.437(6) 1 calc R U P A 2
H35F H -0.027017 0.794343 0.240413 0.071 Uiso 0.437(6) 1 calc R U P A 2
C40 C 0.3906(4) 0.7918(3) 0.0514(3) 0.0480(9) Uani 1 1 d . . . . .
H40A H 0.417593 0.762531 -0.014011 0.072 Uiso 1 1 calc R U . . .
H40B H 0.304051 0.783866 0.086768 0.072 Uiso 1 1 calc R U . . .
H40C H 0.456523 0.750247 0.082029 0.072 Uiso 1 1 calc R U . . .
C41 C 0.3811(4) 0.9132(4) 0.0505(4) 0.0744(16) Uani 1 1 d . . . . .
H41A H 0.312066 0.953938 0.021258 0.089 Uiso 1 1 calc R U . . .
H41B H 0.350201 0.941834 0.117231 0.089 Uiso 1 1 calc R U . . .
C42 C 0.5025(4) 0.9400(3) 0.0007(3) 0.0470(9) Uani 1 1 d . . . . .
H42A H 0.532516 0.911681 -0.065996 0.056 Uiso 1 1 calc R U . . .
H42B H 0.571593 0.897946 0.029510 0.056 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C36 1.775(3) . ?
Fe1 C37 1.784(3) . ?
Fe1 N3 1.951(2) . ?
Fe1 C4 2.046(3) . ?
Fe1 C5 2.134(3) . ?
Fe1 C3 2.150(2) . ?
Fe1 C2 2.201(2) . ?
Fe1 C1 2.397(2) . ?
O1 C1 1.240(3) . ?
O2 C36 1.154(3) . ?
O3 C37 1.148(3) . ?
N1 C2 1.398(3) . ?
N1 C10 1.477(3) . ?
N1 C6 1.480(3) . ?
N2 C3 1.395(3) . ?
N2 C15 1.464(3) . ?
N2 C11 1.477(3) . ?
N3 C38 1.136(3) . ?
C1 C5 1.473(3) . ?
C1 C2 1.488(3) . ?
C2 C3 1.440(3) . ?
C3 C4 1.445(3) . ?
C4 C5 1.453(3) . ?
C4 C16 1.495(3) . ?
C5 C26 1.482(3) . ?
C6 C7 1.526(4) . ?
C7 C8 1.524(4) . ?
C8 C9 1.522(4) . ?
C9 C10 1.524(4) . ?
C11 C12 1.518(4) . ?
C12 C13 1.523(4) . ?
C13 C14 1.530(4) . ?
C14 C15 1.526(4) . ?
C16 C21 1.384(3) . ?
C16 C17 1.396(4) . ?
C17 C18 1.391(4) . ?
C18 C19 1.397(4) . ?
C19 C20 1.386(4) . ?
C19 C22 1.536(4) . ?
C20 C21 1.393(4) . ?
C22 C23 1.533(4) . ?
C22 C25 1.536(4) . ?
C22 C24 1.537(4) . ?
C26 C31 1.400(4) . ?
C26 C27 1.401(4) . ?
C27 C28 1.392(4) . ?
C28 C29 1.392(4) . ?
C29 C30 1.393(4) . ?
C29 C32 1.535(4) . ?
C30 C31 1.386(4) . ?
C32 C33A 1.470(7) . ?
C32 C35A 1.473(8) . ?
C32 C35 1.475(7) . ?
C32 C34 1.498(6) . ?
C32 C33 1.640(6) . ?
C32 C34A 1.658(8) . ?
C38 C39 1.460(4) . ?
C40 C41 1.511(6) . ?
C41 C42 1.463(6) . ?
C42 C42 1.506(8) 2_675 ?

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
C36 Fe1 C37 90.64(12) . . ?
C36 Fe1 N3 102.58(11) . . ?
C37 Fe1 N3 95.90(10) . . ?
C36 Fe1 C4 113.79(11) . . ?
C37 Fe1 C4 100.58(11) . . ?
N3 Fe1 C4 139.58(10) . . ?
C36 Fe1 C5 153.69(11) . . ?
C37 Fe1 C5 99.54(11) . . ?
N3 Fe1 C5 100.43(9) . . ?
C4 Fe1 C5 40.63(9) . . ?
C36 Fe1 C3 89.55(11) . . ?
C37 Fe1 C3 134.92(11) . . ?
N3 Fe1 C3 127.91(9) . . ?
C4 Fe1 C3 40.20(10) . . ?
C5 Fe1 C3 66.10(9) . . ?
C36 Fe1 C2 102.00(11) . . ?
C37 Fe1 C2 164.93(11) . . ?
N3 Fe1 C2 89.38(9) . . ?
C4 Fe1 C2 66.94(9) . . ?
C5 Fe1 C2 65.56(9) . . ?
C3 Fe1 C2 38.62(9) . . ?
C36 Fe1 C1 138.93(10) . . ?
C37 Fe1 C1 130.43(11) . . ?
N3 Fe1 C1 76.98(9) . . ?
C4 Fe1 C1 64.21(9) . . ?
C5 Fe1 C1 37.38(9) . . ?
C3 Fe1 C1 62.36(9) . . ?
C2 Fe1 C1 37.45(8) . . ?
C2 N1 C10 115.9(2) . . ?
C2 N1 C6 118.2(2) . . ?
C10 N1 C6 111.4(2) . . ?
C3 N2 C15 120.3(2) . . ?
C3 N2 C11 113.5(2) . . ?
C15 N2 C11 113.6(2) . . ?
C38 N3 Fe1 169.1(2) . . ?
O1 C1 C5 127.1(2) . . ?
O1 C1 C2 127.6(2) . . ?
C5 C1 C2 104.93(19) . . ?
O1 C1 Fe1 132.86(19) . . ?
C5 C1 Fe1 61.57(13) . . ?
C2 C1 Fe1 64.11(13) . . ?
N1 C2 C3 125.1(2) . . ?
N1 C2 C1 126.2(2) . . ?
C3 C2 C1 107.7(2) . . ?
N1 C2 Fe1 127.50(18) . . ?
C3 C2 Fe1 68.79(13) . . ?
C1 C2 Fe1 78.44(14) . . ?
N2 C3 C2 122.5(2) . . ?
N2 C3 C4 128.7(2) . . ?
C2 C3 C4 108.8(2) . . ?
N2 C3 Fe1 129.28(18) . . ?
C2 C3 Fe1 72.59(14) . . ?
C4 C3 Fe1 65.99(13) . . ?
C3 C4 C5 107.4(2) . . ?
C3 C4 C16 125.2(2) . . ?
C5 C4 C16 125.0(2) . . ?
C3 C4 Fe1 73.80(15) . . ?
C5 C4 Fe1 72.96(15) . . ?
C16 C4 Fe1 132.73(18) . . ?
C4 C5 C1 108.8(2) . . ?
C4 C5 C26 127.6(2) . . ?
C1 C5 C26 122.3(2) . . ?
C4 C5 Fe1 66.42(14) . . ?
C1 C5 Fe1 81.05(15) . . ?
C26 C5 Fe1 129.06(18) . . ?
N1 C6 C7 110.2(2) . . ?
C8 C7 C6 111.3(2) . . ?
C9 C8 C7 109.5(2) . . ?
C8 C9 C10 111.6(2) . . ?
N1 C10 C9 111.6(2) . . ?
N2 C11 C12 110.3(2) . . ?
C11 C12 C13 110.9(2) . . ?
C12 C13 C14 109.9(2) . . ?
C15 C14 C13 110.3(2) . . ?
N2 C15 C14 109.1(2) . . ?
C21 C16 C17 117.2(2) . . ?
C21 C16 C4 124.1(2) . . ?
C17 C16 C4 118.7(2) . . ?
C18 C17 C16 121.1(3) . . ?
C17 C18 C19 121.6(3) . . ?
C20 C19 C18 116.7(2) . . ?
C20 C19 C22 122.2(2) . . ?
C18 C19 C22 121.1(2) . . ?
C19 C20 C21 121.8(2) . . ?
C16 C21 C20 121.4(2) . . ?
C23 C22 C25 109.1(3) . . ?
C23 C22 C19 111.0(2) . . ?
C25 C22 C19 107.7(2) . . ?
C23 C22 C24 107.7(2) . . ?
C25 C22 C24 109.2(3) . . ?
C19 C22 C24 112.0(2) . . ?
C31 C26 C27 116.8(2) . . ?
C31 C26 C5 123.1(2) . . ?
C27 C26 C5 120.1(2) . . ?
C28 C27 C26 121.3(2) . . ?
C29 C28 C27 121.6(2) . . ?
C28 C29 C30 116.9(2) . . ?
C28 C29 C32 121.3(2) . . ?
C30 C29 C32 121.8(2) . . ?
C31 C30 C29 121.9(2) . . ?
C30 C31 C26 121.3(3) . . ?
C33A C32 C35A 115.4(5) . . ?
C35 C32 C34 113.0(4) . . ?
C33A C32 C29 109.8(4) . . ?
C35A C32 C29 114.4(3) . . ?
C35 C32 C29 110.9(3) . . ?
C34 C32 C29 114.1(3) . . ?
C35 C32 C33 107.3(4) . . ?
C34 C32 C33 103.7(4) . . ?
C29 C32 C33 107.2(3) . . ?
C33A C32 C34A 105.2(5) . . ?
C35A C32 C34A 104.8(6) . . ?
C29 C32 C34A 106.1(3) . . ?
O2 C36 Fe1 174.8(2) . . ?
O3 C37 Fe1 177.5(3) . . ?
N3 C38 C39 177.9(3) . . ?
C42 C41 C40 116.7(4) . . ?
C41 C42 C42 118.3(4) . 2_675 ?

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 -52.4(3) . . . . ?
C6 N1 C2 C3 171.5(2) . . . . ?
C10 N1 C2 C1 140.9(2) . . . . ?
C6 N1 C2 C1 4.8(4) . . . . ?
C10 N1 C2 Fe1 36.5(3) . . . . ?
C6 N1 C2 Fe1 -99.5(2) . . . . ?
O1 C1 C2 N1 -2.8(4) . . . . ?
C5 C1 C2 N1 -175.7(2) . . . . ?
Fe1 C1 C2 N1 -128.3(3) . . . . ?
O1 C1 C2 C3 -171.4(3) . . . . ?
C5 C1 C2 C3 15.7(3) . . . . ?
Fe1 C1 C2 C3 63.07(16) . . . . ?
O1 C1 C2 Fe1 125.5(3) . . . . ?
C5 C1 C2 Fe1 -47.39(17) . . . . ?
C15 N2 C3 C2 158.9(2) . . . . ?
C11 N2 C3 C2 -61.6(3) . . . . ?
C15 N2 C3 C4 -23.6(4) . . . . ?
C11 N2 C3 C4 115.8(3) . . . . ?
C15 N2 C3 Fe1 65.4(3) . . . . ?
C11 N2 C3 Fe1 -155.2(2) . . . . ?
N1 C2 C3 N2 -4.2(4) . . . . ?
C1 C2 C3 N2 164.5(2) . . . . ?
Fe1 C2 C3 N2 -125.9(2) . . . . ?
N1 C2 C3 C4 177.9(2) . . . . ?
C1 C2 C3 C4 -13.4(3) . . . . ?
Fe1 C2 C3 C4 56.16(17) . . . . ?
N1 C2 C3 Fe1 121.7(3) . . . . ?
C1 C2 C3 Fe1 -69.55(17) . . . . ?
N2 C3 C4 C5 -172.2(2) . . . . ?
C2 C3 C4 C5 5.6(3) . . . . ?
Fe1 C3 C4 C5 65.73(17) . . . . ?
N2 C3 C4 C16 -9.2(4) . . . . ?
C2 C3 C4 C16 168.5(2) . . . . ?
Fe1 C3 C4 C16 -131.3(3) . . . . ?
N2 C3 C4 Fe1 122.1(3) . . . . ?
C2 C3 C4 Fe1 -60.18(18) . . . . ?
C3 C4 C5 C1 4.5(3) . . . . ?
C16 C4 C5 C1 -158.5(2) . . . . ?
Fe1 C4 C5 C1 70.84(18) . . . . ?
C3 C4 C5 C26 171.6(2) . . . . ?
C16 C4 C5 C26 8.5(4) . . . . ?
Fe1 C4 C5 C26 -122.1(3) . . . . ?
C3 C4 C5 Fe1 -66.30(17) . . . . ?
C16 C4 C5 Fe1 130.7(3) . . . . ?
O1 C1 C5 C4 174.7(3) . . . . ?
C2 C1 C5 C4 -12.4(3) . . . . ?
Fe1 C1 C5 C4 -61.21(17) . . . . ?
O1 C1 C5 C26 6.9(4) . . . . ?
C2 C1 C5 C26 179.8(2) . . . . ?
Fe1 C1 C5 C26 130.9(3) . . . . ?
O1 C1 C5 Fe1 -124.1(3) . . . . ?
C2 C1 C5 Fe1 48.84(17) . . . . ?
C2 N1 C6 C7 -163.6(2) . . . . ?
C10 N1 C6 C7 58.5(3) . . . . ?
N1 C6 C7 C8 -58.0(3) . . . . ?
C6 C7 C8 C9 55.3(3) . . . . ?
C7 C8 C9 C10 -53.5(3) . . . . ?
C2 N1 C10 C9 163.8(2) . . . . ?
C6 N1 C10 C9 -57.2(3) . . . . ?
C8 C9 C10 N1 55.0(3) . . . . ?
C3 N2 C11 C12 159.9(2) . . . . ?
C15 N2 C11 C12 -57.8(3) . . . . ?
N2 C11 C12 C13 54.7(3) . . . . ?
C11 C12 C13 C14 -55.1(3) . . . . ?
C12 C13 C14 C15 56.7(3) . . . . ?
C3 N2 C15 C14 -161.5(2) . . . . ?
C11 N2 C15 C14 59.1(3) . . . . ?
C13 C14 C15 N2 -57.8(3) . . . . ?
C3 C4 C16 C21 107.5(3) . . . . ?
C5 C4 C16 C21 -92.4(3) . . . . ?
Fe1 C4 C16 C21 6.8(4) . . . . ?
C3 C4 C16 C17 -70.0(4) . . . . ?
C5 C4 C16 C17 90.1(3) . . . . ?
Fe1 C4 C16 C17 -170.8(2) . . . . ?
C21 C16 C17 C18 4.1(4) . . . . ?
C4 C16 C17 C18 -178.2(3) . . . . ?
C16 C17 C18 C19 -1.2(5) . . . . ?
C17 C18 C19 C20 -2.1(5) . . . . ?
C17 C18 C19 C22 177.8(3) . . . . ?
C18 C19 C20 C21 2.3(4) . . . . ?
C22 C19 C20 C21 -177.5(3) . . . . ?
C17 C16 C21 C20 -3.9(4) . . . . ?
C4 C16 C21 C20 178.6(3) . . . . ?
C19 C20 C21 C16 0.7(4) . . . . ?
C20 C19 C22 C23 -139.0(3) . . . . ?
C18 C19 C22 C23 41.1(4) . . . . ?
C20 C19 C22 C25 101.6(3) . . . . ?
C18 C19 C22 C25 -78.3(3) . . . . ?
C20 C19 C22 C24 -18.5(4) . . . . ?
C18 C19 C22 C24 161.6(3) . . . . ?
C4 C5 C26 C31 41.1(4) . . . . ?
C1 C5 C26 C31 -153.5(3) . . . . ?
Fe1 C5 C26 C31 -47.5(4) . . . . ?
C4 C5 C26 C27 -140.2(3) . . . . ?
C1 C5 C26 C27 25.3(4) . . . . ?
Fe1 C5 C26 C27 131.3(2) . . . . ?
C31 C26 C27 C28 3.8(4) . . . . ?
C5 C26 C27 C28 -175.0(3) . . . . ?
C26 C27 C28 C29 -0.4(5) . . . . ?
C27 C28 C29 C30 -3.4(4) . . . . ?
C27 C28 C29 C32 175.2(3) . . . . ?
C28 C29 C30 C31 3.9(5) . . . . ?
C32 C29 C30 C31 -174.7(3) . . . . ?
C29 C30 C31 C26 -0.5(5) . . . . ?
C27 C26 C31 C30 -3.3(4) . . . . ?
C5 C26 C31 C30 175.5(3) . . . . ?
C28 C29 C32 C33A -130.2(4) . . . . ?
C30 C29 C32 C33A 48.4(5) . . . . ?
C28 C29 C32 C35A 1.5(6) . . . . ?
C30 C29 C32 C35A -179.9(5) . . . . ?
C28 C29 C32 C35 57.8(5) . . . . ?
C30 C29 C32 C35 -123.6(4) . . . . ?
C28 C29 C32 C34 -173.2(4) . . . . ?
C30 C29 C32 C34 5.3(5) . . . . ?
C28 C29 C32 C33 -59.0(4) . . . . ?
C30 C29 C32 C33 119.5(4) . . . . ?
C28 C29 C32 C34A 116.6(4) . . . . ?
C30 C29 C32 C34A -64.8(5) . . . . ?
C40 C41 C42 C42 -179.3(5) . . . 2_675 ?

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.083


