# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2116935'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2021-10-21 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 H10 Fe3 O18), C3 H12 N2'
_chemical_formula_sum            'C19 H32 Fe6 N2 O36'
_chemical_formula_weight         1199.56
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   28.903(4)
_cell_length_b                   6.9208(11)
_cell_length_c                   20.641(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.589(17)
_cell_angle_gamma                90
_cell_volume                     3977.0(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5980
_cell_measurement_theta_min      3.0910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1544
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9503
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.820
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -48.00   1.00   50.00    --   30.00  54.00  60.00   25
  2  ω     87.00 113.00   1.00   50.00    --   30.00  54.00  60.00   26
  3  ω    -65.00 119.00   1.00   50.00    --   30.00  54.00 -90.00  184
  4  ω      3.00 111.00   1.00   50.00    --   30.00  54.00-180.00  108
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046366000
_diffrn_orient_matrix_UB_12      0.0047599000
_diffrn_orient_matrix_UB_13      -0.0354553000
_diffrn_orient_matrix_UB_21      -0.0249505000
_diffrn_orient_matrix_UB_22      0.0071272000
_diffrn_orient_matrix_UB_23      -0.0029617000
_diffrn_orient_matrix_UB_31      0.0018859000
_diffrn_orient_matrix_UB_32      0.1023194000
_diffrn_orient_matrix_UB_33      0.0019845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5694
_reflns_number_total             9503
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         9503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.1284
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+109.3481P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2718
_refine_ls_wR_factor_ref         0.3275
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.532(7)
 0.468(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Others
 Fixed Sof: H9A(0.5) H9B(0.5)
4.a Rotating group:
 O17(H17A,H17B)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C5(H5), C2(H2), C4(H4), C6(H6), C1(H1), C8(H8)
4.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.53616(8) 0.2562(3) 0.13880(12) 0.0312(7) Uani 1 1 d . . . . .
Fe3 Fe 0.63540(10) 0.3970(3) 0.09958(13) 0.0348(7) Uani 1 1 d . . . . .
Fe2 Fe 0.64413(9) 0.2169(3) 0.25111(13) 0.0338(7) Uani 1 1 d . . . . .
O004 O 0.6053(4) 0.2899(14) 0.1632(6) 0.025(2) Uani 1 1 d . . . . .
O13 O 0.4654(4) 0.2139(17) 0.1124(6) 0.038(3) Uani 1 1 d . . . . .
O8 O 0.5980(5) 0.232(2) 0.0211(7) 0.051(4) Uani 1 1 d . . . . .
O11 O 0.5409(5) -0.0137(17) 0.1775(7) 0.049(4) Uani 1 1 d . . . . .
O9 O 0.5286(5) 0.3719(19) 0.2244(6) 0.048(3) Uani 1 1 d . . . . .
O4 O 0.6964(5) 0.0891(18) 0.2177(6) 0.044(3) Uani 1 1 d . . . . .
O10 O 0.5981(5) 0.324(2) 0.3013(6) 0.051(4) Uani 1 1 d . . . . .
O7 O 0.5344(5) 0.1294(17) 0.0502(6) 0.043(3) Uani 1 1 d . . . . .
O1 O 0.6787(5) 0.5808(17) 0.1635(6) 0.045(3) Uani 1 1 d . . . . .
O14 O 0.3873(5) 0.2689(19) 0.0754(7) 0.048(3) Uani 1 1 d . . . . .
O6 O 0.5223(5) 0.5192(17) 0.0935(7) 0.049(4) Uani 1 1 d . . . . .
O16 O 0.7331(5) -0.0366(19) 0.4210(6) 0.049(4) Uani 1 1 d . . . . .
O12 O 0.6150(5) -0.0494(18) 0.2472(7) 0.048(4) Uani 1 1 d . . . . .
O2 O 0.6788(5) 0.4767(18) 0.2666(7) 0.046(3) Uani 1 1 d . . . . .
O3 O 0.6870(5) 0.1915(19) 0.1121(7) 0.050(4) Uani 1 1 d . . . . .
O17 O 0.6691(4) 0.4978(17) 0.0287(7) 0.045(3) Uani 1 1 d . . . . .
H17A H 0.653830 0.558268 -0.007429 0.068 Uiso 1 1 d R U . . .
H17B H 0.699549 0.496043 0.030838 0.068 Uiso 1 1 d R U . . .
O5 O 0.5886(5) 0.6151(17) 0.0687(7) 0.048(4) Uani 1 1 d . . . . .
O15 O 0.6851(5) 0.1513(18) 0.3447(6) 0.047(3) Uani 1 1 d . . . . .
N1 N 0.6642(6) 0.418(2) 0.4400(8) 0.047(4) Uani 1 1 d . . . . .
H1A H 0.641884 0.496877 0.415750 0.057 Uiso 1 1 calc R U . . .
H1B H 0.652823 0.358269 0.470662 0.057 Uiso 1 1 calc R U . . .
H1C H 0.672084 0.330747 0.413121 0.057 Uiso 1 1 calc R U . . .
C3 C 0.5463(8) 0.635(2) 0.0712(10) 0.045(5) Uani 1 1 d . . . . .
H3 H 0.531269 0.749664 0.054175 0.054 Uiso 1 1 calc R U . . .
C7 C 0.4297(8) 0.316(3) 0.0925(9) 0.046(5) Uani 1 1 d . . . . .
H7 H 0.435611 0.447924 0.090032 0.056 Uiso 1 1 calc R U . . .
C5 C 0.5560(7) 0.378(3) 0.2829(9) 0.044(5) Uani 1 1 d . . . . .
H5 H 0.543116 0.428476 0.316060 0.052 Uiso 1 1 calc R U . . .
C2 C 0.7048(8) 0.087(3) 0.1610(10) 0.048(5) Uani 1 1 d . . . . .
H2 H 0.727047 -0.003720 0.155271 0.058 Uiso 1 1 calc R U . . .
C10 C 0.7065(7) 0.529(3) 0.4735(11) 0.048(5) Uani 1 1 d . . . . .
H10A H 0.699992 0.600579 0.510498 0.058 Uiso 1 1 calc R U . . .
H10B H 0.713274 0.622043 0.442016 0.058 Uiso 1 1 calc R U . . .
C9 C 0.750000 0.403(3) 0.500000 0.038(6) Uani 1 2 d S T P . .
H9A H 0.754818 0.321016 0.464291 0.045 Uiso 0.5 1 calc R U P . .
H9B H 0.745181 0.321027 0.535711 0.045 Uiso 0.5 1 calc R U P . .
C4 C 0.5609(9) 0.131(3) 0.0144(10) 0.057(6) Uani 1 1 d . . . . .
H4 H 0.553217 0.048181 -0.022453 0.069 Uiso 1 1 calc R U . . .
C6 C 0.5746(7) -0.108(3) 0.2174(11) 0.045(5) Uani 1 1 d . . . . .
H6 H 0.568058 -0.236565 0.224809 0.055 Uiso 1 1 calc R U . . .
C1 C 0.6889(8) 0.591(3) 0.2281(12) 0.053(6) Uani 1 1 d . . . . .
H1 H 0.706052 0.699608 0.247514 0.064 Uiso 1 1 calc R U . . .
C8 C 0.7053(7) -0.004(3) 0.3671(10) 0.049(5) Uani 1 1 d . . . . .
H8 H 0.697704 -0.109472 0.338130 0.058 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 O004 1.939(11) . ?
Fe1 O13 1.993(12) . ?
Fe1 O11 2.022(12) . ?
Fe1 O9 2.005(13) . ?
Fe1 O7 2.017(12) . ?
Fe1 O6 2.036(13) . ?
Fe3 O004 1.909(10) . ?
Fe3 O8 2.037(13) . ?
Fe3 O1 2.009(12) . ?
Fe3 O3 2.026(13) . ?
Fe3 O17 2.084(13) . ?
Fe3 O5 2.012(13) . ?
Fe2 O004 1.927(11) . ?
Fe2 O4 2.025(13) . ?
Fe2 O10 2.033(13) . ?
Fe2 O12 2.020(13) . ?
Fe2 O2 2.041(13) . ?
Fe2 O15 2.028(14) . ?
O13 C7 1.23(2) . ?
O8 C4 1.26(2) . ?
O11 C6 1.27(2) . ?
O9 C5 1.25(2) . ?
O4 C2 1.26(2) . ?
O10 C5 1.23(2) . ?
O7 C4 1.20(3) . ?
O1 C1 1.29(3) . ?
O14 C7 1.22(2) . ?
O6 C3 1.23(2) . ?
O16 C8 1.21(2) . ?
O12 C6 1.23(2) . ?
O2 C1 1.21(2) . ?
O3 C2 1.24(2) . ?
O17 H17A 0.8659 . ?
O17 H17B 0.8688 . ?
O5 C3 1.24(2) . ?
O15 C8 1.25(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C10 1.45(2) . ?
C3 H3 0.9300 . ?
C7 H7 0.9300 . ?
C5 H5 0.9300 . ?
C2 H2 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.51(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C1 H1 0.9300 . ?
C8 H8 0.9300 . ?

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
O004 Fe1 O13 178.3(5) . . ?
O004 Fe1 O11 93.0(5) . . ?
O004 Fe1 O9 94.1(5) . . ?
O004 Fe1 O7 93.5(5) . . ?
O004 Fe1 O6 94.2(5) . . ?
O13 Fe1 O11 85.8(5) . . ?
O13 Fe1 O9 87.2(5) . . ?
O13 Fe1 O7 85.1(5) . . ?
O13 Fe1 O6 86.8(5) . . ?
O11 Fe1 O6 172.4(6) . . ?
O9 Fe1 O11 91.8(6) . . ?
O9 Fe1 O7 172.2(6) . . ?
O9 Fe1 O6 89.6(6) . . ?
O7 Fe1 O11 86.5(6) . . ?
O7 Fe1 O6 91.1(6) . . ?
O004 Fe3 O8 95.0(5) . . ?
O004 Fe3 O1 96.4(5) . . ?
O004 Fe3 O3 95.5(5) . . ?
O004 Fe3 O17 176.7(5) . . ?
O004 Fe3 O5 96.7(5) . . ?
O8 Fe3 O17 82.9(5) . . ?
O1 Fe3 O8 168.5(6) . . ?
O1 Fe3 O3 93.1(6) . . ?
O1 Fe3 O17 85.6(5) . . ?
O1 Fe3 O5 88.9(6) . . ?
O3 Fe3 O8 85.6(6) . . ?
O3 Fe3 O17 81.8(5) . . ?
O5 Fe3 O8 90.0(6) . . ?
O5 Fe3 O3 167.3(6) . . ?
O5 Fe3 O17 85.9(5) . . ?
O004 Fe2 O4 95.3(5) . . ?
O004 Fe2 O10 95.1(5) . . ?
O004 Fe2 O12 94.0(5) . . ?
O004 Fe2 O2 93.1(5) . . ?
O004 Fe2 O15 177.7(5) . . ?
O4 Fe2 O10 169.5(5) . . ?
O4 Fe2 O2 93.4(6) . . ?
O4 Fe2 O15 85.9(5) . . ?
O10 Fe2 O2 87.7(6) . . ?
O12 Fe2 O4 85.9(6) . . ?
O12 Fe2 O10 91.7(6) . . ?
O12 Fe2 O2 172.9(6) . . ?
O12 Fe2 O15 88.0(5) . . ?
O15 Fe2 O10 83.8(5) . . ?
O15 Fe2 O2 84.9(6) . . ?
Fe3 O004 Fe1 119.7(6) . . ?
Fe3 O004 Fe2 119.5(6) . . ?
Fe2 O004 Fe1 120.8(5) . . ?
C7 O13 Fe1 135.6(12) . . ?
C4 O8 Fe3 130.8(13) . . ?
C6 O11 Fe1 133.4(12) . . ?
C5 O9 Fe1 132.2(12) . . ?
C2 O4 Fe2 132.1(12) . . ?
C5 O10 Fe2 133.0(12) . . ?
C4 O7 Fe1 133.6(13) . . ?
C1 O1 Fe3 130.1(13) . . ?
C3 O6 Fe1 133.8(14) . . ?
C6 O12 Fe2 130.5(12) . . ?
C1 O2 Fe2 131.8(13) . . ?
C2 O3 Fe3 130.1(13) . . ?
Fe3 O17 H17A 122.7 . . ?
Fe3 O17 H17B 128.2 . . ?
H17A O17 H17B 109.0 . . ?
C3 O5 Fe3 130.7(12) . . ?
C8 O15 Fe2 129.7(13) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C10 N1 H1A 109.5 . . ?
C10 N1 H1B 109.5 . . ?
C10 N1 H1C 109.5 . . ?
O6 C3 O5 127.4(17) . . ?
O6 C3 H3 116.3 . . ?
O5 C3 H3 116.3 . . ?
O13 C7 H7 115.6 . . ?
O14 C7 O13 128.8(17) . . ?
O14 C7 H7 115.6 . . ?
O9 C5 H5 116.5 . . ?
O10 C5 O9 127.0(17) . . ?
O10 C5 H5 116.5 . . ?
O4 C2 H2 116.1 . . ?
O3 C2 O4 127.8(18) . . ?
O3 C2 H2 116.1 . . ?
N1 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
N1 C10 C9 112.3(14) . . ?
H10A C10 H10B 107.9 . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C10 C9 C10 109.3(19) . 2_656 ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 2_656 . ?
C10 C9 H9B 109.8 2_656 . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
O8 C4 H4 116.4 . . ?
O7 C4 O8 127.2(19) . . ?
O7 C4 H4 116.4 . . ?
O11 C6 H6 116.2 . . ?
O12 C6 O11 127.6(17) . . ?
O12 C6 H6 116.2 . . ?
O1 C1 H1 116.0 . . ?
O2 C1 O1 127.9(18) . . ?
O2 C1 H1 116.0 . . ?
O16 C8 O15 129(2) . . ?
O16 C8 H8 115.5 . . ?
O15 C8 H8 115.5 . . ?

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
Fe1 O13 C7 O14 176.9(14) . . . . ?
Fe1 O11 C6 O12 5(4) . . . . ?
Fe1 O9 C5 O10 7(4) . . . . ?
Fe1 O7 C4 O8 -6(4) . . . . ?
Fe1 O6 C3 O5 2(3) . . . . ?
Fe3 O8 C4 O7 12(4) . . . . ?
Fe3 O1 C1 O2 9(3) . . . . ?
Fe3 O3 C2 O4 -3(4) . . . . ?
Fe3 O5 C3 O6 -1(3) . . . . ?
Fe2 O4 C2 O3 13(4) . . . . ?
Fe2 O10 C5 O9 3(4) . . . . ?
Fe2 O12 C6 O11 4(4) . . . . ?
Fe2 O2 C1 O1 2(4) . . . . ?
Fe2 O15 C8 O16 172.5(17) . . . . ?
N1 C10 C9 C10 173(2) . . . 2_656 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.529
_oxdiff_exptl_absorpt_empirical_full_min 0.721
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.532(7)
2 0.468(7)
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 2116937'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2021-10-26 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_audit_creation_date             2021-10-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 H10 Fe3 O18), C7 H20 N2'
_chemical_formula_sum            'C23 H40 Fe6 N2 O36'
_chemical_formula_weight         1255.67
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.1240(17)
_cell_length_b                   6.9163(6)
_cell_length_c                   28.584(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.658(7)
_cell_angle_gamma                90
_cell_volume                     4356.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3687
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7250
_cell_measurement_theta_min      3.1400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7719
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.002
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00 118.00   1.00  100.00    --   30.00  54.00-180.00  134
  2  ω      7.00 111.00   1.00  100.00    --   30.00  54.00  90.00  104
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179975000
_diffrn_orient_matrix_UB_12      -0.0066584000
_diffrn_orient_matrix_UB_13      -0.0249156000
_diffrn_orient_matrix_UB_21      0.0266835000
_diffrn_orient_matrix_UB_22      -0.0035329000
_diffrn_orient_matrix_UB_23      -0.0072984000
_diffrn_orient_matrix_UB_31      0.0003122000
_diffrn_orient_matrix_UB_32      -0.1022956000
_diffrn_orient_matrix_UB_33      0.0019117000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2967
_reflns_number_total             3823
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+12.9230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0979
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C2, N2, C1, C3, C4, C5, N1, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim N2 \\sim C1 \\sim C3 \\sim C4 \\sim C5 \\sim N1 \\sim C6 \\sim C7:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C7) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) C4(0.5) H4A(0.5) H4B(0.5) N2(0.5)
 H2C(0.5) H2D(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) N1(0.5) H1D(0.5) H1E(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
5.a Riding coordinates:
 O18(H18A,H18B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), N2(H2C,H2D), C3(H3A,H3B), N1(H1D,H1E), C5(H5A,H5B),
 C6(H6A,H6B)
5.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C15(H15), C11(H11), C9(H9), C8(H8), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe00 Fe 0.36911(2) 0.76015(8) 0.46412(2) 0.02810(16) Uani 1 1 d . . . . .
Fe1 Fe 0.39863(2) 0.92905(9) 0.36471(2) 0.02916(16) Uani 1 1 d . . . . .
Fe03 Fe 0.25938(2) 0.77946(9) 0.35620(2) 0.03102(17) Uani 1 1 d . . . . .
O1 O 0.34256(11) 0.8229(4) 0.39477(9) 0.0255(6) Uani 1 1 d . . . . .
O6 O 0.32789(14) 0.4984(4) 0.45491(11) 0.0458(8) Uani 1 1 d . . . . .
O4 O 0.39870(13) 0.6865(4) 0.53630(10) 0.0375(7) Uani 1 1 d . . . . .
O11 O 0.28275(13) 0.6536(5) 0.29961(11) 0.0444(8) Uani 1 1 d . . . . .
O7 O 0.25703(14) 0.5061(5) 0.38114(12) 0.0482(8) Uani 1 1 d . . . . .
O13 O 0.34266(14) 1.1356(5) 0.32560(12) 0.0474(8) Uani 1 1 d . . . . .
O15 O 0.44488(13) 0.6230(5) 0.46062(11) 0.0418(8) Uani 1 1 d . . . . .
O17 O 0.43098(15) 1.1320(5) 0.41630(11) 0.0489(8) Uani 1 1 d . . . . .
O5 O 0.44968(14) 0.7263(5) 0.61515(11) 0.0489(9) Uani 1 1 d . . . . .
O8 O 0.29686(13) 0.8802(5) 0.47882(11) 0.0458(8) Uani 1 1 d . . . . .
O10 O 0.37701(14) 0.7490(5) 0.30607(11) 0.0459(8) Uani 1 1 d . . . . .
O16 O 0.41336(14) 1.0138(4) 0.48259(10) 0.0427(8) Uani 1 1 d . . . . .
O18 O 0.46080(12) 1.0342(4) 0.33134(10) 0.0403(7) Uani 1 1 d . . . . .
H18A H 0.442232 1.089346 0.303081 0.060 Uiso 1 1 d R U . . .
H18B H 0.482292 1.129556 0.348511 0.060 Uiso 1 1 d R U . . .
O14 O 0.46747(13) 0.7470(5) 0.39638(12) 0.0490(9) Uani 1 1 d . . . . .
O12 O 0.25029(13) 1.0446(5) 0.32483(12) 0.0474(8) Uani 1 1 d . . . . .
O9 O 0.22378(13) 0.8863(5) 0.40697(11) 0.0487(9) Uani 1 1 d . . . . .
O2 O 0.17236(13) 0.7533(5) 0.31521(12) 0.0506(9) Uani 1 1 d . . . . .
O3 O 0.08843(13) 0.6565(6) 0.26135(11) 0.0563(10) Uani 1 1 d . . . . .
C10 C 0.2884(2) 0.4270(7) 0.41933(17) 0.0431(11) Uani 1 1 d . . . . .
H10 H 0.281376 0.295499 0.421749 0.052 Uiso 1 1 calc R U . . .
C12 C 0.3312(2) 0.6485(7) 0.28926(17) 0.0424(11) Uani 1 1 d . . . . .
H12 H 0.333252 0.557450 0.265868 0.051 Uiso 1 1 calc R U . . .
C15 C 0.43016(19) 1.1410(7) 0.45894(15) 0.0371(10) Uani 1 1 d . . . . .
H15 H 0.443642 1.256181 0.475430 0.045 Uiso 1 1 calc R U . . .
C11 C 0.2443(2) 0.9132(6) 0.45182(16) 0.0382(10) Uani 1 1 d . . . . .
H11 H 0.217431 0.963842 0.467123 0.046 Uiso 1 1 calc R U . . .
C9 C 0.4293(2) 0.7804(7) 0.57197(17) 0.0455(12) Uani 1 1 d . . . . .
H9 H 0.438194 0.907116 0.565631 0.055 Uiso 1 1 calc R U . . .
C8 C 0.14307(19) 0.6433(7) 0.28339(15) 0.0386(10) Uani 1 1 d . . . . .
H8 H 0.163854 0.540328 0.275039 0.046 Uiso 1 1 calc R U . . .
C13 C 0.2873(2) 1.1591(7) 0.31685(16) 0.0420(11) Uani 1 1 d . . . . .
H13 H 0.271800 1.276527 0.302621 0.050 Uiso 1 1 calc R U . . .
C14 C 0.4751(2) 0.6349(7) 0.43155(17) 0.0414(11) Uani 1 1 d . . . . .
H14 H 0.507502 0.549296 0.436792 0.050 Uiso 1 1 calc R U . . .
C2 C 0.3801(8) 1.234(4) 0.6353(6) 0.069(5) Uani 0.5 1 d . U P A -1
H2A H 0.346725 1.301208 0.642238 0.083 Uiso 0.5 1 calc R U P A -1
H2B H 0.383094 1.104839 0.648913 0.083 Uiso 0.5 1 calc R U P A -1
C4 C 0.5029(7) 1.414(2) 0.7355(4) 0.079(4) Uani 0.5 1 d . U P A -1
H4A H 0.514487 1.532072 0.722468 0.094 Uiso 0.5 1 calc R U P A -1
H4B H 0.531034 1.313322 0.732956 0.094 Uiso 0.5 1 calc R U P A -1
N2 N 0.4353(5) 1.3368(17) 0.6551(3) 0.076(3) Uani 0.5 1 d . U P A -1
H2C H 0.433365 1.451435 0.640579 0.091 Uiso 0.5 1 calc R U P A -1
H2D H 0.466105 1.270552 0.650534 0.091 Uiso 0.5 1 calc R U P A -1
C1 C 0.3704(6) 1.2272(19) 0.5765(5) 0.074(3) Uani 0.5 1 d . U P A -1
H1A H 0.333556 1.159237 0.560440 0.111 Uiso 0.5 1 calc R U P A -1
H1B H 0.367958 1.356577 0.563917 0.111 Uiso 0.5 1 calc R U P A -1
H1C H 0.404083 1.161526 0.570548 0.111 Uiso 0.5 1 calc R U P A -1
C3 C 0.4436(6) 1.361(3) 0.7068(5) 0.090(4) Uani 0.5 1 d . U P A -1
H3A H 0.415593 1.459525 0.710719 0.108 Uiso 0.5 1 calc R U P A -1
H3B H 0.432879 1.241008 0.719512 0.108 Uiso 0.5 1 calc R U P A -1
C7 C 0.6129(8) 1.228(3) 0.8806(5) 0.051(4) Uani 0.5 1 d . U P A -1
H7A H 0.641057 1.121811 0.887796 0.077 Uiso 0.5 1 calc R U P A -1
H7B H 0.624207 1.319906 0.906936 0.077 Uiso 0.5 1 calc R U P A -1
H7C H 0.572780 1.180541 0.877019 0.077 Uiso 0.5 1 calc R U P A -1
N1 N 0.5716(4) 1.4911(11) 0.8193(3) 0.0401(17) Uani 0.5 1 d . U P A -1
H1D H 0.572205 1.548547 0.847273 0.048 Uiso 0.5 1 calc R U P A -1
H1E H 0.585128 1.576528 0.801760 0.048 Uiso 0.5 1 calc R U P A -1
C5 C 0.5087(5) 1.4461(17) 0.7924(4) 0.047(3) Uani 0.5 1 d . U P A -1
H5A H 0.482566 1.551557 0.795696 0.057 Uiso 0.5 1 calc R U P A -1
H5B H 0.496135 1.330093 0.805732 0.057 Uiso 0.5 1 calc R U P A -1
C6 C 0.6142(5) 1.3291(17) 0.8310(4) 0.052(2) Uani 0.5 1 d . U P A -1
H6A H 0.654825 1.375329 0.834371 0.063 Uiso 0.5 1 calc R U P A -1
H6B H 0.603302 1.235704 0.804399 0.063 Uiso 0.5 1 calc R U P A -1


_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
Fe00 O1 1.938(2) . ?
Fe00 O6 2.025(3) . ?
Fe00 O4 2.032(3) . ?
Fe00 O15 2.022(3) . ?
Fe00 O8 2.021(3) . ?
Fe00 O16 2.019(3) . ?
Fe1 O1 1.906(3) . ?
Fe1 O13 2.022(3) . ?
Fe1 O17 2.008(3) . ?
Fe1 O10 2.026(3) . ?
Fe1 O18 2.083(3) . ?
Fe1 O14 2.016(3) . ?
Fe03 O1 1.929(2) . ?
Fe03 O11 2.048(3) . ?
Fe03 O7 2.027(3) . ?
Fe03 O12 2.024(3) . ?
Fe03 O9 2.013(3) . ?
Fe03 O2 2.006(3) . ?
O6 C10 1.245(5) . ?
O4 C9 1.235(5) . ?
O11 C12 1.243(5) . ?
O7 C10 1.240(5) . ?
O13 C13 1.237(5) . ?
O15 C14 1.241(5) . ?
O17 C15 1.226(5) . ?
O5 C9 1.238(5) . ?
O8 C11 1.247(5) . ?
O10 C12 1.236(5) . ?
O16 C15 1.242(5) . ?
O18 H18A 0.8785 . ?
O18 H18B 0.8800 . ?
O14 C14 1.239(5) . ?
O12 C13 1.238(5) . ?
O9 C11 1.239(5) . ?
O2 C8 1.221(5) . ?
O3 C8 1.232(5) . ?
C10 H10 0.9300 . ?
C12 H12 0.9300 . ?
C15 H15 0.9300 . ?
C11 H11 0.9300 . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N2 1.42(2) . ?
C2 C1 1.628(18) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.415(19) . ?
C4 C5 1.605(16) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 C3 1.439(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 C6 1.590(15) . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C5 1.457(13) . ?
N1 C6 1.462(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
O1 Fe00 O6 94.39(12) . . ?
O1 Fe00 O4 177.96(12) . . ?
O1 Fe00 O15 93.71(11) . . ?
O1 Fe00 O8 95.47(11) . . ?
O1 Fe00 O16 92.93(11) . . ?
O6 Fe00 O4 84.74(12) . . ?
O15 Fe00 O6 87.41(13) . . ?
O15 Fe00 O4 84.41(12) . . ?
O8 Fe00 O6 90.47(14) . . ?
O8 Fe00 O4 86.39(12) . . ?
O8 Fe00 O15 170.71(12) . . ?
O16 Fe00 O6 172.68(12) . . ?
O16 Fe00 O4 87.96(11) . . ?
O16 Fe00 O15 92.43(13) . . ?
O16 Fe00 O8 88.52(14) . . ?
O1 Fe1 O13 96.46(12) . . ?
O1 Fe1 O17 95.22(12) . . ?
O1 Fe1 O10 96.04(12) . . ?
O1 Fe1 O18 177.79(12) . . ?
O1 Fe1 O14 96.28(12) . . ?
O13 Fe1 O10 91.19(14) . . ?
O13 Fe1 O18 85.13(12) . . ?
O17 Fe1 O13 86.89(15) . . ?
O17 Fe1 O10 168.71(13) . . ?
O17 Fe1 O18 86.39(12) . . ?
O17 Fe1 O14 92.25(15) . . ?
O10 Fe1 O18 82.36(12) . . ?
O14 Fe1 O13 167.26(13) . . ?
O14 Fe1 O10 87.17(14) . . ?
O14 Fe1 O18 82.13(12) . . ?
O1 Fe03 O11 93.51(11) . . ?
O1 Fe03 O7 94.17(12) . . ?
O1 Fe03 O12 93.66(12) . . ?
O1 Fe03 O9 94.92(12) . . ?
O1 Fe03 O2 176.18(14) . . ?
O7 Fe03 O11 85.59(14) . . ?
O12 Fe03 O11 92.97(14) . . ?
O12 Fe03 O7 172.12(12) . . ?
O9 Fe03 O11 171.29(12) . . ?
O9 Fe03 O7 91.62(14) . . ?
O9 Fe03 O12 88.67(14) . . ?
O2 Fe03 O11 87.63(12) . . ?
O2 Fe03 O7 89.56(14) . . ?
O2 Fe03 O12 82.64(14) . . ?
O2 Fe03 O9 84.09(13) . . ?
Fe1 O1 Fe00 119.97(12) . . ?
Fe1 O1 Fe03 119.94(13) . . ?
Fe03 O1 Fe00 120.09(13) . . ?
C10 O6 Fe00 131.4(3) . . ?
C9 O4 Fe00 129.7(3) . . ?
C12 O11 Fe03 132.3(3) . . ?
C10 O7 Fe03 130.6(3) . . ?
C13 O13 Fe1 130.9(3) . . ?
C14 O15 Fe00 132.5(3) . . ?
C15 O17 Fe1 130.6(3) . . ?
C11 O8 Fe00 131.2(3) . . ?
C12 O10 Fe1 129.4(3) . . ?
C15 O16 Fe00 133.7(3) . . ?
Fe1 O18 H18A 111.1 . . ?
Fe1 O18 H18B 111.0 . . ?
H18A O18 H18B 102.9 . . ?
C14 O14 Fe1 130.9(3) . . ?
C13 O12 Fe03 132.6(3) . . ?
C11 O9 Fe03 133.6(3) . . ?
C8 O2 Fe03 136.3(3) . . ?
O6 C10 H10 115.4 . . ?
O7 C10 O6 129.2(4) . . ?
O7 C10 H10 115.4 . . ?
O11 C12 H12 115.9 . . ?
O10 C12 O11 128.3(4) . . ?
O10 C12 H12 115.9 . . ?
O17 C15 O16 127.4(4) . . ?
O17 C15 H15 116.3 . . ?
O16 C15 H15 116.3 . . ?
O8 C11 H11 116.3 . . ?
O9 C11 O8 127.5(4) . . ?
O9 C11 H11 116.3 . . ?
O4 C9 O5 127.8(5) . . ?
O4 C9 H9 116.1 . . ?
O5 C9 H9 116.1 . . ?
O2 C8 O3 125.8(5) . . ?
O2 C8 H8 117.1 . . ?
O3 C8 H8 117.1 . . ?
O13 C13 O12 127.5(4) . . ?
O13 C13 H13 116.2 . . ?
O12 C13 H13 116.2 . . ?
O15 C14 H14 116.1 . . ?
O14 C14 O15 127.9(4) . . ?
O14 C14 H14 116.1 . . ?
H2A C2 H2B 108.9 . . ?
N2 C2 H2A 110.8 . . ?
N2 C2 H2B 110.8 . . ?
N2 C2 C1 104.6(11) . . ?
C1 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
H4A C4 H4B 107.8 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C3 C4 C5 113.2(9) . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C2 N2 H2C 110.3 . . ?
C2 N2 H2D 110.3 . . ?
C2 N2 C3 107.0(11) . . ?
H2C N2 H2D 108.6 . . ?
C3 N2 H2C 110.3 . . ?
C3 N2 H2D 110.3 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C3 N2 115.6(11) . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
N2 C3 H3A 108.4 . . ?
N2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H1D N1 H1E 107.3 . . ?
C5 N1 H1D 108.1 . . ?
C5 N1 H1E 108.1 . . ?
C5 N1 C6 116.8(8) . . ?
C6 N1 H1D 108.1 . . ?
C6 N1 H1E 108.1 . . ?
C4 C5 H5A 109.9 . . ?
C4 C5 H5B 109.9 . . ?
N1 C5 C4 109.1(8) . . ?
N1 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
N1 C6 C7 110.4(10) . . ?
N1 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?

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
Fe00 O6 C10 O7 -10.5(8) . . . . ?
Fe00 O4 C9 O5 -175.2(4) . . . . ?
Fe00 O15 C14 O14 3.6(8) . . . . ?
Fe00 O8 C11 O9 -3.5(8) . . . . ?
Fe00 O16 C15 O17 -11.0(8) . . . . ?
Fe1 O13 C13 O12 -10.6(8) . . . . ?
Fe1 O17 C15 O16 7.4(7) . . . . ?
Fe1 O10 C12 O11 11.7(8) . . . . ?
Fe1 O14 C14 O15 -9.7(8) . . . . ?
Fe03 O11 C12 O10 -14.4(8) . . . . ?
Fe03 O7 C10 O6 5.3(8) . . . . ?
Fe03 O12 C13 O13 2.2(8) . . . . ?
Fe03 O9 C11 O8 1.1(8) . . . . ?
Fe03 O2 C8 O3 -178.0(4) . . . . ?
C2 N2 C3 C4 164.0(17) . . . . ?
C1 C2 N2 C3 175.5(13) . . . . ?
C3 C4 C5 N1 177.5(12) . . . . ?
C5 C4 C3 N2 178.0(14) . . . . ?
C5 N1 C6 C7 -85.4(13) . . . . ?
C6 N1 C5 C4 -77.8(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.693
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2116938'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2021-10-26 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_audit_creation_date             2021-10-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 H10 Fe3 O18), C7 H20 N2'
_chemical_formula_sum            'C23 H40 Fe6 N2 O36'
_chemical_formula_weight         1255.67
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8203(14)
_cell_length_b                   11.744(3)
_cell_length_c                   27.583(3)
_cell_angle_alpha                82.650(14)
_cell_angle_beta                 84.347(13)
_cell_angle_gamma                76.202(18)
_cell_volume                     2122.6(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.8730
_cell_measurement_theta_min      2.7560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1754
_diffrn_reflns_av_unetI/netI     0.3085
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11364
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         3.019
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     83.00 110.00   1.00   15.00    --   30.00  54.00 120.00   27
  2  ω    -72.00  33.00   1.00   15.00    --   30.00  54.00   0.00  105
  3  ω    -72.00  34.00   1.00   15.00    --   30.00  54.00-120.00  106
  4  ω    -74.00  32.00   1.00   15.00    --   30.00  54.00 120.00  106
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0251799000
_diffrn_orient_matrix_UB_12      -0.0532497000
_diffrn_orient_matrix_UB_13      -0.0111407000
_diffrn_orient_matrix_UB_21      0.0563501000
_diffrn_orient_matrix_UB_22      0.0265421000
_diffrn_orient_matrix_UB_23      -0.0193332000
_diffrn_orient_matrix_UB_31      0.0878345000
_diffrn_orient_matrix_UB_32      -0.0192526000
_diffrn_orient_matrix_UB_33      0.0133565000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2847
_reflns_number_total             7383
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.386
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.276
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         7383
_refine_ls_number_restraints     1344
_refine_ls_R_factor_all          0.2521
_refine_ls_R_factor_gt           0.1358
_refine_ls_restrained_S_all      0.893
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1539P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2954
_refine_ls_wR_factor_ref         0.3773
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18A,H18B} of O18, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H36A,H36B} of O36
2. Uiso/Uaniso restraints and constraints
O25 \\sim O11 \\sim O31 \\sim O6 \\sim O19 \\sim O30 \\sim O5 \\sim O3 \\sim
O12 \\sim O24 \\sim O21 \\sim O32 \\sim O13 \\sim O15 \\sim O10 \\sim O8 \\sim
O23 \\sim O9 \\sim O27 \\sim O36 \\sim O26 \\sim O14 \\sim O1 \\sim O2 \\sim O7
\\sim O35 \\sim O22 \\sim O28 \\sim O33 \\sim O16 \\sim O29 \\sim O34 \\sim O18
\\sim O17 \\sim O4 \\sim O20 \\sim C12 \\sim C6 \\sim C3 \\sim C4 \\sim C10
\\sim C2 \\sim C9 \\sim C11 \\sim C15 \\sim C8 \\sim C7 \\sim C1 \\sim C16
\\sim C5 \\sim C14 \\sim C13 \\sim C19 \\sim C22 \\sim C17 \\sim C18 \\sim C20
\\sim C21 \\sim C23 \\sim N1 \\sim N2: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.04 within 3.8A
Uanis(O36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.05
3.a Riding coordinates:
 O36(H36A,H36B), O18(H18A,H18B)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C19(H19A,H19B), C22(H22A,H22B), C18(H18C,H18D),
 C20(H20A,H20B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C3(H3), C4(H4), C10(H10), C2(H2), C9(H9), C11(H11),
 C15(H15), C8(H8), C7(H7), C1(H1), C16(H16), C5(H5), C14(H14), C13(H13)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe5 Fe -0.1322(3) 0.7773(2) 0.96588(9) 0.0198(6) Uani 1 1 d . . . . .
Fe2 Fe 0.6535(3) 0.7263(2) 0.53583(9) 0.0208(6) Uani 1 1 d . . . . .
Fe1 Fe 0.8543(3) 0.5731(2) 0.63685(9) 0.0219(6) Uani 1 1 d . . . . .
Fe4 Fe 0.0071(3) 0.9311(2) 0.86277(9) 0.0230(6) Uani 1 1 d . . . . .
Fe3 Fe 0.5614(3) 0.8415(2) 0.64292(9) 0.0205(6) Uani 1 1 d . . . . .
Fe6 Fe -0.0664(3) 0.6632(2) 0.85811(9) 0.0212(6) Uani 1 1 d . . . . .
O25 O 0.0861(16) 0.8509(10) 0.9826(4) 0.0236(18) Uani 1 1 d . U . . .
O11 O 0.9508(16) 0.6566(11) 0.5184(4) 0.0268(18) Uani 1 1 d . U . . .
O31 O -0.3681(16) 0.7050(10) 0.9613(4) 0.0271(19) Uani 1 1 d . U . . .
O6 O 0.4767(16) 0.7337(10) 0.7020(4) 0.0272(16) Uani 1 1 d . U . . .
O19 O -0.0657(16) 0.7928(10) 0.8955(4) 0.0244(15) Uani 1 1 d . U . . .
O30 O -0.3512(16) 0.6570(10) 0.8847(4) 0.0272(19) Uani 1 1 d . U . . .
O5 O 0.3520(17) 0.7940(11) 0.5438(5) 0.0291(19) Uani 1 1 d . U . . .
O3 O 0.6016(17) 0.9695(11) 0.5907(5) 0.0299(19) Uani 1 1 d . U . . .
O12 O 0.5876(16) 0.5657(10) 0.5400(4) 0.0261(18) Uani 1 1 d . U . . .
O24 O 0.2006(16) 0.9407(10) 0.9118(4) 0.0227(18) Uani 1 1 d . U . . .
O21 O 0.2466(17) 0.8443(11) 0.8225(5) 0.0304(19) Uani 1 1 d . U . . .
O32 O -0.2198(16) 0.7641(10) 1.0386(4) 0.023(2) Uani 1 1 d . U . . .
O13 O 0.7509(17) 0.4572(10) 0.6028(4) 0.0281(19) Uani 1 1 d . U . . .
O15 O 0.6814(17) 0.7083(11) 0.3857(5) 0.033(3) Uani 1 1 d . U . . .
O10 O 1.0905(17) 0.5676(11) 0.5867(5) 0.0292(19) Uani 1 1 d . U . . .
O8 O 0.8211(17) 0.8472(11) 0.6734(4) 0.0281(18) Uani 1 1 d . U . . .
O23 O -0.2037(17) 0.7696(11) 0.8008(5) 0.0302(19) Uani 1 1 d . U . . .
O9 O 0.9893(16) 0.6589(11) 0.6795(4) 0.0270(19) Uani 1 1 d . U . . .
O27 O -0.3294(16) 0.9387(10) 0.9608(4) 0.0270(18) Uani 1 1 d . U . . .
O36 O 0.0731(16) 1.0889(10) 0.8293(4) 0.026(3) Uani 1 1 d . U . . .
H36A H 0.140575 1.081191 0.799306 0.038 Uiso 1 1 d R U . . .
H36B H 0.162905 1.112161 0.845646 0.038 Uiso 1 1 d R U . . .
O26 O -0.2245(17) 1.0490(10) 0.8955(5) 0.0268(19) Uani 1 1 d . U . . .
O14 O 0.6022(16) 0.7366(10) 0.4645(4) 0.026(2) Uani 1 1 d . U . . .
O1 O 0.6907(16) 0.7165(10) 0.6049(4) 0.0275(15) Uani 1 1 d . U . . .
O2 O 0.7093(17) 0.8900(10) 0.5206(4) 0.0265(18) Uani 1 1 d . U . . .
O7 O 0.6467(17) 0.5477(10) 0.6916(4) 0.028(2) Uani 1 1 d . U . . .
O35 O -0.012(2) 0.3931(11) 0.7704(5) 0.037(3) Uani 1 1 d . U . . .
O22 O -0.1739(17) 0.9485(11) 0.8066(5) 0.0308(19) Uani 1 1 d . U . . .
O28 O 0.0643(16) 0.6184(10) 0.9771(4) 0.0263(18) Uani 1 1 d . U . . .
O33 O -0.2350(19) 0.7925(12) 1.1169(5) 0.038(3) Uani 1 1 d . U . . .
O16 O 0.4521(18) 0.9779(11) 0.6838(5) 0.032(2) Uani 1 1 d . U . . .
O29 O 0.0709(17) 0.5359(11) 0.9094(5) 0.0320(19) Uani 1 1 d . U . . .
O34 O -0.0822(18) 0.5256(11) 0.8246(5) 0.035(2) Uani 1 1 d . U . . .
O18 O 1.0292(18) 0.4198(11) 0.6720(5) 0.034(3) Uani 1 1 d . U . . .
H18A H 0.976393 0.382458 0.700364 0.041 Uiso 1 1 d R U . . .
H18B H 1.159953 0.388968 0.659394 0.041 Uiso 1 1 d R U . . .
O17 O 0.254(2) 1.0851(12) 0.7383(5) 0.042(3) Uani 1 1 d . U . . .
O4 O 0.2836(17) 0.8533(10) 0.6218(5) 0.0285(18) Uani 1 1 d . U . . .
O20 O 0.2103(17) 0.6637(11) 0.8232(5) 0.0303(17) Uani 1 1 d . U . . .
C12 C -0.339(3) 1.0288(16) 0.9333(7) 0.026(2) Uani 1 1 d . U . . .
H12 H -0.444429 1.091821 0.940924 0.031 Uiso 1 1 calc R U . . .
C6 C 1.103(3) 0.6055(16) 0.5409(7) 0.026(2) Uani 1 1 d . U . . .
H6 H 1.229501 0.594480 0.524034 0.032 Uiso 1 1 calc R U . . .
C3 C 0.504(3) 0.6237(16) 0.7110(7) 0.029(2) Uani 1 1 d . U . . .
H3 H 0.412252 0.595031 0.733790 0.035 Uiso 1 1 calc R U . . .
N1 N 0.324(2) 0.6965(14) 0.1623(6) 0.037(3) Uani 1 1 d . U . . .
H1A H 0.209944 0.674242 0.172516 0.045 Uiso 1 1 calc R U . . .
H1B H 0.292377 0.770391 0.148221 0.045 Uiso 1 1 calc R U . . .
C4 C 0.962(3) 0.7629(16) 0.6853(7) 0.028(2) Uani 1 1 d . U . . .
H4 H 1.062070 0.781819 0.701126 0.034 Uiso 1 1 calc R U . . .
C10 C -0.245(3) 0.8761(16) 0.7896(7) 0.028(2) Uani 1 1 d . U . . .
H10 H -0.338978 0.905371 0.766244 0.033 Uiso 1 1 calc R U . . .
N2 N 0.367(2) 0.8175(13) 0.3297(6) 0.033(3) Uani 1 1 d . U . . .
H2A H 0.435168 0.790391 0.356279 0.039 Uiso 1 1 calc R U . . .
H2B H 0.384157 0.889897 0.319718 0.039 Uiso 1 1 calc R U . . .
C2 C 0.235(3) 0.8292(16) 0.5815(7) 0.027(2) Uani 1 1 d . U . . .
H2 H 0.097354 0.838214 0.578704 0.033 Uiso 1 1 calc R U . . .
C9 C 0.311(3) 0.7387(16) 0.8152(7) 0.026(2) Uani 1 1 d . U . . .
H9 H 0.444384 0.715211 0.802838 0.032 Uiso 1 1 calc R U . . .
C11 C 0.212(2) 0.9063(15) 0.9564(6) 0.026(2) Uani 1 1 d . U . . .
H11 H 0.316842 0.921107 0.972030 0.031 Uiso 1 1 calc R U . . .
C15 C -0.157(2) 0.7954(15) 1.0747(6) 0.022(3) Uani 1 1 d . U . . .
H15 H -0.039468 0.823731 1.069114 0.027 Uiso 1 1 calc R U . . .
C8 C 0.296(3) 1.0016(16) 0.7147(7) 0.029(2) Uani 1 1 d . U . . .
H8 H 0.209009 0.950453 0.719027 0.035 Uiso 1 1 calc R U . . .
C7 C 0.727(3) 0.7079(16) 0.4284(7) 0.028(2) Uani 1 1 d . U . . .
H7 H 0.863313 0.684750 0.434326 0.034 Uiso 1 1 calc R U . . .
C1 C 0.672(2) 0.9738(16) 0.5460(7) 0.026(2) Uani 1 1 d . U . . .
H1 H 0.696676 1.045240 0.531351 0.031 Uiso 1 1 calc R U . . .
C16 C 0.004(3) 0.4822(18) 0.7851(7) 0.035(3) Uani 1 1 d . U . . .
H16 H 0.086881 0.524897 0.765810 0.042 Uiso 1 1 calc R U . . .
C5 C 0.634(2) 0.4738(16) 0.5676(6) 0.025(2) Uani 1 1 d . U . . .
H5 H 0.580038 0.411112 0.562456 0.030 Uiso 1 1 calc R U . . .
C14 C -0.447(3) 0.6737(16) 0.9273(7) 0.028(2) Uani 1 1 d . U . . .
H14 H -0.578036 0.662185 0.932765 0.034 Uiso 1 1 calc R U . . .
C13 C 0.124(2) 0.5374(16) 0.9521(7) 0.026(2) Uani 1 1 d . U . . .
H13 H 0.216389 0.471471 0.965164 0.031 Uiso 1 1 calc R U . . .
C19 C 0.450(3) 0.7375(17) 0.2893(7) 0.035(3) Uani 1 1 d . U . . .
H19A H 0.591272 0.738895 0.281270 0.042 Uiso 1 1 calc R U . . .
H19B H 0.444981 0.657296 0.302114 0.042 Uiso 1 1 calc R U . . .
C22 C 0.439(3) 0.6195(17) 0.1264(8) 0.038(3) Uani 1 1 d . U . . .
H22A H 0.465751 0.538286 0.141191 0.045 Uiso 1 1 calc R U . . .
H22B H 0.568304 0.640087 0.117190 0.045 Uiso 1 1 calc R U . . .
C17 C 0.078(3) 0.8825(19) 0.3880(9) 0.053(6) Uani 1 1 d . U . . .
H17A H 0.091206 0.962824 0.382283 0.080 Uiso 1 1 calc R U . . .
H17B H 0.157673 0.841927 0.414430 0.080 Uiso 1 1 calc R U . . .
H17C H -0.061510 0.881107 0.396275 0.080 Uiso 1 1 calc R U . . .
C18 C 0.152(3) 0.8217(17) 0.3416(8) 0.040(3) Uani 1 1 d . U . . .
H18C H 0.130776 0.742100 0.346549 0.048 Uiso 1 1 calc R U . . .
H18D H 0.075092 0.864311 0.314502 0.048 Uiso 1 1 calc R U . . .
C20 C 0.343(3) 0.7683(17) 0.2436(8) 0.038(3) Uani 1 1 d . U . . .
H20A H 0.205220 0.758995 0.250172 0.046 Uiso 1 1 calc R U . . .
H20B H 0.338755 0.849988 0.231294 0.046 Uiso 1 1 calc R U . . .
C21 C 0.450(3) 0.6910(17) 0.2069(8) 0.039(3) Uani 1 1 d . U . . .
H21A H 0.482627 0.610404 0.222231 0.047 Uiso 1 1 calc R U . . .
H21B H 0.575693 0.713267 0.195352 0.047 Uiso 1 1 calc R U . . .
C23 C 0.322(3) 0.6306(17) 0.0795(8) 0.049(6) Uani 1 1 d . U . . .
H23A H 0.395358 0.574515 0.058015 0.073 Uiso 1 1 calc R U . . .
H23B H 0.307162 0.708921 0.062940 0.073 Uiso 1 1 calc R U . . .
H23C H 0.190108 0.615349 0.088734 0.073 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
Fe5 O25 2.006(11) . ?
Fe5 O31 2.012(12) . ?
Fe5 O19 1.946(12) . ?
Fe5 O32 2.032(12) . ?
Fe5 O27 2.043(11) . ?
Fe5 O28 2.029(11) . ?
Fe2 O11 2.032(12) . ?
Fe2 O5 2.021(11) . ?
Fe2 O12 2.028(12) . ?
Fe2 O14 2.016(11) . ?
Fe2 O1 1.933(12) . ?
Fe2 O2 2.032(12) . ?
Fe1 O13 2.037(12) . ?
Fe1 O10 2.012(13) . ?
Fe1 O9 2.051(12) . ?
Fe1 O1 1.943(11) . ?
Fe1 O7 2.010(12) . ?
Fe1 O18 2.089(11) . ?
Fe4 O19 1.902(12) . ?
Fe4 O24 2.011(11) . ?
Fe4 O21 2.020(12) . ?
Fe4 O36 2.090(12) . ?
Fe4 O26 2.055(12) . ?
Fe4 O22 2.036(12) . ?
Fe3 O6 2.055(13) . ?
Fe3 O3 1.995(13) . ?
Fe3 O8 2.054(11) . ?
Fe3 O1 1.903(12) . ?
Fe3 O16 2.031(13) . ?
Fe3 O4 2.005(11) . ?
Fe6 O19 1.945(12) . ?
Fe6 O30 2.022(12) . ?
Fe6 O23 2.042(12) . ?
Fe6 O29 2.042(12) . ?
Fe6 O34 1.991(13) . ?
Fe6 O20 2.034(13) . ?
O25 C11 1.31(2) . ?
O11 C6 1.247(18) . ?
O31 C14 1.26(2) . ?
O6 C3 1.26(2) . ?
O30 C14 1.30(2) . ?
O5 C2 1.29(2) . ?
O3 C1 1.27(2) . ?
O12 C5 1.232(19) . ?
O24 C11 1.25(2) . ?
O21 C9 1.25(2) . ?
O32 C15 1.251(19) . ?
O13 C5 1.282(18) . ?
O15 C7 1.25(2) . ?
O10 C6 1.29(2) . ?
O8 C4 1.238(19) . ?
O23 C10 1.22(2) . ?
O9 C4 1.22(2) . ?
O27 C12 1.21(2) . ?
O36 H36A 0.9099 . ?
O36 H36B 0.9053 . ?
O26 C12 1.27(2) . ?
O14 C7 1.27(2) . ?
O2 C1 1.24(2) . ?
O7 C3 1.28(2) . ?
O35 C16 1.20(2) . ?
O22 C10 1.23(2) . ?
O28 C13 1.22(2) . ?
O33 C15 1.23(2) . ?
O16 C8 1.30(2) . ?
O29 C13 1.27(2) . ?
O34 C16 1.29(2) . ?
O18 H18A 0.9301 . ?
O18 H18B 0.9300 . ?
O17 C8 1.21(2) . ?
O4 C2 1.27(2) . ?
O20 C9 1.23(2) . ?
C12 H12 0.9300 . ?
C6 H6 0.9300 . ?
C3 H3 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C22 1.47(2) . ?
N1 C21 1.55(2) . ?
C4 H4 0.9300 . ?
C10 H10 0.9300 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C19 1.53(2) . ?
N2 C18 1.46(2) . ?
C2 H2 0.9300 . ?
C9 H9 0.9300 . ?
C11 H11 0.9300 . ?
C15 H15 0.9300 . ?
C8 H8 0.9300 . ?
C7 H7 0.9300 . ?
C1 H1 0.9300 . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.48(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.56(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 C18 1.53(3) . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.47(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?

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
O25 Fe5 O31 170.2(5) . . ?
O25 Fe5 O32 87.2(5) . . ?
O25 Fe5 O27 90.3(5) . . ?
O25 Fe5 O28 87.6(5) . . ?
O31 Fe5 O32 83.0(5) . . ?
O31 Fe5 O27 88.0(5) . . ?
O31 Fe5 O28 93.3(5) . . ?
O19 Fe5 O25 95.5(5) . . ?
O19 Fe5 O31 94.3(5) . . ?
O19 Fe5 O32 176.5(4) . . ?
O19 Fe5 O27 91.0(5) . . ?
O19 Fe5 O28 93.6(5) . . ?
O32 Fe5 O27 86.7(5) . . ?
O28 Fe5 O32 88.8(5) . . ?
O28 Fe5 O27 175.0(5) . . ?
O11 Fe2 O2 88.9(5) . . ?
O5 Fe2 O11 172.4(5) . . ?
O5 Fe2 O12 87.0(5) . . ?
O5 Fe2 O2 91.6(5) . . ?
O12 Fe2 O11 91.4(5) . . ?
O12 Fe2 O2 171.1(5) . . ?
O14 Fe2 O11 88.8(5) . . ?
O14 Fe2 O5 83.7(5) . . ?
O14 Fe2 O12 84.3(5) . . ?
O14 Fe2 O2 86.8(5) . . ?
O1 Fe2 O11 93.5(5) . . ?
O1 Fe2 O5 94.1(5) . . ?
O1 Fe2 O12 94.7(5) . . ?
O1 Fe2 O14 177.6(5) . . ?
O1 Fe2 O2 94.1(5) . . ?
O13 Fe1 O9 168.1(5) . . ?
O13 Fe1 O18 83.5(5) . . ?
O10 Fe1 O13 90.9(5) . . ?
O10 Fe1 O9 89.5(5) . . ?
O10 Fe1 O18 86.1(5) . . ?
O9 Fe1 O18 84.6(5) . . ?
O1 Fe1 O13 97.0(5) . . ?
O1 Fe1 O10 94.5(5) . . ?
O1 Fe1 O9 94.8(5) . . ?
O1 Fe1 O7 96.3(5) . . ?
O1 Fe1 O18 179.3(5) . . ?
O7 Fe1 O13 85.9(5) . . ?
O7 Fe1 O10 169.1(5) . . ?
O7 Fe1 O9 91.5(5) . . ?
O7 Fe1 O18 83.2(5) . . ?
O19 Fe4 O24 95.4(5) . . ?
O19 Fe4 O21 95.3(5) . . ?
O19 Fe4 O36 176.6(5) . . ?
O19 Fe4 O26 96.1(5) . . ?
O19 Fe4 O22 95.2(5) . . ?
O24 Fe4 O21 88.0(5) . . ?
O24 Fe4 O36 84.6(4) . . ?
O24 Fe4 O26 92.1(5) . . ?
O24 Fe4 O22 169.4(5) . . ?
O21 Fe4 O36 88.0(5) . . ?
O21 Fe4 O26 168.5(5) . . ?
O21 Fe4 O22 90.9(5) . . ?
O26 Fe4 O36 80.6(5) . . ?
O22 Fe4 O36 84.8(5) . . ?
O22 Fe4 O26 86.9(5) . . ?
O3 Fe3 O6 169.2(5) . . ?
O3 Fe3 O8 90.9(5) . . ?
O3 Fe3 O16 83.3(5) . . ?
O3 Fe3 O4 90.4(5) . . ?
O8 Fe3 O6 92.3(5) . . ?
O1 Fe3 O6 95.3(5) . . ?
O1 Fe3 O3 94.8(5) . . ?
O1 Fe3 O8 94.4(5) . . ?
O1 Fe3 O16 174.1(5) . . ?
O1 Fe3 O4 95.0(5) . . ?
O16 Fe3 O6 87.1(5) . . ?
O16 Fe3 O8 80.1(5) . . ?
O4 Fe3 O6 84.8(5) . . ?
O4 Fe3 O8 170.3(5) . . ?
O4 Fe3 O16 90.6(5) . . ?
O19 Fe6 O30 92.0(5) . . ?
O19 Fe6 O23 94.5(5) . . ?
O19 Fe6 O29 94.3(5) . . ?
O19 Fe6 O34 175.1(5) . . ?
O19 Fe6 O20 94.1(5) . . ?
O30 Fe6 O23 84.9(5) . . ?
O30 Fe6 O29 94.9(5) . . ?
O30 Fe6 O20 172.6(5) . . ?
O23 Fe6 O29 171.2(5) . . ?
O34 Fe6 O30 83.9(5) . . ?
O34 Fe6 O23 87.8(5) . . ?
O34 Fe6 O29 83.4(5) . . ?
O34 Fe6 O20 90.2(5) . . ?
O20 Fe6 O23 90.5(5) . . ?
O20 Fe6 O29 88.9(5) . . ?
C11 O25 Fe5 133.7(11) . . ?
C6 O11 Fe2 136.7(13) . . ?
C14 O31 Fe5 135.6(13) . . ?
C3 O6 Fe3 133.1(12) . . ?
Fe5 O19 Fe6 119.5(6) . . ?
Fe4 O19 Fe5 121.0(6) . . ?
Fe4 O19 Fe6 119.4(6) . . ?
C14 O30 Fe6 132.4(11) . . ?
C2 O5 Fe2 131.5(11) . . ?
C1 O3 Fe3 135.3(12) . . ?
C5 O12 Fe2 133.6(11) . . ?
C11 O24 Fe4 133.0(11) . . ?
C9 O21 Fe4 133.5(12) . . ?
C15 O32 Fe5 132.5(12) . . ?
C5 O13 Fe1 131.2(12) . . ?
C6 O10 Fe1 132.3(11) . . ?
C4 O8 Fe3 127.2(12) . . ?
C10 O23 Fe6 133.6(12) . . ?
C4 O9 Fe1 131.7(11) . . ?
C12 O27 Fe5 134.2(12) . . ?
Fe4 O36 H36A 112.7 . . ?
Fe4 O36 H36B 111.9 . . ?
H36A O36 H36B 101.4 . . ?
C12 O26 Fe4 127.9(11) . . ?
C7 O14 Fe2 129.1(11) . . ?
Fe2 O1 Fe1 119.2(6) . . ?
Fe3 O1 Fe2 121.5(6) . . ?
Fe3 O1 Fe1 119.3(6) . . ?
C1 O2 Fe2 130.1(13) . . ?
C3 O7 Fe1 129.2(12) . . ?
C10 O22 Fe4 131.5(12) . . ?
C13 O28 Fe5 132.7(11) . . ?
C8 O16 Fe3 132.5(12) . . ?
C13 O29 Fe6 133.8(12) . . ?
C16 O34 Fe6 134.5(13) . . ?
Fe1 O18 H18A 120.0 . . ?
Fe1 O18 H18B 120.0 . . ?
H18A O18 H18B 120.0 . . ?
C2 O4 Fe3 128.2(11) . . ?
C9 O20 Fe6 132.8(13) . . ?
O27 C12 O26 128.9(17) . . ?
O27 C12 H12 115.6 . . ?
O26 C12 H12 115.6 . . ?
O11 C6 O10 122.5(17) . . ?
O11 C6 H6 118.8 . . ?
O10 C6 H6 118.8 . . ?
O6 C3 O7 125.4(18) . . ?
O6 C3 H3 117.3 . . ?
O7 C3 H3 117.3 . . ?
H1A N1 H1B 108.1 . . ?
C22 N1 H1A 109.5 . . ?
C22 N1 H1B 109.5 . . ?
C22 N1 C21 110.9(14) . . ?
C21 N1 H1A 109.5 . . ?
C21 N1 H1B 109.5 . . ?
O8 C4 H4 114.9 . . ?
O9 C4 O8 130.2(17) . . ?
O9 C4 H4 114.9 . . ?
O23 C10 O22 126.0(16) . . ?
O23 C10 H10 117.0 . . ?
O22 C10 H10 117.0 . . ?
H2A N2 H2B 108.1 . . ?
C19 N2 H2A 109.6 . . ?
C19 N2 H2B 109.6 . . ?
C18 N2 H2A 109.6 . . ?
C18 N2 H2B 109.6 . . ?
C18 N2 C19 110.3(14) . . ?
O5 C2 H2 115.7 . . ?
O4 C2 O5 128.7(16) . . ?
O4 C2 H2 115.7 . . ?
O21 C9 H9 117.7 . . ?
O20 C9 O21 124.6(18) . . ?
O20 C9 H9 117.7 . . ?
O25 C11 H11 117.9 . . ?
O24 C11 O25 124.1(15) . . ?
O24 C11 H11 117.9 . . ?
O32 C15 H15 116.8 . . ?
O33 C15 O32 126.5(17) . . ?
O33 C15 H15 116.8 . . ?
O16 C8 H8 117.5 . . ?
O17 C8 O16 125.1(18) . . ?
O17 C8 H8 117.5 . . ?
O15 C7 O14 125.4(16) . . ?
O15 C7 H7 117.3 . . ?
O14 C7 H7 117.3 . . ?
O3 C1 H1 117.4 . . ?
O2 C1 O3 125.2(18) . . ?
O2 C1 H1 117.4 . . ?
O35 C16 O34 127(2) . . ?
O35 C16 H16 116.3 . . ?
O34 C16 H16 116.3 . . ?
O12 C5 O13 125.6(16) . . ?
O12 C5 H5 117.2 . . ?
O13 C5 H5 117.2 . . ?
O31 C14 O30 122.1(17) . . ?
O31 C14 H14 119.0 . . ?
O30 C14 H14 119.0 . . ?
O28 C13 O29 125.0(16) . . ?
O28 C13 H13 117.5 . . ?
O29 C13 H13 117.5 . . ?
N2 C19 H19A 108.4 . . ?
N2 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 N2 115.5(15) . . ?
C20 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
N1 C22 H22A 109.3 . . ?
N1 C22 H22B 109.3 . . ?
N1 C22 C23 111.6(14) . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
N2 C18 C17 110.4(16) . . ?
N2 C18 H18C 109.6 . . ?
N2 C18 H18D 109.6 . . ?
C17 C18 H18C 109.6 . . ?
C17 C18 H18D 109.6 . . ?
H18C C18 H18D 108.1 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 C19 109.4(16) . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
N1 C21 H21A 108.9 . . ?
N1 C21 H21B 108.9 . . ?
C20 C21 N1 113.2(15) . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

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
Fe5 O25 C11 O24 11(3) . . . . ?
Fe5 O31 C14 O30 18(3) . . . . ?
Fe5 O32 C15 O33 172.7(12) . . . . ?
Fe5 O27 C12 O26 3(3) . . . . ?
Fe5 O28 C13 O29 0(3) . . . . ?
Fe2 O11 C6 O10 11(3) . . . . ?
Fe2 O5 C2 O4 16(3) . . . . ?
Fe2 O12 C5 O13 -2(3) . . . . ?
Fe2 O14 C7 O15 174.1(13) . . . . ?
Fe2 O2 C1 O3 6(2) . . . . ?
Fe1 O13 C5 O12 15(3) . . . . ?
Fe1 O10 C6 O11 -1(3) . . . . ?
Fe1 O9 C4 O8 13(3) . . . . ?
Fe1 O7 C3 O6 -7(3) . . . . ?
Fe4 O24 C11 O25 0(3) . . . . ?
Fe4 O21 C9 O20 18(3) . . . . ?
Fe4 O26 C12 O27 6(3) . . . . ?
Fe4 O22 C10 O23 -8(3) . . . . ?
Fe3 O6 C3 O7 24(3) . . . . ?
Fe3 O3 C1 O2 12(3) . . . . ?
Fe3 O8 C4 O9 5(3) . . . . ?
Fe3 O16 C8 O17 176.4(13) . . . . ?
Fe3 O4 C2 O5 -2(3) . . . . ?
Fe6 O30 C14 O31 4(3) . . . . ?
Fe6 O23 C10 O22 16(3) . . . . ?
Fe6 O29 C13 O28 17(3) . . . . ?
Fe6 O34 C16 O35 175.3(13) . . . . ?
Fe6 O20 C9 O21 -10(3) . . . . ?
N2 C19 C20 C21 175.0(17) . . . . ?
C19 N2 C18 C17 169.6(15) . . . . ?
C19 C20 C21 N1 166.8(17) . . . . ?
C22 N1 C21 C20 178.9(18) . . . . ?
C18 N2 C19 C20 56(2) . . . . ?
C21 N1 C22 C23 -175.9(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.594
####################################################################### 
# 
# 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_2_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2116936'
loop_
_audit_author_name
_audit_author_address
'Jiong-Peng Zhao'
;Tianjin University Of Technology
China
;
_audit_update_record             
;
2021-10-21 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 H10 Fe3 O18), C4 H14 N2'
_chemical_formula_sum            'C20 H34 Fe6 N2 O36'
_chemical_formula_weight         1213.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20h34N2Fe6O36
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   22.208(7)
_cell_length_b                   6.841(2)
_cell_length_c                   28.961(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.34(3)
_cell_angle_gamma                90
_cell_volume                     4098(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0500
_cell_measurement_theta_min      3.1490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 10 6 0.2354
-30 0 25 0.0425
30 1 -24 0.0372
-5 -10 4 0.4894
4 0 -40 0.0588
-4 0 39 0.0328
31 -1 -21 0.0490
27 0 7 0.0198
-23 0 -15 0.0902
15 0 26 0.0231

_exptl_crystal_size_max          0.742
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.093
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
-0.8840 9.5770 5.5224 0.1762 -0.0374 0.9836
-29.9462 0.4493 24.9602 0.9753 -0.2073 -0.0767
29.8334 1.3635 -23.9599 -0.9437 0.2006 0.2631
-4.9994 -9.5219 3.7341 0.0705 0.0970 -0.9928
3.8728 0.0629 -39.5420 -0.5869 -0.8078 -0.0555
-3.9577 0.1303 39.0810 0.5846 0.7922 0.0737
30.9893 -1.0265 -21.1070 -0.9543 0.3311 0.0322
26.9855 0.0733 6.9673 -0.4998 0.8554 0.1810
-22.9967 -0.0944 -14.9893 0.3105 -0.9360 -0.1768
15.0141 0.1187 26.0239 0.0043 0.9827 0.1560

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_av_unetI/netI     0.1883
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14752
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.885
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  56.00   1.00   75.55    --   30.00  54.00-150.00   66
  2  ω    -63.00 119.00   1.00   75.55    --   30.00  54.00 120.00  182
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0218309000
_diffrn_orient_matrix_UB_12      0.0090462000
_diffrn_orient_matrix_UB_13      0.0127182000
_diffrn_orient_matrix_UB_21      0.0258158000
_diffrn_orient_matrix_UB_22      -0.0147511000
_diffrn_orient_matrix_UB_23      0.0229331000
_diffrn_orient_matrix_UB_31      0.0058762000
_diffrn_orient_matrix_UB_32      0.1020170000
_diffrn_orient_matrix_UB_33      0.0021407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3505
_reflns_number_total             7057
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.896
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.0983
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1029P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2624
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
3.a Riding coordinates:
 O36(H36A,H36B), O18(H18A,H18B)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C3(H3A,H3B), C2(H2C,H2D), C1(H1D,H1E)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C16(H16), C8(H8), C7(H7), C13(H13), C17(H17), C5(H5),
 C6(H6), C20(H20), C10(H10), C19(H19), C9(H9), C11(H11), C18(H18), C12(H12)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Fe4 Fe 0.38028(8) 0.4581(3) 0.40282(5) 0.0302(4) Uani 1 1 d . . . . .
Fe6 Fe 0.49208(8) 0.4596(3) 0.35044(5) 0.0315(4) Uani 1 1 d . . . . .
Fe2 Fe 0.14037(8) 0.1207(3) 0.45420(5) 0.0329(4) Uani 1 1 d . . . . .
Fe1 Fe -0.00359(8) -0.0729(3) 0.39162(5) 0.0321(4) Uani 1 1 d . . . . .
Fe3 Fe 0.10681(7) -0.0370(3) 0.33845(5) 0.0301(4) Uani 1 1 d . . . . .
Fe5 Fe 0.34340(8) 0.3080(3) 0.28594(5) 0.0319(4) Uani 1 1 d . . . . .
O19 O 0.4043(3) 0.4067(11) 0.3454(2) 0.0257(16) Uani 1 1 d . . . . .
O16 O 0.1358(4) -0.0902(13) 0.2806(3) 0.042(2) Uani 1 1 d . . . . .
O25 O 0.4643(4) 0.5884(12) 0.2821(3) 0.040(2) Uani 1 1 d . . . . .
O9 O 0.1911(4) -0.1584(14) 0.3806(2) 0.045(2) Uani 1 1 d . . . . .
O32 O 0.3524(4) 0.5176(13) 0.4603(3) 0.040(2) Uani 1 1 d . . . . .
O7 O 0.1471(4) 0.2275(13) 0.3421(3) 0.045(2) Uani 1 1 d . . . . .
O1 O 0.0815(3) 0.0064(11) 0.3951(2) 0.0297(18) Uani 1 1 d . . . . .
O3 O 0.0296(4) -0.2052(14) 0.4595(3) 0.046(2) Uani 1 1 d . . . . .
O36 O 0.2734(4) 0.2181(13) 0.2181(2) 0.041(2) Uani 1 1 d . . . . .
H36A H 0.258997 0.103296 0.221237 0.062 Uiso 1 1 d R U . . .
H36B H 0.291017 0.200756 0.196227 0.062 Uiso 1 1 d R U . . .
O4 O -0.0208(4) 0.1826(13) 0.4188(3) 0.042(2) Uani 1 1 d . . . . .
O21 O 0.3351(4) 0.1979(13) 0.3960(3) 0.049(2) Uani 1 1 d . . . . .
O27 O 0.5024(4) 0.1950(13) 0.3251(3) 0.041(2) Uani 1 1 d . . . . .
O34 O 0.5836(4) 0.4888(13) 0.3534(3) 0.045(2) Uani 1 1 d . . . . .
O30 O 0.4593(4) 0.3363(14) 0.4541(2) 0.046(2) Uani 1 1 d . . . . .
O29 O 0.4233(4) 0.7229(12) 0.4165(3) 0.044(2) Uani 1 1 d . . . . .
O22 O 0.2978(4) 0.5924(13) 0.3607(3) 0.044(2) Uani 1 1 d . . . . .
O18 O 0.2050(4) 0.2387(13) 0.5193(3) 0.048(2) Uani 1 1 d . . . . .
H18A H 0.241260 0.291844 0.523775 0.072 Uiso 1 1 d R U . . .
H18B H 0.201230 0.245044 0.547455 0.072 Uiso 1 1 d R U . . .
O31 O 0.5353(4) 0.3548(14) 0.4204(3) 0.047(2) Uani 1 1 d . . . . .
O13 O 0.0727(4) -0.3078(13) 0.3261(3) 0.046(2) Uani 1 1 d . . . . .
O26 O 0.4026(4) 0.1085(13) 0.2746(3) 0.049(2) Uani 1 1 d . . . . .
O28 O 0.4945(4) 0.7332(12) 0.3782(3) 0.043(2) Uani 1 1 d . . . . .
O24 O 0.3627(4) 0.5042(14) 0.2401(3) 0.049(2) Uani 1 1 d . . . . .
O2 O 0.1246(4) -0.0717(14) 0.5011(3) 0.049(2) Uani 1 1 d . . . . .
O14 O -0.0926(4) -0.1409(14) 0.3876(3) 0.047(2) Uani 1 1 d . . . . .
O10 O 0.0238(4) 0.0683(14) 0.2882(3) 0.052(3) Uani 1 1 d . . . . .
O11 O -0.0515(4) 0.0322(14) 0.3226(3) 0.052(2) Uani 1 1 d . . . . .
O17 O 0.1813(4) -0.0308(14) 0.2248(3) 0.048(2) Uani 1 1 d . . . . .
O6 O 0.1718(4) 0.3343(13) 0.4206(3) 0.044(2) Uani 1 1 d . . . . .
O5 O 0.0766(4) 0.3100(13) 0.4626(3) 0.052(2) Uani 1 1 d . . . . .
O20 O 0.3100(4) 0.0982(14) 0.3181(3) 0.048(2) Uani 1 1 d . . . . .
O8 O 0.2167(4) -0.0464(14) 0.4581(3) 0.048(2) Uani 1 1 d . . . . .
O23 O 0.2695(4) 0.4880(14) 0.2827(3) 0.053(3) Uani 1 1 d . . . . .
O33 O 0.3040(5) 0.4560(14) 0.5142(3) 0.058(3) Uani 1 1 d . . . . .
O12 O 0.0004(4) -0.3387(14) 0.3628(3) 0.055(3) Uani 1 1 d . . . . .
O35 O 0.6709(4) 0.6283(17) 0.3483(3) 0.066(3) Uani 1 1 d . . . . .
O15 O -0.1681(5) -0.3116(18) 0.4030(3) 0.079(4) Uani 1 1 d . . . . .
N1 N 0.1907(5) 0.8941(16) 0.6788(3) 0.050(3) Uani 1 1 d . . . . .
H1A H 0.151756 0.948284 0.670416 0.060 Uiso 1 1 calc R U . . .
H1B H 0.220911 0.985552 0.690838 0.060 Uiso 1 1 calc R U . . .
H1C H 0.195395 0.803114 0.701862 0.060 Uiso 1 1 calc R U . . .
C15 C 0.4614(5) 0.0836(16) 0.2951(4) 0.029(2) Uani 1 1 d . U . . .
H15 H 0.477533 -0.032455 0.287494 0.035 Uiso 1 1 calc R U . . .
C14 C 0.3154(6) 0.0788(18) 0.3616(4) 0.039(3) Uani 1 1 d . . . . .
H14 H 0.302976 -0.042102 0.369808 0.047 Uiso 1 1 calc R U . . .
C16 C 0.4114(6) 0.6038(18) 0.2471(4) 0.035(3) Uani 1 1 d . . . . .
H16 H 0.408346 0.700814 0.223895 0.042 Uiso 1 1 calc R U . . .
C8 C 0.1698(6) 0.347(2) 0.3769(4) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.187411 0.460702 0.369240 0.057 Uiso 1 1 calc R U . . .
N2 N 0.3263(5) 0.7640(18) 0.5776(4) 0.055(3) Uani 1 1 d . . . . .
H2A H 0.355921 0.709128 0.603966 0.066 Uiso 1 1 calc R U . . .
H2B H 0.324886 0.694880 0.551141 0.066 Uiso 1 1 calc R U . . .
C7 C 0.2262(6) -0.1548(19) 0.4254(4) 0.046(3) Uani 1 1 d . . . . .
H7 H 0.261920 -0.237146 0.435831 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2645(6) 0.5932(19) 0.3165(4) 0.043(3) Uani 1 1 d . . . . .
H13 H 0.230978 0.683889 0.306773 0.051 Uiso 1 1 calc R U . . .
C17 C 0.5163(6) 0.3169(18) 0.4558(3) 0.034(3) Uani 1 1 d . . . . .
H17 H 0.546958 0.271328 0.485195 0.041 Uiso 1 1 calc R U . . .
C5 C 0.0819(7) -0.199(2) 0.4943(4) 0.045(3) Uani 1 1 d . . . . .
H5 H 0.090336 -0.297791 0.517756 0.054 Uiso 1 1 calc R U . . .
C6 C 0.0140(6) 0.311(2) 0.4434(4) 0.044(3) Uani 1 1 d . . . . .
H6 H -0.006468 0.421657 0.449069 0.053 Uiso 1 1 calc R U . . .
C20 C 0.3274(7) 0.4105(19) 0.4826(4) 0.048(3) Uani 1 1 d . . . . .
H20 H 0.325925 0.278219 0.474848 0.058 Uiso 1 1 calc R U . . .
C10 C -0.0319(6) 0.088(2) 0.2875(4) 0.055(4) Uani 1 1 d . . . . .
H10 H -0.062027 0.146800 0.259697 0.066 Uiso 1 1 calc R U . . .
C19 C 0.6135(6) 0.626(2) 0.3408(4) 0.048(3) Uani 1 1 d . . . . .
H19 H 0.589274 0.733832 0.324705 0.058 Uiso 1 1 calc R U . . .
C9 C 0.0332(6) -0.4029(19) 0.3386(4) 0.045(3) Uani 1 1 d . . . . .
H9 H 0.027442 -0.533631 0.329231 0.053 Uiso 1 1 calc R U . . .
C11 C 0.1578(7) 0.025(2) 0.2548(4) 0.048(3) Uani 1 1 d . . . . .
H11 H 0.155562 0.159125 0.259429 0.057 Uiso 1 1 calc R U . . .
C18 C 0.4634(7) 0.802(2) 0.4022(4) 0.053(4) Uani 1 1 d . . . . .
H18 H 0.471492 0.933278 0.410773 0.064 Uiso 1 1 calc R U . . .
C3 C 0.2622(6) 0.748(2) 0.5829(4) 0.056(4) Uani 1 1 d . . . . .
H3A H 0.251136 0.610267 0.582718 0.067 Uiso 1 1 calc R U . . .
H3B H 0.229740 0.808694 0.554517 0.067 Uiso 1 1 calc R U . . .
C12 C -0.1159(7) -0.277(3) 0.4022(6) 0.090(6) Uani 1 1 d . . . . .
H12 H -0.086304 -0.376807 0.415734 0.108 Uiso 1 1 calc R U . . .
C4 C 0.3478(8) 0.963(2) 0.5723(5) 0.071(5) Uani 1 1 d . . . . .
H4A H 0.317279 1.022834 0.543176 0.107 Uiso 1 1 calc R U . . .
H4B H 0.389443 0.957449 0.569233 0.107 Uiso 1 1 calc R U . . .
H4C H 0.350886 1.038820 0.600926 0.107 Uiso 1 1 calc R U . . .
C2 C 0.2600(6) 0.841(3) 0.6298(4) 0.063(4) Uani 1 1 d . . . . .
H2C H 0.294561 0.787807 0.658333 0.076 Uiso 1 1 calc R U . . .
H2D H 0.266725 0.980455 0.628815 0.076 Uiso 1 1 calc R U . . .
C1 C 0.1975(8) 0.804(2) 0.6348(5) 0.069(5) Uani 1 1 d . . . . .
H1D H 0.191694 0.663486 0.636301 0.083 Uiso 1 1 calc R U . . .
H1E H 0.163298 0.852179 0.605472 0.083 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
Fe4 O19 1.954(6) . ?
Fe4 O32 2.019(6) . ?
Fe4 O21 2.018(8) . ?
Fe4 O30 2.021(8) . ?
Fe4 O29 2.019(8) . ?
Fe4 O22 2.015(8) . ?
Fe6 O19 1.935(6) . ?
Fe6 O25 2.047(7) . ?
Fe6 O27 1.997(8) . ?
Fe6 O34 2.013(8) . ?
Fe6 O31 2.031(7) . ?
Fe6 O28 2.030(8) . ?
Fe2 O1 1.903(7) . ?
Fe2 O18 2.072(7) . ?
Fe2 O2 2.011(8) . ?
Fe2 O6 2.016(8) . ?
Fe2 O5 1.998(9) . ?
Fe2 O8 2.013(8) . ?
Fe1 O1 1.933(7) . ?
Fe1 O3 2.042(7) . ?
Fe1 O4 2.009(8) . ?
Fe1 O14 1.994(8) . ?
Fe1 O11 2.023(8) . ?
Fe1 O12 2.016(9) . ?
Fe3 O16 2.034(7) . ?
Fe3 O9 2.005(8) . ?
Fe3 O7 2.004(8) . ?
Fe3 O1 1.941(6) . ?
Fe3 O13 1.984(9) . ?
Fe3 O10 2.019(9) . ?
Fe5 O19 1.886(6) . ?
Fe5 O36 2.106(7) . ?
Fe5 O26 2.003(8) . ?
Fe5 O24 2.040(8) . ?
Fe5 O20 1.995(8) . ?
Fe5 O23 2.027(8) . ?
O16 C11 1.297(13) . ?
O25 C16 1.245(13) . ?
O9 C7 1.246(13) . ?
O32 C20 1.234(14) . ?
O7 C8 1.254(15) . ?
O3 C5 1.230(14) . ?
O36 H36A 0.8647 . ?
O36 H36B 0.8652 . ?
O4 C6 1.214(14) . ?
O21 C14 1.237(13) . ?
O27 C15 1.261(13) . ?
O34 C19 1.279(15) . ?
O30 C17 1.256(13) . ?
O29 C18 1.236(14) . ?
O22 C13 1.222(12) . ?
O18 H18A 0.8496 . ?
O18 H18B 0.8508 . ?
O31 C17 1.268(12) . ?
O13 C9 1.247(14) . ?
O26 C15 1.234(13) . ?
O28 C18 1.237(14) . ?
O24 C16 1.230(13) . ?
O2 C5 1.247(14) . ?
O14 C12 1.211(18) . ?
O10 C10 1.237(14) . ?
O11 C10 1.302(14) . ?
O17 C11 1.229(13) . ?
O6 C8 1.254(12) . ?
O5 C6 1.296(14) . ?
O20 C14 1.228(13) . ?
O8 C7 1.279(13) . ?
O23 C13 1.253(13) . ?
O33 C20 1.245(12) . ?
O12 C9 1.259(13) . ?
O35 C19 1.212(14) . ?
O15 C12 1.194(17) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.473(13) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C16 H16 0.9300 . ?
C8 H8 0.9300 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C3 1.491(15) . ?
N2 C4 1.470(17) . ?
C7 H7 0.9300 . ?
C13 H13 0.9300 . ?
C17 H17 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C20 H20 0.9300 . ?
C10 H10 0.9300 . ?
C19 H19 0.9300 . ?
C9 H9 0.9300 . ?
C11 H11 0.9300 . ?
C18 H18 0.9300 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.516(15) . ?
C12 H12 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C1 1.470(17) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?

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
O19 Fe4 O32 177.7(3) . . ?
O19 Fe4 O21 92.2(3) . . ?
O19 Fe4 O30 96.7(3) . . ?
O19 Fe4 O29 94.1(3) . . ?
O19 Fe4 O22 92.1(3) . . ?
O32 Fe4 O30 85.5(3) . . ?
O32 Fe4 O29 85.6(3) . . ?
O21 Fe4 O32 88.1(3) . . ?
O21 Fe4 O30 88.6(4) . . ?
O21 Fe4 O29 173.7(3) . . ?
O29 Fe4 O30 90.2(4) . . ?
O22 Fe4 O32 85.6(3) . . ?
O22 Fe4 O21 91.9(4) . . ?
O22 Fe4 O30 171.1(3) . . ?
O22 Fe4 O29 88.3(4) . . ?
O19 Fe6 O25 93.8(3) . . ?
O19 Fe6 O27 92.9(3) . . ?
O19 Fe6 O34 174.6(3) . . ?
O19 Fe6 O31 96.1(3) . . ?
O19 Fe6 O28 94.7(3) . . ?
O27 Fe6 O25 94.0(3) . . ?
O27 Fe6 O34 81.7(3) . . ?
O27 Fe6 O31 88.3(3) . . ?
O27 Fe6 O28 172.3(3) . . ?
O34 Fe6 O25 86.7(3) . . ?
O34 Fe6 O31 83.7(3) . . ?
O34 Fe6 O28 90.6(3) . . ?
O31 Fe6 O25 169.7(3) . . ?
O28 Fe6 O25 86.6(3) . . ?
O28 Fe6 O31 89.8(3) . . ?
O1 Fe2 O18 178.7(3) . . ?
O1 Fe2 O2 96.1(3) . . ?
O1 Fe2 O6 96.3(3) . . ?
O1 Fe2 O5 95.2(3) . . ?
O1 Fe2 O8 96.1(3) . . ?
O2 Fe2 O18 82.8(3) . . ?
O2 Fe2 O6 167.5(3) . . ?
O2 Fe2 O8 86.6(4) . . ?
O6 Fe2 O18 84.8(3) . . ?
O5 Fe2 O18 85.6(3) . . ?
O5 Fe2 O2 92.1(4) . . ?
O5 Fe2 O6 88.6(4) . . ?
O5 Fe2 O8 168.7(4) . . ?
O8 Fe2 O18 83.1(3) . . ?
O8 Fe2 O6 90.3(4) . . ?
O1 Fe1 O3 94.0(3) . . ?
O1 Fe1 O4 93.3(3) . . ?
O1 Fe1 O14 177.2(4) . . ?
O1 Fe1 O11 96.0(3) . . ?
O1 Fe1 O12 94.9(3) . . ?
O4 Fe1 O3 93.6(4) . . ?
O4 Fe1 O11 88.3(4) . . ?
O4 Fe1 O12 171.8(3) . . ?
O14 Fe1 O3 87.5(3) . . ?
O14 Fe1 O4 84.2(3) . . ?
O14 Fe1 O11 82.6(3) . . ?
O14 Fe1 O12 87.6(4) . . ?
O11 Fe1 O3 169.7(3) . . ?
O12 Fe1 O3 86.7(4) . . ?
O12 Fe1 O11 89.9(4) . . ?
O9 Fe3 O16 85.6(3) . . ?
O9 Fe3 O10 172.4(3) . . ?
O7 Fe3 O16 86.3(3) . . ?
O7 Fe3 O9 92.4(4) . . ?
O7 Fe3 O10 89.4(4) . . ?
O1 Fe3 O16 177.8(3) . . ?
O1 Fe3 O9 92.4(3) . . ?
O1 Fe3 O7 94.5(3) . . ?
O1 Fe3 O13 94.9(3) . . ?
O1 Fe3 O10 94.9(3) . . ?
O13 Fe3 O16 84.2(3) . . ?
O13 Fe3 O9 86.2(4) . . ?
O13 Fe3 O7 170.5(3) . . ?
O13 Fe3 O10 90.8(4) . . ?
O10 Fe3 O16 87.1(3) . . ?
O19 Fe5 O36 176.0(3) . . ?
O19 Fe5 O26 95.6(3) . . ?
O19 Fe5 O24 96.2(3) . . ?
O19 Fe5 O20 95.5(3) . . ?
O19 Fe5 O23 97.2(3) . . ?
O26 Fe5 O36 87.4(3) . . ?
O26 Fe5 O24 92.0(4) . . ?
O26 Fe5 O23 167.2(3) . . ?
O24 Fe5 O36 81.0(3) . . ?
O20 Fe5 O36 87.2(3) . . ?
O20 Fe5 O26 87.9(4) . . ?
O20 Fe5 O24 168.2(3) . . ?
O20 Fe5 O23 91.5(4) . . ?
O23 Fe5 O36 79.9(3) . . ?
O23 Fe5 O24 85.9(4) . . ?
Fe6 O19 Fe4 118.8(3) . . ?
Fe5 O19 Fe4 120.9(3) . . ?
Fe5 O19 Fe6 120.2(3) . . ?
C11 O16 Fe3 131.5(8) . . ?
C16 O25 Fe6 133.3(7) . . ?
C7 O9 Fe3 135.8(8) . . ?
C20 O32 Fe4 130.1(8) . . ?
C8 O7 Fe3 132.5(8) . . ?
Fe2 O1 Fe1 120.1(3) . . ?
Fe2 O1 Fe3 120.5(4) . . ?
Fe1 O1 Fe3 119.4(3) . . ?
C5 O3 Fe1 132.5(8) . . ?
Fe5 O36 H36A 110.0 . . ?
Fe5 O36 H36B 110.2 . . ?
H36A O36 H36B 103.7 . . ?
C6 O4 Fe1 133.3(8) . . ?
C14 O21 Fe4 132.6(8) . . ?
C15 O27 Fe6 130.6(8) . . ?
C19 O34 Fe6 133.0(9) . . ?
C17 O30 Fe4 131.7(7) . . ?
C18 O29 Fe4 132.6(9) . . ?
C13 O22 Fe4 134.9(8) . . ?
Fe2 O18 H18A 127.6 . . ?
Fe2 O18 H18B 127.9 . . ?
H18A O18 H18B 104.5 . . ?
C17 O31 Fe6 134.6(8) . . ?
C9 O13 Fe3 134.2(8) . . ?
C15 O26 Fe5 131.1(8) . . ?
C18 O28 Fe6 129.4(9) . . ?
C16 O24 Fe5 129.6(8) . . ?
C5 O2 Fe2 131.2(8) . . ?
C12 O14 Fe1 134.3(10) . . ?
C10 O10 Fe3 134.1(7) . . ?
C10 O11 Fe1 132.1(8) . . ?
C8 O6 Fe2 130.4(9) . . ?
C6 O5 Fe2 130.3(8) . . ?
C14 O20 Fe5 130.0(8) . . ?
C7 O8 Fe2 130.6(8) . . ?
C13 O23 Fe5 127.8(8) . . ?
C9 O12 Fe1 131.8(8) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
O27 C15 H15 115.8 . . ?
O26 C15 O27 128.4(10) . . ?
O26 C15 H15 115.8 . . ?
O21 C14 H14 115.5 . . ?
O20 C14 O21 129.0(12) . . ?
O20 C14 H14 115.5 . . ?
O25 C16 H16 116.6 . . ?
O24 C16 O25 126.8(11) . . ?
O24 C16 H16 116.6 . . ?
O7 C8 O6 128.3(13) . . ?
O7 C8 H8 115.8 . . ?
O6 C8 H8 115.8 . . ?
H2A N2 H2B 107.4 . . ?
C3 N2 H2A 108.3 . . ?
C3 N2 H2B 108.3 . . ?
C4 N2 H2A 108.3 . . ?
C4 N2 H2B 108.3 . . ?
C4 N2 C3 116.1(12) . . ?
O9 C7 O8 124.9(12) . . ?
O9 C7 H7 117.6 . . ?
O8 C7 H7 117.6 . . ?
O22 C13 O23 128.6(13) . . ?
O22 C13 H13 115.7 . . ?
O23 C13 H13 115.7 . . ?
O30 C17 O31 125.0(10) . . ?
O30 C17 H17 117.5 . . ?
O31 C17 H17 117.5 . . ?
O3 C5 O2 126.2(12) . . ?
O3 C5 H5 116.9 . . ?
O2 C5 H5 116.9 . . ?
O4 C6 O5 127.2(12) . . ?
O4 C6 H6 116.4 . . ?
O5 C6 H6 116.4 . . ?
O32 C20 O33 128.6(12) . . ?
O32 C20 H20 115.7 . . ?
O33 C20 H20 115.7 . . ?
O10 C10 O11 124.9(11) . . ?
O10 C10 H10 117.6 . . ?
O11 C10 H10 117.6 . . ?
O34 C19 H19 117.3 . . ?
O35 C19 O34 125.4(14) . . ?
O35 C19 H19 117.3 . . ?
O13 C9 O12 126.2(12) . . ?
O13 C9 H9 116.9 . . ?
O12 C9 H9 116.9 . . ?
O16 C11 H11 117.8 . . ?
O17 C11 O16 124.4(13) . . ?
O17 C11 H11 117.8 . . ?
O29 C18 O28 129.6(14) . . ?
O29 C18 H18 115.2 . . ?
O28 C18 H18 115.2 . . ?
N2 C3 H3A 108.8 . . ?
N2 C3 H3B 108.8 . . ?
N2 C3 C2 113.9(11) . . ?
H3A C3 H3B 107.7 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
O14 C12 H12 112.8 . . ?
O15 C12 O14 134.4(17) . . ?
O15 C12 H12 112.8 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C2 H2C 109.5 . . ?
C3 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
C1 C2 C3 110.9(11) . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 H1E 108.7 . . ?
C2 C1 N1 114.3(12) . . ?
C2 C1 H1D 108.7 . . ?
C2 C1 H1E 108.7 . . ?
H1D C1 H1E 107.6 . . ?

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
Fe4 O32 C20 O33 -171.0(10) . . . . ?
Fe4 O21 C14 O20 -11(2) . . . . ?
Fe4 O30 C17 O31 -8.5(19) . . . . ?
Fe4 O29 C18 O28 -8(2) . . . . ?
Fe4 O22 C13 O23 8(2) . . . . ?
Fe6 O25 C16 O24 -18.4(19) . . . . ?
Fe6 O27 C15 O26 -2.6(18) . . . . ?
Fe6 O34 C19 O35 174.3(9) . . . . ?
Fe6 O31 C17 O30 1(2) . . . . ?
Fe6 O28 C18 O29 1(2) . . . . ?
Fe2 O2 C5 O3 -19(2) . . . . ?
Fe2 O6 C8 O7 0(2) . . . . ?
Fe2 O5 C6 O4 7.6(19) . . . . ?
Fe2 O8 C7 O9 9.9(19) . . . . ?
Fe1 O3 C5 O2 17(2) . . . . ?
Fe1 O4 C6 O5 -5(2) . . . . ?
Fe1 O14 C12 O15 173.6(14) . . . . ?
Fe1 O11 C10 O10 8(2) . . . . ?
Fe1 O12 C9 O13 -1(2) . . . . ?
Fe3 O16 C11 O17 170.2(9) . . . . ?
Fe3 O9 C7 O8 -6(2) . . . . ?
Fe3 O7 C8 O6 -2(2) . . . . ?
Fe3 O13 C9 O12 4(2) . . . . ?
Fe3 O10 C10 O11 -3(2) . . . . ?
Fe5 O26 C15 O27 -10.5(18) . . . . ?
Fe5 O24 C16 O25 10.3(19) . . . . ?
Fe5 O20 C14 O21 11(2) . . . . ?
Fe5 O23 C13 O22 -11(2) . . . . ?
O26 Fe5 O19 Fe4 -135.7(5) . . . . ?
O26 Fe5 O19 Fe6 44.5(5) . . . . ?
O24 Fe5 O19 Fe4 131.6(5) . . . . ?
O24 Fe5 O19 Fe6 -48.1(5) . . . . ?
O20 Fe5 O19 Fe4 -47.2(5) . . . . ?
O20 Fe5 O19 Fe6 133.0(5) . . . . ?
O23 Fe5 O19 Fe4 45.0(5) . . . . ?
O23 Fe5 O19 Fe6 -134.8(5) . . . . ?
N2 C3 C2 C1 -174.9(13) . . . . ?
C3 C2 C1 N1 -178.4(13) . . . . ?
C4 N2 C3 C2 -64.3(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.336
_oxdiff_exptl_absorpt_empirical_full_min 0.444
