# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

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

data_M-173
_database_code_depnum_ccdc_archive 'CCDC 2311804'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_M-173               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT020_M-173               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.509 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT031_M-173               
;
PROBLEM: Refined Extinction Parameter Within Range of ...      2.000 Sigma
RESPONSE: The extinction parameter has been used to model dynamic scatter contribution to the observed intensities during refinement with a model based on kinematic approximation.
;
_vrf_PLAT082_M-173               
;
PROBLEM: High R1 Value ..................................       0.18 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_vrf_PLAT084_M-173               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.40 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_vrf_PLAT341_M-173               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.016 Ang.
RESPONSE: Low C-C bond precision is the results of larger unit cell dimension ESD observed in 3D-ED data and disorder present in the crystal structures
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(m3-1,2,3-methyltriazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C18 H18 Fe3 N18'
_chemical_formula_sum            'C18 H18 Fe3 N18'
_chemical_formula_weight         654.00
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      173(1)
_chemical_oxdiff_formula         'Fe C H N O'
_chemical_oxdiff_usercomment     -100C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   16.84(8)
_cell_length_b                   16.84(8)
_cell_length_c                   16.84(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4773(68)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1289
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      0.8780
_cell_measurement_theta_min      0.1200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             927
_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  0.5094
_diffrn_reflns_av_unetI/netI     0.1846
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.896
_diffrn_reflns_theta_min         0.074
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  53.00   0.25    0.25    --    0.00   0.00   0.00  424
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004632000
_diffrn_orient_matrix_UB_12      0.0013871000
_diffrn_orient_matrix_UB_13      -0.0002738000
_diffrn_orient_matrix_UB_21      -0.0001645000
_diffrn_orient_matrix_UB_22      0.0002400000
_diffrn_orient_matrix_UB_23      0.0014643000
_diffrn_orient_matrix_UB_31      0.0014082000
_diffrn_orient_matrix_UB_32      0.0004857000
_diffrn_orient_matrix_UB_33      0.0000814000
_diffrn_oxdiff_ac6_digest_hkl_ed 
;
11a4c870201f240baf46587a33f87442315731
;
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                188
_reflns_number_total             270
_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 1.171.43.86a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.9a 64-bit (release 17-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       70(35)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1904
_refine_ls_R_factor_gt           0.1779
_refine_ls_restrained_S_all      1.310
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3804
_refine_ls_wR_factor_ref         0.3978
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C6(0.25) H6A(0.25) H6B(0.25) H6C(0.25)
3.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_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
Fe1 Fe 0.125000 0.625000 0.625000 0.029(2) Uani 1 24 d S T P . .
Fe2 Fe 0.250000 0.750000 0.500000 0.052(2) Uani 1 12 d S T P . .
N3 N 0.2487(6) 0.625000 0.625000 0.045(3) Uani 1 4 d S T P . .
N4 N 0.2935(5) 0.6697(4) 0.5803(4) 0.061(3) Uani 1 2 d S T P A .
C5 C 0.3689(7) 0.6542(6) 0.5958(6) 0.094(5) Uani 1 2 d S T P . .
C6 C 0.4450(14) 0.6921(16) 0.5881(15) 0.061(9) Uani 0.25 1 d . . P A -1
H6A H 0.472390 0.670599 0.542957 0.092 Uiso 0.25 1 calc R U P A -1
H6B H 0.475693 0.682717 0.635217 0.092 Uiso 0.25 1 calc R U P A -1
H6C H 0.437643 0.748156 0.580999 0.092 Uiso 0.25 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
Fe1 N3 2.083(14) . ?
Fe1 N3 2.083(14) 6_456 ?
Fe1 N3 2.083(14) 77_455 ?
Fe1 N3 2.083(14) 82_545 ?
Fe1 N3 2.083(14) 50_464 ?
Fe1 N3 2.083(14) 57_455 ?
Fe2 N4 2.048(14) 155_665 ?
Fe2 N4 2.048(14) . ?
Fe2 N4 2.048(14) 128_565 ?
Fe2 N4 2.048(14) 35_455 ?
Fe2 N4 2.048(14) 169_566 ?
Fe2 N4 2.048(14) 56 ?
N3 N4 1.303(12) . ?
N3 N4 1.303(12) 76_456 ?
N4 C5 1.322(16) . ?
C5 C5 1.39(3) 76_456 ?
C5 C6 1.44(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
N3 Fe1 N3 90.000(1) . 82_545 ?
N3 Fe1 N3 90.000(2) 50_464 6_456 ?
N3 Fe1 N3 90.000(1) 50_464 57_455 ?
N3 Fe1 N3 180.0 . 50_464 ?
N3 Fe1 N3 90.000(1) . 57_455 ?
N3 Fe1 N3 90.000(2) 82_545 50_464 ?
N3 Fe1 N3 90.000(1) 82_545 6_456 ?
N3 Fe1 N3 90.000(2) . 77_455 ?
N3 Fe1 N3 180.0 77_455 6_456 ?
N3 Fe1 N3 90.0 82_545 77_455 ?
N3 Fe1 N3 180.0 82_545 57_455 ?
N3 Fe1 N3 90.000(1) 50_464 77_455 ?
N3 Fe1 N3 90.000(1) 77_455 57_455 ?
N3 Fe1 N3 90.000(1) . 6_456 ?
N3 Fe1 N3 90.000(1) 6_456 57_455 ?
N4 Fe2 N4 180.0 155_665 35_455 ?
N4 Fe2 N4 180.0 56 128_565 ?
N4 Fe2 N4 92.1(3) 56 . ?
N4 Fe2 N4 92.1(3) 155_665 169_566 ?
N4 Fe2 N4 92.1(3) 35_455 . ?
N4 Fe2 N4 87.9(3) 35_455 169_566 ?
N4 Fe2 N4 92.1(3) 169_566 128_565 ?
N4 Fe2 N4 87.9(3) 155_665 56 ?
N4 Fe2 N4 87.9(3) 155_665 . ?
N4 Fe2 N4 92.1(3) 35_455 56 ?
N4 Fe2 N4 180.0(3) 169_566 . ?
N4 Fe2 N4 87.9(3) 169_566 56 ?
N4 Fe2 N4 87.9(3) 128_565 . ?
N4 Fe2 N4 92.1(3) 155_665 128_565 ?
N4 Fe2 N4 87.9(3) 35_455 128_565 ?
N4 N3 Fe1 125.3(6) 76_456 . ?
N4 N3 Fe1 125.3(6) . . ?
N4 N3 N4 109.4(12) . 76_456 ?
N3 N4 Fe2 123.8(7) . . ?
N3 N4 C5 109.1(10) . . ?
C5 N4 Fe2 127.1(7) . . ?
N4 C5 C5 106.2(6) . 76_456 ?
N4 C5 C6 138.7(16) . . ?
C5 C5 C6 112.2(13) 76_456 . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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
Fe1 N3 N4 Fe2 0.000(1) . . . . ?
Fe1 N3 N4 C5 180.000(1) . . . . ?
Fe2 N4 C5 C5 180.000(2) . . . 76_456 ?
Fe2 N4 C5 C6 22.3(14) . . . . ?
N3 N4 C5 C5 0.000(2) . . . 76_456 ?
N3 N4 C5 C6 -157.7(14) . . . . ?
N4 N3 N4 Fe2 180.000(1) 76_456 . . . ?
N4 N3 N4 C5 0.000(2) 76_456 . . . ?

_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 7.520
_oxdiff_exptl_absorpt_empirical_full_min 0.141
####################################################################### 
# 
# 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_M-293
_database_code_depnum_ccdc_archive 'CCDC 2311806'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_M-293               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT020_M-293               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.414 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT031_M-293               
;
PROBLEM: Refined Extinction Parameter Within Range of ...      2.393 Sigma
RESPONSE: The extinction parameter has been used to model dynamic scatter contribution to the observed intensities during refinement with a model based on kinematic approximation
;
_vrf_PLAT084_M-293               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: he high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_audit_creation_date             2023-06-29
_audit_creation_method           
;
Olex2 1.5-ac6-011
(compiled 2023.03.09 svn.rbb2c1857 for Rigaku Oxford Diffraction, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(m3-1,2,3-methyltriazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C18 H18 Fe3 N18'
_chemical_formula_sum            'C18 H18 Fe3 N18'
_chemical_formula_weight         654.00
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      293(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   17.26(9)
_cell_length_b                   17.26(9)
_cell_length_c                   17.26(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5146(78)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.8290
_cell_measurement_theta_min      0.0720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             927
_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  0.4135
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.897
_diffrn_reflns_theta_min         0.072
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  60.00   0.50    0.50    --    0.00   0.00   0.00  240
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001745000
_diffrn_orient_matrix_UB_12      -0.0008835000
_diffrn_orient_matrix_UB_13      0.0011357000
_diffrn_orient_matrix_UB_21      -0.0002640000
_diffrn_orient_matrix_UB_22      -0.0011485000
_diffrn_orient_matrix_UB_23      -0.0008550000
_diffrn_orient_matrix_UB_31      0.0014212000
_diffrn_orient_matrix_UB_32      -0.0001039000
_diffrn_orient_matrix_UB_33      -0.0003004000
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                208
_reflns_number_total             291
_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 1.171.43.76a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-011 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-011 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       67(28)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         291
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.1209
_refine_ls_restrained_S_all      1.211
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3453
_refine_ls_wR_factor_ref         0.3803
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25)
4.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_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
Fe1 Fe 0.375000 0.375000 0.375000 0.041(2) Uani 1 24 d S T P . .
N1 N 0.375000 0.375000 0.2482(5) 0.059(3) Uani 1 4 d S T P . .
N2 N 0.4191(4) 0.3309(4) 0.2058(4) 0.076(3) Uani 1 2 d S T P A .
C1 C 0.4024(5) 0.3476(5) 0.1301(6) 0.103(4) Uani 1 2 d S T P . .
C3 C 0.4416(14) 0.3405(16) 0.0572(12) 0.080(9) Uani 0.25 1 d . . P A -1
H3A H 0.480069 0.300554 0.060543 0.120 Uiso 0.25 1 calc R U P A -1
H3B H 0.404761 0.327528 0.017568 0.120 Uiso 0.25 1 calc R U P A -1
H3C H 0.466072 0.388837 0.044547 0.120 Uiso 0.25 1 calc R U P A -1
Fe2 Fe 0.500000 0.250000 0.250000 0.064(2) Uani 1 12 d S T P . .


_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 N1 2.190(14) . ?
Fe1 N1 2.190(14) 9 ?
Fe1 N1 2.190(14) 31_554 ?
Fe1 N1 2.190(14) 59_455 ?
Fe1 N1 2.190(14) 75_545 ?
Fe1 N1 2.190(14) 5 ?
N1 N2 1.301(11) 26_554 ?
N1 N2 1.301(11) . ?
N2 C1 1.368(15) . ?
N2 Fe2 2.117(14) . ?
C1 C1 1.34(2) 26_554 ?
C1 C3 1.43(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 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
N1 Fe1 N1 90.0 . 59_455 ?
N1 Fe1 N1 90.000(1) 75_545 31_554 ?
N1 Fe1 N1 90.000(1) 5 9 ?
N1 Fe1 N1 180.0 . 75_545 ?
N1 Fe1 N1 90.0 . 9 ?
N1 Fe1 N1 90.0 59_455 75_545 ?
N1 Fe1 N1 90.000(1) 59_455 31_554 ?
N1 Fe1 N1 90.000(1) . 5 ?
N1 Fe1 N1 180.0 5 31_554 ?
N1 Fe1 N1 90.0 59_455 5 ?
N1 Fe1 N1 90.0 75_545 9 ?
N1 Fe1 N1 90.0 75_545 5 ?
N1 Fe1 N1 90.0 31_554 9 ?
N1 Fe1 N1 90.0 . 31_554 ?
N1 Fe1 N1 180.0 59_455 9 ?
N2 N1 Fe1 124.2(5) . . ?
N2 N1 Fe1 124.2(5) 26_554 . ?
N2 N1 N2 111.6(9) 26_554 . ?
N1 N2 C1 106.9(8) . . ?
N1 N2 Fe2 124.7(6) . . ?
C1 N2 Fe2 128.4(6) . . ?
N2 C1 C3 136.2(14) . . ?
C1 C1 N2 107.3(5) 26_554 . ?
C1 C1 C3 113.1(12) 26_554 . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 Fe2 N2 92.3(3) . 82_545 ?
N2 Fe2 N2 87.7(3) 82_545 121_655 ?
N2 Fe2 N2 87.7(3) 31_554 121_655 ?
N2 Fe2 N2 92.3(3) 31_554 82_545 ?
N2 Fe2 N2 87.7(3) 31_554 154_565 ?
N2 Fe2 N2 180.0 . 121_655 ?
N2 Fe2 N2 87.7(3) 103_656 82_545 ?
N2 Fe2 N2 87.7(3) . 103_656 ?
N2 Fe2 N2 180.0(4) 154_565 82_545 ?
N2 Fe2 N2 92.3(3) . 31_554 ?
N2 Fe2 N2 92.3(3) 103_656 121_655 ?
N2 Fe2 N2 180.0(5) 103_656 31_554 ?
N2 Fe2 N2 92.3(3) 154_565 121_655 ?
N2 Fe2 N2 87.7(3) . 154_565 ?
N2 Fe2 N2 92.3(3) 103_656 154_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.581
_oxdiff_exptl_absorpt_empirical_full_min 0.448
####################################################################### 
# 
# 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_M-233
_database_code_depnum_ccdc_archive 'CCDC 2311805'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_M-233               
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT020_M-233               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.249 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT084_M-233               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components
;
_vrf_PLAT341_M-233               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: Low C-C bond precision is the results of larger unit cell dimension ESD observed in 3D-ED data and disorder present in the crystal structures
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(m3-1,2,3-methyltriazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C18 H18 Fe3 N18'
_chemical_formula_sum            'C18 H18 Fe3 N18'
_chemical_formula_weight         654.00
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      233(1)
_chemical_oxdiff_formula         'Fe C H N O'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   17.0(4)
_cell_length_b                   17.0(4)
_cell_length_c                   17.0(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4936(316)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    300
_cell_measurement_temperature    233(1)
_cell_measurement_theta_max      0.7830
_cell_measurement_theta_min      0.1150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.9a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             927
_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  0.2492
_diffrn_reflns_av_unetI/netI     0.1670
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1808
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.898
_diffrn_reflns_theta_min         0.073
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -19.75   0.25    0.25    --    0.00   0.00   0.00  141
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0005107000
_diffrn_orient_matrix_UB_12      0.0002450500
_diffrn_orient_matrix_UB_13      -0.0013631500
_diffrn_orient_matrix_UB_21      0.0001506500
_diffrn_orient_matrix_UB_22      -0.0014506000
_diffrn_orient_matrix_UB_23      -0.0002125500
_diffrn_orient_matrix_UB_31      -0.0013761500
_diffrn_orient_matrix_UB_32      -0.0000710000
_diffrn_orient_matrix_UB_33      -0.0005270500
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                134
_reflns_number_total             267
_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 1.171.44.9a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.44.9a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.44.9a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.098
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       85(33)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.1198
_refine_ls_restrained_S_all      1.117
_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)+(0.1823P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3236
_refine_ls_wR_factor_ref         0.3815
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C6(0.25) H6A(0.25) H6B(0.25) H6C(0.25)
3.a Me refined with riding coordinates:
 C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_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
Fe2 Fe 0.500000 0.500000 0.500000 0.064(3) Uani 1 12 d S T P . .
Fe1 Fe 0.375000 0.375000 0.375000 0.040(3) Uani 1 24 d S T P . .
N3 N 0.375000 0.5015(7) 0.375000 0.063(4) Uani 1 4 d S T P . .
N4 N 0.4194(5) 0.5442(7) 0.4194(5) 0.076(4) Uani 1 2 d S T P A .
C5 C 0.4025(6) 0.6184(10) 0.4025(6) 0.109(5) Uani 1 2 d S T P . .
C6 C 0.442(3) 0.6995(18) 0.408(3) 0.15(3) Uani 0.25 1 d . . P A -1
H6A H 0.406775 0.738883 0.388175 0.220 Uiso 0.25 1 calc R U P A -1
H6B H 0.454382 0.710788 0.461804 0.220 Uiso 0.25 1 calc R U P A -1
H6C H 0.489293 0.699502 0.377360 0.220 Uiso 0.25 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
Fe2 N4 2.08(5) . ?
Fe2 N4 2.08(5) 101_666 ?
Fe2 N4 2.08(5) 5 ?
Fe2 N4 2.08(5) 105_666 ?
Fe2 N4 2.08(5) 9 ?
Fe2 N4 2.08(5) 97_666 ?
Fe1 N3 2.15(5) 82_545 ?
Fe1 N3 2.15(5) . ?
Fe1 N3 2.15(5) 54_455 ?
Fe1 N3 2.15(5) 9 ?
Fe1 N3 2.15(5) 26_554 ?
Fe1 N3 2.15(5) 5 ?
N3 N4 1.29(3) . ?
N3 N4 1.29(3) 75_545 ?
N4 C5 1.33(3) . ?
C5 C5 1.33(4) 75_545 ?
C5 C6 1.54(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
N4 Fe2 N4 87.6(4) . 105_666 ?
N4 Fe2 N4 87.6(4) 9 101_666 ?
N4 Fe2 N4 87.6(4) 9 97_666 ?
N4 Fe2 N4 92.4(4) . 9 ?
N4 Fe2 N4 180.0(3) . 97_666 ?
N4 Fe2 N4 180.0(3) 105_666 9 ?
N4 Fe2 N4 92.4(4) 105_666 101_666 ?
N4 Fe2 N4 92.4(4) . 5 ?
N4 Fe2 N4 180.0(3) 5 101_666 ?
N4 Fe2 N4 87.6(4) 105_666 5 ?
N4 Fe2 N4 92.4(4) 105_666 97_666 ?
N4 Fe2 N4 92.4(4) 9 5 ?
N4 Fe2 N4 87.6(4) 5 97_666 ?
N4 Fe2 N4 87.6(4) . 101_666 ?
N4 Fe2 N4 92.4(4) 101_666 97_666 ?
N3 Fe1 N3 180.0 82_545 9 ?
N3 Fe1 N3 180.0 5 54_455 ?
N3 Fe1 N3 90.000(1) 5 . ?
N3 Fe1 N3 90.000(2) 82_545 26_554 ?
N3 Fe1 N3 90.000(2) 9 . ?
N3 Fe1 N3 90.000(1) 9 26_554 ?
N3 Fe1 N3 90.000(1) 26_554 54_455 ?
N3 Fe1 N3 90.000(1) 82_545 5 ?
N3 Fe1 N3 90.000(1) 82_545 . ?
N3 Fe1 N3 90.000(1) 9 5 ?
N3 Fe1 N3 180.0 26_554 . ?
N3 Fe1 N3 90.0 26_554 5 ?
N3 Fe1 N3 90.0 54_455 . ?
N3 Fe1 N3 90.000(1) 82_545 54_455 ?
N3 Fe1 N3 90.000(1) 9 54_455 ?
N4 N3 Fe1 124.2(7) 75_545 . ?
N4 N3 Fe1 124.2(7) . . ?
N4 N3 N4 111.6(15) . 75_545 ?
N3 N4 Fe2 124.6(9) . . ?
N3 N4 C5 106.3(11) . . ?
C5 N4 Fe2 129.1(9) . . ?
N4 C5 C5 107.9(7) . 75_545 ?
N4 C5 C6 138.3(16) . . ?
C5 C5 C6 110.6(13) 75_545 . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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
Fe2 N4 C5 C5 180.000(4) . . . 75_545 ?
Fe2 N4 C5 C6 24(3) . . . . ?
Fe1 N3 N4 Fe2 0.000(2) . . . . ?
Fe1 N3 N4 C5 180.000(2) . . . . ?
N3 N4 C5 C5 0.000(2) . . . 75_545 ?
N3 N4 C5 C6 -156(3) . . . . ?
N4 N3 N4 Fe2 180.000(1) 75_545 . . . ?
N4 N3 N4 C5 0.000(3) 75_545 . . . ?

_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 9.085
_oxdiff_exptl_absorpt_empirical_full_min 0.543
####################################################################### 
# 
# 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_M-373
_database_code_depnum_ccdc_archive 'CCDC 2311807'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_M-373               
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT020_M-373               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.236 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT213_M-373               
;
PROBLEM: Atom C6              has ADP max/min Ratio .....        4.8 prolat
RESPONSE: a disorder could not be model better for the high temperature structure (373K)
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(m3-1,2,3-methyltriazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C18 H18 Fe3 N18'
_chemical_formula_sum            'C18 H18 Fe3 N18'
_chemical_formula_weight         654.00
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      373(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   17.26(8)
_cell_length_b                   17.26(8)
_cell_length_c                   17.26(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5140(74)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1369
_cell_measurement_temperature    373(1)
_cell_measurement_theta_max      0.8980
_cell_measurement_theta_min      0.1160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             927
_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  0.2358
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.898
_diffrn_reflns_theta_min         0.072
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  50.00   0.25    0.25    --    0.00   0.00   0.00  400
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0013456000
_diffrn_orient_matrix_UB_12      -0.0002194000
_diffrn_orient_matrix_UB_13      -0.0005002000
_diffrn_orient_matrix_UB_21      0.0001847000
_diffrn_orient_matrix_UB_22      0.0014356000
_diffrn_orient_matrix_UB_23      -0.0001544000
_diffrn_orient_matrix_UB_31      0.0005161000
_diffrn_orient_matrix_UB_32      0.0000885000
_diffrn_orient_matrix_UB_33      0.0013578000
_diffrn_oxdiff_ac6_digest_hkl_ed 
;
1161d5e68abf78989352d0b526dfb123ae7d53
;
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                251
_reflns_number_total             291
_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 1.171.43.86a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.9a 64-bit (release 17-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       128(43)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         291
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.1218
_refine_ls_restrained_S_all      1.285
_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)+(0.1729P)²+1.9642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3406
_refine_ls_wR_factor_ref         0.3491
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C6(0.25) H6A(0.25) H6B(0.25) H6C(0.25)
4.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_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
Fe1 Fe 0.375000 0.375000 0.375000 0.038(2) Uani 1 24 d S T P . .
Fe2 Fe 0.500000 0.500000 0.500000 0.066(2) Uani 1 12 d S T P . .
N3 N 0.375000 0.375000 0.5024(5) 0.060(3) Uani 1 4 d S T P . .
N4 N 0.4186(3) 0.4186(3) 0.5442(4) 0.076(3) Uani 1 2 d S T P A .
C5 C 0.4036(5) 0.4036(5) 0.6184(6) 0.119(5) Uani 1 2 d S T P . .
C6 C 0.431(3) 0.424(5) 0.6909(14) 0.18(2) Uani 0.25 1 d . . P A -1
H6A H 0.485413 0.436220 0.687259 0.273 Uiso 0.25 1 calc R U P A -1
H6B H 0.424562 0.380936 0.725884 0.273 Uiso 0.25 1 calc R U P A -1
H6C H 0.403321 0.467802 0.709941 0.273 Uiso 0.25 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
Fe1 N3 2.198(13) 59_455 ?
Fe1 N3 2.198(13) 31_554 ?
Fe1 N3 2.198(13) 5 ?
Fe1 N3 2.198(13) 9 ?
Fe1 N3 2.198(13) 75_545 ?
Fe1 N3 2.198(13) . ?
Fe2 N4 2.129(13) . ?
Fe2 N4 2.129(13) 97_666 ?
Fe2 N4 2.129(13) 101_666 ?
Fe2 N4 2.129(13) 105_666 ?
Fe2 N4 2.129(13) 9 ?
Fe2 N4 2.129(13) 5 ?
N3 N4 1.285(10) 26_554 ?
N3 N4 1.285(10) . ?
N4 C5 1.331(14) . ?
C5 C5 1.39(2) 26_554 ?
C5 C6 1.38(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
N3 Fe1 N3 180.0 59_455 9 ?
N3 Fe1 N3 90.000(1) 75_545 31_554 ?
N3 Fe1 N3 180.0 75_545 . ?
N3 Fe1 N3 90.0 59_455 75_545 ?
N3 Fe1 N3 90.0 59_455 . ?
N3 Fe1 N3 90.0 9 75_545 ?
N3 Fe1 N3 90.0 9 31_554 ?
N3 Fe1 N3 90.0 59_455 5 ?
N3 Fe1 N3 180.0 5 31_554 ?
N3 Fe1 N3 90.000(1) 9 5 ?
N3 Fe1 N3 90.0 9 . ?
N3 Fe1 N3 90.0 75_545 5 ?
N3 Fe1 N3 90.0 5 . ?
N3 Fe1 N3 90.000(1) 59_455 31_554 ?
N3 Fe1 N3 90.000(1) 31_554 . ?
N4 Fe2 N4 87.8(3) . 105_666 ?
N4 Fe2 N4 180.0(2) 5 101_666 ?
N4 Fe2 N4 87.8(3) 5 97_666 ?
N4 Fe2 N4 92.2(3) . 9 ?
N4 Fe2 N4 92.2(3) 105_666 97_666 ?
N4 Fe2 N4 180.0 105_666 9 ?
N4 Fe2 N4 87.8(3) 9 101_666 ?
N4 Fe2 N4 92.2(3) . 5 ?
N4 Fe2 N4 180.0 . 97_666 ?
N4 Fe2 N4 87.8(3) 105_666 5 ?
N4 Fe2 N4 87.8(3) 9 97_666 ?
N4 Fe2 N4 92.2(3) 9 5 ?
N4 Fe2 N4 92.2(3) 101_666 97_666 ?
N4 Fe2 N4 87.8(3) . 101_666 ?
N4 Fe2 N4 92.2(3) 105_666 101_666 ?
N4 N3 Fe1 124.2(5) 26_554 . ?
N4 N3 Fe1 124.2(5) . . ?
N4 N3 N4 111.6(9) 26_554 . ?
N3 N4 Fe2 124.8(6) . . ?
N3 N4 C5 108.3(8) . . ?
C5 N4 Fe2 127.0(6) . . ?
N4 C5 C5 106.0(5) . 26_554 ?
N4 C5 C6 138.9(16) . . ?
C6 C5 C5 115.0(16) . 26_554 ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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
Fe1 N3 N4 Fe2 0.000(1) . . . . ?
Fe1 N3 N4 C5 180.000(1) . . . . ?
Fe2 N4 C5 C5 180.000(1) . . . 26_554 ?
Fe2 N4 C5 C6 -6(6) . . . . ?
N3 N4 C5 C5 0.000(1) . . . 26_554 ?
N3 N4 C5 C6 174(6) . . . . ?
N4 N3 N4 Fe2 180.000(0) 26_554 . . . ?
N4 N3 N4 C5 0.000(1) 26_554 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.419
_oxdiff_exptl_absorpt_empirical_full_min 0.431
####################################################################### 
# 
# 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_C-293
_database_code_depnum_ccdc_archive 'CCDC 2311810'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_C-293               
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT020_C-293               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.199 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT082_C-293               
;
PROBLEM: High R1 Value ..................................       0.20 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_vrf_PLAT084_C-293               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.44 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_vrf_PLAT341_C-293               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01667 Ang.
RESPONSE: Low C-C bond precision is the result of larger unit cell dimension ESD observed in 3D-ED data and disorder present in the crystal structures.
;
_audit_creation_date             2023-12-03
_audit_creation_method           
;
Olex2 1.5-ac6-014
(compiled 2023.11.29 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6869)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(1,4,5,6-tetrahydrocyclopenta[d][1,2,3]triazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H36 Fe3 N18'
_chemical_formula_sum            'C30 H36 Fe3 N18'
_chemical_formula_weight         816.28
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      293(2)
_chemical_oxdiff_formula         'C H N Fe'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   18.19(10)
_cell_length_b                   18.19(10)
_cell_length_c                   18.19(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6017(99)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1028
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.8970
_cell_measurement_theta_min      0.0670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.76a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1244
_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  0.1988
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.898
_diffrn_reflns_theta_min         0.068
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  16.00   0.50    0.50    --    0.00   0.00   0.00  132
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0012428000
_diffrn_orient_matrix_UB_12      -0.0005900000
_diffrn_orient_matrix_UB_13      0.0000119000
_diffrn_orient_matrix_UB_21      -0.0004225000
_diffrn_orient_matrix_UB_22      0.0008996000
_diffrn_orient_matrix_UB_23      0.0009609000
_diffrn_orient_matrix_UB_31      -0.0004211000
_diffrn_orient_matrix_UB_32      0.0008653000
_diffrn_orient_matrix_UB_33      -0.0009915000
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                306
_reflns_number_total             333
_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 1.171.43.76a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.76a 64-bit (release 21-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       944(323)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2030
_refine_ls_R_factor_gt           0.1956
_refine_ls_restrained_S_all      1.841
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4352
_refine_ls_wR_factor_ref         0.4417
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H7A(0.25) H7B(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
;
_atom_sites_solution_hydrogens   geom
_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
Fe1 Fe 0.625000 0.125000 0.625000 0.026(3) Uani 1 24 d S T P . .
Fe2 Fe 0.500000 0.250000 0.750000 0.027(3) Uani 1 12 d S T P . .
N3 N 0.5825(4) 0.2878(5) 0.6675(4) 0.038(4) Uani 1 2 d S T P . .
N5 N 0.625000 0.2471(7) 0.625000 0.039(4) Uani 1 4 d S T P . .
C4 C 0.5979(5) 0.3573(5) 0.6521(5) 0.038(4) Uani 1 2 d S T P . .
C6 C 0.5763(5) 0.4316(7) 0.6737(5) 0.052(4) Uani 1 2 d S T P . .
H6A H 0.585899 0.440003 0.725513 0.062 Uiso 0.5 1 calc R U P . .
H6B H 0.524487 0.440003 0.664101 0.062 Uiso 0.5 1 calc R U P . .
C7 C 0.625000 0.4816(11) 0.625000 0.091(9) Uani 1 4 d S T P . .
H7A H 0.594410 0.512793 0.594410 0.109 Uiso 0.5 2 calc R U P . .
H7B H 0.655590 0.512794 0.655590 0.109 Uiso 0.5 2 calc R U P . .


_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 N5 2.221(17) . ?
Fe1 N5 2.221(17) 54_455 ?
Fe1 N5 2.221(17) 29_545 ?
Fe1 N5 2.221(17) 58_545 ?
Fe1 N5 2.221(17) 50_554 ?
Fe1 N5 2.221(17) 81_545 ?
Fe2 N3 2.231(15) . ?
Fe2 N3 2.231(15) 121_656 ?
Fe2 N3 2.231(15) 79 ?
Fe2 N3 2.231(15) 178_566 ?
Fe2 N3 2.231(15) 58_545 ?
Fe2 N3 2.231(15) 151_556 ?
N3 N5 1.319(14) . ?
N3 C4 1.325(15) . ?
C4 C4 1.39(3) 27_645 ?
C4 C6 1.461(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.55(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 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
N5 Fe1 N5 90.000(1) . 58_545 ?
N5 Fe1 N5 90.000(1) 50_554 54_455 ?
N5 Fe1 N5 90.000(1) 50_554 81_545 ?
N5 Fe1 N5 180.0 . 50_554 ?
N5 Fe1 N5 90.000(2) . 81_545 ?
N5 Fe1 N5 90.000(2) 58_545 50_554 ?
N5 Fe1 N5 90.000(1) 58_545 54_455 ?
N5 Fe1 N5 90.000(1) . 29_545 ?
N5 Fe1 N5 180.0 29_545 54_455 ?
N5 Fe1 N5 90.000(1) 58_545 29_545 ?
N5 Fe1 N5 180.0 58_545 81_545 ?
N5 Fe1 N5 90.000(1) 50_554 29_545 ?
N5 Fe1 N5 90.000(2) 29_545 81_545 ?
N5 Fe1 N5 90.000(1) . 54_455 ?
N5 Fe1 N5 90.0 54_455 81_545 ?
N3 Fe2 N3 92.2(3) . 178_566 ?
N3 Fe2 N3 92.2(3) 58_545 151_556 ?
N3 Fe2 N3 92.2(3) 79 121_656 ?
N3 Fe2 N3 87.8(3) . 58_545 ?
N3 Fe2 N3 87.8(3) 178_566 121_656 ?
N3 Fe2 N3 180.0(3) 178_566 58_545 ?
N3 Fe2 N3 87.8(3) 178_566 151_556 ?
N3 Fe2 N3 87.8(3) . 79 ?
N3 Fe2 N3 180.0(4) 79 151_556 ?
N3 Fe2 N3 92.2(3) 178_566 79 ?
N3 Fe2 N3 92.2(3) 58_545 121_656 ?
N3 Fe2 N3 87.8(3) 58_545 79 ?
N3 Fe2 N3 87.8(3) 151_556 121_656 ?
N3 Fe2 N3 92.2(3) . 151_556 ?
N3 Fe2 N3 180.0(2) . 121_656 ?
N5 N3 Fe2 128.0(7) . . ?
N5 N3 C4 106.7(9) . . ?
C4 N3 Fe2 125.3(8) . . ?
N3 N5 Fe1 124.1(6) 27_645 . ?
N3 N5 Fe1 124.1(6) . . ?
N3 N5 N3 111.9(12) . 27_645 ?
N3 C4 C4 107.4(7) . 27_645 ?
N3 C4 C6 140.2(11) . . ?
C4 C4 C6 112.4(7) 27_645 . ?
C4 C6 H6A 111.0 . . ?
C4 C6 H6B 111.0 . . ?
C4 C6 C7 103.6(10) . . ?
H6A C6 H6B 109.0 . . ?
C7 C6 H6A 111.1 . . ?
C7 C6 H6B 111.0 . . ?
C6 C7 C6 108.1(15) 27_645 . ?
C6 C7 H7A 110.1 27_645 . ?
C6 C7 H7A 110.1 . . ?
C6 C7 H7B 110.1 . . ?
C6 C7 H7B 110.1 27_645 . ?
H7A C7 H7B 108.4 . . ?

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
Fe2 N3 N5 Fe1 0.000(2) . . . . ?
Fe2 N3 N5 N3 180.000(1) . . . 27_645 ?
Fe2 N3 C4 C4 180.001(3) . . . 27_645 ?
Fe2 N3 C4 C6 -0.001(6) . . . . ?
N3 C4 C6 C7 180.002(4) . . . . ?
N5 N3 C4 C4 0.002(1) . . . 27_645 ?
N5 N3 C4 C6 180.000(4) . . . . ?
C4 N3 N5 Fe1 179.999(2) . . . . ?
C4 N3 N5 N3 -0.001(3) . . . 27_645 ?
C4 C4 C6 C7 0.000(3) 27_645 . . . ?
C4 C6 C7 C6 0.000(4) . . . 27_645 ?

_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 2.125
_oxdiff_exptl_absorpt_empirical_full_min 0.600
####################################################################### 
# 
# 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_C-173
_database_code_depnum_ccdc_archive 'CCDC 2311808'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_C-173               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT020_C-173               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.311 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT213_C-173               
;
PROBLEM: Atom C7              has ADP max/min Ratio .....        7.1 prolat
RESPONSE: The disorder model of carbon atoms is hard to model due to dynamic scatter intensities
;
_vrf_PLAT084_C-173               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: he high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_vrf_PLAT250_C-173               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.5 Note
RESPONSE: The disorder model of carbon atoms is hard to model due to dynamic scatter intensities
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(1,4,5,6-tetrahydrocyclopenta[d][1,2,3]triazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H36 Fe3 N18'
_chemical_formula_sum            'C30 H36 Fe3 N18'
_chemical_formula_weight         816.28
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      173(1)
_chemical_oxdiff_formula         'C8 H5 N5 Fe2 '
_chemical_oxdiff_usercomment     '173.15K '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   18.06(7)
_cell_length_b                   18.06(7)
_cell_length_c                   18.06(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5893(65)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1560
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      0.8930
_cell_measurement_theta_min      0.0680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1244
_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  0.3114
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6138
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.896
_diffrn_reflns_theta_min         0.069
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  50.00   0.25    0.25    --    0.00   0.00   0.00  400
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0009305000
_diffrn_orient_matrix_UB_12      0.0006218000
_diffrn_orient_matrix_UB_13      0.0008219000
_diffrn_orient_matrix_UB_21      -0.0009422000
_diffrn_orient_matrix_UB_22      0.0009653000
_diffrn_orient_matrix_UB_23      0.0003347000
_diffrn_orient_matrix_UB_31      -0.0004233000
_diffrn_orient_matrix_UB_32      -0.0007806000
_diffrn_orient_matrix_UB_33      0.0010703000
_diffrn_oxdiff_ac6_digest_hkl_ed 
;
117916b4fb1c40fc098883efd638ca9a428275
;
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                310
_reflns_number_total             327
_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 1.171.43.86a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.9a 64-bit (release 17-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       86(25)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         327
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.1479
_refine_ls_restrained_S_all      1.216
_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)+(0.1426P)²+26.0047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3612
_refine_ls_wR_factor_ref         0.3655
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C6 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
3. Rigid body (RIGU) restrains
 N4, N3, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) C7(0.25) H7A(0.25) H7B(0.25)
5.a Riding coordinates:
 C7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
;
_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
Fe1 Fe 0.375000 0.375000 0.375000 0.007(3) Uani 1 24 d S T P . .
Fe2 Fe 0.500000 0.500000 0.500000 0.013(2) Uani 1 12 d S T P . .
N4 N 0.4179(4) 0.5377(5) 0.4179(4) 0.019(3) Uani 1 2 d S T P A .
N3 N 0.375000 0.4963(6) 0.375000 0.017(3) Uani 1 4 d S T P . .
C5 C 0.4025(4) 0.6076(6) 0.4025(4) 0.024(3) Uani 1 2 d S T P . .
C6 C 0.422(2) 0.6825(6) 0.4254(18) 0.032(4) Uani 0.5 1 d . U P A -1
H6A H 0.398222 0.695262 0.472003 0.038 Uiso 0.5 1 calc R U P A -1
H6B H 0.474779 0.688539 0.430074 0.038 Uiso 0.5 1 calc R U P A -1
C7 C 0.393(3) 0.7263(11) 0.366(3) 0.028(6) Uani 0.25 1 d . U P A -1
H7A H 0.372024 0.770836 0.387433 0.033 Uiso 0.25 1 d R U P A -1
H7B H 0.430024 0.739806 0.329424 0.033 Uiso 0.25 1 d 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
Fe1 N3 2.191(14) 82_545 ?
Fe1 N3 2.191(14) 54_455 ?
Fe1 N3 2.191(14) 5 ?
Fe1 N3 2.191(14) . ?
Fe1 N3 2.191(14) 26_554 ?
Fe1 N3 2.191(14) 9 ?
Fe2 N4 2.205(12) 105_666 ?
Fe2 N4 2.205(12) . ?
Fe2 N4 2.205(12) 5 ?
Fe2 N4 2.205(12) 9 ?
Fe2 N4 2.205(12) 97_666 ?
Fe2 N4 2.205(12) 101_666 ?
N4 N3 1.327(12) . ?
N4 C5 1.322(14) . ?
C5 C5 1.41(2) 75_545 ?
C5 C6 1.456(16) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.43(5) . ?
C7 H7A 0.9697 . ?
C7 H7B 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
N3 Fe1 N3 90.000(1) 82_545 . ?
N3 Fe1 N3 90.0 26_554 54_455 ?
N3 Fe1 N3 90.0 26_554 9 ?
N3 Fe1 N3 90.000(2) 82_545 26_554 ?
N3 Fe1 N3 180.0 82_545 9 ?
N3 Fe1 N3 180.0 . 26_554 ?
N3 Fe1 N3 90.0 . 54_455 ?
N3 Fe1 N3 90.000(1) 82_545 5 ?
N3 Fe1 N3 180.0 5 54_455 ?
N3 Fe1 N3 90.0 . 5 ?
N3 Fe1 N3 90.000(2) . 9 ?
N3 Fe1 N3 90.000(1) 26_554 5 ?
N3 Fe1 N3 90.000(2) 5 9 ?
N3 Fe1 N3 90.000(1) 82_545 54_455 ?
N3 Fe1 N3 90.0 54_455 9 ?
N4 Fe2 N4 180.0(2) 105_666 9 ?
N4 Fe2 N4 180.0(2) 5 101_666 ?
N4 Fe2 N4 87.9(3) 5 . ?
N4 Fe2 N4 87.9(3) 105_666 97_666 ?
N4 Fe2 N4 87.9(3) 9 . ?
N4 Fe2 N4 92.1(3) 9 97_666 ?
N4 Fe2 N4 92.1(3) 9 101_666 ?
N4 Fe2 N4 92.1(3) 105_666 5 ?
N4 Fe2 N4 92.1(3) 105_666 . ?
N4 Fe2 N4 87.9(3) 9 5 ?
N4 Fe2 N4 180.0 97_666 . ?
N4 Fe2 N4 92.1(3) 97_666 5 ?
N4 Fe2 N4 92.1(3) 101_666 . ?
N4 Fe2 N4 87.9(3) 105_666 101_666 ?
N4 Fe2 N4 87.9(3) 97_666 101_666 ?
N3 N4 Fe2 127.7(7) . . ?
C5 N4 Fe2 125.3(7) . . ?
C5 N4 N3 107.0(9) . . ?
N4 N3 Fe1 124.3(6) 75_545 . ?
N4 N3 Fe1 124.3(6) . . ?
N4 N3 N4 111.4(11) 75_545 . ?
N4 C5 C5 107.3(6) . 75_545 ?
N4 C5 C6 141.1(11) . . ?
C5 C5 C6 111.6(7) 75_545 . ?
C5 C6 H6A 111.3 . . ?
C5 C6 H6B 111.3 . . ?
H6A C6 H6B 109.2 . . ?
C7 C6 C5 102.4(17) . . ?
C7 C6 H6A 111.3 . . ?
C7 C6 H6B 111.3 . . ?
C6 C7 H7A 107.1 . . ?
C6 C7 H7B 113.2 . . ?
H7A C7 H7B 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
Fe2 N4 N3 Fe1 0.000(2) . . . . ?
Fe2 N4 N3 N4 180.000(1) . . . 75_545 ?
Fe2 N4 C5 C5 180.000(2) . . . 75_545 ?
Fe2 N4 C5 C6 -3(3) . . . . ?
N4 C5 C6 C7 165.6(13) . . . . ?
N3 N4 C5 C5 0.000(2) . . . 75_545 ?
N3 N4 C5 C6 177(3) . . . . ?
C5 N4 N3 Fe1 180.000(2) . . . . ?
C5 N4 N3 N4 0.000(3) . . . 75_545 ?
C5 C5 C6 C7 -18(3) 75_545 . . . ?

_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 7.263
_oxdiff_exptl_absorpt_empirical_full_min 0.470
####################################################################### 
# 
# 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_C-233
_database_code_depnum_ccdc_archive 'CCDC 2311809'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT211_C-233               
;
PROBLEM: ADP of Atom C7        is N.P.D. or (nearly) 2D .     Please Check
RESPONSE: The disorder model of carbon atoms is hard to model due to dynamic scatter intensities
;
_vrf_RINTA01_C-233               
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT020_C-233               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.207 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure. 
;
_vrf_PLAT084_C-233               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components
;
_vrf_PLAT213_C-233               
;
PROBLEM: Atom N3              has ADP max/min Ratio .....        5.0 prolat
RESPONSE: The disorder model of carbon atoms is hard to model due to dynamic scatter intensities
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(1,4,5,6-tetrahydrocyclopenta[d][1,2,3]triazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H36 Fe3 N18'
_chemical_formula_sum            'C30 H36 Fe3 N18'
_chemical_formula_weight         816.28
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      233(1)
_chemical_oxdiff_formula         'C8 H5 N5 Fe2 '
_chemical_oxdiff_usercomment     233,15K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   18.08(16)
_cell_length_b                   18.08(16)
_cell_length_c                   18.08(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5907(158)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1286
_cell_measurement_temperature    233(1)
_cell_measurement_theta_max      0.8760
_cell_measurement_theta_min      0.0700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.9a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1244
_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  0.2070
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6134
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.896
_diffrn_reflns_theta_min         0.069
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  50.00   0.25    0.25    --    0.00   0.00   0.00  400
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0006240000
_diffrn_orient_matrix_UB_12      -0.0009266500
_diffrn_orient_matrix_UB_13      0.0008165500
_diffrn_orient_matrix_UB_21      0.0009633500
_diffrn_orient_matrix_UB_22      0.0009436000
_diffrn_orient_matrix_UB_23      0.0003332500
_diffrn_orient_matrix_UB_31      -0.0007786500
_diffrn_orient_matrix_UB_32      0.0004188001
_diffrn_orient_matrix_UB_33      0.0010720501
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                306
_reflns_number_total             327
_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 1.171.44.9a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.44.9a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.44.9a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       54(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.352
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         327
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.1434
_refine_ls_restrained_S_all      1.264
_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)+(0.1399P)²+24.3691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3535
_refine_ls_wR_factor_ref         0.3568
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
N4 \\sim N3 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.009 and sigma
for terminal atoms of 0.009 within 2A
3. Rigid body (RIGU) restrains
 N4, N3, C5, C6, C7
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Others
 Fixed Sof: C5(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.25) H7A(0.25) H7B(0.25)
5.a Riding coordinates:
 C7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
;
_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
Fe1 Fe 0.375000 0.375000 0.375000 0.004(3) Uani 1 24 d S T P . .
Fe2 Fe 0.500000 0.500000 0.500000 0.013(2) Uani 1 12 d S T P . .
N4 N 0.4180(4) 0.5376(5) 0.4180(4) 0.014(2) Uani 1 2 d S TU P . .
N3 N 0.375000 0.4954(6) 0.375000 0.012(3) Uani 1 4 d S TU P A .
C5 C 0.3976(17) 0.6072(6) 0.4066(17) 0.013(4) Uani 0.5 1 d . U P A -1
C6 C 0.4152(11) 0.6815(6) 0.4304(10) 0.014(4) Uani 0.5 1 d . U P A -1
H6A H 0.467738 0.686973 0.439801 0.017 Uiso 0.5 1 calc R U P A -1
H6B H 0.387921 0.694753 0.474663 0.017 Uiso 0.5 1 calc R U P A -1
C7 C 0.392(2) 0.7273(10) 0.366(2) 0.012(5) Uani 0.25 1 d . U P A -1
H7A H 0.376892 0.770958 0.393467 0.015 Uiso 0.25 1 d R U P A -1
H7B H 0.434892 0.739928 0.335457 0.015 Uiso 0.25 1 d 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
Fe1 N3 2.18(2) 82_545 ?
Fe1 N3 2.18(2) 54_455 ?
Fe1 N3 2.18(2) 5 ?
Fe1 N3 2.18(2) . ?
Fe1 N3 2.18(2) 26_554 ?
Fe1 N3 2.18(2) 9 ?
Fe2 N4 2.20(2) . ?
Fe2 N4 2.20(2) 9 ?
Fe2 N4 2.20(2) 101_666 ?
Fe2 N4 2.20(2) 105_666 ?
Fe2 N4 2.20(2) 97_666 ?
Fe2 N4 2.20(2) 5 ?
N4 N3 1.339(16) . ?
N4 C5 1.328(18) . ?
C5 C6 1.45(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.49(4) . ?
C7 H7A 0.9695 . ?
C7 H7B 0.9858 . ?

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
N3 Fe1 N3 90.000(1) 82_545 . ?
N3 Fe1 N3 90.0 26_554 54_455 ?
N3 Fe1 N3 90.0 26_554 9 ?
N3 Fe1 N3 90.000(2) 82_545 26_554 ?
N3 Fe1 N3 180.0 82_545 9 ?
N3 Fe1 N3 180.0 . 26_554 ?
N3 Fe1 N3 90.0 . 54_455 ?
N3 Fe1 N3 90.000(1) 82_545 5 ?
N3 Fe1 N3 180.0 5 54_455 ?
N3 Fe1 N3 90.0 . 5 ?
N3 Fe1 N3 90.0 . 9 ?
N3 Fe1 N3 90.000(1) 26_554 5 ?
N3 Fe1 N3 90.000(2) 5 9 ?
N3 Fe1 N3 90.000(1) 82_545 54_455 ?
N3 Fe1 N3 90.0 54_455 9 ?
N4 Fe2 N4 92.1(3) . 105_666 ?
N4 Fe2 N4 180.0(2) 5 101_666 ?
N4 Fe2 N4 87.9(3) 5 9 ?
N4 Fe2 N4 180.0(2) . 97_666 ?
N4 Fe2 N4 180.0(2) 105_666 9 ?
N4 Fe2 N4 87.9(3) 105_666 97_666 ?
N4 Fe2 N4 87.9(3) 97_666 101_666 ?
N4 Fe2 N4 87.9(3) . 5 ?
N4 Fe2 N4 87.9(3) . 9 ?
N4 Fe2 N4 92.1(3) 105_666 5 ?
N4 Fe2 N4 92.1(3) 97_666 9 ?
N4 Fe2 N4 92.1(3) 97_666 5 ?
N4 Fe2 N4 92.1(3) 101_666 9 ?
N4 Fe2 N4 92.1(3) . 101_666 ?
N4 Fe2 N4 87.9(3) 105_666 101_666 ?
N3 N4 Fe2 127.3(7) . . ?
C5 N4 Fe2 125.8(7) . . ?
C5 N4 N3 106.7(9) . . ?
N4 N3 Fe1 124.7(6) . . ?
N4 N3 Fe1 124.7(6) 75_545 . ?
N4 N3 N4 110.5(11) 75_545 . ?
N4 C5 C6 140.6(11) . . ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C5 C6 C7 102.7(16) . . ?
H6A C6 H6B 109.1 . . ?
C7 C6 H6A 111.2 . . ?
C7 C6 H6B 111.2 . . ?
C6 C7 H7A 97.5 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.4 . . ?

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
Fe2 N4 N3 Fe1 0.000(2) . . . . ?
Fe2 N4 N3 N4 180.000(1) . . . 75_545 ?
Fe2 N4 C5 C6 5(6) . . . . ?
N4 C5 C6 C7 154(5) . . . . ?
N3 N4 C5 C6 180(4) . . . . ?
C5 N4 N3 Fe1 -174.8(19) . . . . ?
C5 N4 N3 N4 5.2(19) . . . 75_545 ?

_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.907
####################################################################### 
# 
# 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_C-373
_database_code_depnum_ccdc_archive 'CCDC 2311811'
loop_
_audit_author_name
_audit_author_address
'Jakub Wojciechowski'
;Rigaku Europe SE
Germany
;
_audit_update_record             
;
2023-12-03 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_C-373               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT020_C-373               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.473 Report
RESPONSE: The high Rint is the result of the presence of dynamic scatter intensities and high symmetry of crystal structure
;
_vrf_PLAT084_C-373               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: The high R1 and wR2 values are common for refinement using a model based on kinematic approximation on observed intensities with dynamic scatter components. 
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
catena-[hexakis(1,4,5,6-tetrahydrocyclopenta[d][1,2,3]triazolate)-tri-iron)]
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H36 Fe3 N18'
_chemical_formula_sum            'C30 H36 Fe3 N18'
_chemical_formula_weight         816.28
_chemical_melting_point          ?
_exptl_crystal_description       'nano grain'
_exptl_crystal_colour            ?
_diffrn_ambient_temperature      373(1)
_chemical_oxdiff_formula         'C8 H5 N5 Fe2 '
_chemical_oxdiff_usercomment     373.2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+1/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'z, x, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z, x'
'-y+1/4, z+1/2, -x+3/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+1/4, x+1/2'
'y+3/4, x+1/4, -z+1/2'
'-y, -x, -z'
'y+1/4, -x+1/2, z+3/4'
'-y+1/2, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+1/4'
'-x, -z, -y'
'x+1/4, -z+1/2, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'z+1/4, -y+1/2, x+3/4'
'-z+1/2, y+3/4, x+1/4'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+1/4, y+1, -z+5/4'
'x+1/2, -y+5/4, -z+3/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+5/4, -y+3/4'
'-z+3/4, -x+3/4, y+1'
'-z+1/4, x+1, -y+5/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1, -x+5/4'
'y+1/2, -z+5/4, -x+3/4'
'-y+3/4, -z+3/4, x+1'
'y+3/4, x+3/4, -z+1'
'-y, -x+1/2, -z+1/2'
'y+1/4, -x+1, z+5/4'
'-y+1/2, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1'
'-x+1/2, z+5/4, y+3/4'
'-x, -z+1/2, -y+1/2'
'x+1/4, -z+1, y+5/4'
'z+3/4, y+3/4, -x+1'
'z+1/4, -y+1, x+5/4'
'-z+1/2, y+5/4, x+3/4'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+5/4, -y+1/4, z+1'
'-x+3/4, y+1/2, -z+5/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1, -x+3/4, -y+3/4'
'-z+5/4, -x+1/4, y+1'
'-z+3/4, x+1/2, -y+5/4'
'y+1/2, z, x+1/2'
'-y+3/4, z+1/2, -x+5/4'
'y+1, -z+3/4, -x+3/4'
'-y+5/4, -z+1/4, x+1'
'y+5/4, x+1/4, -z+1'
'-y+1/2, -x, -z+1/2'
'y+3/4, -x+1/2, z+5/4'
'-y+1, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1'
'-x+1, z+3/4, y+3/4'
'-x+1/2, -z, -y+1/2'
'x+3/4, -z+1/2, y+5/4'
'z+5/4, y+1/4, -x+1'
'z+3/4, -y+1/2, x+5/4'
'-z+1, y+3/4, x+3/4'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+5/4, -y+3/4, z+1/2'
'-x+3/4, y+1, -z+3/4'
'x+1, -y+5/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1, -x+5/4, -y+1/4'
'-z+5/4, -x+3/4, y+1/2'
'-z+3/4, x+1, -y+3/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1, -x+3/4'
'y+1, -z+5/4, -x+1/4'
'-y+5/4, -z+3/4, x+1/2'
'y+5/4, x+3/4, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y+3/4, -x+1, z+3/4'
'-y+1, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+1/2'
'-x+1, z+5/4, y+1/4'
'-x+1/2, -z+1/2, -y'
'x+3/4, -z+1, y+3/4'
'z+5/4, y+3/4, -x+1/2'
'z+3/4, -y+1, x+3/4'
'-z+1, y+5/4, x+1/4'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x-3/4, y-1/4, -z-1/2'
'x-1/4, -y-1/2, z-3/4'
'-x-1/2, y-3/4, z-1/4'
'-z, -x, -y'
'-z-1/2, x-3/4, y-1/4'
'z-3/4, x-1/4, -y-1/2'
'z-1/4, -x-1/2, y-3/4'
'-y, -z, -x'
'y-1/4, -z-1/2, x-3/4'
'-y-1/2, z-3/4, x-1/4'
'y-3/4, z-1/4, -x-1/2'
'-y-3/4, -x-1/4, z-1/2'
'y, x, z'
'-y-1/4, x-1/2, -z-3/4'
'y-1/2, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/2'
'x-1/2, -z-3/4, -y-1/4'
'x, z, y'
'-x-1/4, z-1/2, -y-3/4'
'-z-3/4, -y-1/4, x-1/2'
'-z-1/4, y-1/2, -x-3/4'
'z-1/2, -y-3/4, -x-1/4'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x-3/4, y+1/4, -z'
'x-1/4, -y, z-1/4'
'-x-1/2, y-1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x-1/4, y+1/4'
'z-3/4, x+1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z, x-1/4'
'-y-1/2, z-1/4, x+1/4'
'y-3/4, z+1/4, -x'
'-y-3/4, -x+1/4, z'
'y, x+1/2, z+1/2'
'-y-1/4, x, -z-1/4'
'y-1/2, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y'
'x-1/2, -z-1/4, -y+1/4'
'x, z+1/2, y+1/2'
'-x-1/4, z, -y-1/4'
'-z-3/4, -y+1/4, x'
'-z-1/4, y, -x-1/4'
'z-1/2, -y-1/4, -x+1/4'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-1/4, -z'
'x+1/4, -y-1/2, z-1/4'
'-x, y-3/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-3/4, y+1/4'
'z-1/4, x-1/4, -y'
'z+1/4, -x-1/2, y-1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z-1/2, x-1/4'
'-y, z-3/4, x+1/4'
'y-1/4, z-1/4, -x'
'-y-1/4, -x-1/4, z'
'y+1/2, x, z+1/2'
'-y+1/4, x-1/2, -z-1/4'
'y, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y'
'x, -z-3/4, -y+1/4'
'x+1/2, z, y+1/2'
'-x+1/4, z-1/2, -y-1/4'
'-z-1/4, -y-1/4, x'
'-z+1/4, y-1/2, -x-1/4'
'z, -y-3/4, -x+1/4'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x-1/4, y+1/4, -z-1/2'
'x+1/4, -y, z-3/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x+1/4, -y-1/2'
'z+1/4, -x, y-3/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z, x-3/4'
'-y, z-1/4, x-1/4'
'y-1/4, z+1/4, -x-1/2'
'-y-1/4, -x+1/4, z-1/2'
'y+1/2, x+1/2, z'
'-y+1/4, x, -z-3/4'
'y, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y-1/2'
'x, -z-1/4, -y-1/4'
'x+1/2, z+1/2, y'
'-x+1/4, z, -y-3/4'
'-z-1/4, -y+1/4, x-1/2'
'-z+1/4, y, -x-3/4'
'z, -y-1/4, -x-1/4'
'z+1/2, y+1/2, x'

_cell_length_a                   18.10(10)
_cell_length_b                   18.10(10)
_cell_length_c                   18.10(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5932(99)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    791
_cell_measurement_temperature    377(1)
_cell_measurement_theta_max      0.8900
_cell_measurement_theta_min      0.0680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1244
_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  0.4731
_diffrn_reflns_av_unetI/netI     0.1909
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4241
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.899
_diffrn_reflns_theta_min         0.069
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  26.00   0.25    0.25    --    0.00   0.00   0.00  320
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0009350000
_diffrn_orient_matrix_UB_12      -0.0006053000
_diffrn_orient_matrix_UB_13      -0.0008248000
_diffrn_orient_matrix_UB_21      -0.0009260000
_diffrn_orient_matrix_UB_22      -0.0009711000
_diffrn_orient_matrix_UB_23      -0.0003446000
_diffrn_orient_matrix_UB_31      -0.0004271000
_diffrn_orient_matrix_UB_32      0.0007836000
_diffrn_orient_matrix_UB_33      -0.0010636000
_diffrn_oxdiff_ac6_digest_hkl_ed 
;
1117b53d759539ca21422ded22bb8d1c520fcc
;
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'LaB6 electron gun'
_diffrn_source_type              JEM-2300ED
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                250
_reflns_number_total             328
_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 1.171.43.86a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.9a 64-bit (release 17-08-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.86a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       72(26)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         328
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1734
_refine_ls_R_factor_gt           0.1434
_refine_ls_restrained_S_all      1.194
_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)+(0.1515P)²+6.7345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3380
_refine_ls_wR_factor_ref         0.3659
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C6 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
3. Rigid body (RIGU) restrains
 N4, N3, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C6(0.5) H6B(0.5) H6A(0.5) C7(0.25) H7B(0.25) H7A(0.25)
5.a Riding coordinates:
 C7(H7B,H7A)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6B,H6A)
;
_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
Fe1 Fe 0.375000 0.375000 0.375000 0.013(2) Uani 1 24 d S T P . .
Fe2 Fe 0.500000 0.500000 0.500000 0.020(2) Uani 1 12 d S T P . .
N3 N 0.4959(6) 0.375000 0.375000 0.023(3) Uani 1 4 d S T P . .
N4 N 0.5377(4) 0.4178(3) 0.4178(3) 0.026(3) Uani 1 2 d S T P A .
C5 C 0.6072(5) 0.4013(4) 0.4013(4) 0.032(3) Uani 1 2 d S T P . .
C6 C 0.6809(6) 0.4144(10) 0.4318(10) 0.026(5) Uani 0.5 1 d . U P A -1
H6B H 0.690837 0.383253 0.474290 0.031 Uiso 0.5 1 calc R U P A -1
H6A H 0.688285 0.465792 0.445040 0.031 Uiso 0.5 1 calc R U P A -1
C7 C 0.7255(9) 0.393(2) 0.367(2) 0.025(6) Uani 0.25 1 d . U P A -1
H7B H 0.737740 0.430196 0.330626 0.030 Uiso 0.25 1 d R U P A -1
H7A H 0.770550 0.372826 0.387966 0.030 Uiso 0.25 1 d 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
Fe1 N3 2.188(16) 82_545 ?
Fe1 N3 2.188(16) 54_455 ?
Fe1 N3 2.188(16) 5 ?
Fe1 N3 2.188(16) 9 ?
Fe1 N3 2.188(16) 26_554 ?
Fe1 N3 2.188(16) . ?
Fe2 N4 2.212(15) 105_666 ?
Fe2 N4 2.213(15) . ?
Fe2 N4 2.212(15) 5 ?
Fe2 N4 2.212(15) 9 ?
Fe2 N4 2.212(15) 97_666 ?
Fe2 N4 2.212(15) 101_666 ?
N3 N4 1.332(13) 52_455 ?
N3 N4 1.332(13) . ?
N4 C5 1.328(13) . ?
C5 C5 1.35(2) 52_455 ?
C5 C6 1.463(16) . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 C7 1.48(5) . ?
C7 H7B 0.9699 . ?
C7 H7A 0.9697 . ?

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
N3 Fe1 N3 180.0 82_545 9 ?
N3 Fe1 N3 90.000(1) 26_554 54_455 ?
N3 Fe1 N3 180.0 26_554 . ?
N3 Fe1 N3 90.000(1) 82_545 26_554 ?
N3 Fe1 N3 90.0 82_545 . ?
N3 Fe1 N3 90.0 9 26_554 ?
N3 Fe1 N3 90.0 9 54_455 ?
N3 Fe1 N3 90.0 82_545 5 ?
N3 Fe1 N3 180.0 5 54_455 ?
N3 Fe1 N3 90.000(1) 9 5 ?
N3 Fe1 N3 90.000(1) 9 . ?
N3 Fe1 N3 90.000(1) 26_554 5 ?
N3 Fe1 N3 90.000(2) 5 . ?
N3 Fe1 N3 90.000(1) 82_545 54_455 ?
N3 Fe1 N3 90.0 54_455 . ?
N4 Fe2 N4 180.0 105_666 9 ?
N4 Fe2 N4 180.0 5 101_666 ?
N4 Fe2 N4 87.9(3) 5 . ?
N4 Fe2 N4 87.9(3) 105_666 97_666 ?
N4 Fe2 N4 87.9(3) 9 . ?
N4 Fe2 N4 92.1(3) 9 97_666 ?
N4 Fe2 N4 92.1(3) 9 101_666 ?
N4 Fe2 N4 92.1(3) 105_666 5 ?
N4 Fe2 N4 92.1(3) 105_666 . ?
N4 Fe2 N4 87.9(3) 9 5 ?
N4 Fe2 N4 180.0 97_666 . ?
N4 Fe2 N4 92.1(3) 97_666 5 ?
N4 Fe2 N4 92.1(3) 101_666 . ?
N4 Fe2 N4 87.9(3) 105_666 101_666 ?
N4 Fe2 N4 87.9(3) 97_666 101_666 ?
N4 N3 Fe1 124.7(5) 52_455 . ?
N4 N3 Fe1 124.7(5) . . ?
N4 N3 N4 110.6(10) 52_455 . ?
N3 N4 Fe2 127.3(6) . . ?
C5 N4 Fe2 126.5(7) . . ?
C5 N4 N3 106.1(8) . . ?
N4 C5 C5 108.6(6) . 52_455 ?
N4 C5 C6 137.9(10) . . ?
C5 C5 C6 112.4(7) 52_455 . ?
C5 C6 H6B 112.0 . . ?
C5 C6 H6A 112.0 . . ?
C5 C6 C7 98.9(15) . . ?
H6B C6 H6A 109.7 . . ?
C7 C6 H6B 112.0 . . ?
C7 C6 H6A 112.0 . . ?
C6 C7 H7B 118.6 . . ?
C6 C7 H7A 104.3 . . ?
H7B C7 H7A 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
Fe1 N3 N4 Fe2 0.000(1) . . . . ?
Fe1 N3 N4 C5 180.000(1) . . . . ?
Fe2 N4 C5 C5 180.000(1) . . . 52_455 ?
Fe2 N4 C5 C6 13.2(13) . . . . ?
N3 N4 C5 C5 0.000(1) . . . 52_455 ?
N3 N4 C5 C6 -166.8(13) . . . . ?
N4 N3 N4 Fe2 180.000(0) 52_455 . . . ?
N4 N3 N4 C5 0.000(1) 52_455 . . . ?
N4 C5 C6 C7 -165.8(11) . . . . ?
C5 C5 C6 C7 27.7(18) 52_455 . . . ?

_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 5.629
_oxdiff_exptl_absorpt_empirical_full_min 0.316
