# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_4_2_rb20_145_1c_250K
_database_code_depnum_ccdc_archive 'CCDC 2259418'
loop_
_audit_author_name
_audit_author_address
'Joachim Kusz'
;University of Silesia
Poland
;
_audit_update_record             
;
2023-04-27 deposited with the CCDC.	2026-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C22 H24 Fe N16, 2(B F4), 0.95(C H4 O)
;
_chemical_formula_sum            'C22.95 H27.80 B2 F8 Fe N16 O0.95'
_chemical_formula_weight         772.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.7542(7)
_cell_length_b                   12.9367(6)
_cell_length_c                   15.6423(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.243(5)
_cell_angle_gamma                90
_cell_volume                     3137.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(1)
_cell_measurement_reflns_used    5249
_cell_measurement_theta_min      3.4010
_cell_measurement_theta_max      25.6000

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_F_000             1572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.579
_shelx_estimated_absorpt_T_min   0.908
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            26053
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.149
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3210
_reflns_number_gt                2408
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0957P)²+8.0813P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3210
_refine_ls_number_parameters     238
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1936
_refine_ls_wR_factor_gt          0.1690
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.250000 0.250000 0.000000 0.0332(3) Uani 1 2 d S . P . .
N1 N 0.17978(18) 0.1638(2) -0.1122(2) 0.0365(7) Uani 1 1 d . . . . .
C2 C 0.1905(2) 0.0609(3) -0.1063(3) 0.0391(8) Uani 1 1 d . . . . .
C3 C 0.1650(3) -0.0035(3) -0.1752(3) 0.0550(11) Uani 1 1 d . . . . .
H3 H 0.175837 -0.074832 -0.169825 0.066 Uiso 1 1 calc R U . . .
C4 C 0.1235(3) 0.0368(4) -0.2519(3) 0.0582(11) Uani 1 1 d . . . . .
H4 H 0.104611 -0.006180 -0.299922 0.070 Uiso 1 1 calc R U . . .
C5 C 0.1100(3) 0.1413(3) -0.2574(3) 0.0519(10) Uani 1 1 d . . . . .
H5 H 0.080880 0.170923 -0.309210 0.062 Uiso 1 1 calc R U . . .
C6 C 0.1392(2) 0.2018(3) -0.1872(3) 0.0436(9) Uani 1 1 d . . . . .
H6 H 0.130234 0.273586 -0.192034 0.052 Uiso 1 1 calc R U . . .
N11 N 0.27379(18) -0.0654(2) 0.0870(2) 0.0393(7) Uani 1 1 d . . . . .
N12 N 0.2326(2) -0.0712(3) 0.0036(2) 0.0440(8) Uani 1 1 d . . . . .
C13 C 0.2310(2) 0.0244(3) -0.0210(3) 0.0365(8) Uani 1 1 d . . . . .
N14 N 0.26835(19) 0.0912(2) 0.0406(2) 0.0368(7) Uani 1 1 d . . . . .
C15 C 0.2947(2) 0.0316(3) 0.1074(3) 0.0403(8) Uani 1 1 d . . . . .
H15 H 0.324040 0.054217 0.161810 0.048 Uiso 1 1 calc R U . . .
C16 C 0.2966(2) -0.1585(3) 0.1380(3) 0.0457(10) Uani 1 1 d . . . . .
H16A H 0.247497 -0.206153 0.129708 0.055 Uiso 1 1 calc R U . . .
H16B H 0.310508 -0.140610 0.199775 0.055 Uiso 1 1 calc R U . . .
C17 C 0.3738(3) -0.2108(3) 0.1105(3) 0.0533(11) Uani 1 1 d . . . . .
H17A H 0.387714 -0.274243 0.144319 0.064 Uiso 1 1 calc R U . . .
H17B H 0.359384 -0.229924 0.048961 0.064 Uiso 1 1 calc R U . . .
C18 C 0.4497(2) -0.1414(3) 0.1240(3) 0.0463(9) Uani 1 1 d . . . . .
H18B H 0.438483 -0.082217 0.084438 0.056 Uiso 1 1 calc R U . . .
H18A H 0.459469 -0.114994 0.183654 0.056 Uiso 1 1 calc R U . . .
N21 N 0.5267(2) -0.1955(3) 0.1084(2) 0.0447(8) Uani 1 1 d . . . . .
N22 N 0.5687(3) -0.2605(3) 0.1666(3) 0.0691(13) Uani 1 1 d . . . . .
N23 N 0.6348(2) -0.2904(4) 0.1375(3) 0.0654(12) Uani 1 1 d . . . . .
N24 N 0.6379(2) -0.2444(2) 0.0616(2) 0.0372(7) Uani 1 1 d . . . . .
C25 C 0.5689(2) -0.1873(3) 0.0444(2) 0.0379(8) Uani 1 1 d . . . . .
H25 H 0.552434 -0.146911 -0.005824 0.046 Uiso 1 1 calc R U . . .
B1 B 0.4089(4) -0.0782(4) -0.1411(4) 0.0575(13) Uani 1 1 d . . . . .
F1 F 0.4874(2) -0.1187(3) -0.1450(2) 0.0962(12) Uani 1 1 d . . . . .
F2 F 0.4101(2) -0.0351(2) -0.06251(18) 0.0731(8) Uani 1 1 d . . . . .
F3 F 0.3457(3) -0.1480(3) -0.1593(3) 0.1212(16) Uani 1 1 d . . . . .
F4 F 0.3922(2) -0.0002(3) -0.2027(2) 0.0977(11) Uani 1 1 d . . . . .
O98 O 0.002(2) 0.0128(17) 0.009(3) 0.188(8) Uiso 0.475(10) 1 d D . P A -1
H98 H 0.016803 0.052542 0.050887 0.282 Uiso 0.475(10) 1 d DR U P A -1
C99 C 0.0350(10) -0.0902(13) 0.0191(14) 0.135(8) Uani 0.475(10) 1 d D . P A -1
H99A H 0.044708 -0.115565 -0.036744 0.202 Uiso 0.475(10) 1 calc R U P A -1
H99B H -0.006162 -0.134648 0.040536 0.202 Uiso 0.475(10) 1 calc R U P A -1
H99C H 0.089020 -0.090230 0.059999 0.202 Uiso 0.475(10) 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 N14 2.154(3) . ?
Fe1 N14 2.154(3) 7 ?
Fe1 N24 2.158(3) 5_655 ?
Fe1 N24 2.158(3) 3_455 ?
Fe1 N1 2.204(3) 7 ?
Fe1 N1 2.204(3) . ?
N1 C6 1.327(5) . ?
N1 C2 1.342(5) . ?
C2 C3 1.365(6) . ?
C2 C13 1.452(5) . ?
C3 C4 1.363(6) . ?
C3 H3 0.9400 . ?
C4 C5 1.368(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.360(6) . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
N11 C15 1.322(5) . ?
N11 N12 1.351(5) . ?
N11 C16 1.454(5) . ?
N12 C13 1.293(5) . ?
C13 N14 1.349(5) . ?
N14 C15 1.306(5) . ?
C15 H15 0.9400 . ?
C16 C17 1.519(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.481(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N21 1.458(5) . ?
C18 H18B 0.9800 . ?
C18 H18A 0.9800 . ?
N21 C25 1.302(5) . ?
N21 N22 1.327(5) . ?
N22 N23 1.268(5) . ?
N23 N24 1.336(5) . ?
N24 C25 1.302(4) . ?
C25 H25 0.9400 . ?
B1 F3 1.336(6) . ?
B1 F2 1.347(6) . ?
B1 F1 1.354(6) . ?
B1 F4 1.388(7) . ?
O98 C99 1.430(2) . ?
O98 H98 0.8300 . ?
C99 H99A 0.9700 . ?
C99 H99B 0.9700 . ?
C99 H99C 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
N14 Fe1 N14 180.0 . 7 ?
N14 Fe1 N24 91.26(11) . 5_655 ?
N14 Fe1 N24 88.74(11) 7 5_655 ?
N14 Fe1 N24 88.74(11) . 3_455 ?
N14 Fe1 N24 91.26(11) 7 3_455 ?
N24 Fe1 N24 180.0(2) 5_655 3_455 ?
N14 Fe1 N1 103.07(11) . 7 ?
N14 Fe1 N1 76.93(11) 7 7 ?
N24 Fe1 N1 92.18(11) 5_655 7 ?
N24 Fe1 N1 87.82(11) 3_455 7 ?
N14 Fe1 N1 76.94(11) . . ?
N14 Fe1 N1 103.06(11) 7 . ?
N24 Fe1 N1 87.83(11) 5_655 . ?
N24 Fe1 N1 92.17(11) 3_455 . ?
N1 Fe1 N1 180.0 7 . ?
C6 N1 C2 117.6(3) . . ?
C6 N1 Fe1 127.6(3) . . ?
C2 N1 Fe1 114.1(2) . . ?
N1 C2 C3 122.4(4) . . ?
N1 C2 C13 114.5(3) . . ?
C3 C2 C13 123.1(4) . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 118.5(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
N1 C6 C5 122.7(4) . . ?
N1 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C15 N11 N12 110.0(3) . . ?
C15 N11 C16 128.8(3) . . ?
N12 N11 C16 120.9(3) . . ?
C13 N12 N11 102.5(3) . . ?
N12 C13 N14 114.6(3) . . ?
N12 C13 C2 124.6(4) . . ?
N14 C13 C2 120.8(3) . . ?
C15 N14 C13 103.2(3) . . ?
C15 N14 Fe1 143.7(3) . . ?
C13 N14 Fe1 112.5(2) . . ?
N14 C15 N11 109.7(4) . . ?
N14 C15 H15 125.2 . . ?
N11 C15 H15 125.2 . . ?
N11 C16 C17 110.2(3) . . ?
N11 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
N11 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C18 C17 C16 110.9(3) . . ?
C18 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
N21 C18 C17 111.1(3) . . ?
N21 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
N21 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
H18B C18 H18A 108.0 . . ?
C25 N21 N22 108.6(3) . . ?
C25 N21 C18 130.0(3) . . ?
N22 N21 C18 121.2(3) . . ?
N23 N22 N21 106.7(3) . . ?
N22 N23 N24 110.2(3) . . ?
C25 N24 N23 106.0(3) . . ?
C25 N24 Fe1 130.2(3) . 3_545 ?
N23 N24 Fe1 123.0(2) . 3_545 ?
N21 C25 N24 108.4(3) . . ?
N21 C25 H25 125.8 . . ?
N24 C25 H25 125.8 . . ?
F3 B1 F2 111.3(5) . . ?
F3 B1 F1 112.4(5) . . ?
F2 B1 F1 109.7(5) . . ?
F3 B1 F4 107.5(5) . . ?
F2 B1 F4 107.6(4) . . ?
F1 B1 F4 108.2(4) . . ?
C99 O98 H98 116.4 . . ?
O98 C99 H99A 109.5 . . ?
O98 C99 H99B 109.5 . . ?
H99A C99 H99B 109.5 . . ?
O98 C99 H99C 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 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
C6 N1 C2 C3 3.2(5) . . . . ?
Fe1 N1 C2 C3 -168.2(3) . . . . ?
C6 N1 C2 C13 -176.7(3) . . . . ?
Fe1 N1 C2 C13 11.9(4) . . . . ?
N1 C2 C3 C4 -3.1(7) . . . . ?
C13 C2 C3 C4 176.8(4) . . . . ?
C2 C3 C4 C5 0.9(7) . . . . ?
C3 C4 C5 C6 0.9(7) . . . . ?
C2 N1 C6 C5 -1.2(6) . . . . ?
Fe1 N1 C6 C5 168.9(3) . . . . ?
C4 C5 C6 N1 -0.9(7) . . . . ?
C15 N11 N12 C13 -0.3(4) . . . . ?
C16 N11 N12 C13 -174.4(3) . . . . ?
N11 N12 C13 N14 0.1(4) . . . . ?
N11 N12 C13 C2 -177.9(3) . . . . ?
N1 C2 C13 N12 166.2(3) . . . . ?
C3 C2 C13 N12 -13.6(6) . . . . ?
N1 C2 C13 N14 -11.6(5) . . . . ?
C3 C2 C13 N14 168.5(4) . . . . ?
N12 C13 N14 C15 0.1(4) . . . . ?
C2 C13 N14 C15 178.2(3) . . . . ?
N12 C13 N14 Fe1 -173.2(2) . . . . ?
C2 C13 N14 Fe1 4.9(4) . . . . ?
C13 N14 C15 N11 -0.3(4) . . . . ?
Fe1 N14 C15 N11 169.2(3) . . . . ?
N12 N11 C15 N14 0.4(4) . . . . ?
C16 N11 C15 N14 173.9(3) . . . . ?
C15 N11 C16 C17 -97.7(5) . . . . ?
N12 N11 C16 C17 75.3(4) . . . . ?
N11 C16 C17 C18 60.5(5) . . . . ?
C16 C17 C18 N21 172.6(3) . . . . ?
C17 C18 N21 C25 107.9(5) . . . . ?
C17 C18 N21 N22 -76.9(5) . . . . ?
C25 N21 N22 N23 0.0(6) . . . . ?
C18 N21 N22 N23 -176.2(4) . . . . ?
N21 N22 N23 N24 1.2(6) . . . . ?
N22 N23 N24 C25 -1.9(6) . . . . ?
N22 N23 N24 Fe1 168.5(3) . . . 3_545 ?
N22 N21 C25 N24 -1.2(5) . . . . ?
C18 N21 C25 N24 174.6(4) . . . . ?
N23 N24 C25 N21 1.8(5) . . . . ?
Fe1 N24 C25 N21 -167.6(3) 3_545 . . . ?

_refine_diff_density_max         0.896
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.083

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

data_1_1_rb22_v43cd_2a_100K
_database_code_depnum_ccdc_archive 'CCDC 2259411'
loop_
_audit_author_name
_audit_author_address
'Joachim Kusz'
;University of Silesia
Poland
;
_audit_update_record             
;
2023-04-27 deposited with the CCDC.	2026-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 Fe N18, 2(B F4)'
_chemical_formula_sum            'C20 H22 B2 F8 Fe N18'
_chemical_formula_weight         744.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.9524(3)
_cell_length_b                   8.8207(2)
_cell_length_c                   9.9917(3)
_cell_angle_alpha                86.989(2)
_cell_angle_beta                 84.475(3)
_cell_angle_gamma                85.069(3)
_cell_volume                     694.35(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    4210
_cell_measurement_theta_min      3.3490
_cell_measurement_theta_max      36.3660

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.650
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            5862
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.027
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2831
_reflns_number_gt                2617
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0408P)²+0.6654P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2831
_refine_ls_number_parameters     233
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.000000 1.000000 0.01015(11) Uani 1 2 d S . P . .
F3 F 0.17252(16) 0.46775(15) 0.42247(12) 0.0303(3) Uani 1 1 d D . . . .
F4A F 0.20938(18) 0.44566(17) 0.19488(13) 0.0324(3) Uani 0.9523(18) 1 d D . P A
1
F2A F 0.36851(19) 0.29317(16) 0.33015(14) 0.0344(4) Uani 0.9523(18) 1 d D . P A
1
F1A F 0.4112(2) 0.5440(2) 0.30109(17) 0.0502(5) Uani 0.9523(18) 1 d D . P A 1
F1B F 0.4537(10) 0.432(3) 0.3650(17) 0.0502(5) Uani 0.0477(18) 1 d D . P A 2
F4B F 0.284(2) 0.5856(14) 0.2370(14) 0.0324(3) Uani 0.0477(18) 1 d D . P A 2
F2B F 0.272(2) 0.3268(16) 0.2356(15) 0.0344(4) Uani 0.0477(18) 1 d D . P A 2
N1 N 0.34145(19) 0.14126(16) 0.89683(15) 0.0127(3) Uani 1 1 d . . . . .
N22 N 0.73040(19) 0.29712(17) 0.19332(15) 0.0135(3) Uani 1 1 d . . . . .
N14 N 0.64024(19) 0.01973(17) 0.82759(15) 0.0132(3) Uani 1 1 d . . . . .
N24 N 0.60344(19) 0.17390(17) 0.06681(15) 0.0129(3) Uani 1 1 d . . . . .
N13 N 0.8010(2) -0.02038(18) 0.77617(16) 0.0165(3) Uani 1 1 d . . . . .
N23 N 0.6820(2) 0.16141(17) 0.17873(15) 0.0145(3) Uani 1 1 d . . . . .
N11 N 0.6747(2) 0.10868(17) 0.62307(15) 0.0144(3) Uani 1 1 d . . . . .
N21 N 0.6895(2) 0.40005(18) 0.09752(16) 0.0186(3) Uani 1 1 d . . . . .
N12 N 0.8222(2) 0.03250(18) 0.65272(16) 0.0176(3) Uani 1 1 d . . . . .
C15 C 0.5633(2) 0.10002(19) 0.73170(18) 0.0131(4) Uani 1 1 d . . . . .
C2 C 0.3894(2) 0.16338(19) 0.76305(18) 0.0133(4) Uani 1 1 d . . . . .
C6 C 0.1877(2) 0.1997(2) 0.94297(19) 0.0171(4) Uani 1 1 d . . . . .
H6 H 0.153960 0.189126 1.036585 0.021 Uiso 1 1 calc R U . . .
C3 C 0.2833(2) 0.2341(2) 0.67299(19) 0.0153(4) Uani 1 1 d . . . . .
H3 H 0.319419 0.243972 0.579746 0.018 Uiso 1 1 calc R U . . .
C17 C 0.8310(2) 0.2097(2) 0.41594(18) 0.0159(4) Uani 1 1 d . . . . .
H17A H 0.911808 0.233591 0.479802 0.019 Uiso 1 1 calc R U . . .
H17B H 0.873590 0.112106 0.375428 0.019 Uiso 1 1 calc R U . . .
C4 C 0.1219(2) 0.2903(2) 0.72286(19) 0.0165(4) Uani 1 1 d . . . . .
H4 H 0.044803 0.338255 0.663731 0.020 Uiso 1 1 calc R U . . .
C5 C 0.0750(2) 0.2756(2) 0.8592(2) 0.0184(4) Uani 1 1 d . . . . .
H5 H -0.033099 0.316794 0.895455 0.022 Uiso 1 1 calc R U . . .
C18 C 0.8238(3) 0.3344(2) 0.30609(19) 0.0181(4) Uani 1 1 d . . . . .
H18A H 0.769127 0.429042 0.345419 0.022 Uiso 1 1 calc R U . . .
H18B H 0.940961 0.354250 0.270970 0.022 Uiso 1 1 calc R U . . .
C16 C 0.6582(2) 0.1921(2) 0.49235(18) 0.0164(4) Uani 1 1 d . . . . .
H16A H 0.599349 0.294099 0.507632 0.020 Uiso 1 1 calc R U . . .
H16B H 0.588695 0.136405 0.437560 0.020 Uiso 1 1 calc R U . . .
C25 C 0.6099(2) 0.3193(2) 0.01950(19) 0.0170(4) Uani 1 1 d . . . . .
H25 H 0.562901 0.359035 -0.060244 0.020 Uiso 1 1 calc R U . . .
B1 B 0.2906(3) 0.4397(2) 0.3132(2) 0.0189(4) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N14 1.9681(15) . ?
Fe1 N14 1.9681(15) 2_657 ?
Fe1 N24 1.9763(15) 2_656 ?
Fe1 N24 1.9763(15) 1_556 ?
Fe1 N1 2.0125(15) 2_657 ?
Fe1 N1 2.0125(15) . ?
F3 B1 1.387(2) . ?
F4A B1 1.397(2) . ?
F2A B1 1.394(2) . ?
F1A B1 1.377(3) . ?
F1B B1 1.437(8) . ?
F4B B1 1.460(8) . ?
F2B B1 1.321(7) . ?
N1 C6 1.335(2) . ?
N1 C2 1.363(2) . ?
N22 N23 1.308(2) . ?
N22 N21 1.328(2) . ?
N22 C18 1.474(2) . ?
N14 C15 1.327(2) . ?
N14 N13 1.356(2) . ?
N24 N23 1.328(2) . ?
N24 C25 1.347(2) . ?
N13 N12 1.296(2) . ?
N11 C15 1.337(2) . ?
N11 N12 1.352(2) . ?
N11 C16 1.476(2) . ?
N21 C25 1.322(2) . ?
C15 C2 1.458(3) . ?
C2 C3 1.381(2) . ?
C6 C5 1.391(3) . ?
C6 H6 0.9500 . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C17 C18 1.514(3) . ?
C17 C16 1.523(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C25 H25 0.9500 . ?

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
N14 Fe1 N14 180.0 . 2_657 ?
N14 Fe1 N24 89.94(6) . 2_656 ?
N14 Fe1 N24 90.06(6) 2_657 2_656 ?
N14 Fe1 N24 90.06(6) . 1_556 ?
N14 Fe1 N24 89.94(6) 2_657 1_556 ?
N24 Fe1 N24 180.00(5) 2_656 1_556 ?
N14 Fe1 N1 99.64(6) . 2_657 ?
N14 Fe1 N1 80.36(6) 2_657 2_657 ?
N24 Fe1 N1 91.36(6) 2_656 2_657 ?
N24 Fe1 N1 88.64(6) 1_556 2_657 ?
N14 Fe1 N1 80.36(6) . . ?
N14 Fe1 N1 99.64(6) 2_657 . ?
N24 Fe1 N1 88.64(6) 2_656 . ?
N24 Fe1 N1 91.36(6) 1_556 . ?
N1 Fe1 N1 180.00(9) 2_657 . ?
C6 N1 C2 117.58(15) . . ?
C6 N1 Fe1 126.29(13) . . ?
C2 N1 Fe1 115.64(12) . . ?
N23 N22 N21 114.68(15) . . ?
N23 N22 C18 123.24(15) . . ?
N21 N22 C18 122.08(15) . . ?
C15 N14 N13 107.24(14) . . ?
C15 N14 Fe1 114.31(12) . . ?
N13 N14 Fe1 138.38(12) . . ?
N23 N24 C25 106.72(15) . . ?
N23 N24 Fe1 121.75(12) . 1_554 ?
C25 N24 Fe1 131.51(13) . 1_554 ?
N12 N13 N14 109.32(14) . . ?
N22 N23 N24 105.08(14) . . ?
C15 N11 N12 108.24(15) . . ?
C15 N11 C16 129.98(15) . . ?
N12 N11 C16 121.65(15) . . ?
C25 N21 N22 101.75(15) . . ?
N13 N12 N11 107.50(15) . . ?
N14 C15 N11 107.70(15) . . ?
N14 C15 C2 118.44(16) . . ?
N11 C15 C2 133.80(16) . . ?
N1 C2 C3 123.24(17) . . ?
N1 C2 C15 110.26(15) . . ?
C3 C2 C15 126.48(17) . . ?
N1 C6 C5 122.50(18) . . ?
N1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C2 C3 C4 118.03(17) . . ?
C2 C3 H3 121.0 . . ?
C4 C3 H3 121.0 . . ?
C18 C17 C16 112.05(15) . . ?
C18 C17 H17A 109.2 . . ?
C16 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C16 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C5 C4 C3 119.23(17) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 119.28(18) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
N22 C18 C17 113.46(15) . . ?
N22 C18 H18A 108.9 . . ?
C17 C18 H18A 108.9 . . ?
N22 C18 H18B 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
N11 C16 C17 111.21(15) . . ?
N11 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
N11 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N21 C25 N24 111.76(16) . . ?
N21 C25 H25 124.1 . . ?
N24 C25 H25 124.1 . . ?
F2B B1 F3 119.0(7) . . ?
F1A B1 F3 111.37(18) . . ?
F1A B1 F2A 109.71(18) . . ?
F3 B1 F2A 108.74(17) . . ?
F1A B1 F4A 109.22(18) . . ?
F3 B1 F4A 109.99(16) . . ?
F2A B1 F4A 107.74(17) . . ?
F2B B1 F1B 113.7(7) . . ?
F3 B1 F1B 105.9(6) . . ?
F2B B1 F4B 111.1(7) . . ?
F3 B1 F4B 102.7(6) . . ?
F1B B1 F4B 102.8(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N14 N13 N12 -0.3(2) . . . . ?
Fe1 N14 N13 N12 -176.94(14) . . . . ?
N21 N22 N23 N24 -0.2(2) . . . . ?
C18 N22 N23 N24 -179.87(16) . . . . ?
C25 N24 N23 N22 0.19(19) . . . . ?
Fe1 N24 N23 N22 -178.67(11) 1_554 . . . ?
N23 N22 N21 C25 0.1(2) . . . . ?
C18 N22 N21 C25 179.80(17) . . . . ?
N14 N13 N12 N11 0.3(2) . . . . ?
C15 N11 N12 N13 -0.2(2) . . . . ?
C16 N11 N12 N13 175.99(16) . . . . ?
N13 N14 C15 N11 0.18(19) . . . . ?
Fe1 N14 C15 N11 177.71(11) . . . . ?
N13 N14 C15 C2 -177.32(15) . . . . ?
Fe1 N14 C15 C2 0.2(2) . . . . ?
N12 N11 C15 N14 0.0(2) . . . . ?
C16 N11 C15 N14 -175.78(17) . . . . ?
N12 N11 C15 C2 176.99(19) . . . . ?
C16 N11 C15 C2 1.2(3) . . . . ?
C6 N1 C2 C3 -4.3(3) . . . . ?
Fe1 N1 C2 C3 168.21(14) . . . . ?
C6 N1 C2 C15 176.75(15) . . . . ?
Fe1 N1 C2 C15 -10.77(18) . . . . ?
N14 C15 C2 N1 7.0(2) . . . . ?
N11 C15 C2 N1 -169.72(18) . . . . ?
N14 C15 C2 C3 -171.95(17) . . . . ?
N11 C15 C2 C3 11.3(3) . . . . ?
C2 N1 C6 C5 2.6(3) . . . . ?
Fe1 N1 C6 C5 -168.98(14) . . . . ?
N1 C2 C3 C4 2.5(3) . . . . ?
C15 C2 C3 C4 -178.67(17) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C4 C5 C6 -2.5(3) . . . . ?
N1 C6 C5 C4 0.7(3) . . . . ?
N23 N22 C18 C17 -10.3(3) . . . . ?
N21 N22 C18 C17 170.04(17) . . . . ?
C16 C17 C18 N22 -68.9(2) . . . . ?
C15 N11 C16 C17 162.34(17) . . . . ?
N12 N11 C16 C17 -13.0(2) . . . . ?
C18 C17 C16 N11 -161.73(15) . . . . ?
N22 N21 C25 N24 0.0(2) . . . . ?
N23 N24 C25 N21 -0.1(2) . . . . ?
Fe1 N24 C25 N21 178.58(13) 1_554 . . . ?

_refine_diff_density_max         0.899
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.064

