# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

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

data_FeL6(BF4)3_295K
_database_code_depnum_ccdc_archive 'CCDC 2098447'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-12-09 deposited with the CCDC.	2022-01-05 downloaded from the CCDC.
;
_audit_creation_date             2021-12-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H42 Fe1 N6 O6, 3(B F4), 0.8[C5H12]'
_chemical_formula_sum            'C36 H42 B3 F12 Fe N6 O6'
_chemical_formula_weight         971.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
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'

_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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   14.5511(4)
_cell_length_b                   14.5511(4)
_cell_length_c                   39.000(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7151.3(6)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6488
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      26.9210
_cell_measurement_theta_min      3.1960

_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            24775
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.209
_diffrn_ambient_temperature      295.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1367
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1165
_reflns_number_total             1412
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1412
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0494
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0990P)²+6.9398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1607
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F2
 1.35 with sigma of 0.01
 B1-F1
 1.35 with sigma of 0.008
 B1-F3 = B1-F5
 1.35 with sigma of 0.005
 B1-F4 = B1-F6
 1.34 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
Uanis(B1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
4. Others
 Fixed Sof: F1(0.75) F2(0.35) F3(0.34) F4(0.24) F5(0.15) F6(0.17)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.333333 0.666667 0.416667 0.0541(3) Uani 1 6 d S T P . .
O1 O 0.39695(13) 0.60009(12) 0.44612(6) 0.0669(6) Uani 1 1 d . . . . .
N1 N 0.44643(18) 0.47870(17) 0.45616(5) 0.0626(6) Uani 1 1 d . . . . .
H1 H 0.510663 0.528841 0.452959 0.075 Uiso 1 1 calc R U . . .
C2 C 0.36780(19) 0.50394(19) 0.45425(6) 0.0591(6) Uani 1 1 d . . . . .
C3 C 0.2647(2) 0.4227(2) 0.46118(8) 0.0730(8) Uani 1 1 d . . . . .
H3 H 0.208563 0.436104 0.460828 0.088 Uiso 1 1 calc R U . . .
C4 C 0.2472(3) 0.3235(2) 0.46847(9) 0.0871(10) Uani 1 1 d . . . . .
H4 H 0.178536 0.269450 0.473195 0.105 Uiso 1 1 calc R U . . .
C5 C 0.3300(3) 0.3017(2) 0.46896(9) 0.0882(10) Uani 1 1 d . . . . .
H5 H 0.316178 0.233200 0.473572 0.106 Uiso 1 1 calc R U . . .
C6 C 0.4302(3) 0.3795(2) 0.46277(7) 0.0734(8) Uani 1 1 d . . . . .
C7 C 0.5240(3) 0.3650(3) 0.46172(10) 0.1003(11) Uani 1 1 d . . . . .
H7A H 0.536261 0.351627 0.438542 0.150 Uiso 1 1 calc R U . . .
H7B H 0.511312 0.305920 0.475919 0.150 Uiso 1 1 calc R U . . .
H7C H 0.585072 0.428094 0.470002 0.150 Uiso 1 1 calc R U . . .
B1 B 0.7186(4) 0.666667 0.416667 0.115(2) Uani 1 2 d DS TU P . .
F1 F 0.6511(5) 0.6511(5) 0.44226(18) 0.174(2) Uani 0.75 1 d D . P A 1
F2 F 0.7454(10) 0.5918(9) 0.4126(4) 0.188(7) Uani 0.35 1 d D U P A 2
F3 F 0.6674(13) 0.6033(12) 0.4433(4) 0.179(6) Uani 0.34 1 d D U P A 3
F4 F 0.7048(16) 0.5765(11) 0.4021(5) 0.176(9) Uani 0.24 1 d D U P A 4
F5 F 0.8107(5) 0.666667 0.416667 0.187(12) Uani 0.3 2 d DS T P A 5
F6 F 0.655(2) 0.5763(12) 0.3995(6) 0.185(10) Uani 0.17 1 d D U P A 6


_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 O1 2.0030(18) 2_665 ?
Fe1 O1 2.0029(18) 11_565 ?
Fe1 O1 2.0030(18) 10_455 ?
Fe1 O1 2.0030(18) 3_565 ?
Fe1 O1 2.0030(18) . ?
Fe1 O1 2.0029(18) 12 ?
O1 C2 1.282(3) . ?
N1 H1 0.8600 . ?
N1 C2 1.367(3) . ?
N1 C6 1.366(3) . ?
C2 C3 1.395(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.364(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.347(5) . ?
C6 C7 1.482(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
B1 F1 1.339(5) . ?
B1 F1 1.339(5) 11_565 ?
B1 F2 1.338(8) 11_565 ?
B1 F2 1.338(8) . ?
B1 F3 1.340(5) 11_565 ?
B1 F3 1.341(5) . ?
B1 F4 1.349(4) . ?
B1 F4 1.349(4) 11_565 ?
B1 F5 1.340(5) . ?
B1 F6 1.348(4) 11_565 ?
B1 F6 1.348(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 90.37(9) 2_665 3_565 ?
O1 Fe1 O1 88.76(11) . 12 ?
O1 Fe1 O1 90.51(11) . 11_565 ?
O1 Fe1 O1 90.37(9) 2_665 . ?
O1 Fe1 O1 88.76(11) 2_665 11_565 ?
O1 Fe1 O1 90.37(9) 3_565 . ?
O1 Fe1 O1 90.51(11) 3_565 12 ?
O1 Fe1 O1 90.51(11) 2_665 10_455 ?
O1 Fe1 O1 90.37(9) 10_455 12 ?
O1 Fe1 O1 88.76(11) 3_565 10_455 ?
O1 Fe1 O1 178.76(9) 3_565 11_565 ?
O1 Fe1 O1 178.77(9) . 10_455 ?
O1 Fe1 O1 90.38(9) 12 11_565 ?
O1 Fe1 O1 178.77(9) 2_665 12 ?
O1 Fe1 O1 90.37(9) 10_455 11_565 ?
C2 O1 Fe1 133.53(16) . . ?
C2 N1 H1 117.7 . . ?
C6 N1 H1 117.7 . . ?
C6 N1 C2 124.6(2) . . ?
O1 C2 N1 116.2(2) . . ?
O1 C2 C3 126.9(2) . . ?
N1 C2 C3 116.8(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C5 121.3(3) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
N1 C6 C7 117.4(3) . . ?
C5 C6 N1 117.7(3) . . ?
C5 C6 C7 124.9(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
F1 B1 F1 98.9(8) . 11_565 ?
F1 B1 F3 121.8(9) . 11_565 ?
F1 B1 F4 114.2(11) 11_565 11_565 ?
F1 B1 F4 91.6(8) . 11_565 ?
F1 B1 F6 67.9(12) . 11_565 ?
F1 B1 F6 96.6(14) 11_565 11_565 ?
F2 B1 F2 91.3(12) 11_565 . ?
F2 B1 F6 59.0(14) 11_565 11_565 ?
F2 B1 F6 142.7(16) . 11_565 ?
F3 B1 F3 155.5(15) 11_565 . ?
F3 B1 F6 80.7(15) 11_565 11_565 ?
F3 B1 F6 94.4(13) . 11_565 ?
F4 B1 F4 140.6(16) 11_565 . ?
F5 B1 F6 101.6(14) . 11_565 ?
F6 B1 F6 157(3) 11_565 . ?

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 O1 C2 N1 141.3(2) . . . . ?
Fe1 O1 C2 C3 -38.4(4) . . . . ?
O1 C2 C3 C4 178.0(3) . . . . ?
N1 C2 C3 C4 -1.7(4) . . . . ?
C2 N1 C6 C5 -2.3(4) . . . . ?
C2 N1 C6 C7 176.2(3) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C3 C4 C5 C6 1.2(5) . . . . ?
C4 C5 C6 N1 0.0(5) . . . . ?
C4 C5 C6 C7 -178.3(3) . . . . ?
C6 N1 C2 O1 -176.7(2) . . . . ?
C6 N1 C2 C3 3.1(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 210 electrons were 
found in a volume of 888Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[C5H12] per Formula Unit 
which account for 202 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 148.2 34.7 '0.8 C5H12'
2 0.000 0.000 0.500 148.2 34.7 '0.8 C5H12'
3 0.333 0.667 0.667 148.2 34.7 '0.8 C5H12'
4 0.333 0.667 0.167 148.2 34.7 '0.8 C5H12'
5 0.667 0.333 0.333 148.2 34.7 '0.8 C5H12'
6 0.667 0.333 0.833 148.2 34.7 '0.8 C5H12'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_FeL6(BF4)3_125K
_database_code_depnum_ccdc_archive 'CCDC 2098448'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-12-09 deposited with the CCDC.	2022-01-05 downloaded from the CCDC.
;
_audit_creation_date             2021-03-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H42 Fe1 N6 O6, 3(B F4), 0.8[C5H12]'
_chemical_formula_sum            'C36 H42 B3 F12 Fe N6 O6'
_chemical_formula_weight         971.03
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
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'

_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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   14.3913(7)
_cell_length_b                   14.3913(7)
_cell_length_c                   38.125(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6838.3(10)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    125
_cell_measurement_theta_max      22.8160
_cell_measurement_theta_min      3.9000

_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.533
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.186
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            18022
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.440
_diffrn_ambient_temperature      125
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1367
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                744
_reflns_number_total             1341
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0826
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1073P)²+58.3106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2693
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C5(H5)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

# start Validation Reply Form
_vrf_PLAT250_FeL6BF43_125K       
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.1 Note  
RESPONSE: The whole structure is slightly disordered (ADPs are elongated
in the same direction).
;
# end Validation Reply Form

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 0.666667 0.333333 0.583333 0.0688(9) Uani 1 6 d S T P . .
O1 O 0.5986(3) 0.3964(3) 0.55281(14) 0.0795(15) Uani 1 1 d . . . . .
N1 N 0.4747(4) 0.4442(4) 0.54265(17) 0.084(2) Uani 1 1 d . . . . .
H1 H 0.526758 0.511129 0.544967 0.101 Uiso 1 1 calc R U . . .
C2 C 0.5005(5) 0.3662(5) 0.5451(2) 0.079(2) Uani 1 1 d . . . . .
C3 C 0.4179(5) 0.2597(5) 0.5395(2) 0.086(2) Uani 1 1 d . . . . .
H3 H 0.432289 0.202118 0.540274 0.103 Uiso 1 1 calc R U . . .
C4 C 0.3174(5) 0.2411(6) 0.5329(3) 0.106(3) Uani 1 1 d . . . . .
H4 H 0.261495 0.169484 0.528929 0.127 Uiso 1 1 calc R U . . .
C5 C 0.2935(6) 0.3237(6) 0.5318(3) 0.106(3) Uani 1 1 d . . . . .
H5 H 0.222103 0.308260 0.527693 0.128 Uiso 1 1 calc R U . . .
C6 C 0.3731(5) 0.4264(6) 0.5368(2) 0.090(3) Uani 1 1 d . . . . .
C7 C 0.3593(6) 0.5236(6) 0.5368(3) 0.111(3) Uani 1 1 d . . . . .
H7A H 0.422316 0.584138 0.547611 0.167 Uiso 1 1 calc R U . . .
H7B H 0.294998 0.507848 0.550250 0.167 Uiso 1 1 calc R U . . .
H7C H 0.351693 0.541963 0.512651 0.167 Uiso 1 1 calc R U . . .
B1 B 0.666667 0.7169(8) 0.583333 0.159(10) Uani 1 2 d S T P . .
F1 F 0.6408(5) 0.6504(4) 0.5552(2) 0.173(3) Uani 1 1 d . . . . .
F2 F 0.7507(7) 0.8131(5) 0.5752(4) 0.318(7) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.007(4) 2_655 ?
Fe1 O1 2.007(4) 18_655 ?
Fe1 O1 2.007(4) 16_545 ?
Fe1 O1 2.007(4) 3_665 ?
Fe1 O1 2.007(4) . ?
Fe1 O1 2.007(4) 17 ?
O1 C2 1.285(7) . ?
N1 H1 0.8800 . ?
N1 C2 1.352(8) . ?
N1 C6 1.372(7) . ?
C2 C3 1.409(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.356(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.355(10) . ?
C6 C7 1.507(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
B1 F1 1.361(9) . ?
B1 F1 1.360(9) 18_655 ?
B1 F2 1.342(10) 18_655 ?
B1 F2 1.342(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 89.7(2) 2_655 3_665 ?
O1 Fe1 O1 91.7(2) . 18_655 ?
O1 Fe1 O1 89.7(2) 16_545 17 ?
O1 Fe1 O1 89.7(2) 2_655 . ?
O1 Fe1 O1 91.7(2) 2_655 17 ?
O1 Fe1 O1 89.7(2) 3_665 . ?
O1 Fe1 O1 88.8(3) 3_665 18_655 ?
O1 Fe1 O1 88.8(3) 2_655 16_545 ?
O1 Fe1 O1 89.7(2) 16_545 18_655 ?
O1 Fe1 O1 91.7(2) 3_665 16_545 ?
O1 Fe1 O1 88.8(3) . 17 ?
O1 Fe1 O1 178.0(2) . 16_545 ?
O1 Fe1 O1 89.8(2) 18_655 17 ?
O1 Fe1 O1 178.0(2) 2_655 18_655 ?
O1 Fe1 O1 178.0(2) 3_665 17 ?
C2 O1 Fe1 132.8(4) . . ?
C2 N1 H1 117.7 . . ?
C2 N1 C6 124.5(6) . . ?
C6 N1 H1 117.7 . . ?
O1 C2 N1 116.5(5) . . ?
O1 C2 C3 126.2(6) . . ?
N1 C2 C3 117.4(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.7(6) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.0(6) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.5(6) . . ?
C6 C5 H5 120.3 . . ?
N1 C6 C7 116.7(6) . . ?
C5 C6 N1 117.8(6) . . ?
C5 C6 C7 125.5(6) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
F1 B1 F1 110.9(10) . 18_655 ?
F2 B1 F1 109.4(7) 18_655 18_655 ?
F2 B1 F1 109.1(5) . 18_655 ?
F2 B1 F1 109.4(7) . . ?
F2 B1 F1 109.1(5) 18_655 . ?
F2 B1 F2 108.9(13) . 18_655 ?

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 O1 C2 N1 141.4(6) . . . . ?
Fe1 O1 C2 C3 -37.9(12) . . . . ?
O1 C2 C3 C4 177.5(9) . . . . ?
N1 C2 C3 C4 -1.8(13) . . . . ?
C2 N1 C6 C5 -2.5(14) . . . . ?
C2 N1 C6 C7 176.7(8) . . . . ?
C2 C3 C4 C5 -0.4(15) . . . . ?
C3 C4 C5 C6 1.4(15) . . . . ?
C4 C5 C6 N1 0.0(14) . . . . ?
C4 C5 C6 C7 -179.1(9) . . . . ?
C6 N1 C2 O1 -176.0(8) . . . . ?
C6 N1 C2 C3 3.4(13) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 210 electrons were 
found in a volume of 762Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[C5H12] per Formula Unit 
which account for 202 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 127.4 34.8 '0.8 C5H12'
2 0.000 0.000 0.500 127.4 34.8 '0.8 C5H12'
3 0.333 0.667 0.667 127.4 34.8 '0.8 C5H12'
4 0.333 0.667 0.167 127.4 34.8 '0.8 C5H12'
5 0.667 0.333 0.333 127.4 34.8 '0.8 C5H12'
6 0.667 0.333 0.833 127.4 34.8 '0.8 C5H12'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
