# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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#######################################################################

data_EFB57_a
_database_code_depnum_ccdc_archive 'CCDC 1825247'
_audit_update_record             
;
2018-02-22 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H60 B3 F15 Fe3 N48'
_chemical_formula_weight         2082.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
B B 0.0020 0.0008 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0076 0.0040 'Calculated using XDISP in WinGX (Farrugia, 1999)'
F F 0.0211 0.0125 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Fe Fe 0.3555 0.9930 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_H-M_alt        'P 4/n c c'
_space_group_name_Hall           '-P 4a 2ac'

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

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

_cell_length_a                   19.9412(9)
_cell_length_b                   19.9412(9)
_cell_length_c                   24.1342(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9597.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9241
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      33.61

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_F_000             4224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.683
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS, Madison WI'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   
;
Advanced Light Source, station 11.3.1
;
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            118782
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.151
_diffrn_reflns_theta_max         33.636
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7361
_reflns_number_gt                5653
_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.
;
_vrf_PLAT084_EFB57_a             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.55 Report
RESPONSE: This is correct, this crystal was found to have a supercell, which
has lead to elevated wR2 values due to the low intensities of the reflections
that indicate that the larger supercell is present.
;
_vrf_PLAT934_EFB57_a             
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         45 Check 
RESPONSE: We attribute this to the supercell causing poor correlation between
predicted and observed reflections. Some of these disagreeable reflections may
also be due to the disordered solvent in the pores of the crystal, which have
not been modelled. No attempt has been made to omit these disagreeable
reflections from the refinement.
;
_vrf_PLAT973_EFB57_a             
;
PROBLEM: Check Calcd Positive Residual Density on     Fe1       2.48 eA-3  
RESPONSE: 
These larger than ideal peaks of electron density disappear when the
cutoff resolution of the data is lowered from 0.7 A to 0.8 A through use of a
SHEL 999 0.8 command. Below is presented the intensity statistics for the
dataset. We were reluctant to cut the data to lower resolution simply to make
these peaks disappear, given that the Mean I/s values were still above 9 at
the higher resolution, and the Rmerge value for the 0.71 to 0.70 shell is
0.0838.

 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma

  Inf - 3.11     123    129     95.3    21.48     94.58   66.75  0.0302  0.0123
 3.11 - 2.00     291    291    100.0    18.85     37.03   56.54  0.0315  0.0124
 2.00 - 1.56     415    415    100.0    17.86     29.91   54.79  0.0252  0.0167
 1.56 - 1.35     414    414    100.0    17.84     16.13   46.36  0.0261  0.0152
 1.35 - 1.22     415    415    100.0    17.29     12.77   39.46  0.0283  0.0155
 1.22 - 1.13     403    403    100.0    17.15      8.77   37.29  0.0332  0.0154
 1.13 - 1.06     409    409    100.0    16.99      7.27   35.24  0.0354  0.0167
 1.06 - 1.00     450    450    100.0    16.10      7.77   31.93  0.0385  0.0181
 1.00 - 0.96     364    364    100.0    15.21      7.97   27.57  0.0384  0.0180
 0.96 - 0.92     430    430    100.0    15.38      6.51   25.06  0.0405  0.0184
 0.92 - 0.88     500    501     99.8    15.28      3.67   19.07  0.0493  0.0218
 0.88 - 0.86     285    285    100.0    15.02      3.47   17.20  0.0508  0.0228
 0.86 - 0.83     475    475    100.0    15.03      2.87   17.31  0.0569  0.0247
 0.83 - 0.81     371    371    100.0    14.32      2.73   15.69  0.0634  0.0269
 0.81 - 0.79     402    402    100.0    14.15      2.60   14.21  0.0695  0.0279
 0.79 - 0.77     440    440    100.0    13.82      2.46   13.01  0.0703  0.0292
 0.77 - 0.75     493    493    100.0    13.80      1.98   11.19  0.0804  0.0330
 0.75 - 0.73     538    538    100.0    13.30      1.76   10.95  0.0905  0.0375
 0.73 - 0.72     302    302    100.0    12.58      1.74   10.64  0.0878  0.0371
 0.72 - 0.71     300    300    100.0    12.40      1.72   10.47  0.1012  0.0396
 0.71 - 0.70     361    372     97.0    11.09      1.71    9.73  0.1056  0.0446
#------------------------------------------------------------------------------
 0.80 - 0.70    2643   2654     99.6    13.02      1.98   11.38  0.0838  0.0349
  Inf - 0.70    8181   8199     99.8    15.28      8.97   25.52  0.0338  0.0171

The large peaks may be an artefact of the supercell, due to slight variations in
the location of the Fe centres.
;

_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
An initial data collection revealed that the crystal contained a supercell.
The second data collection involved two complete datasets, one at a collection
tome of 1 s, the second at a collection time of 5 s. Both datasets were
integrated together, and the full first dataset was treated as a fast scan in
sadabs. This was done so that any overloaded reflections corresponding to the
smaller cell could be scaled in.

A solution was obtained in four space groups: P4/ncc, P4cc, P42(1)2, and
P-42(1)c. The initial R1 values were as follows:
 R1  Rweak Alpha   Orientation     Space group  Flack_x  
 0.315 0.002 0.067     as input      P4/ncc               
 0.224 0.002 0.017     as input      P4cc           0.50  
 0.283 0.001 0.062     as input      P42(1)2        0.50 
 0.270 0.002 0.071     as input      P-42(1)c       0.49 
A complete refinement was conducted in P4/ncc, which showed that one of the two
unique ligands was positionally disordered, while the other had some rotational
disorder of the cntral aromatic ring. The positional disorder was modelled over
two sites of complementary occupancy, with pairs of equivalent atoms constrained
to have equal Uij values and SAME and SADI commands were used to ensure that the
bond lengths and angles were equivalent for both orientations. The rotational
disorder was modelled by generating remainder of the central -CH-C6H4-CH- from
symmetry equivalent atoms and refining the entire unit with an occupancy of 50%.
SADI commands were used to constrain equivalent bonds to have the same length.

Before modelling the BF4 anions, a SQUEEZE analysis was performed. This showed
the following:
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.250  0.750  0.217       903       379 ' '
   2  0.250  0.750  0.250         7         0 ' '
   3  0.250  0.750  0.750         7         0 ' '
   4  0.750  0.250  0.781       903       379 ' '
   5  0.750  0.250  0.750         7         0 ' '
   6  0.750  0.250  0.250         7         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
As there were still anions needing to be modelled, no refinement was performed
using SQUEEZEd data, this was done for an estimate of residual electron density
only. The above corresponds to 758 electrons per unit cell, or 63 electrons per
Fe centre unaccounted for. One BF4 contributes 42 electron, so this leaves 21 
electrons, or approximately 0.8 ethanol molecules unaccounted for. The bulk of
the solvent used in the synthesis was ethanol, however, as there is a possibility
that there may be small amounts of water present, these solvent molecules have
not been included in the final molecular formula.

One BF4 anion was modelled, and successive positions of the disordered BF4 were
added as more peaks of electron density appeared in the region. The BF4 anions
were refined with a common B-F bond length, which was refined as a free variable,
and an F...F separation that was fixed at 1.633 times this value. Each BF4 site
was given a variable occupancy, with these constrained to sum to 0.75. Equivalent
atoms were constrained to have equal Uij values.

As there were multiple potential space groups, one of which (P4cc) had a
significantly lower initial R1 than the current model, the framework atoms were
modelled for each of the other three potential solutions. The resulting R1 
values, Flack parameters and BASF values are as follows:
P4cc		0.1502		0.52(10)	0.52085	
P42(1)1		0.1482		0.52(13)	0.51576
P-42(1)c	0.1513		0.51(12)	0.50817
In all cases, the R1 values are comparable to the current solution, and the Flack 
and BASF parameters indicate that the crystal is either centrosymmetric or a
racemic twin. None of these lower symmetry space groups resulted in the ordering
of the disordered ligands. As such, the space group P4/ncc was selected as the
correct space group. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0048(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7361
_refine_ls_number_parameters     439
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.1301
_refine_ls_wR_factor_ref         0.5509
_refine_ls_wR_factor_gt          0.4997
_refine_ls_goodness_of_fit_ref   2.717
_refine_ls_restrained_S_all      2.711
_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
C1 C 0.6323(2) 0.6747(2) 0.57047(15) 0.0386(9) Uani 1 1 d . . . . .
H1 H 0.6637 0.6531 0.5469 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5394(2) 0.7087(3) 0.6076(2) 0.0530(12) Uani 1 1 d . . . . .
H2 H 0.4931 0.7151 0.6149 0.064 Uiso 1 1 calc R U . . .
N4_1 N 0.5222(3) 0.6370(3) 0.5291(2) 0.0460(13) Uani 0.739(4) 1 d D . P A 1
C3_1 C 0.5531(3) 0.5975(3) 0.4974(2) 0.0398(11) Uani 0.739(4) 1 d D . P A 1
H3_1 H 0.6003 0.5925 0.5005 0.048 Uiso 0.739(4) 1 calc R U P A 1
C4_1 C 0.5156(2) 0.5593(3) 0.4556(2) 0.0446(13) Uani 0.739(4) 1 d D . P A 1
C5_1 C 0.4462(3) 0.5626(4) 0.4516(3) 0.0528(15) Uani 0.739(4) 1 d D . P A 1
H5_1 H 0.4218 0.5910 0.4759 0.063 Uiso 0.739(4) 1 calc R U P A 1
C6_1 C 0.4126(3) 0.5246(3) 0.4124(2) 0.0496(14) Uani 0.739(4) 1 d D . P A 1
H6_1 H 0.3652 0.5270 0.4095 0.059 Uiso 0.739(4) 1 calc R U P A 1
C7_1 C 0.4491(2) 0.4827(3) 0.3770(2) 0.0416(12) Uani 0.739(4) 1 d D . P A 1
C8_1 C 0.5192(3) 0.4796(3) 0.3811(2) 0.0450(12) Uani 0.739(4) 1 d D . P A 1
H8_1 H 0.5440 0.4515 0.3569 0.054 Uiso 0.739(4) 1 calc R U P A 1
C9_1 C 0.5519(3) 0.5177(3) 0.4205(2) 0.0465(13) Uani 0.739(4) 1 d D . P A 1
H9_1 H 0.5993 0.5154 0.4237 0.056 Uiso 0.739(4) 1 calc R U P A 1
C10_1 C 0.4134(3) 0.4425(3) 0.3361(2) 0.0411(13) Uani 0.739(4) 1 d D . P A 1
H10_1 H 0.3658 0.4402 0.3359 0.049 Uiso 0.739(4) 1 calc R U P A 1
N5_1 N 0.4481(3) 0.4105(4) 0.3007(2) 0.0421(13) Uani 0.739(4) 1 d D . P A 1
N4_2 N 0.5462(6) 0.6292(11) 0.5198(7) 0.0460(13) Uani 0.261(4) 1 d D . P A 2
C3_2 C 0.4839(5) 0.6250(7) 0.5115(5) 0.0398(11) Uani 0.261(4) 1 d D . P A 2
H3_2 H 0.4534 0.6492 0.5342 0.048 Uiso 0.261(4) 1 calc R U P A 2
C4_2 C 0.4591(5) 0.5823(7) 0.4663(5) 0.0446(13) Uani 0.261(4) 1 d D . P A 2
C5_2 C 0.3915(5) 0.5811(8) 0.4524(6) 0.0528(15) Uani 0.261(4) 1 d D . P A 2
H5_2 H 0.3610 0.6104 0.4706 0.063 Uiso 0.261(4) 1 calc R U P A 2
C6_2 C 0.3687(5) 0.5372(8) 0.4123(6) 0.0496(14) Uani 0.261(4) 1 d D . P A 2
H6_2 H 0.3220 0.5332 0.4053 0.059 Uiso 0.261(4) 1 calc R U P A 2
C7_2 C 0.4146(5) 0.4987(7) 0.3818(5) 0.0416(12) Uani 0.261(4) 1 d D . P A 2
C8_2 C 0.4829(5) 0.5014(7) 0.3950(5) 0.0450(12) Uani 0.261(4) 1 d D . P A 2
H8_2 H 0.5141 0.4735 0.3761 0.054 Uiso 0.261(4) 1 calc R U P A 2
C9_2 C 0.5048(5) 0.5449(8) 0.4359(6) 0.0465(13) Uani 0.261(4) 1 d D . P A 2
H9_2 H 0.5514 0.5493 0.4431 0.056 Uiso 0.261(4) 1 calc R U P A 2
C10_2 C 0.3890(7) 0.4566(9) 0.3372(7) 0.0411(13) Uani 0.261(4) 1 d D . P A 2
H10_2 H 0.3422 0.4558 0.3297 0.049 Uiso 0.261(4) 1 calc R U P A 2
N5_2 N 0.4284(8) 0.4212(10) 0.3083(8) 0.0421(13) Uani 0.261(4) 1 d D . P A 2
C11 C 0.4420(2) 0.3422(2) 0.22144(18) 0.0456(10) Uani 1 1 d . . . . .
H11 H 0.4884 0.3466 0.2131 0.055 Uiso 1 1 calc R U . . .
C12 C 0.3446(2) 0.3546(2) 0.26116(16) 0.0390(9) Uani 1 1 d . . . . .
H12 H 0.3098 0.3692 0.2851 0.047 Uiso 1 1 calc R U . . .
C13 C 0.6891(2) 0.61863(19) 0.90213(15) 0.0357(8) Uani 1 1 d . . . . .
H13 H 0.6565 0.6459 0.8843 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7491(2) 0.5337(2) 0.92619(17) 0.0442(10) Uani 1 1 d . . . . .
H14 H 0.7666 0.4895 0.9282 0.053 Uiso 1 1 calc R U . . .
C15 C 0.6748(6) 0.4580(5) 0.8417(5) 0.044(3) Uani 0.5 1 d D . P B -1
H15 H 0.7061 0.4350 0.8645 0.053 Uiso 0.5 1 calc R U P B -1
C16 C 0.6383(5) 0.4221(5) 0.7964(5) 0.041(2) Uani 0.5 1 d D . P B -1
C17 C 0.5849(9) 0.4541(10) 0.7681(9) 0.029(3) Uani 0.5 1 d D . P B -1
H17 H 0.5714 0.4987 0.7763 0.035 Uiso 0.5 1 calc R U P B -1
C18 C 0.5537(11) 0.4157(12) 0.7278(11) 0.045(6) Uani 0.5 1 d D . P B -1
H18 H 0.5228 0.4376 0.7040 0.054 Uiso 0.5 1 calc R U P B -1
C19 C 0.5638(7) 0.3493(6) 0.7198(6) 0.055(3) Uani 0.5 1 d D . P B -1
C20 C 0.6159(10) 0.3215(8) 0.7475(9) 0.103(7) Uani 0.5 1 d D . P B -1
H20 H 0.6284 0.2771 0.7378 0.124 Uiso 0.5 1 calc R U P B -1
C21 C 0.6522(8) 0.3530(7) 0.7890(7) 0.080(5) Uani 0.5 1 d D . P B -1
H21 H 0.6843 0.3299 0.8110 0.096 Uiso 0.5 1 calc R U P B -1
C22 C 0.5292(6) 0.3109(6) 0.6752(5) 0.047(3) Uani 0.5 1 d D . P B -1
H22 H 0.5443 0.2674 0.6652 0.057 Uiso 0.5 1 calc R U P B -1
N1 N 0.64824(16) 0.71416(18) 0.61176(13) 0.0367(8) Uani 1 1 d . . . . .
N2 N 0.5886(2) 0.7363(2) 0.63576(16) 0.0483(9) Uani 1 1 d . . . . .
N3 N 0.56506(19) 0.6692(2) 0.56611(13) 0.0436(9) Uani 1 1 d D . . . .
N6 N 0.41039(19) 0.3738(2) 0.26386(13) 0.0454(9) Uani 1 1 d D . . . .
N7 N 0.33810(16) 0.31269(16) 0.21977(13) 0.0344(7) Uani 1 1 d . . . . .
N9 N 0.73015(17) 0.63934(17) 0.94121(12) 0.0359(7) Uani 1 1 d . . . . .
N8 N 0.39997(17) 0.30511(19) 0.19373(15) 0.0415(8) Uani 1 1 d . . . . .
N10 N 0.7694(2) 0.58344(19) 0.95686(16) 0.0435(8) Uani 1 1 d . . . . .
N11 N 0.69979(17) 0.55303(16) 0.89101(13) 0.0376(8) Uani 1 1 d . . . . .
N12 N 0.66284(17) 0.52084(18) 0.84914(14) 0.0404(8) Uani 1 1 d D . . . .
F1 F 0.7500 0.7500 0.7021(2) 0.0195(13) Uani 1 4 d S T P . .
F2 F 0.7500 0.7500 0.8686(2) 0.0191(13) Uani 1 4 d S T P . .
F3 F 0.7500 0.7500 1.0339(3) 0.0205(13) Uani 1 4 d S T P . .
Fe1 Fe 0.7500 0.7500 0.62159(5) 0.0184(5) Uani 1 4 d S T P . .
Fe2 Fe 0.7500 0.7500 0.78878(5) 0.0179(5) Uani 1 4 d S T P . .
Fe3 Fe 0.7500 0.7500 0.95293(6) 0.0196(5) Uani 1 4 d S T P . .
B1_3 B 0.6270(8) 0.3456(8) 0.1720(7) 0.103(7) Uiso 0.120(7) 1 d D . P C 4
F4_3 F 0.6718(12) 0.3986(11) 0.1644(14) 0.125(6) Uiso 0.120(7) 1 d D . P C 4
F5_3 F 0.6620(13) 0.2850(9) 0.1705(14) 0.114(5) Uiso 0.120(7) 1 d D . P C 4
F6_3 F 0.5790(11) 0.3464(17) 0.1300(8) 0.101(4) Uiso 0.120(7) 1 d D . P C 4
F7_3 F 0.5954(13) 0.3524(16) 0.2233(7) 0.091(4) Uiso 0.120(7) 1 d D . P C 4
B1_4 B 0.6694(6) 0.3610(6) 0.3802(5) 0.103(7) Uiso 0.204(8) 1 d D . P D 1
F4_4 F 0.7312(8) 0.3287(10) 0.3751(10) 0.125(6) Uiso 0.204(8) 1 d D . P D 1
F5_4 F 0.6179(9) 0.3138(9) 0.3771(10) 0.114(5) Uiso 0.204(8) 1 d D . P D 1
F6_4 F 0.6622(12) 0.4075(9) 0.3374(7) 0.101(4) Uiso 0.204(8) 1 d D . P D 1
F7_4 F 0.6664(11) 0.3940(9) 0.4311(6) 0.091(4) Uiso 0.204(8) 1 d D . P D 1
B1_5 B 0.6621(7) 0.3553(7) 0.3524(6) 0.103(7) Uiso 0.177(7) 1 d D . P E 2
F4_5 F 0.7020(10) 0.3035(9) 0.3318(10) 0.125(6) Uiso 0.177(7) 1 d D . P E 2
F5_5 F 0.6922(11) 0.3826(11) 0.3995(7) 0.114(5) Uiso 0.177(7) 1 d D . P E 2
F6_5 F 0.5990(8) 0.3301(11) 0.3662(10) 0.101(4) Uiso 0.177(7) 1 d D . P E 2
F7_5 F 0.6552(12) 0.4049(8) 0.3121(8) 0.091(4) Uiso 0.177(7) 1 d D . P E 2
B1_6 B 0.6239(7) 0.3714(7) 0.28326(13) 0.103(7) Uiso 0.082(6) 1 d D . P F 3
F4_6 F 0.6667(6) 0.3333(6) 0.2500 0.125(6) Uiso 0.164(11) 2 d DS . P F 3
F5_6 F 0.5859(6) 0.4141(6) 0.2500 0.114(5) Uiso 0.164(11) 2 d DS . P F 3
F6_6 F 0.6618(10) 0.4093(10) 0.3204(6) 0.101(4) Uiso 0.082(6) 1 d D . P F 3
F7_6 F 0.5813(10) 0.3288(10) 0.3127(8) 0.091(4) Uiso 0.082(6) 1 d D . P F 3
B1_7 B 0.6732(7) 0.3621(7) 0.3834(6) 0.103(7) Uiso 0.167(8) 1 d D . P G 5
F4_7 F 0.7076(13) 0.3790(14) 0.4317(7) 0.125(6) Uiso 0.167(8) 1 d D . P G 5
F5_7 F 0.6129(9) 0.3308(12) 0.3971(12) 0.114(5) Uiso 0.167(8) 1 d D . P G 5
F6_7 F 0.6601(14) 0.4201(9) 0.3529(10) 0.101(4) Uiso 0.167(8) 1 d D . P G 5
F7_7 F 0.7123(11) 0.3184(10) 0.3518(9) 0.091(4) Uiso 0.167(8) 1 d D . P G 5


_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
C1 N1 1.308(5) . ?
C1 N3 1.350(6) . ?
C1 H1 0.9500 . ?
C2 N2 1.313(6) . ?
C2 N3 1.373(6) . ?
C2 H2 0.9500 . ?
N4_1 C3_1 1.259(7) . ?
N4_1 N3 1.394(5) . ?
C3_1 C4_1 1.469(7) . ?
C3_1 H3_1 0.9500 . ?
C4_1 C9_1 1.387(6) . ?
C4_1 C5_1 1.388(6) . ?
C5_1 C6_1 1.387(6) . ?
C5_1 H5_1 0.9500 . ?
C6_1 C7_1 1.398(5) . ?
C6_1 H6_1 0.9500 . ?
C7_1 C8_1 1.402(5) . ?
C7_1 C10_1 1.458(6) . ?
C8_1 C9_1 1.381(5) . ?
C8_1 H8_1 0.9500 . ?
C9_1 H9_1 0.9500 . ?
C10_1 N5_1 1.269(8) . ?
C10_1 H10_1 0.9500 . ?
N5_1 N6 1.376(5) . ?
N4_2 C3_2 1.261(8) . ?
N4_2 N3 1.425(11) . ?
C3_2 C4_2 1.471(8) . ?
C3_2 H3_2 0.9500 . ?
C4_2 C9_2 1.387(6) . ?
C4_2 C5_2 1.389(6) . ?
C5_2 C6_2 1.383(6) . ?
C5_2 H5_2 0.9500 . ?
C6_2 C7_2 1.403(6) . ?
C6_2 H6_2 0.9500 . ?
C7_2 C8_2 1.401(6) . ?
C7_2 C10_2 1.456(7) . ?
C8_2 C9_2 1.384(6) . ?
C8_2 H8_2 0.9500 . ?
C9_2 H9_2 0.9500 . ?
C10_2 N5_2 1.267(9) . ?
C10_2 H10_2 0.9500 . ?
N5_2 N6 1.474(10) . ?
C11 N8 1.303(6) . ?
C11 N6 1.357(6) . ?
C11 H11 0.9500 . ?
C12 N7 1.309(5) . ?
C12 N6 1.367(5) . ?
C12 H12 0.9500 . ?
C13 N9 1.316(5) . ?
C13 N11 1.352(5) . ?
C13 H13 0.9500 . ?
C14 N10 1.302(6) . ?
C14 N11 1.355(5) . ?
C14 H14 0.9500 . ?
C15 N12 1.287(10) . ?
C15 C16 1.496(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.416(13) . ?
C16 C21 1.417(13) . ?
C17 C18 1.386(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.353(17) . ?
C18 H18 0.9500 . ?
C19 C20 1.353(16) . ?
C19 C22 1.491(13) . ?
C20 C21 1.387(10) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 N12 1.272(10) 8_666 ?
C22 H22 0.9500 . ?
N1 N2 1.394(5) . ?
N1 Fe1 2.164(3) . ?
N7 N8 1.393(5) . ?
N7 Fe2 2.166(3) 9_666 ?
N9 N10 1.414(5) . ?
N9 Fe3 2.260(3) . ?
N11 N12 1.406(4) . ?
N12 C22 1.272(10) 8_666 ?
F1 Fe1 1.943(6) . ?
F1 Fe2 2.092(6) . ?
F2 Fe2 1.927(6) . ?
F2 Fe3 2.035(5) . ?
F3 Fe3 1.953(6) . ?
F3 Fe1 2.117(6) 13_576 ?
Fe1 F3 2.117(6) 13_575 ?
Fe1 N1 2.164(3) 2_665 ?
Fe1 N1 2.164(3) 3_655 ?
Fe1 N1 2.164(3) 4_565 ?
Fe2 N7 2.166(3) 9_666 ?
Fe2 N7 2.166(3) 10_666 ?
Fe2 N7 2.166(3) 11_666 ?
Fe2 N7 2.166(3) 12_666 ?
Fe3 N9 2.260(3) 2_665 ?
Fe3 N9 2.260(3) 4_565 ?
Fe3 N9 2.260(3) 3_655 ?
B1_3 F4_3 1.395(4) . ?
B1_3 F7_3 1.395(4) . ?
B1_3 F5_3 1.395(4) . ?
B1_3 F6_3 1.395(4) . ?
B1_4 F5_4 1.395(4) . ?
B1_4 F4_4 1.395(4) . ?
B1_4 F6_4 1.395(4) . ?
B1_4 F7_4 1.395(4) . ?
B1_5 F6_5 1.395(4) . ?
B1_5 F5_5 1.395(4) . ?
B1_5 F7_5 1.395(4) . ?
B1_5 F4_5 1.395(4) . ?
B1_6 F7_6 1.395(4) . ?
B1_6 F5_6 1.395(4) . ?
B1_6 F6_6 1.395(4) . ?
B1_6 F4_6 1.395(4) . ?
B1_6 B1_6 1.611(6) 8_665 ?
F4_6 B1_6 1.395(4) 8_665 ?
F5_6 B1_6 1.395(4) 8_665 ?
B1_7 F5_7 1.395(4) . ?
B1_7 F4_7 1.395(4) . ?
B1_7 F7_7 1.395(4) . ?
B1_7 F6_7 1.395(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
N1 C1 N3 110.5(4) . . ?
N1 C1 H1 124.8 . . ?
N3 C1 H1 124.8 . . ?
N2 C2 N3 109.9(4) . . ?
N2 C2 H2 125.1 . . ?
N3 C2 H2 125.1 . . ?
C3_1 N4_1 N3 112.2(5) . . ?
N4_1 C3_1 C4_1 119.5(4) . . ?
N4_1 C3_1 H3_1 120.2 . . ?
C4_1 C3_1 H3_1 120.2 . . ?
C9_1 C4_1 C5_1 120.4(5) . . ?
C9_1 C4_1 C3_1 117.6(4) . . ?
C5_1 C4_1 C3_1 121.9(4) . . ?
C6_1 C5_1 C4_1 120.1(5) . . ?
C6_1 C5_1 H5_1 119.9 . . ?
C4_1 C5_1 H5_1 119.9 . . ?
C5_1 C6_1 C7_1 119.5(5) . . ?
C5_1 C6_1 H6_1 120.2 . . ?
C7_1 C6_1 H6_1 120.2 . . ?
C6_1 C7_1 C8_1 120.1(5) . . ?
C6_1 C7_1 C10_1 119.3(4) . . ?
C8_1 C7_1 C10_1 120.7(4) . . ?
C9_1 C8_1 C7_1 119.7(5) . . ?
C9_1 C8_1 H8_1 120.2 . . ?
C7_1 C8_1 H8_1 120.2 . . ?
C8_1 C9_1 C4_1 120.1(5) . . ?
C8_1 C9_1 H9_1 119.9 . . ?
C4_1 C9_1 H9_1 119.9 . . ?
N5_1 C10_1 C7_1 117.8(5) . . ?
N5_1 C10_1 H10_1 121.1 . . ?
C7_1 C10_1 H10_1 121.1 . . ?
C10_1 N5_1 N6 113.9(5) . . ?
C3_2 N4_2 N3 114.9(10) . . ?
N4_2 C3_2 C4_2 119.1(7) . . ?
N4_2 C3_2 H3_2 120.4 . . ?
C4_2 C3_2 H3_2 120.4 . . ?
C9_2 C4_2 C5_2 120.1(6) . . ?
C9_2 C4_2 C3_2 118.9(6) . . ?
C5_2 C4_2 C3_2 121.0(6) . . ?
C6_2 C5_2 C4_2 119.9(6) . . ?
C6_2 C5_2 H5_2 120.1 . . ?
C4_2 C5_2 H5_2 120.1 . . ?
C5_2 C6_2 C7_2 120.0(6) . . ?
C5_2 C6_2 H6_2 120.0 . . ?
C7_2 C6_2 H6_2 120.0 . . ?
C8_2 C7_2 C6_2 119.5(6) . . ?
C8_2 C7_2 C10_2 122.1(7) . . ?
C6_2 C7_2 C10_2 118.3(7) . . ?
C9_2 C8_2 C7_2 119.5(6) . . ?
C9_2 C8_2 H8_2 120.2 . . ?
C7_2 C8_2 H8_2 120.2 . . ?
C8_2 C9_2 C4_2 120.5(6) . . ?
C8_2 C9_2 H9_2 119.8 . . ?
C4_2 C9_2 H9_2 119.8 . . ?
N5_2 C10_2 C7_2 120.7(9) . . ?
N5_2 C10_2 H10_2 119.7 . . ?
C7_2 C10_2 H10_2 119.7 . . ?
C10_2 N5_2 N6 127.4(11) . . ?
N8 C11 N6 110.6(4) . . ?
N8 C11 H11 124.7 . . ?
N6 C11 H11 124.7 . . ?
N7 C12 N6 108.1(4) . . ?
N7 C12 H12 126.0 . . ?
N6 C12 H12 126.0 . . ?
N9 C13 N11 110.3(4) . . ?
N9 C13 H13 124.8 . . ?
N11 C13 H13 124.8 . . ?
N10 C14 N11 111.4(4) . . ?
N10 C14 H14 124.3 . . ?
N11 C14 H14 124.3 . . ?
N12 C15 C16 118.5(10) . . ?
N12 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C17 C16 C21 121.6(11) . . ?
C17 C16 C15 120.1(10) . . ?
C21 C16 C15 117.5(9) . . ?
C18 C17 C16 115.3(13) . . ?
C18 C17 H17 122.4 . . ?
C16 C17 H17 122.4 . . ?
C19 C18 C17 125.0(13) . . ?
C19 C18 H18 117.5 . . ?
C17 C18 H18 117.5 . . ?
C18 C19 C20 116.4(15) . . ?
C18 C19 C22 122.5(13) . . ?
C20 C19 C22 120.1(10) . . ?
C19 C20 C21 124.9(11) . . ?
C19 C20 H20 117.6 . . ?
C21 C20 H20 117.6 . . ?
C20 C21 C16 115.4(11) . . ?
C20 C21 H21 122.3 . . ?
C16 C21 H21 122.3 . . ?
N12 C22 C19 119.0(10) 8_666 . ?
N12 C22 H22 120.5 8_666 . ?
C19 C22 H22 120.5 . . ?
C1 N1 N2 107.4(3) . . ?
C1 N1 Fe1 120.6(3) . . ?
N2 N1 Fe1 130.5(3) . . ?
C2 N2 N1 106.8(4) . . ?
C1 N3 C2 105.4(3) . . ?
C1 N3 N4_1 134.2(4) . . ?
C2 N3 N4_1 120.3(4) . . ?
C1 N3 N4_2 111.6(6) . . ?
C2 N3 N4_2 142.8(6) . . ?
C11 N6 C12 106.3(3) . . ?
C11 N6 N5_1 118.7(4) . . ?
C12 N6 N5_1 134.7(4) . . ?
C11 N6 N5_2 137.1(7) . . ?
C12 N6 N5_2 116.6(7) . . ?
C12 N7 N8 109.0(3) . . ?
C12 N7 Fe2 121.5(3) . 9_666 ?
N8 N7 Fe2 127.8(2) . 9_666 ?
C13 N9 N10 106.8(3) . . ?
C13 N9 Fe3 120.4(3) . . ?
N10 N9 Fe3 129.8(3) . . ?
C11 N8 N7 106.1(3) . . ?
C14 N10 N9 106.1(4) . . ?
C13 N11 C14 105.4(3) . . ?
C13 N11 N12 120.1(3) . . ?
C14 N11 N12 134.5(3) . . ?
C22 N12 C15 25.3(6) 8_666 . ?
C22 N12 N11 118.3(6) 8_666 . ?
C15 N12 N11 116.6(6) . . ?
Fe1 F1 Fe2 180.0 . . ?
Fe2 F2 Fe3 180.0 . . ?
Fe3 F3 Fe1 180.0 . 13_576 ?
F1 Fe1 F3 180.0 . 13_575 ?
F1 Fe1 N1 96.30(9) . . ?
F3 Fe1 N1 83.70(9) 13_575 . ?
F1 Fe1 N1 96.30(9) . 2_665 ?
F3 Fe1 N1 83.70(9) 13_575 2_665 ?
N1 Fe1 N1 167.40(18) . 2_665 ?
F1 Fe1 N1 96.30(9) . 3_655 ?
F3 Fe1 N1 83.70(9) 13_575 3_655 ?
N1 Fe1 N1 89.31(2) . 3_655 ?
N1 Fe1 N1 89.31(2) 2_665 3_655 ?
F1 Fe1 N1 96.30(9) . 4_565 ?
F3 Fe1 N1 83.70(9) 13_575 4_565 ?
N1 Fe1 N1 89.31(2) . 4_565 ?
N1 Fe1 N1 89.31(2) 2_665 4_565 ?
N1 Fe1 N1 167.40(18) 3_655 4_565 ?
F2 Fe2 F1 180.0 . . ?
F2 Fe2 N7 95.46(9) . 9_666 ?
F1 Fe2 N7 84.54(9) . 9_666 ?
F2 Fe2 N7 95.46(9) . 10_666 ?
F1 Fe2 N7 84.54(9) . 10_666 ?
N7 Fe2 N7 169.08(18) 9_666 10_666 ?
F2 Fe2 N7 95.46(9) . 11_666 ?
F1 Fe2 N7 84.54(9) . 11_666 ?
N7 Fe2 N7 89.481(17) 9_666 11_666 ?
N7 Fe2 N7 89.481(17) 10_666 11_666 ?
F2 Fe2 N7 95.46(9) . 12_666 ?
F1 Fe2 N7 84.54(9) . 12_666 ?
N7 Fe2 N7 89.481(17) 9_666 12_666 ?
N7 Fe2 N7 89.481(17) 10_666 12_666 ?
N7 Fe2 N7 169.08(18) 11_666 12_666 ?
F3 Fe3 F2 180.0 . . ?
F3 Fe3 N9 97.19(8) . 2_665 ?
F2 Fe3 N9 82.81(8) . 2_665 ?
F3 Fe3 N9 97.19(8) . 4_565 ?
F2 Fe3 N9 82.81(8) . 4_565 ?
N9 Fe3 N9 89.10(2) 2_665 4_565 ?
F3 Fe3 N9 97.19(8) . 3_655 ?
F2 Fe3 N9 82.81(8) . 3_655 ?
N9 Fe3 N9 89.10(2) 2_665 3_655 ?
N9 Fe3 N9 165.62(16) 4_565 3_655 ?
F3 Fe3 N9 97.19(8) . . ?
F2 Fe3 N9 82.81(8) . . ?
N9 Fe3 N9 165.62(16) 2_665 . ?
N9 Fe3 N9 89.10(2) 4_565 . ?
N9 Fe3 N9 89.10(2) 3_655 . ?
F4_3 B1_3 F7_3 109.47(15) . . ?
F4_3 B1_3 F5_3 109.48(15) . . ?
F7_3 B1_3 F5_3 109.45(15) . . ?
F4_3 B1_3 F6_3 109.48(15) . . ?
F7_3 B1_3 F6_3 109.48(15) . . ?
F5_3 B1_3 F6_3 109.47(15) . . ?
F5_4 B1_4 F4_4 109.47(15) . . ?
F5_4 B1_4 F6_4 109.48(15) . . ?
F4_4 B1_4 F6_4 109.48(15) . . ?
F5_4 B1_4 F7_4 109.46(15) . . ?
F4_4 B1_4 F7_4 109.45(15) . . ?
F6_4 B1_4 F7_4 109.49(15) . . ?
F6_5 B1_5 F5_5 109.46(15) . . ?
F6_5 B1_5 F7_5 109.47(15) . . ?
F5_5 B1_5 F7_5 109.49(15) . . ?
F6_5 B1_5 F4_5 109.45(15) . . ?
F5_5 B1_5 F4_5 109.50(15) . . ?
F7_5 B1_5 F4_5 109.46(15) . . ?
F7_6 B1_6 F5_6 109.47(15) . . ?
F7_6 B1_6 F6_6 109.48(15) . . ?
F5_6 B1_6 F6_6 109.46(15) . . ?
F7_6 B1_6 F4_6 109.46(15) . . ?
F5_6 B1_6 F4_6 109.49(15) . . ?
F6_6 B1_6 F4_6 109.46(15) . . ?
F7_6 B1_6 B1_6 125.27(18) . 8_665 ?
F5_6 B1_6 B1_6 54.75(8) . 8_665 ?
F6_6 B1_6 B1_6 125.26(19) . 8_665 ?
F4_6 B1_6 B1_6 54.74(8) . 8_665 ?
B1_6 F4_6 B1_6 70.52(15) 8_665 . ?
B1_6 F5_6 B1_6 70.52(15) . 8_665 ?
F5_7 B1_7 F4_7 109.48(15) . . ?
F5_7 B1_7 F7_7 109.46(15) . . ?
F4_7 B1_7 F7_7 109.47(15) . . ?
F5_7 B1_7 F6_7 109.49(15) . . ?
F4_7 B1_7 F6_7 109.47(15) . . ?
F7_7 B1_7 F6_7 109.46(15) . . ?

_refine_diff_density_max         1.603
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.193

_shelxl_version_number           2014/6

