# Electronic Supplementary Material (ESI) for Chemical Science.
# 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. 
# 
#######################################################################

data_Fe-depe2_BArF4
_database_code_depnum_ccdc_archive 'CCDC 1451414'
_audit_update_record             
;
2017-07-27 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C20 H48 Fe P4'
_chemical_formula_sum            'C52 H60 B F24 Fe P4'
_chemical_formula_weight         1331.54

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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. 
;

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

_cell_length_a                   13.2989(3)
_cell_length_b                   13.2989(3)
_cell_length_c                   17.4417(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3084.75(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3131
_cell_measurement_theta_min      2.4730
_cell_measurement_theta_max      25.9500

_exptl_crystal_description       'tabular plates'
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_F_000             1358
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.454
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            11440
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.064
_diffrn_reflns_theta_max         29.134
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3536
_reflns_number_gt                2993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_max     0.923
_reflns_Friedel_fraction_full    0.999

_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,
_computing_cell_refinement       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0403P)²+3.1240P] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.03(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3536
_refine_ls_number_parameters     266
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.001
_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 1.0000 0.5000 0.2500 0.0360(3) Uani 1 4 d S T P . .
P1 P 0.8432(6) 0.5608(6) 0.2516(5) 0.0415(11) Uani 0.5 1 d D U P A -1
C2 C 0.7516(8) 0.4563(7) 0.2303(9) 0.088(5) Uani 0.5 1 d D . P A -1
H2A H 0.6876 0.4691 0.2577 0.105 Uiso 0.5 1 calc R U P A -1
H2B H 0.7371 0.4548 0.1746 0.105 Uiso 0.5 1 calc R U P A -1
C3 C 0.7945(7) 0.3549(7) 0.2553(10) 0.090(4) Uani 0.5 1 d D . P A -1
H3A H 0.7605 0.3003 0.2268 0.108 Uiso 0.5 1 calc R U P A -1
H3B H 0.7818 0.3448 0.3107 0.108 Uiso 0.5 1 calc R U P A -1
P4 P 0.9325(7) 0.3497(8) 0.2365(7) 0.064(2) Uani 0.5 1 d D U P A -1
C5 C 0.8052(18) 0.6024(14) 0.3467(8) 0.081(6) Uani 0.5 1 d D . P A -1
H5A H 0.8211 0.6748 0.3520 0.097 Uiso 0.5 1 calc R U P A -1
H5B H 0.7314 0.5949 0.3514 0.097 Uiso 0.5 1 calc R U P A -1
C6 C 0.855(3) 0.545(3) 0.4119(9) 0.114(12) Uani 0.5 1 d D . P A -1
H6A H 0.8313 0.5716 0.4611 0.171 Uiso 0.5 1 calc R U P A -1
H6B H 0.8385 0.4737 0.4080 0.171 Uiso 0.5 1 calc R U P A -1
H6C H 0.9284 0.5537 0.4086 0.171 Uiso 0.5 1 calc R U P A -1
C7 C 0.7971(7) 0.6582(7) 0.1880(6) 0.060(3) Uani 0.5 1 d D . P A -1
H7A H 0.8347 0.7208 0.1991 0.072 Uiso 0.5 1 calc R U P A -1
H7B H 0.8133 0.6383 0.1347 0.072 Uiso 0.5 1 calc R U P A -1
C8 C 0.6841(8) 0.6819(10) 0.1922(9) 0.083(4) Uani 0.5 1 d D . P A -1
H8A H 0.6679 0.7354 0.1555 0.125 Uiso 0.5 1 calc R U P A -1
H8B H 0.6454 0.6214 0.1796 0.125 Uiso 0.5 1 calc R U P A -1
H8C H 0.6669 0.7042 0.2441 0.125 Uiso 0.5 1 calc R U P A -1
C9 C 0.9684(10) 0.2442(7) 0.3006(7) 0.076(3) Uani 0.5 1 d D . P A -1
H9A H 1.0385 0.2247 0.2888 0.092 Uiso 0.5 1 calc R U P A -1
H9B H 0.9670 0.2687 0.3542 0.092 Uiso 0.5 1 calc R U P A -1
C10 C 0.9017(13) 0.1497(9) 0.2951(9) 0.106(5) Uani 0.5 1 d D . P A -1
H10A H 0.9265 0.0985 0.3309 0.160 Uiso 0.5 1 calc R U P A -1
H10B H 0.8322 0.1673 0.3083 0.160 Uiso 0.5 1 calc R U P A -1
H10C H 0.9040 0.1232 0.2427 0.160 Uiso 0.5 1 calc R U P A -1
C11 C 0.9384(16) 0.2948(19) 0.1410(8) 0.092(8) Uani 0.5 1 d D . P A -1
H11A H 1.0046 0.2618 0.1345 0.110 Uiso 0.5 1 calc R U P A -1
H11B H 0.8860 0.2423 0.1367 0.110 Uiso 0.5 1 calc R U P A -1
C12 C 0.924(3) 0.370(3) 0.0767(11) 0.108(11) Uani 0.5 1 d D . P A -1
H12A H 0.9279 0.3358 0.0272 0.162 Uiso 0.5 1 calc R U P A -1
H12B H 0.8578 0.4023 0.0818 0.162 Uiso 0.5 1 calc R U P A -1
H12C H 0.9765 0.4219 0.0796 0.162 Uiso 0.5 1 calc R U P A -1
B20 B 1.0000 0.5000 0.7500 0.0269(13) Uani 1 4 d S T P . .
C21 C 0.9149(2) 0.4553(3) 0.69184(19) 0.0286(7) Uani 1 1 d . . . . .
C22 C 0.9326(3) 0.3669(3) 0.6500(2) 0.0337(8) Uani 1 1 d . . . . .
H22A H 0.9922 0.3298 0.6599 0.040 Uiso 1 1 calc R U . . .
C23 C 0.8667(3) 0.3320(3) 0.5950(2) 0.0376(8) Uani 1 1 d . . . . .
C24 C 0.7793(3) 0.3843(3) 0.5783(2) 0.0409(9) Uani 1 1 d . . . . .
H24A H 0.7338 0.3607 0.5404 0.049 Uiso 1 1 calc R U . . .
C25 C 0.7602(3) 0.4723(3) 0.6188(2) 0.0389(9) Uani 1 1 d . . . . .
C26 C 0.8269(3) 0.5059(3) 0.6736(2) 0.0330(8) Uani 1 1 d . . . . .
H26A H 0.8120 0.5665 0.7001 0.040 Uiso 1 1 calc R U . . .
C27 C 0.8904(4) 0.2367(4) 0.5523(3) 0.0541(12) Uani 1 1 d D . . . .
F27A F 0.9724(4) 0.2423(4) 0.5133(3) 0.121(3) Uani 0.907(9) 1 d D . P B 1
F27B F 0.9032(5) 0.1603(3) 0.5992(3) 0.113(3) Uani 0.907(9) 1 d D . P B 1
F27C F 0.8199(4) 0.2072(4) 0.5065(4) 0.127(3) Uani 0.907(9) 1 d D . P B 1
F27D F 0.889(2) 0.257(2) 0.4799(10) 0.055(10) Uiso 0.093(9) 1 d D . P B 2
F27E F 0.9766(14) 0.198(2) 0.5672(15) 0.043(9) Uiso 0.093(9) 1 d D . P B 2
F27F F 0.8245(17) 0.1696(19) 0.5620(18) 0.054(10) Uiso 0.093(9) 1 d D . P B 2
C28 C 0.6675(4) 0.5322(4) 0.6025(3) 0.0640(14) Uani 1 1 d D . . . .
F28A F 0.6074(5) 0.4921(5) 0.5536(5) 0.138(4) Uani 0.872(9) 1 d D . P C 1
F28B F 0.6128(3) 0.5491(4) 0.6671(3) 0.103(2) Uani 0.872(9) 1 d D . P C 1
F28C F 0.6887(4) 0.6269(3) 0.5808(3) 0.0830(15) Uani 0.872(9) 1 d D U P C 1
F28D F 0.665(2) 0.5311(19) 0.5230(9) 0.071(9) Uiso 0.128(9) 1 d D . P C 2
F28E F 0.5905(17) 0.4811(18) 0.6214(16) 0.076(9) Uiso 0.128(9) 1 d D . P C 2
F28F F 0.667(2) 0.6210(15) 0.6239(17) 0.082(7) Uiso 0.128(9) 1 d D U P C 2


_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 P4 2.204(10) . ?
Fe1 P1 2.237(8) . ?
P1 C7 1.811(11) . ?
P1 C5 1.819(13) . ?
P1 C2 1.885(12) . ?
C2 C3 1.528(13) . ?
C3 P4 1.865(12) . ?
P4 C11 1.820(15) . ?
P4 C9 1.856(12) . ?
C5 C6 1.522(18) . ?
C7 C8 1.538(12) . ?
C9 C10 1.541(14) . ?
C11 C12 1.519(19) . ?
B20 C21 1.632(4) 7_566 ?
B20 C21 1.632(3) 8_646 ?
B20 C21 1.632(4) 2_765 ?
B20 C21 1.632(4) . ?
C21 C26 1.387(5) . ?
C21 C22 1.403(5) . ?
C22 C23 1.380(5) . ?
C23 C24 1.385(6) . ?
C23 C27 1.504(6) . ?
C24 C25 1.389(6) . ?
C25 C26 1.380(5) . ?
C25 C28 1.496(6) . ?
C27 F27F 1.261(16) . ?
C27 F27E 1.282(16) . ?
C27 F27A 1.288(6) . ?
C27 F27C 1.292(6) . ?
C27 F27D 1.292(16) . ?
C27 F27B 1.315(7) . ?
C28 F28F 1.238(16) . ?
C28 F28E 1.272(16) . ?
C28 F28A 1.284(6) . ?
C28 F28C 1.345(7) . ?
C28 F28B 1.359(7) . ?
C28 F28D 1.386(16) . ?

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
P4 Fe1 P1 87.1(5) . . ?
C7 P1 C5 104.3(7) . . ?
C7 P1 C2 100.8(6) . . ?
C5 P1 C2 102.9(8) . . ?
C7 P1 Fe1 124.5(5) . . ?
C5 P1 Fe1 112.4(8) . . ?
C2 P1 Fe1 109.5(5) . . ?
C3 C2 P1 110.7(7) . . ?
C2 C3 P4 110.5(7) . . ?
C11 P4 C9 103.7(9) . . ?
C11 P4 C3 102.6(8) . . ?
C9 P4 C3 100.1(7) . . ?
C11 P4 Fe1 116.3(10) . . ?
C9 P4 Fe1 121.1(6) . . ?
C3 P4 Fe1 110.4(6) . . ?
C6 C5 P1 114.1(14) . . ?
C8 C7 P1 116.6(8) . . ?
C10 C9 P4 115.6(10) . . ?
C12 C11 P4 113.9(14) . . ?
C21 B20 C21 103.1(2) 7_566 8_646 ?
C21 B20 C21 112.72(12) 7_566 2_765 ?
C21 B20 C21 112.72(12) 8_646 2_765 ?
C21 B20 C21 112.73(12) 7_566 . ?
C21 B20 C21 112.72(12) 8_646 . ?
C21 B20 C21 103.1(2) 2_765 . ?
C26 C21 C22 115.4(3) . . ?
C26 C21 B20 123.4(3) . . ?
C22 C21 B20 120.8(3) . . ?
C23 C22 C21 122.5(4) . . ?
C22 C23 C24 120.6(4) . . ?
C22 C23 C27 119.7(4) . . ?
C24 C23 C27 119.7(4) . . ?
C23 C24 C25 118.0(3) . . ?
C26 C25 C24 120.5(4) . . ?
C26 C25 C28 119.3(4) . . ?
C24 C25 C28 120.2(4) . . ?
C25 C26 C21 122.9(4) . . ?
F27F C27 F27E 108.2(14) . . ?
F27A C27 F27C 107.7(5) . . ?
F27F C27 F27D 105.9(15) . . ?
F27E C27 F27D 106.8(14) . . ?
F27A C27 F27B 105.3(5) . . ?
F27C C27 F27B 104.1(5) . . ?
F27F C27 C23 112.6(14) . . ?
F27E C27 C23 115.1(13) . . ?
F27A C27 C23 113.0(4) . . ?
F27C C27 C23 114.2(4) . . ?
F27D C27 C23 107.7(14) . . ?
F27B C27 C23 111.8(4) . . ?
F28F C28 F28E 115.0(16) . . ?
F28A C28 F28C 109.5(6) . . ?
F28A C28 F28B 106.6(6) . . ?
F28C C28 F28B 100.9(5) . . ?
F28F C28 F28D 108.2(15) . . ?
F28E C28 F28D 103.6(14) . . ?
F28F C28 C25 117.3(16) . . ?
F28E C28 C25 109.3(13) . . ?
F28A C28 C25 114.7(5) . . ?
F28C C28 C25 112.3(5) . . ?
F28B C28 C25 111.8(4) . . ?
F28D C28 C25 101.7(14) . . ?

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.045

