# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1446568'
_audit_update_record             
;
2016-02-27 deposited with the CCDC.
2016-03-14 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         ?
_chemical_formula_sum            'C50 H36 F18 Fe N O S4'
_chemical_formula_weight         1192.89

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'
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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.8972(5)
_cell_length_b                   13.8972(5)
_cell_length_c                   16.3109(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2728.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7261
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      25.32

_exptl_crystal_description       Prism-heXagonal
_exptl_crystal_colour            black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             1206
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.148
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   0.875
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   fine-focus,
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 0.83
_diffrn_reflns_number            16013
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.103
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_full        25.242
_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             3349
_reflns_number_gt                2698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 The trifluoromethyl groups and Methylgroup fo DMSO solvent are 
disordered and 
were refined in two major contributors, using a variable site 
occupatiuonal factor (SOF). 
The ratio of SOF was 0.55/0.45 for F1, F2, and F3, 0.46/0.54 for
F4, F5 and F6, and 0.60/0.40 for CH3 of DMSO.
249 restriction were applied; 61 restriction for SAME/SADI, 
26 for DELU and 162 for SIMU insrtructions.

 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       'APEX2 V2012 (Bruker, 2012)'
_computing_cell_refinement       'APEX2 V2012 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.27B  (Bruker, 2012)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'SHELXTL  (Sheldrick, 2013)'
_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)+(0.0593P)²+2.1122P] 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         3349
_refine_ls_number_parameters     302
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1281
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.156
_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
S1 S 0.43465(6) 0.57787(7) 0.68646(4) 0.0447(2) Uani 1 1 d . . . . .
Fe1 Fe 0.3333 0.6667 0.67854(4) 0.0336(2) Uani 1 3 d S T P . .
O1 O 0.3333 0.6667 0.8066(2) 0.0654(11) Uani 1 3 d S T P C .
N1 N 0.3333 0.6667 0.5396(2) 0.0268(7) Uani 1 3 d S T P . .
C1 C 0.5278(2) 0.6271(2) 0.60309(15) 0.0320(6) Uani 1 1 d . . . . .
C2 C 0.4907(2) 0.6272(2) 0.52294(15) 0.0295(5) Uani 1 1 d . . . . .
C3 C 0.5645(2) 0.6575(2) 0.45806(16) 0.0329(6) Uani 1 1 d . . . . .
H3 H 0.5385 0.6559 0.4052 0.039 Uiso 1 1 calc R U . . .
C4 C 0.6755(2) 0.6902(2) 0.46896(17) 0.0365(6) Uani 1 1 d . . . . .
C5 C 0.7112(2) 0.6910(2) 0.54859(17) 0.0377(6) Uani 1 1 d . . . . .
H5 H 0.7854 0.7125 0.5574 0.045 Uiso 1 1 calc R U . . .
C6 C 0.6403(2) 0.6608(2) 0.61523(16) 0.0337(6) Uani 1 1 d . . . . .
C7 C 0.3705(2) 0.5900(2) 0.50666(15) 0.0302(6) Uani 1 1 d . . . . .
H7A H 0.3580 0.5828 0.4479 0.036 Uiso 1 1 calc R U . . .
H7B H 0.3249 0.5171 0.5308 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7545(3) 0.7232(3) 0.3976(2) 0.0531(8) Uani 1 1 d . . . . .
H8A H 0.7227 0.6674 0.3557 0.080 Uiso 1 1 calc R U . . .
H8B H 0.8235 0.7302 0.4156 0.080 Uiso 1 1 calc R U . . .
H8C H 0.7677 0.7930 0.3760 0.080 Uiso 1 1 calc R U . . .
C9 C 0.6871(2) 0.6668(2) 0.69892(17) 0.0387(6) Uani 1 1 d . . . . .
C10 C 0.6901(3) 0.7408(3) 0.7570(2) 0.0597(9) Uani 1 1 d . . . . .
H10 H 0.6578 0.7839 0.7454 0.072 Uiso 1 1 calc R U . . .
C11 C 0.7404(3) 0.7513(3) 0.8320(2) 0.0679(11) Uani 1 1 d . . . . .
C12 C 0.7869(3) 0.6863(3) 0.8509(2) 0.0635(10) Uani 1 1 d . . . . .
H12 H 0.8202 0.6929 0.9016 0.076 Uiso 1 1 calc R U . . .
C13 C 0.7836(2) 0.6120(3) 0.79391(18) 0.0461(7) Uani 1 1 d . . . . .
C14 C 0.7351(2) 0.6029(2) 0.71812(17) 0.0397(6) Uani 1 1 d . . . . .
H14 H 0.7346 0.5533 0.6796 0.048 Uiso 1 1 calc R U . . .
C15 C 0.7463(6) 0.8344(5) 0.8936(3) 0.1176(17) Uani 1 1 d D U . . .
F1 F 0.7232(12) 0.9056(8) 0.8639(6) 0.160(3) Uani 0.549(8) 1 d D U P A 1
F2 F 0.6724(10) 0.7787(9) 0.9536(6) 0.185(4) Uani 0.549(8) 1 d D U P A 1
F3 F 0.8453(7) 0.8885(8) 0.9296(6) 0.146(3) Uani 0.549(8) 1 d D U P A 1
F1A F 0.8240(11) 0.9382(7) 0.8711(8) 0.179(4) Uani 0.451(8) 1 d D U P A 2
F2A F 0.6510(9) 0.8350(10) 0.8973(7) 0.140(3) Uani 0.451(8) 1 d D U P A 2
F3A F 0.7599(13) 0.8130(11) 0.9682(4) 0.152(3) Uani 0.451(8) 1 d D U P A 2
C16 C 0.8340(3) 0.5417(3) 0.81339(19) 0.0671(9) Uani 1 1 d D U . . .
F4 F 0.7903(10) 0.4503(8) 0.7691(7) 0.098(3) Uani 0.455(14) 1 d D U P B 1
F5 F 0.9402(5) 0.5959(7) 0.7927(8) 0.102(3) Uani 0.455(14) 1 d D U P B 1
F6 F 0.8301(12) 0.5137(12) 0.8889(3) 0.110(3) Uani 0.455(14) 1 d D U P B 1
F4A F 0.7744(8) 0.4687(7) 0.8720(5) 0.103(2) Uani 0.545(14) 1 d D U P B 2
F5A F 0.8380(10) 0.4822(9) 0.7531(4) 0.099(2) Uani 0.545(14) 1 d D U P B 2
F6A F 0.9333(6) 0.5970(6) 0.8451(9) 0.128(3) Uani 0.545(14) 1 d D U P B 2
S2 S 0.2805(3) 0.5742(3) 0.86120(18) 0.0820(9) Uani 0.3333 1 d D U P . .
C17 C 0.171(3) 0.572(4) 0.9147(19) 0.117(9) Uani 0.33(4) 1 d D U P C 1
H17A H 0.1383 0.5086 0.9505 0.140 Uiso 0.33(4) 1 calc R U P C 1
H17B H 0.1986 0.6386 0.9465 0.140 Uiso 0.33(4) 1 calc R U P C 1
H17C H 0.1163 0.5672 0.8766 0.140 Uiso 0.33(4) 1 calc R U P C 1
C17A C 0.228(5) 0.620(3) 0.939(2) 0.163(13) Uani 0.33(4) 1 d D U P C 2
H17D H 0.1911 0.5623 0.9789 0.195 Uiso 0.33(4) 1 calc R U P C 2
H17E H 0.2883 0.6842 0.9650 0.195 Uiso 0.33(4) 1 calc R U P C 2
H17F H 0.1767 0.6400 0.9165 0.195 Uiso 0.33(4) 1 calc R 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
S1 C1 1.763(3) . ?
S1 Fe1 2.2933(7) . ?
Fe1 O1 2.088(4) . ?
Fe1 N1 2.266(3) . ?
Fe1 S1 2.2933(7) 2_665 ?
Fe1 S1 2.2933(7) 3_565 ?
O1 S2 1.429(4) 3_565 ?
O1 S2 1.429(4) . ?
O1 S2 1.429(4) 2_665 ?
N1 C7 1.498(3) 3_565 ?
N1 C7 1.498(3) 2_665 ?
N1 C7 1.498(3) . ?
C1 C6 1.404(4) . ?
C1 C2 1.405(3) . ?
C2 C3 1.384(4) . ?
C2 C7 1.505(3) . ?
C3 C4 1.384(4) . ?
C4 C5 1.389(4) . ?
C4 C8 1.506(4) . ?
C5 C6 1.384(4) . ?
C6 C9 1.496(4) . ?
C9 C10 1.383(4) . ?
C9 C14 1.388(4) . ?
C10 C11 1.379(4) . ?
C11 C12 1.383(5) . ?
C11 C15 1.502(6) . ?
C12 C13 1.372(4) . ?
C13 C14 1.383(4) . ?
C13 C16 1.494(4) . ?
C15 F1 1.278(8) . ?
C15 F3A 1.288(9) . ?
C15 F2A 1.329(9) . ?
C15 F3 1.330(8) . ?
C15 F2 1.348(9) . ?
C15 F1A 1.351(10) . ?
C16 F6 1.285(5) . ?
C16 F5A 1.304(6) . ?
C16 F6A 1.304(5) . ?
C16 F4 1.316(6) . ?
C16 F5 1.322(5) . ?
C16 F4A 1.338(5) . ?
S2 C17A 1.737(12) . ?
S2 C17 1.739(12) . ?
S2 C17A 1.76(3) 2_665 ?
S2 S2 1.935(6) 3_565 ?
S2 S2 1.935(6) 2_665 ?
S2 C17 2.09(4) 2_665 ?

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
C1 S1 Fe1 106.08(9) . . ?
O1 Fe1 N1 180.0 . . ?
O1 Fe1 S1 86.77(2) . 2_665 ?
N1 Fe1 S1 93.23(2) . 2_665 ?
O1 Fe1 S1 86.77(2) . 3_565 ?
N1 Fe1 S1 93.23(2) . 3_565 ?
S1 Fe1 S1 119.689(5) 2_665 3_565 ?
O1 Fe1 S1 86.77(2) . . ?
N1 Fe1 S1 93.23(2) . . ?
S1 Fe1 S1 119.685(5) 2_665 . ?
S1 Fe1 S1 119.684(5) 3_565 . ?
S2 O1 S2 85.2(3) 3_565 . ?
S2 O1 S2 85.2(3) 3_565 2_665 ?
S2 O1 S2 85.2(3) . 2_665 ?
S2 O1 Fe1 128.58(18) 3_565 . ?
S2 O1 Fe1 128.58(18) . . ?
S2 O1 Fe1 128.58(18) 2_665 . ?
C7 N1 C7 107.86(17) 3_565 2_665 ?
C7 N1 C7 107.86(17) 3_565 . ?
C7 N1 C7 107.86(17) 2_665 . ?
C7 N1 Fe1 111.04(16) 3_565 . ?
C7 N1 Fe1 111.04(16) 2_665 . ?
C7 N1 Fe1 111.04(16) . . ?
C6 C1 C2 118.6(2) . . ?
C6 C1 S1 119.99(19) . . ?
C2 C1 S1 121.3(2) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C7 119.7(2) . . ?
C1 C2 C7 120.5(2) . . ?
C2 C3 C4 122.4(2) . . ?
C3 C4 C5 117.3(2) . . ?
C3 C4 C8 121.6(3) . . ?
C5 C4 C8 121.1(2) . . ?
C6 C5 C4 122.3(2) . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C9 118.4(2) . . ?
C1 C6 C9 121.8(2) . . ?
N1 C7 C2 114.28(19) . . ?
C10 C9 C14 118.4(3) . . ?
C10 C9 C6 121.2(2) . . ?
C14 C9 C6 120.3(2) . . ?
C11 C10 C9 120.8(3) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 C15 120.3(3) . . ?
C12 C11 C15 119.3(3) . . ?
C13 C12 C11 119.3(3) . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 C16 119.8(3) . . ?
C14 C13 C16 119.8(3) . . ?
C13 C14 C9 120.7(3) . . ?
F3A C15 F2A 102.7(8) . . ?
F1 C15 F3 108.6(7) . . ?
F1 C15 F2 107.8(8) . . ?
F3 C15 F2 106.3(7) . . ?
F3A C15 F1A 111.9(8) . . ?
F2A C15 F1A 105.8(8) . . ?
F1 C15 C11 113.7(5) . . ?
F3A C15 C11 114.4(6) . . ?
F2A C15 C11 111.3(6) . . ?
F3 C15 C11 111.9(5) . . ?
F2 C15 C11 108.1(6) . . ?
F1A C15 C11 110.2(7) . . ?
F5A C16 F6A 107.7(5) . . ?
F6 C16 F4 107.7(6) . . ?
F6 C16 F5 106.4(5) . . ?
F4 C16 F5 104.8(5) . . ?
F5A C16 F4A 105.3(5) . . ?
F6A C16 F4A 103.5(4) . . ?
F6 C16 C13 116.1(5) . . ?
F5A C16 C13 115.9(5) . . ?
F6A C16 C13 113.8(4) . . ?
F4 C16 C13 111.9(6) . . ?
F5 C16 C13 109.2(4) . . ?
F4A C16 C13 109.5(5) . . ?
O1 S2 C17A 104.2(11) . . ?
O1 S2 C17 112.3(12) . . ?
O1 S2 C17A 103.2(7) . 2_665 ?
C17A S2 C17A 78(5) . 2_665 ?
O1 S2 S2 47.39(13) . 3_565 ?
C17A S2 S2 56.9(11) . 3_565 ?
C17 S2 S2 69.2(14) . 3_565 ?
C17A S2 S2 93.9(18) 2_665 3_565 ?
O1 S2 S2 47.39(13) . 2_665 ?
C17A S2 S2 95(2) . 2_665 ?
C17 S2 S2 120.3(17) . 2_665 ?
C17A S2 S2 55.9(7) 2_665 2_665 ?
S2 S2 S2 59.999(2) 3_565 2_665 ?
O1 S2 C17 95.2(9) . 2_665 ?
C17 S2 C17 125(2) . 2_665 ?
S2 S2 C17 104.7(6) 3_565 2_665 ?
S2 S2 C17 51.0(7) 2_665 2_665 ?

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.052


####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1446569'
_audit_update_record             
;
2016-02-27 deposited with the CCDC.
2016-03-14 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         ?
_chemical_formula_sum            'C52 H38 F18 Fe N O S3'
_chemical_formula_weight         1186.86

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'
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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   14.0497(9)
_cell_length_b                   14.0497(9)
_cell_length_c                   16.3511(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2795.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      25.35

_exptl_crystal_description       Prism-Hexagonal
_exptl_crystal_colour            black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_F_000             1202
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.118
_exptl_absorpt_coefficient_mu    0.478
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   fine-focus,
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 0.83
_diffrn_reflns_number            23780
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.086
_diffrn_reflns_theta_max         25.413
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3369
_reflns_number_gt                2740
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 The trifluoromethyl groups and THF  are disordered and 
were refined in two major contributors, using a variable site 
occupational factor (SOF).
The ratio of SOF was 0.57/0.43 for F1, F2, and F3, 0.7/0.25 for
F4, F5 and F6, and 0.56/0.44 for CH2-CH2 of THF.
 
328 restriction were applied; 63 restriction for SAME/SADI, 
30 for DELU and 234 for SIMU insrtructions.
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
 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       'APEX2 V2012 (Bruker, 2012)'
_computing_cell_refinement       'APEX2 V2012 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.27B  (Bruker, 2012)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'SHELXTL  (Sheldrick, 2013)'
_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)+(0.0658P)²+2.4082P] 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         3369
_refine_ls_number_parameters     320
_refine_ls_number_restraints     327
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1377
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.176
_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 0.6667 0.3333 0.32355(4) 0.0415(2) Uani 1 3 d S T P C .
S1 S 0.56350(6) 0.41910(7) 0.31324(4) 0.0519(2) Uani 1 1 d . . . . .
N1 N 0.6667 0.3333 0.4599(2) 0.0315(7) Uani 1 3 d S T P . .
C1 C 0.4709(2) 0.3707(2) 0.39654(15) 0.0352(5) Uani 1 1 d . . . . .
C2 C 0.5086(2) 0.37198(19) 0.47625(15) 0.0329(5) Uani 1 1 d . . . . .
C3 C 0.4354(2) 0.3427(2) 0.54120(15) 0.0357(6) Uani 1 1 d . . . . .
H3 H 0.4612 0.3447 0.5939 0.043 Uiso 1 1 calc R U . . .
C4 C 0.3242(2) 0.3102(2) 0.53048(16) 0.0395(6) Uani 1 1 d . . . . .
C5 C 0.2883(2) 0.3087(2) 0.45145(17) 0.0418(6) Uani 1 1 d . . . . .
H5 H 0.2149 0.2875 0.4428 0.050 Uiso 1 1 calc R U . . .
C6 C 0.3584(2) 0.3377(2) 0.38477(16) 0.0381(6) Uani 1 1 d . . . . .
C7 C 0.6287(2) 0.40980(19) 0.49240(16) 0.0348(5) Uani 1 1 d . . . . .
H7A H 0.6734 0.4817 0.4679 0.042 Uiso 1 1 calc R U . . .
H7B H 0.6414 0.4178 0.5510 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2463(3) 0.2783(3) 0.6020(2) 0.0579(8) Uani 1 1 d . . . . .
H8A H 0.2371 0.2119 0.6262 0.087 Uiso 1 1 calc R U . . .
H8B H 0.1764 0.2665 0.5835 0.087 Uiso 1 1 calc R U . . .
H8C H 0.2759 0.3361 0.6420 0.087 Uiso 1 1 calc R U . . .
C9 C 0.3110(2) 0.3320(2) 0.30201(16) 0.0422(6) Uani 1 1 d . . . . .
C10 C 0.3076(3) 0.2581(3) 0.2434(2) 0.0635(9) Uani 1 1 d . . . . .
H10 H 0.3392 0.2150 0.2543 0.076 Uiso 1 1 calc R U . . .
C11 C 0.2570(4) 0.2493(3) 0.1690(2) 0.0755(11) Uani 1 1 d . . . . .
C12 C 0.2100(3) 0.3141(3) 0.1514(2) 0.0686(10) Uani 1 1 d . . . . .
H12 H 0.1760 0.3074 0.1012 0.082 Uiso 1 1 calc R U . . .
C13 C 0.2142(2) 0.3881(3) 0.20861(18) 0.0500(7) Uani 1 1 d . . . . .
C14 C 0.2636(2) 0.3963(2) 0.28354(17) 0.0433(6) Uani 1 1 d . . . . .
H14 H 0.2652 0.4455 0.3223 0.052 Uiso 1 1 calc R U . . .
C15 C 0.2510(6) 0.1707(7) 0.1042(5) 0.131(3) Uani 0.568(7) 1 d D U P A 1
F1 F 0.2836(9) 0.1020(7) 0.1310(5) 0.160(3) Uani 0.568(7) 1 d D U P A 1
F2 F 0.3158(8) 0.2250(6) 0.0411(5) 0.189(3) Uani 0.568(7) 1 d D U P A 1
F3 F 0.1492(6) 0.1077(7) 0.0759(6) 0.168(3) Uani 0.568(7) 1 d D U P A 1
C15A C 0.2508(8) 0.1631(9) 0.1105(6) 0.132(3) Uani 0.432(7) 1 d D U P A 2
F1A F 0.1820(10) 0.0610(7) 0.1357(6) 0.181(4) Uani 0.432(7) 1 d D U P A 2
F2A F 0.3491(8) 0.1722(10) 0.0996(7) 0.163(3) Uani 0.432(7) 1 d D U P A 2
F3A F 0.2178(12) 0.1746(10) 0.0366(5) 0.162(4) Uani 0.432(7) 1 d D U P A 2
C16 C 0.1624(3) 0.4575(3) 0.19008(19) 0.0698(9) Uani 1 1 d D U . . .
F4 F 0.1955(5) 0.5110(4) 0.1221(2) 0.1229(17) Uani 0.777(5) 1 d D U P B 1
F5 F 0.0547(3) 0.3994(3) 0.1895(4) 0.1314(18) Uani 0.777(5) 1 d D U P B 1
F6 F 0.1852(4) 0.5352(3) 0.2460(2) 0.1015(14) Uani 0.777(5) 1 d D U P B 1
F4A F 0.2358(9) 0.5589(7) 0.1732(10) 0.119(4) Uani 0.223(5) 1 d D U P B 2
F5A F 0.1022(11) 0.4216(10) 0.1221(6) 0.095(3) Uani 0.223(5) 1 d D U P B 2
F6A F 0.0987(12) 0.4579(14) 0.2456(6) 0.106(3) Uani 0.223(5) 1 d D U P B 2
O1 O 0.6667 0.3333 0.1878(2) 0.0780(12) Uani 1 3 d DS TU P . .
C17 C 0.717(2) 0.4346(10) 0.1410(7) 0.117(4) Uani 0.363(13) 1 d D U P C 1
H17A H 0.6877 0.4806 0.1596 0.140 Uiso 0.363(13) 1 calc R U P C 1
H17B H 0.7954 0.4740 0.1506 0.140 Uiso 0.363(13) 1 calc R U P C 1
C18 C 0.697(3) 0.4151(16) 0.0578(6) 0.129(5) Uani 0.363(13) 1 d D U P C 1
H18A H 0.7499 0.4756 0.0244 0.193 Uiso 0.363(13) 1 calc R U P C 1
H18B H 0.6227 0.3956 0.0424 0.193 Uiso 0.363(13) 1 calc R U P C 1
C17A C 0.648(3) 0.4076(17) 0.1362(8) 0.110(3) Uani 0.304(13) 1 d D U P C 2
H17C H 0.5822 0.4071 0.1537 0.132 Uiso 0.304(13) 1 calc R U P C 2
H17D H 0.7096 0.4820 0.1419 0.132 Uiso 0.304(13) 1 calc R U P C 2
C18A C 0.638(3) 0.376(3) 0.0549(7) 0.130(5) Uani 0.304(13) 1 d D U P C 2
H18D H 0.6450 0.4325 0.0175 0.195 Uiso 0.304(13) 1 calc R U P C 2
H18E H 0.5704 0.3075 0.0441 0.195 Uiso 0.304(13) 1 calc R 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 O1 2.220(4) . ?
Fe1 N1 2.229(3) . ?
Fe1 S1 2.3083(7) 2_655 ?
Fe1 S1 2.3083(7) 3_665 ?
Fe1 S1 2.3083(7) . ?
S1 C1 1.768(3) . ?
N1 C7 1.514(3) 3_665 ?
N1 C7 1.514(3) 2_655 ?
N1 C7 1.514(3) . ?
C1 C2 1.403(3) . ?
C1 C6 1.420(4) . ?
C2 C3 1.389(3) . ?
C2 C7 1.518(3) . ?
C3 C4 1.403(4) . ?
C4 C5 1.383(4) . ?
C4 C8 1.509(4) . ?
C5 C6 1.388(4) . ?
C6 C9 1.493(4) . ?
C9 C10 1.396(4) . ?
C9 C14 1.398(4) . ?
C10 C11 1.383(4) . ?
C11 C12 1.397(5) . ?
C11 C15 1.501(10) . ?
C11 C15A 1.511(12) . ?
C12 C13 1.378(5) . ?
C13 C14 1.384(4) . ?
C13 C16 1.510(4) . ?
C15 F1 1.332(7) . ?
C15 F3 1.333(7) . ?
C15 F2 1.334(7) . ?
C15A F3A 1.332(7) . ?
C15A F1A 1.333(7) . ?
C15A F2A 1.334(7) . ?
C16 F6A 1.278(6) . ?
C16 F4 1.292(4) . ?
C16 F4A 1.304(7) . ?
C16 F5 1.312(4) . ?
C16 F5A 1.334(6) . ?
C16 F6 1.335(4) . ?
O1 C17 1.450(9) . ?
O1 C17 1.450(9) 3_665 ?
O1 C17 1.450(9) 2_655 ?
O1 C17A 1.461(10) . ?
O1 C17A 1.462(10) 3_665 ?
O1 C17A 1.462(10) 2_655 ?
C17 C18 1.389(13) . ?
C18 C18 1.74(3) 3_665 ?
C17A C18A 1.387(13) . ?
C18A C18A 1.51(4) 3_665 ?

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 N1 180.0 . . ?
O1 Fe1 S1 85.81(2) . 2_655 ?
N1 Fe1 S1 94.19(2) . 2_655 ?
O1 Fe1 S1 85.81(2) . 3_665 ?
N1 Fe1 S1 94.19(2) . 3_665 ?
S1 Fe1 S1 119.472(6) 2_655 3_665 ?
O1 Fe1 S1 85.81(2) . . ?
N1 Fe1 S1 94.19(2) . . ?
S1 Fe1 S1 119.471(6) 2_655 . ?
S1 Fe1 S1 119.473(6) 3_665 . ?
C1 S1 Fe1 106.04(8) . . ?
C7 N1 C7 108.37(16) 3_665 2_655 ?
C7 N1 C7 108.37(16) 3_665 . ?
C7 N1 C7 108.37(16) 2_655 . ?
C7 N1 Fe1 110.55(16) 3_665 . ?
C7 N1 Fe1 110.55(16) 2_655 . ?
C7 N1 Fe1 110.55(16) . . ?
C2 C1 C6 118.7(2) . . ?
C2 C1 S1 120.69(19) . . ?
C6 C1 S1 120.40(19) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C7 119.9(2) . . ?
C1 C2 C7 120.8(2) . . ?
C2 C3 C4 122.6(2) . . ?
C5 C4 C3 117.4(2) . . ?
C5 C4 C8 121.0(2) . . ?
C3 C4 C8 121.6(2) . . ?
C4 C5 C6 121.9(2) . . ?
C5 C6 C1 120.1(2) . . ?
C5 C6 C9 117.6(2) . . ?
C1 C6 C9 122.3(2) . . ?
N1 C7 C2 114.51(18) . . ?
C10 C9 C14 118.8(2) . . ?
C10 C9 C6 120.7(2) . . ?
C14 C9 C6 120.4(2) . . ?
C11 C10 C9 119.7(3) . . ?
C10 C11 C12 120.8(3) . . ?
C10 C11 C15 121.6(4) . . ?
C12 C11 C15 117.6(4) . . ?
C10 C11 C15A 116.8(4) . . ?
C12 C11 C15A 122.4(4) . . ?
C13 C12 C11 119.7(3) . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 C16 119.9(3) . . ?
C14 C13 C16 120.5(3) . . ?
C13 C14 C9 121.2(3) . . ?
F1 C15 F3 106.1(6) . . ?
F1 C15 F2 106.6(7) . . ?
F3 C15 F2 108.0(7) . . ?
F1 C15 C11 112.8(6) . . ?
F3 C15 C11 112.4(7) . . ?
F2 C15 C11 110.7(6) . . ?
F3A C15A F1A 107.6(7) . . ?
F3A C15A F2A 105.9(7) . . ?
F1A C15A F2A 107.7(7) . . ?
F3A C15A C11 111.1(8) . . ?
F1A C15A C11 112.8(8) . . ?
F2A C15A C11 111.4(8) . . ?
F6A C16 F4A 108.6(6) . . ?
F4 C16 F5 108.8(4) . . ?
F6A C16 F5A 106.3(6) . . ?
F4A C16 F5A 104.0(6) . . ?
F4 C16 F6 104.2(3) . . ?
F5 C16 F6 104.1(3) . . ?
F6A C16 C13 115.2(6) . . ?
F4 C16 C13 113.5(3) . . ?
F4A C16 C13 112.0(7) . . ?
F5 C16 C13 112.3(3) . . ?
F5A C16 C13 110.0(5) . . ?
F6 C16 C13 113.3(3) . . ?
C17 O1 C17 94.8(8) . 3_665 ?
C17 O1 C17 94.8(8) . 2_655 ?
C17 O1 C17 94.8(8) 3_665 2_655 ?
C17A O1 C17A 90.0(9) . 3_665 ?
C17A O1 C17A 90.0(9) . 2_655 ?
C17A O1 C17A 90.0(9) 3_665 2_655 ?
C17 O1 Fe1 121.8(6) . . ?
C17 O1 Fe1 121.8(6) 3_665 . ?
C17 O1 Fe1 121.8(6) 2_655 . ?
C17A O1 Fe1 125.3(7) . . ?
C17A O1 Fe1 125.3(7) 3_665 . ?
C17A O1 Fe1 125.3(7) 2_655 . ?
C18 C17 O1 111.8(9) . . ?
C17 C18 C18 94.1(14) . 3_665 ?
C18A C17A O1 110.5(10) . . ?
C17A C18A C18A 95.0(16) . 3_665 ?

_refine_diff_density_max         0.704
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.051



####################################################################### 
# 
# 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_amd-161bb3
_database_code_depnum_ccdc_archive 'CCDC 1446571'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H32 F18 Fe N O4'
_chemical_formula_sum            'C48 H32 F18 Fe N O4'
_chemical_formula_weight         1084.59

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.3142(11)
_cell_length_b                   14.3683(9)
_cell_length_c                   16.5139(16)
_cell_angle_alpha                65.449(8)
_cell_angle_beta                 66.267(8)
_cell_angle_gamma                61.594(7)
_cell_volume                     2626.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    4693
_cell_measurement_theta_min      3.4279
_cell_measurement_theta_max      29.5587

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_F_000             1094
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 -1 13 0.0908
-14 -16 0 0.1201
-15 1 -13 0.0908
14 16 0 0.1201
0 13 17 0.0478
0 -13 -17 0.0478

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_T_max  0.965
_shelx_estimated_absorpt_T_min   0.902
_shelx_estimated_absorpt_T_max   0.966

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.4685
_diffrn_orient_matrix_ub_11      -0.0220084
_diffrn_orient_matrix_ub_12      0.0153706
_diffrn_orient_matrix_ub_13      -0.0372561
_diffrn_orient_matrix_ub_21      0.0476483
_diffrn_orient_matrix_ub_22      -0.0403481
_diffrn_orient_matrix_ub_23      -0.0190926
_diffrn_orient_matrix_ub_31      -0.0253565
_diffrn_orient_matrix_ub_32      -0.0393821
_diffrn_orient_matrix_ub_33      0.0251948
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.3557
_diffrn_reflns_number            22532
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.832
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.832
_reflns_Friedel_coverage         0
_reflns_number_total             12225
_reflns_number_gt                5772
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    
;
      'SHELXS-2014 (Sheldrick, 2008)'
      G. M. Sheldrick, Acta Crystallogr., Sect. A: 
      Found. Crystallogr., 2008, 64, 112-122.
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
          'Ortep-3 for Windows (Farrugia, 1997)'
      L. J. Farrugia, J. Appl. Crystallogr., 1997, 30, 565.
;
_computing_publication_material  
;	
        'WinGX publication routines (Farrugia, 1999)'				 
	L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.
;


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         12225
_refine_ls_number_parameters     653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.179
_refine_ls_R_factor_gt           0.129
_refine_ls_wR_factor_ref         0.398
_refine_ls_wR_factor_gt          0.3601
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.109

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.1307(6) 0.3015(7) 0.0495(5) 0.076(2) Uani 1 1 d . . . . .
C2 C 0.1924(6) 0.3047(7) -0.0400(5) 0.080(2) Uani 1 1 d . . . . .
C3 C 0.3182(6) 0.2733(7) -0.0645(5) 0.076(2) Uani 1 1 d . . . . .
H3A H 0.3535 0.1941 -0.0346 0.091 Uiso 1 1 calc R U . . .
H3B H 0.3485 0.2858 -0.132 0.091 Uiso 1 1 calc R U . . .
C4 C 0.2821(6) 0.4585(6) -0.0659(5) 0.0711(18) Uani 1 1 d . . . . .
H4A H 0.2026 0.4731 -0.0382 0.085 Uiso 1 1 calc R U . . .
H4B H 0.2951 0.4785 -0.1335 0.085 Uiso 1 1 calc R U . . .
C5 C 0.3123(7) 0.5323(6) -0.0435(4) 0.0723(19) Uani 1 1 d . . . . .
C6 C 0.3111(7) 0.5130(6) 0.0497(4) 0.076(2) Uani 1 1 d . . . . .
C7 C 0.3139(4) 0.5918(5) 0.0725(4) 0.0493(13) Uani 1 1 d . . . . .
C8 C 0.3019(4) 0.5812(5) 0.1702(4) 0.0497(13) Uani 1 1 d . . . . .
C9 C 0.2189(5) 0.6637(5) 0.2121(5) 0.0585(15) Uani 1 1 d . . . . .
H9 H 0.1713 0.727 0.1781 0.07 Uiso 1 1 calc R U . . .
C10 C 0.2064(5) 0.6533(6) 0.3018(5) 0.0629(16) Uani 1 1 d . . . . .
C11 C 0.1118(7) 0.7422(9) 0.3459(6) 0.088(2) Uani 1 1 d . . . . .
C12 C 0.2761(6) 0.5669(7) 0.3505(5) 0.077(2) Uani 1 1 d . . . . .
H12 H 0.2686 0.5621 0.4118 0.093 Uiso 1 1 calc R U . . .
C13 C 0.3581(6) 0.4857(6) 0.3104(4) 0.0701(17) Uani 1 1 d . . . . .
C14 C 0.4435(11) 0.3969(10) 0.3595(6) 0.114(3) Uani 1 1 d . . . . .
C15 C 0.3714(5) 0.4925(5) 0.2193(4) 0.0598(15) Uani 1 1 d . . . . .
H15 H 0.4281 0.4359 0.1923 0.072 Uiso 1 1 calc R U . . .
C16 C 0.3246(5) 0.6870(5) 0.0021(4) 0.0574(14) Uani 1 1 d . . . . .
H16 H 0.325 0.7428 0.0184 0.069 Uiso 1 1 calc R U . . .
C17 C 0.3342(5) 0.7039(5) -0.0863(4) 0.0574(14) Uani 1 1 d . . . . .
C18 C 0.3327(5) 0.6247(5) -0.1104(4) 0.0643(16) Uani 1 1 d . . . . .
H18 H 0.3456 0.6325 -0.1736 0.077 Uiso 1 1 calc R U . . .
C19 C 0.3549(8) 0.8036(6) -0.1608(5) 0.089(2) Uani 1 1 d . . . . .
H19A H 0.3779 0.7918 -0.2214 0.134 Uiso 1 1 calc R U . . .
H19B H 0.4129 0.8143 -0.1527 0.134 Uiso 1 1 calc R U . . .
H19C H 0.2873 0.869 -0.1566 0.134 Uiso 1 1 calc R U . . .
C20 C 0.4658(6) 0.3170(7) -0.0662(5) 0.080(2) Uani 1 1 d . . . . .
H20A H 0.4827 0.3562 -0.04 0.096 Uiso 1 1 calc R U . . .
H20B H 0.4854 0.3468 -0.1341 0.096 Uiso 1 1 calc R U . . .
C21 C 0.5367(6) 0.1956(6) -0.0408(5) 0.0752(19) Uani 1 1 d . . . . .
C22 C 0.5173(6) 0.1319(6) 0.0495(4) 0.0690(17) Uani 1 1 d . . . . .
C23 C 0.5970(5) 0.0249(5) 0.0736(4) 0.0556(14) Uani 1 1 d . . . . .
C24 C 0.5865(5) -0.0426(5) 0.1704(5) 0.0625(16) Uani 1 1 d . . . . .
C25 C 0.6721(5) -0.0875(5) 0.2102(5) 0.0625(16) Uani 1 1 d . . . . .
H25 H 0.7374 -0.073 0.1748 0.075 Uiso 1 1 calc R U . . .
C26 C 0.6660(6) -0.1531(6) 0.3002(5) 0.0717(18) Uani 1 1 d . . . . .
C27 C 0.7597(10) -0.1952(9) 0.3443(7) 0.102(3) Uani 1 1 d . . . . .
C28 C 0.5776(7) -0.1831(7) 0.3498(6) 0.087(2) Uani 1 1 d . . . . .
H28 H 0.5755 -0.2322 0.4101 0.104 Uiso 1 1 calc R U . . .
C29 C 0.4897(7) -0.1407(8) 0.3110(5) 0.088(2) Uani 1 1 d . . . . .
C30 C 0.3960(9) -0.1760(12) 0.3656(8) 0.128(4) Uani 1 1 d . . . . .
C31 C 0.4935(6) -0.0683(6) 0.2216(5) 0.0748(19) Uani 1 1 d . . . . .
H31 H 0.4326 -0.037 0.1963 0.09 Uiso 1 1 calc R U . . .
C32 C 0.6866(5) -0.0115(6) 0.0049(5) 0.0639(16) Uani 1 1 d . . . . .
H32 H 0.7433 -0.0803 0.0215 0.077 Uiso 1 1 calc R U . . .
C33 C 0.6980(5) 0.0459(6) -0.0854(5) 0.0692(18) Uani 1 1 d . . . . .
C34 C 0.6235(6) 0.1476(6) -0.1081(5) 0.0760(19) Uani 1 1 d . . . . .
H34 H 0.6298 0.1881 -0.1712 0.091 Uiso 1 1 calc R U . . .
C35 C 0.7982(7) -0.0035(8) -0.1599(6) 0.101(3) Uani 1 1 d . . . . .
H35A H 0.7832 -0.0521 -0.1765 0.152 Uiso 1 1 calc R U . . .
H35B H 0.8634 -0.0457 -0.1356 0.152 Uiso 1 1 calc R U . . .
H35C H 0.8113 0.0563 -0.2146 0.152 Uiso 1 1 calc R U . . .
C36 C 0.1420(6) 0.3320(6) -0.1065(6) 0.0762(19) Uani 1 1 d . . . . .
H36 H 0.1811 0.3469 -0.1695 0.091 Uiso 1 1 calc R U . . .
C37 C 0.0362(6) 0.3379(6) -0.0834(6) 0.0754(19) Uani 1 1 d . . . . .
C38 C -0.0201(6) 0.3251(6) 0.0062(6) 0.077(2) Uani 1 1 d . . . . .
H38 H -0.0927 0.3274 0.0226 0.092 Uiso 1 1 calc R U . . .
C39 C 0.0218(5) 0.3088(5) 0.0756(5) 0.0684(19) Uani 1 1 d . . . . .
C40 C -0.0439(5) 0.2930(5) 0.1727(5) 0.0666(18) Uani 1 1 d . . . . .
C41 C -0.0854(6) 0.3679(6) 0.2202(5) 0.0682(17) Uani 1 1 d . . . . .
H41 H -0.0666 0.4314 0.1924 0.082 Uiso 1 1 calc R U . . .
C42 C -0.1564(6) 0.3536(6) 0.3105(5) 0.0751(19) Uani 1 1 d . . . . .
C43 C -0.2040(13) 0.4405(12) 0.3553(7) 0.130(4) Uani 1 1 d . . . . .
C44 C -0.1787(7) 0.2587(7) 0.3524(6) 0.096(3) Uani 1 1 d . . . . .
H44 H -0.217 0.2425 0.4156 0.116 Uiso 1 1 calc R U . . .
C45 C -0.1443(7) 0.1858(6) 0.3007(6) 0.086(2) Uani 1 1 d . . . . .
C46 C -0.1734(10) 0.0852(10) 0.3462(7) 0.110(3) Uani 1 1 d . . . . .
C47 C -0.0791(6) 0.2036(6) 0.2121(6) 0.082(2) Uani 1 1 d . . . . .
H47 H -0.0576 0.1551 0.177 0.098 Uiso 1 1 calc R U . . .
C48 C -0.0132(9) 0.3638(11) -0.1603(8) 0.126(4) Uani 1 1 d . . . . .
H48A H -0.0883 0.3646 -0.1336 0.19 Uiso 1 1 calc R U . . .
H48B H 0.0315 0.3074 -0.1935 0.19 Uiso 1 1 calc R U . . .
H48C H -0.0147 0.4361 -0.203 0.19 Uiso 1 1 calc R U . . .
F1 F 0.0360(6) 0.7016(7) 0.4059(6) 0.185(4) Uani 1 1 d . . . . .
F2 F 0.0609(5) 0.8269(6) 0.2896(5) 0.131(2) Uani 1 1 d . . . . .
F3 F 0.1412(5) 0.7757(6) 0.3879(6) 0.158(3) Uani 1 1 d . . . . .
F4 F 0.4708(9) 0.3024(7) 0.3479(6) 0.200(4) Uani 1 1 d . . . . .
F5 F 0.5406(7) 0.4065(10) 0.3323(6) 0.194(4) Uani 1 1 d . . . . .
F6 F 0.4156(7) 0.3921(6) 0.4477(4) 0.173(3) Uani 1 1 d . . . . .
F7 F 0.7953(6) -0.3032(5) 0.3789(5) 0.150(3) Uani 1 1 d . . . . .
F8 F 0.7332(7) -0.1467(7) 0.4032(6) 0.158(3) Uani 1 1 d . . . . .
F9 F 0.8475(5) -0.1761(7) 0.2836(5) 0.152(3) Uani 1 1 d . . . . .
F10 F 0.2997(6) -0.0901(9) 0.3532(6) 0.210(5) Uani 1 1 d . . . . .
F11 F 0.3985(10) -0.2542(12) 0.3418(8) 0.247(6) Uani 1 1 d . . . . .
F12 F 0.3822(6) -0.2104(9) 0.4521(5) 0.194(4) Uani 1 1 d . . . . .
F13 F -0.2740(8) 0.5354(7) 0.3128(6) 0.181(4) Uani 1 1 d . . . . .
F14 F -0.1277(9) 0.4708(10) 0.3528(9) 0.233(5) Uani 1 1 d . . . . .
F15 F -0.2684(10) 0.4166(7) 0.4399(4) 0.213(5) Uani 1 1 d . . . . .
F16 F -0.1501(7) 0.0304(6) 0.2877(6) 0.158(3) Uani 1 1 d . . . . .
F17 F -0.2831(6) 0.1147(6) 0.3780(6) 0.160(3) Uani 1 1 d . . . . .
F18 F -0.1209(9) 0.0138(6) 0.4101(6) 0.183(3) Uani 1 1 d . . . . .
Fe1 Fe 0.30048(6) 0.29161(6) 0.11652(5) 0.0489(3) Uani 1 1 d . . . . .
N1 N 0.3434(3) 0.3411(3) -0.0330(3) 0.0416(9) Uani 1 1 d . . . . .
O1 O 0.1761(5) 0.2769(6) 0.1200(4) 0.107(2) Uani 1 1 d . . . . .
O2 O 0.2908(5) 0.4254(4) 0.1154(3) 0.0864(16) Uani 1 1 d . . . . .
O1W O 0.2613(5) 0.2475(5) 0.2505(3) 0.1026(19) Uani 1 1 d . . . . .
H1WA H 0.1927 0.2779 0.2894 0.154 Uiso 1 1 d R U . . .
H1WB H 0.3074 0.1916 0.2886 0.154 Uiso 1 1 d R U . . .
O3 O 0.4335(5) 0.1704(4) 0.1146(3) 0.0912(16) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C2 1.376(10) . ?
C1 O1 1.397(9) . ?
C1 C39 1.402(9) . ?
C2 C36 1.375(10) . ?
C2 C3 1.550(10) . ?
C3 N1 1.503(8) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 N1 1.457(9) . ?
C4 C5 1.529(9) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C18 1.400(8) . ?
C5 C6 1.442(9) . ?
C6 O2 1.344(7) . ?
C6 C7 1.354(8) . ?
C7 C16 1.407(8) . ?
C7 C8 1.501(8) . ?
C8 C15 1.362(8) . ?
C8 C9 1.406(8) . ?
C9 C10 1.369(9) . ?
C9 H9 0.95 . ?
C10 C12 1.350(11) . ?
C10 C11 1.526(11) . ?
C11 F3 1.263(10) . ?
C11 F2 1.278(11) . ?
C11 F1 1.325(10) . ?
C12 C13 1.375(10) . ?
C12 H12 0.95 . ?
C13 C15 1.405(9) . ?
C13 C14 1.494(14) . ?
C14 F4 1.298(13) . ?
C14 F6 1.327(10) . ?
C14 F5 1.335(14) . ?
C15 H15 0.95 . ?
C16 C17 1.335(9) . ?
C16 H16 0.95 . ?
C17 C18 1.364(8) . ?
C17 C19 1.517(9) . ?
C18 H18 0.95 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 N1 1.515(8) . ?
C20 C21 1.517(11) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.384(9) . ?
C21 C34 1.401(10) . ?
C22 O3 1.313(8) . ?
C22 C23 1.419(9) . ?
C23 C32 1.374(9) . ?
C23 C24 1.475(9) . ?
C24 C25 1.376(9) . ?
C24 C31 1.387(9) . ?
C25 C26 1.383(10) . ?
C25 H25 0.95 . ?
C26 C28 1.361(10) . ?
C26 C27 1.531(12) . ?
C27 F8 1.261(11) . ?
C27 F7 1.318(11) . ?
C27 F9 1.321(12) . ?
C28 C29 1.400(11) . ?
C28 H28 0.95 . ?
C29 C31 1.407(10) . ?
C29 C30 1.471(12) . ?
C30 F12 1.266(13) . ?
C30 F11 1.318(18) . ?
C30 F10 1.365(14) . ?
C31 H31 0.95 . ?
C32 C33 1.356(10) . ?
C32 H32 0.95 . ?
C33 C34 1.341(10) . ?
C33 C35 1.553(10) . ?
C34 H34 0.95 . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C36 C37 1.373(10) . ?
C36 H36 0.95 . ?
C37 C38 1.352(11) . ?
C37 C48 1.527(12) . ?
C38 C39 1.388(11) . ?
C38 H38 0.95 . ?
C39 C40 1.481(10) . ?
C40 C41 1.357(9) . ?
C40 C47 1.409(9) . ?
C41 C42 1.423(10) . ?
C41 H41 0.95 . ?
C42 C44 1.376(11) . ?
C42 C43 1.457(16) . ?
C43 F15 1.335(13) . ?
C43 F14 1.336(15) . ?
C43 F13 1.351(15) . ?
C44 C45 1.409(12) . ?
C44 H44 0.95 . ?
C45 C47 1.376(11) . ?
C45 C46 1.499(13) . ?
C46 F18 1.318(13) . ?
C46 F16 1.337(13) . ?
C46 F17 1.345(12) . ?
C47 H47 0.95 . ?
C48 H48A 0.98 . ?
C48 H48B 0.98 . ?
C48 H48C 0.98 . ?
Fe1 O2 1.853(4) . ?
Fe1 O1 1.867(5) . ?
Fe1 O3 1.871(5) . ?
Fe1 O1W 1.946(4) . ?
Fe1 N1 2.171(4) . ?
O1W H1WA 0.9409 . ?
O1W H1WB 0.9409 . ?

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
C2 C1 O1 122.4(6) . . ?
C2 C1 C39 120.3(7) . . ?
O1 C1 C39 116.8(6) . . ?
C36 C2 C1 119.4(7) . . ?
C36 C2 C3 120.4(6) . . ?
C1 C2 C3 120.2(7) . . ?
N1 C3 C2 110.4(6) . . ?
N1 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 C5 114.0(6) . . ?
N1 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
N1 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.6 . . ?
C18 C5 C6 118.4(6) . . ?
C18 C5 C4 121.4(6) . . ?
C6 C5 C4 120.0(5) . . ?
O2 C6 C7 120.5(6) . . ?
O2 C6 C5 119.5(6) . . ?
C7 C6 C5 119.2(5) . . ?
C6 C7 C16 118.1(5) . . ?
C6 C7 C8 121.7(5) . . ?
C16 C7 C8 120.2(5) . . ?
C15 C8 C9 118.9(5) . . ?
C15 C8 C7 120.8(5) . . ?
C9 C8 C7 120.2(6) . . ?
C10 C9 C8 120.4(6) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C12 C10 C9 121.1(6) . . ?
C12 C10 C11 120.3(7) . . ?
C9 C10 C11 118.5(7) . . ?
F3 C11 F2 107.4(9) . . ?
F3 C11 F1 108.1(8) . . ?
F2 C11 F1 104.6(9) . . ?
F3 C11 C10 113.0(8) . . ?
F2 C11 C10 114.4(7) . . ?
F1 C11 C10 108.8(7) . . ?
C10 C12 C13 119.2(6) . . ?
C10 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C15 121.0(7) . . ?
C12 C13 C14 119.4(7) . . ?
C15 C13 C14 119.0(6) . . ?
F4 C14 F6 112.3(10) . . ?
F4 C14 F5 102.2(11) . . ?
F6 C14 F5 100.0(11) . . ?
F4 C14 C13 111.4(10) . . ?
F6 C14 C13 113.0(9) . . ?
F5 C14 C13 117.2(10) . . ?
C8 C15 C13 119.3(6) . . ?
C8 C15 H15 120.4 . . ?
C13 C15 H15 120.4 . . ?
C17 C16 C7 124.2(5) . . ?
C17 C16 H16 117.9 . . ?
C7 C16 H16 117.9 . . ?
C16 C17 C18 118.4(5) . . ?
C16 C17 C19 122.2(6) . . ?
C18 C17 C19 119.3(6) . . ?
C17 C18 C5 121.0(6) . . ?
C17 C18 H18 119.5 . . ?
C5 C18 H18 119.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 C21 114.2(6) . . ?
N1 C20 H20A 108.7 . . ?
C21 C20 H20A 108.7 . . ?
N1 C20 H20B 108.7 . . ?
C21 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C22 C21 C34 119.6(7) . . ?
C22 C21 C20 120.0(7) . . ?
C34 C21 C20 120.4(6) . . ?
O3 C22 C21 122.4(7) . . ?
O3 C22 C23 119.2(6) . . ?
C21 C22 C23 118.1(6) . . ?
C32 C23 C22 118.0(6) . . ?
C32 C23 C24 121.2(6) . . ?
C22 C23 C24 120.7(6) . . ?
C25 C24 C31 118.4(6) . . ?
C25 C24 C23 120.4(5) . . ?
C31 C24 C23 121.1(6) . . ?
C24 C25 C26 122.0(6) . . ?
C24 C25 H25 119 . . ?
C26 C25 H25 119 . . ?
C28 C26 C25 120.2(7) . . ?
C28 C26 C27 119.2(7) . . ?
C25 C26 C27 120.6(7) . . ?
F8 C27 F7 111.9(9) . . ?
F8 C27 F9 104.9(9) . . ?
F7 C27 F9 104.1(10) . . ?
F8 C27 C26 111.6(9) . . ?
F7 C27 C26 111.7(8) . . ?
F9 C27 C26 112.2(7) . . ?
C26 C28 C29 119.3(7) . . ?
C26 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C28 C29 C31 120.0(7) . . ?
C28 C29 C30 118.0(7) . . ?
C31 C29 C30 121.9(8) . . ?
F12 C30 F11 105.8(11) . . ?
F12 C30 F10 104.3(11) . . ?
F11 C30 F10 105.8(12) . . ?
F12 C30 C29 116.7(11) . . ?
F11 C30 C29 113.1(12) . . ?
F10 C30 C29 110.3(9) . . ?
C24 C31 C29 119.9(7) . . ?
C24 C31 H31 120.1 . . ?
C29 C31 H31 120.1 . . ?
C33 C32 C23 123.3(6) . . ?
C33 C32 H32 118.3 . . ?
C23 C32 H32 118.3 . . ?
C34 C33 C32 118.5(6) . . ?
C34 C33 C35 121.0(7) . . ?
C32 C33 C35 120.5(7) . . ?
C33 C34 C21 121.4(7) . . ?
C33 C34 H34 119.3 . . ?
C21 C34 H34 119.3 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C2 121.2(7) . . ?
C37 C36 H36 119.4 . . ?
C2 C36 H36 119.4 . . ?
C38 C37 C36 117.8(7) . . ?
C38 C37 C48 123.5(7) . . ?
C36 C37 C48 118.6(7) . . ?
C37 C38 C39 123.9(6) . . ?
C37 C38 H38 118.1 . . ?
C39 C38 H38 118.1 . . ?
C38 C39 C1 116.5(7) . . ?
C38 C39 C40 120.9(6) . . ?
C1 C39 C40 122.5(7) . . ?
C41 C40 C47 118.4(6) . . ?
C41 C40 C39 123.8(5) . . ?
C47 C40 C39 117.1(6) . . ?
C40 C41 C42 121.7(6) . . ?
C40 C41 H41 119.1 . . ?
C42 C41 H41 119.1 . . ?
C44 C42 C41 118.9(7) . . ?
C44 C42 C43 122.1(8) . . ?
C41 C42 C43 119.0(7) . . ?
F15 C43 F14 113.0(12) . . ?
F15 C43 F13 101.9(12) . . ?
F14 C43 F13 103.2(12) . . ?
F15 C43 C42 112.9(10) . . ?
F14 C43 C42 111.8(12) . . ?
F13 C43 C42 113.3(10) . . ?
C42 C44 C45 119.4(7) . . ?
C42 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C47 C45 C44 120.1(7) . . ?
C47 C45 C46 121.1(8) . . ?
C44 C45 C46 118.7(8) . . ?
F18 C46 F16 106.2(11) . . ?
F18 C46 F17 112.9(9) . . ?
F16 C46 F17 101.9(10) . . ?
F18 C46 C45 112.1(10) . . ?
F16 C46 C45 113.4(7) . . ?
F17 C46 C45 109.9(9) . . ?
C45 C47 C40 120.8(7) . . ?
C45 C47 H47 119.6 . . ?
C40 C47 H47 119.6 . . ?
C37 C48 H48A 109.5 . . ?
C37 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C37 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O2 Fe1 O1 119.8(3) . . ?
O2 Fe1 O3 120.9(3) . . ?
O1 Fe1 O3 119.3(3) . . ?
O2 Fe1 O1W 90.0(2) . . ?
O1 Fe1 O1W 89.3(3) . . ?
O3 Fe1 O1W 90.5(2) . . ?
O2 Fe1 N1 90.03(18) . . ?
O1 Fe1 N1 90.5(2) . . ?
O3 Fe1 N1 89.68(19) . . ?
O1W Fe1 N1 179.7(2) . . ?
C4 N1 C3 111.6(5) . . ?
C4 N1 C20 110.4(5) . . ?
C3 N1 C20 109.2(5) . . ?
C4 N1 Fe1 109.3(3) . . ?
C3 N1 Fe1 108.6(3) . . ?
C20 N1 Fe1 107.6(4) . . ?
C1 O1 Fe1 131.0(4) . . ?
C6 O2 Fe1 135.1(4) . . ?
Fe1 O1W H1WA 126.5 . . ?
Fe1 O1W H1WB 126.4 . . ?
H1WA O1W H1WB 107.1 . . ?
C22 O3 Fe1 134.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C36 -178.5(7) . . . . ?
C39 C1 C2 C36 9.9(12) . . . . ?
O1 C1 C2 C3 4.0(12) . . . . ?
C39 C1 C2 C3 -167.6(7) . . . . ?
C36 C2 C3 N1 127.8(7) . . . . ?
C1 C2 C3 N1 -54.7(9) . . . . ?
N1 C4 C5 C18 132.9(7) . . . . ?
N1 C4 C5 C6 -52.4(9) . . . . ?
C18 C5 C6 O2 179.4(7) . . . . ?
C4 C5 C6 O2 4.5(12) . . . . ?
C18 C5 C6 C7 9.4(12) . . . . ?
C4 C5 C6 C7 -165.4(7) . . . . ?
O2 C6 C7 C16 -173.7(6) . . . . ?
C5 C6 C7 C16 -3.8(10) . . . . ?
O2 C6 C7 C8 4.1(11) . . . . ?
C5 C6 C7 C8 174.0(6) . . . . ?
C6 C7 C8 C15 56.7(8) . . . . ?
C16 C7 C8 C15 -125.4(6) . . . . ?
C6 C7 C8 C9 -123.7(7) . . . . ?
C16 C7 C8 C9 54.1(7) . . . . ?
C15 C8 C9 C10 -1.8(8) . . . . ?
C7 C8 C9 C10 178.7(5) . . . . ?
C8 C9 C10 C12 3.2(9) . . . . ?
C8 C9 C10 C11 -177.1(5) . . . . ?
C12 C10 C11 F3 47.5(11) . . . . ?
C9 C10 C11 F3 -132.2(9) . . . . ?
C12 C10 C11 F2 170.9(7) . . . . ?
C9 C10 C11 F2 -8.9(10) . . . . ?
C12 C10 C11 F1 -72.6(10) . . . . ?
C9 C10 C11 F1 107.7(9) . . . . ?
C9 C10 C12 C13 -2.8(10) . . . . ?
C11 C10 C12 C13 177.5(6) . . . . ?
C10 C12 C13 C15 1.1(11) . . . . ?
C10 C12 C13 C14 172.8(8) . . . . ?
C12 C13 C14 F4 142.4(9) . . . . ?
C15 C13 C14 F4 -45.7(13) . . . . ?
C12 C13 C14 F6 15.0(15) . . . . ?
C15 C13 C14 F6 -173.2(9) . . . . ?
C12 C13 C14 F5 -100.5(10) . . . . ?
C15 C13 C14 F5 71.4(13) . . . . ?
C9 C8 C15 C13 0.1(8) . . . . ?
C7 C8 C15 C13 179.6(5) . . . . ?
C12 C13 C15 C8 0.2(10) . . . . ?
C14 C13 C15 C8 -171.5(8) . . . . ?
C6 C7 C16 C17 -1.2(10) . . . . ?
C8 C7 C16 C17 -179.1(6) . . . . ?
C7 C16 C17 C18 0.6(10) . . . . ?
C7 C16 C17 C19 -174.9(6) . . . . ?
C16 C17 C18 C5 5.3(10) . . . . ?
C19 C17 C18 C5 -179.1(7) . . . . ?
C6 C5 C18 C17 -10.2(11) . . . . ?
C4 C5 C18 C17 164.5(7) . . . . ?
N1 C20 C21 C22 -51.6(9) . . . . ?
N1 C20 C21 C34 129.6(7) . . . . ?
C34 C21 C22 O3 -176.0(7) . . . . ?
C20 C21 C22 O3 5.2(11) . . . . ?
C34 C21 C22 C23 10.3(10) . . . . ?
C20 C21 C22 C23 -168.4(6) . . . . ?
O3 C22 C23 C32 -177.0(6) . . . . ?
C21 C22 C23 C32 -3.1(9) . . . . ?
O3 C22 C23 C24 0.0(9) . . . . ?
C21 C22 C23 C24 173.9(6) . . . . ?
C32 C23 C24 C25 49.8(8) . . . . ?
C22 C23 C24 C25 -127.1(7) . . . . ?
C32 C23 C24 C31 -126.0(7) . . . . ?
C22 C23 C24 C31 57.1(9) . . . . ?
C31 C24 C25 C26 -2.8(10) . . . . ?
C23 C24 C25 C26 -178.6(6) . . . . ?
C24 C25 C26 C28 5.8(11) . . . . ?
C24 C25 C26 C27 -175.8(7) . . . . ?
C28 C26 C27 F8 -73.9(11) . . . . ?
C25 C26 C27 F8 107.7(10) . . . . ?
C28 C26 C27 F7 52.2(12) . . . . ?
C25 C26 C27 F7 -126.2(9) . . . . ?
C28 C26 C27 F9 168.7(8) . . . . ?
C25 C26 C27 F9 -9.7(12) . . . . ?
C25 C26 C28 C29 -4.4(12) . . . . ?
C27 C26 C28 C29 177.2(8) . . . . ?
C26 C28 C29 C31 0.2(14) . . . . ?
C26 C28 C29 C30 179.1(11) . . . . ?
C28 C29 C30 F12 23.2(19) . . . . ?
C31 C29 C30 F12 -158.0(11) . . . . ?
C28 C29 C30 F11 -99.8(13) . . . . ?
C31 C29 C30 F11 79.0(14) . . . . ?
C28 C29 C30 F10 141.9(11) . . . . ?
C31 C29 C30 F10 -39.2(17) . . . . ?
C25 C24 C31 C29 -1.5(11) . . . . ?
C23 C24 C31 C29 174.4(7) . . . . ?
C28 C29 C31 C24 2.8(13) . . . . ?
C30 C29 C31 C24 -176.1(11) . . . . ?
C22 C23 C32 C33 -5.4(9) . . . . ?
C24 C23 C32 C33 177.6(6) . . . . ?
C23 C32 C33 C34 6.3(10) . . . . ?
C23 C32 C33 C35 -176.4(7) . . . . ?
C32 C33 C34 C21 1.4(11) . . . . ?
C35 C33 C34 C21 -175.9(7) . . . . ?
C22 C21 C34 C33 -9.7(11) . . . . ?
C20 C21 C34 C33 169.0(7) . . . . ?
C1 C2 C36 C37 -11.0(12) . . . . ?
C3 C2 C36 C37 166.4(7) . . . . ?
C2 C36 C37 C38 5.4(12) . . . . ?
C2 C36 C37 C48 -177.5(9) . . . . ?
C36 C37 C38 C39 1.5(11) . . . . ?
C48 C37 C38 C39 -175.5(8) . . . . ?
C37 C38 C39 C1 -2.5(10) . . . . ?
C37 C38 C39 C40 -178.7(7) . . . . ?
C2 C1 C39 C38 -3.3(10) . . . . ?
O1 C1 C39 C38 -175.3(6) . . . . ?
C2 C1 C39 C40 172.8(7) . . . . ?
O1 C1 C39 C40 0.8(10) . . . . ?
C38 C39 C40 C41 -110.8(8) . . . . ?
C1 C39 C40 C41 73.2(10) . . . . ?
C38 C39 C40 C47 58.8(9) . . . . ?
C1 C39 C40 C47 -117.2(8) . . . . ?
C47 C40 C41 C42 4.7(11) . . . . ?
C39 C40 C41 C42 174.2(7) . . . . ?
C40 C41 C42 C44 3.4(12) . . . . ?
C40 C41 C42 C43 -175.9(9) . . . . ?
C44 C42 C43 F15 1.1(17) . . . . ?
C41 C42 C43 F15 -179.7(10) . . . . ?
C44 C42 C43 F14 129.8(11) . . . . ?
C41 C42 C43 F14 -50.9(15) . . . . ?
C44 C42 C43 F13 -114.1(11) . . . . ?
C41 C42 C43 F13 65.2(13) . . . . ?
C41 C42 C44 C45 -9.1(13) . . . . ?
C43 C42 C44 C45 170.2(10) . . . . ?
C42 C44 C45 C47 6.7(14) . . . . ?
C42 C44 C45 C46 -177.4(9) . . . . ?
C47 C45 C46 F18 107.3(11) . . . . ?
C44 C45 C46 F18 -68.5(13) . . . . ?
C47 C45 C46 F16 -13.0(15) . . . . ?
C44 C45 C46 F16 171.2(10) . . . . ?
C47 C45 C46 F17 -126.3(10) . . . . ?
C44 C45 C46 F17 57.9(13) . . . . ?
C44 C45 C47 C40 1.5(13) . . . . ?
C46 C45 C47 C40 -174.2(8) . . . . ?
C41 C40 C47 C45 -7.1(12) . . . . ?
C39 C40 C47 C45 -177.3(7) . . . . ?
C5 C4 N1 C3 -174.6(5) . . . . ?
C5 C4 N1 C20 -52.8(7) . . . . ?
C5 C4 N1 Fe1 65.3(6) . . . . ?
C2 C3 N1 C4 -52.0(7) . . . . ?
C2 C3 N1 C20 -174.4(6) . . . . ?
C2 C3 N1 Fe1 68.6(6) . . . . ?
C21 C20 N1 C4 -176.0(6) . . . . ?
C21 C20 N1 C3 -52.8(7) . . . . ?
C21 C20 N1 Fe1 64.9(6) . . . . ?
C2 C1 O1 Fe1 24.6(12) . . . . ?
C39 C1 O1 Fe1 -163.5(6) . . . . ?
O2 Fe1 O1 C1 84.8(8) . . . . ?
O3 Fe1 O1 C1 -95.4(8) . . . . ?
O1W Fe1 O1 C1 174.4(8) . . . . ?
N1 Fe1 O1 C1 -5.5(8) . . . . ?
C7 C6 O2 Fe1 -168.4(6) . . . . ?
C5 C6 O2 Fe1 21.7(12) . . . . ?
O1 Fe1 O2 C6 -95.6(8) . . . . ?
O3 Fe1 O2 C6 84.6(8) . . . . ?
O1W Fe1 O2 C6 175.2(8) . . . . ?
N1 Fe1 O2 C6 -5.1(8) . . . . ?
C21 C22 O3 Fe1 17.9(12) . . . . ?
C23 C22 O3 Fe1 -168.5(5) . . . . ?
O2 Fe1 O3 C22 -90.0(8) . . . . ?
O1 Fe1 O3 C22 90.2(7) . . . . ?
O1W Fe1 O3 C22 179.7(7) . . . . ?
N1 Fe1 O3 C22 -0.1(7) . . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 0.000 0.000 125 7 ' '
2 0.044 0.038 0.500 383 12 ' '
3 0.499 0.500 0.500 23 0 ' '
_platon_squeeze_details          
;
;
