# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_gunt07o08_h
_database_code_depnum_ccdc_archive 'CCDC 1508837'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             2015-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C16 H4 F24 Fe2 O16)'
_chemical_formula_sum            'C8 H2 F12 Fe O8'
_chemical_formula_weight         509.95
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.658(6)
_cell_length_b                   9.753(3)
_cell_length_c                   8.341(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.571(4)
_cell_angle_gamma                90
_cell_volume                     1581.3(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2077
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.891
_cell_measurement_theta_min      2.337
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.494737
_exptl_absorpt_correction_T_min  0.353389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1216 before and 0.0520 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1184 before and 0.0573 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 12369 reflections, Rint = 0.0552
 (7755 with I > 3sig(I), Rint = 0.0521)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'crystallized from trifluoroacetic acid'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.228
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (10 s exposure) covering -0.300° degrees in ω.
 The crystal to detector distance was 4.956 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2370
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.547
_diffrn_reflns_theta_min         2.095
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Platform with a Apex I-detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2111
_reflns_number_total             2370
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+0.7184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1408
_refine_special_details          
'All crystals examined were twinned by a 180 deg. rotation around the [301] direction in real space, which corresponds to the [100] direction in reciprocal space. The volume ratio of the two domains of this crystal is 0.453:0.547. All CF3-are disordered and were describded by two sets of fluorine atoms each. The hydrogen atom at O4 has been found in the difference fourier map and he refinement has been done according to the riding model.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.546(2) 0.454(2)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, F1, F2, F3, F4, F5, F6, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
5.a Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.5000 0.60845(5) 0.7500 0.02476(16) Uani 1 2 d S T P . .
O1 O 0.44840(11) 0.4606(3) 0.8598(3) 0.0414(5) Uani 1 1 d . . . . .
O2 O 0.41424(10) 0.3653(2) 1.0745(2) 0.0282(4) Uani 1 1 d . . . . .
O3 O 0.45401(12) 0.7659(3) 0.8815(3) 0.0419(6) Uani 1 1 d . . . . .
O4 O 0.35093(11) 0.8111(2) 0.7393(3) 0.0388(5) Uani 1 1 d . . . . .
H4 H 0.3641 0.7599 0.6691 0.058 Uiso 1 1 calc GR . . . .
C1 C 0.40596(14) 0.4089(3) 0.9319(3) 0.0280(5) Uani 1 1 d . U . . .
C2 C 0.33258(16) 0.3957(3) 0.8393(4) 0.0400(7) Uani 1 1 d . U . . .
C3 C 0.39964(15) 0.8256(3) 0.8582(3) 0.0323(6) Uani 1 1 d . U . . .
C4 C 0.38351(19) 0.9350(4) 0.9804(4) 0.0433(7) Uani 1 1 d . U . . .
F1 F 0.3052(4) 0.5224(8) 0.8212(8) 0.0599(13) Uani 0.79(3) 1 d . U . A 1
F2 F 0.2927(3) 0.3230(14) 0.9200(13) 0.073(3) Uani 0.79(3) 1 d . U . A 1
F3 F 0.3348(5) 0.3447(12) 0.6954(10) 0.0693(19) Uani 0.79(3) 1 d . U . A 1
F4 F 0.4243(4) 0.9171(10) 1.1208(6) 0.074(2) Uani 0.731(19) 1 d . U . B 1
F5 F 0.3963(7) 1.0542(5) 0.9280(9) 0.086(3) Uani 0.731(19) 1 d . U . B 1
F6 F 0.3210(3) 0.9252(10) 1.0094(12) 0.075(2) Uani 0.731(19) 1 d . U . B 1
F1A F 0.2942(11) 0.489(3) 0.857(4) 0.057(4) Uani 0.21(3) 1 d . U . A 2
F2A F 0.3039(12) 0.282(2) 0.875(3) 0.048(4) Uani 0.21(3) 1 d . U . A 2
F3A F 0.3281(12) 0.382(3) 0.680(3) 0.043(4) Uani 0.21(3) 1 d . U . A 2
F4A F 0.4346(7) 0.978(2) 1.073(3) 0.070(4) Uani 0.269(19) 1 d . U . B 2
F5A F 0.3533(13) 1.0462(16) 0.9023(14) 0.065(4) Uani 0.269(19) 1 d . U . B 2
F6A F 0.3362(12) 0.897(2) 1.053(3) 0.061(4) Uani 0.269(19) 1 d . U . B 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 2.055(2) 2_656 ?
Fe1 O1 2.055(2) . ?
Fe1 O2 2.077(2) 5_667 ?
Fe1 O2 2.077(2) 6_565 ?
Fe1 O3 2.162(2) 2_656 ?
Fe1 O3 2.162(2) . ?
O1 C1 1.209(3) . ?
O2 Fe1 2.077(2) 5_667 ?
O2 C1 1.251(3) . ?
O3 C3 1.207(4) . ?
O4 H4 0.8400 . ?
O4 C3 1.279(4) . ?
C1 C2 1.537(4) . ?
C2 F1 1.347(7) . ?
C2 F2 1.314(6) . ?
C2 F3 1.307(8) . ?
C2 F1A 1.204(19) . ?
C2 F2A 1.300(19) . ?
C2 F3A 1.33(2) . ?
C3 C4 1.541(4) . ?
C4 F4 1.329(6) . ?
C4 F5 1.280(6) . ?
C4 F6 1.292(7) . ?
C4 F4A 1.246(13) . ?
C4 F5A 1.355(12) . ?
C4 F6A 1.241(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 90.89(15) 2_656 . ?
O1 Fe1 O2 89.86(8) . 6_565 ?
O1 Fe1 O2 100.08(8) 2_656 6_565 ?
O1 Fe1 O2 100.08(8) . 5_667 ?
O1 Fe1 O2 89.86(8) 2_656 5_667 ?
O1 Fe1 O3 174.81(8) . 2_656 ?
O1 Fe1 O3 90.06(11) 2_656 2_656 ?
O1 Fe1 O3 174.81(8) 2_656 . ?
O1 Fe1 O3 90.05(11) . . ?
O2 Fe1 O2 165.86(11) 5_667 6_565 ?
O2 Fe1 O3 84.95(8) 6_565 2_656 ?
O2 Fe1 O3 85.02(8) 5_667 2_656 ?
O2 Fe1 O3 85.02(8) 6_565 . ?
O2 Fe1 O3 84.95(8) 5_667 . ?
O3 Fe1 O3 89.46(14) 2_656 . ?
C1 O1 Fe1 159.6(2) . . ?
C1 O2 Fe1 127.25(18) . 5_667 ?
C3 O3 Fe1 133.5(2) . . ?
C3 O4 H4 109.5 . . ?
O1 C1 O2 127.8(3) . . ?
O1 C1 C2 116.8(3) . . ?
O2 C1 C2 115.4(2) . . ?
F1 C2 C1 108.0(4) . . ?
F2 C2 C1 112.0(4) . . ?
F2 C2 F1 107.1(5) . . ?
F3 C2 C1 109.6(5) . . ?
F3 C2 F1 108.3(6) . . ?
F3 C2 F2 111.7(7) . . ?
F1A C2 C1 115.7(11) . . ?
F1A C2 F2A 108.5(13) . . ?
F1A C2 F3A 104.4(15) . . ?
F2A C2 C1 111.2(10) . . ?
F2A C2 F3A 100.3(14) . . ?
F3A C2 C1 115.4(11) . . ?
O3 C3 O4 127.9(3) . . ?
O3 C3 C4 119.5(3) . . ?
O4 C3 C4 112.7(3) . . ?
F4 C4 C3 109.6(4) . . ?
F5 C4 C3 109.4(3) . . ?
F5 C4 F4 107.3(5) . . ?
F5 C4 F6 111.9(5) . . ?
F6 C4 C3 111.6(5) . . ?
F6 C4 F4 107.0(5) . . ?
F4A C4 C3 114.8(7) . . ?
F4A C4 F5A 106.3(9) . . ?
F5A C4 C3 110.8(5) . . ?
F6A C4 C3 111.2(11) . . ?
F6A C4 F4A 113.0(13) . . ?
F6A C4 F5A 99.6(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O1 C1 O2 -107.9(6) . . . . ?
Fe1 O1 C1 C2 71.5(7) . . . . ?
Fe1 O2 C1 O1 9.7(4) 5_667 . . . ?
Fe1 O2 C1 C2 -169.62(19) 5_667 . . . ?
Fe1 O3 C3 O4 -0.5(5) . . . . ?
Fe1 O3 C3 C4 -179.9(2) . . . . ?
O1 C1 C2 F1 -70.4(5) . . . . ?
O1 C1 C2 F2 171.9(9) . . . . ?
O1 C1 C2 F3 47.3(7) . . . . ?
O1 C1 C2 F1A -93(2) . . . . ?
O1 C1 C2 F2A 142.7(14) . . . . ?
O1 C1 C2 F3A 29.4(13) . . . . ?
O2 C1 C2 F1 109.0(5) . . . . ?
O2 C1 C2 F2 -8.7(9) . . . . ?
O2 C1 C2 F3 -133.3(7) . . . . ?
O2 C1 C2 F1A 87(2) . . . . ?
O2 C1 C2 F2A -37.8(15) . . . . ?
O2 C1 C2 F3A -151.2(13) . . . . ?
O3 C3 C4 F4 -19.3(7) . . . . ?
O3 C3 C4 F5 98.1(8) . . . . ?
O3 C3 C4 F6 -137.6(6) . . . . ?
O3 C3 C4 F4A 17.4(15) . . . . ?
O3 C3 C4 F5A 137.8(13) . . . . ?
O3 C3 C4 F6A -112.5(12) . . . . ?
O4 C3 C4 F4 161.2(6) . . . . ?
O4 C3 C4 F5 -81.4(7) . . . . ?
O4 C3 C4 F6 42.9(7) . . . . ?
O4 C3 C4 F4A -162.2(15) . . . . ?
O4 C3 C4 F5A -41.7(13) . . . . ?
O4 C3 C4 F6A 68.0(12) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.546(2)
2 0.454(2)

####################################################################### 
# 
# 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_gunt05o04_100k
_database_code_depnum_ccdc_archive 'CCDC 1508836'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             2015-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H8 Co F6 O8'
_chemical_formula_sum            'C4 H8 Co F6 O8'
_chemical_formula_weight         357.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co1 C4 O8 F6 H8 '
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'
Co Co 0.3494 0.9721 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1360(4)
_cell_length_b                   9.0331(7)
_cell_length_c                   9.2695(5)
_cell_angle_alpha                75.139(6)
_cell_angle_beta                 64.574(6)
_cell_angle_gamma                71.426(6)
_cell_volume                     577.49(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5674
_cell_measurement_temperature    103(5)
_cell_measurement_theta_max      31.8010
_cell_measurement_theta_min      2.9940
_shelx_estimated_absorpt_T_max   0.783
_shelx_estimated_absorpt_T_min   0.620
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. The HKLF 5-file with two components contains 7015 reflections unique reflections, merged from 20573 measured reflections.
R-int. for all components is 0.033, Rsigma 0.049.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             354
_exptl_crystal_recrystallization_method 
'crystallized from toluene/ethanole-mixture'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         2.977
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(5)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -31.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -91.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -77.0000  120.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
  4 omega  -56.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   77.0000   60.0000 46

#__ type_ start__ end____ width___ exp.time_
  5 omega  -35.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   66.0000  -30.0000 76

#__ type_ start__ end____ width___ exp.time_
  6 omega  -95.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -77.0000  -30.0000 98

#__ type_ start__ end____ width___ exp.time_
  7 omega  -94.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -66.0000 -165.0000 88

#__ type_ start__ end____ width___ exp.time_
  8 omega  -31.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  9 omega   19.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000  -60.0000 50

#__ type_ start__ end____ width___ exp.time_
 10 omega  -17.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega  -24.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 12 omega  -24.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000  150.0000 95
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0759819000
_diffrn_orient_matrix_UB_12      -0.0121997000
_diffrn_orient_matrix_UB_13      0.0236698000
_diffrn_orient_matrix_UB_21      -0.0204254000
_diffrn_orient_matrix_UB_22      0.0821346000
_diffrn_orient_matrix_UB_23      0.0015292000
_diffrn_orient_matrix_UB_31      -0.0607527000
_diffrn_orient_matrix_UB_32      -0.0101911000
_diffrn_orient_matrix_UB_33      0.0822138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'While cooling form 275 K to 100 K the crystal experiences a phase transition to an ordered phase, where the rotation of the trifluoromethyl-groups freezes. The crystal system changes from monoclinic to triclinic, the resulting crystal at 100 K is twinned with a volume ration of the individuals of about 1:1.'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5604
_reflns_number_total             7011
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         7011
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0712
_refine_special_details          
'All hydrogen atom positions were found in the diffrerence fourier map and refined freely.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5106(6) 0.4894(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Co1 Co 0.16052(3) 0.59412(3) 0.11239(3) 0.01274(7) Uani 1 1 d . . . . .
F2 F -0.10789(17) 0.16518(13) 0.44633(15) 0.0364(3) Uani 1 1 d . . . . .
F6 F 0.36535(19) 1.04155(15) -0.29647(14) 0.0426(3) Uani 1 1 d . . . . .
F4 F 0.45462(16) 1.10042(13) -0.13621(15) 0.0321(3) Uani 1 1 d . . . . .
F1 F -0.36288(17) 0.30582(14) 0.59405(13) 0.0346(3) Uani 1 1 d . . . . .
F3 F -0.32011(17) 0.29387(15) 0.35183(13) 0.0341(3) Uani 1 1 d . . . . .
O2 O -0.21269(17) 0.55158(14) 0.46226(13) 0.0199(3) Uani 1 1 d . . . . .
O1 O -0.01312(16) 0.43381(13) 0.24430(13) 0.0156(2) Uani 1 1 d . . . . .
O4 O 0.15849(16) 0.97235(13) 0.05320(15) 0.0211(3) Uani 1 1 d . . . . .
O7 O -0.02937(16) 0.71350(14) -0.00123(15) 0.0151(2) Uani 1 1 d . . . . .
O8 O 0.35892(16) 0.47349(14) 0.21487(15) 0.0145(2) Uani 1 1 d . . . . .
O5 O 0.03205(18) 0.73582(15) 0.29246(16) 0.0181(3) Uani 1 1 d . . . . .
O6 O 0.29946(18) 0.44617(15) -0.06319(15) 0.0178(3) Uani 1 1 d . . . . .
C1 C -0.1460(2) 0.44348(19) 0.38023(19) 0.0155(3) Uani 1 1 d . . . . .
C3 C 0.2981(2) 0.89049(19) -0.0383(2) 0.0159(3) Uani 1 1 d . . . . .
C4 C 0.4341(2) 0.9802(2) -0.1811(2) 0.0224(4) Uani 1 1 d . . . . .
F5 F 0.60310(16) 0.88954(13) -0.24548(16) 0.0433(4) Uani 1 1 d . . . . .
O3 O 0.34331(15) 0.74370(12) -0.03480(13) 0.0152(2) Uani 1 1 d . . . . .
C2 C -0.2355(3) 0.2996(2) 0.4452(2) 0.0207(4) Uani 1 1 d . . . . .
H6A H 0.405(3) 0.440(3) -0.113(3) 0.031 Uiso 1 1 d R . . . .
H6B H 0.253(3) 0.385(3) -0.067(3) 0.031 Uiso 1 1 d R . . . .
H8A H 0.414(3) 0.391(3) 0.188(3) 0.037(7) Uiso 1 1 d . . . . .
H5A H -0.059(3) 0.714(3) 0.356(3) 0.039(7) Uiso 1 1 d . . . . .
H8B H 0.319(3) 0.466(3) 0.327(3) 0.053(8) Uiso 1 1 d . . . . .
H5B H 0.044(3) 0.824(3) 0.256(3) 0.050(8) Uiso 1 1 d . . . . .
H7A H -0.004(3) 0.688(3) -0.090(3) 0.033(6) Uiso 1 1 d . . . . .
H7B H -0.068(3) 0.814(3) -0.013(3) 0.032(6) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.1213(11) . ?
Co1 O7 2.1006(12) . ?
Co1 O8 2.0882(12) . ?
Co1 O5 2.0646(12) . ?
Co1 O6 2.0703(12) . ?
Co1 O3 2.1192(11) . ?
F2 C2 1.323(2) . ?
F6 C4 1.332(2) . ?
F4 C4 1.337(2) . ?
F1 C2 1.3247(19) . ?
F3 C2 1.335(2) . ?
O2 C1 1.2309(19) . ?
O1 C1 1.2611(18) . ?
O4 C3 1.231(2) . ?
C1 C2 1.552(2) . ?
C3 C4 1.549(2) . ?
C3 O3 1.2539(19) . ?
C4 F5 1.322(2) . ?

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
O7 Co1 O1 88.49(5) . . ?
O7 Co1 O3 90.87(5) . . ?
O8 Co1 O1 92.83(5) . . ?
O8 Co1 O7 177.35(5) . . ?
O8 Co1 O3 87.64(4) . . ?
O5 Co1 O1 92.74(5) . . ?
O5 Co1 O7 93.57(5) . . ?
O5 Co1 O8 88.67(5) . . ?
O5 Co1 O6 177.10(6) . . ?
O5 Co1 O3 91.80(5) . . ?
O6 Co1 O1 87.47(5) . . ?
O6 Co1 O7 89.32(5) . . ?
O6 Co1 O8 88.44(5) . . ?
O6 Co1 O3 88.02(5) . . ?
O3 Co1 O1 175.44(4) . . ?
C1 O1 Co1 127.49(10) . . ?
O2 C1 O1 128.43(15) . . ?
O2 C1 C2 118.06(14) . . ?
O1 C1 C2 113.49(14) . . ?
O4 C3 C4 116.11(14) . . ?
O4 C3 O3 128.89(15) . . ?
O3 C3 C4 114.96(14) . . ?
F6 C4 F4 106.86(15) . . ?
F6 C4 C3 109.74(15) . . ?
F4 C4 C3 111.54(14) . . ?
F5 C4 F6 108.01(16) . . ?
F5 C4 F4 107.33(15) . . ?
F5 C4 C3 113.10(15) . . ?
C3 O3 Co1 123.78(10) . . ?
F2 C2 F1 107.61(15) . . ?
F2 C2 F3 107.50(15) . . ?
F2 C2 C1 111.55(14) . . ?
F1 C2 F3 107.51(14) . . ?
F1 C2 C1 112.23(14) . . ?
F3 C2 C1 110.23(14) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5106(6)
2 0.4894(6)

####################################################################### 
# 
# 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_gunt18o05_new3
_database_code_depnum_ccdc_archive 'CCDC 1508835'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             2015-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H4 F24 Mn2 O16'
_chemical_formula_sum            'C16 H4 F24 Mn2 O16'
_chemical_formula_weight         1018.07
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3229(17)
_cell_length_b                   13.518(2)
_cell_length_c                   13.940(2)
_cell_angle_alpha                105.172(2)
_cell_angle_beta                 111.289(2)
_cell_angle_gamma                107.081(2)
_cell_volume                     1577.4(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.448
_cell_measurement_theta_min      2.235
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0816 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.8037.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'from trifluoroacetic acid'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.133
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (10 s exposure) covering -0.300° degrees in ω.
 The crystal to detector distance was 4.956 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16256
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.479
_diffrn_reflns_theta_min         1.722
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5807
_reflns_number_total             7786
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7786
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0473
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0589P)²+1.8305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1262
_refine_special_details          'several CF3-groups show significant disorder'
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O15) = Uanis(O15A)
Uanis(O7) = Uanis(O7A)
2. Rigid body (RIGU) restrains
 C3, C4, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C13, C14, F19, F20, F21, F19A, F20A, F21A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, C10, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(3)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(3)
 Sof(O15A)=1-FVAR(4)
 Sof(O15)=FVAR(4)
 Sof(O7)=1-FVAR(5)
 Sof(O7A)=FVAR(5)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mn1 Mn 1.01132(5) 0.61949(3) 0.66138(4) 0.01826(11) Uani 1 1 d . . . . .
Mn2 Mn 0.84286(5) 0.88104(3) 0.54816(3) 0.01736(11) Uani 1 1 d . . . . .
F1 F 1.4342(3) 0.6741(2) 1.05219(17) 0.0458(6) Uani 1 1 d . . . . .
F2 F 1.3770(3) 0.52796(17) 0.91264(19) 0.0499(6) Uani 1 1 d . . . . .
F3 F 1.5696(2) 0.6836(2) 0.9672(2) 0.0480(6) Uani 1 1 d . . . . .
F7 F 0.6233(2) 0.25105(17) 0.5155(2) 0.0431(5) Uani 1 1 d . . . . .
F8 F 0.6293(3) 0.1924(2) 0.36172(18) 0.0581(7) Uani 1 1 d . . . . .
F9 F 0.7812(3) 0.18235(17) 0.5057(2) 0.0497(6) Uani 1 1 d . . . . .
F10 F 0.6062(3) 0.4550(2) 0.3038(2) 0.0588(7) Uani 1 1 d . . . . .
F11 F 0.5472(3) 0.42600(16) 0.42795(18) 0.0451(6) Uani 1 1 d . . . . .
F12 F 0.4414(2) 0.50485(17) 0.3319(2) 0.0521(7) Uani 1 1 d . . . . .
F16 F 0.6691(3) 0.9505(2) 0.8760(2) 0.0566(7) Uani 1 1 d . . . . .
F17 F 0.6405(3) 0.78464(19) 0.78857(18) 0.0514(6) Uani 1 1 d . . . . .
F18 F 0.8559(3) 0.9039(2) 0.92987(18) 0.0498(6) Uani 1 1 d . . . . .
F22 F 1.2173(3) 1.05250(19) 0.8770(2) 0.0568(7) Uani 1 1 d . . . . .
F23 F 1.3955(2) 1.00016(17) 0.8846(2) 0.0528(7) Uani 1 1 d . . . . .
F24 F 1.3011(3) 1.05971(18) 0.7604(2) 0.0494(6) Uani 1 1 d . . . . .
O1 O 1.3840(3) 0.7825(2) 0.9065(2) 0.0501(8) Uani 1 1 d . . . . .
H1 H 1.325(6) 0.800(4) 0.869(4) 0.071(17) Uiso 1 1 d . . . . .
O2 O 1.2003(2) 0.60572(16) 0.79432(17) 0.0226(4) Uani 1 1 d . . . . .
O3 O 0.9295(2) 0.62959(17) 0.78859(18) 0.0258(5) Uani 1 1 d . . . . .
O4 O 0.8541(3) 0.45515(19) 0.7847(2) 0.0310(5) Uani 1 1 d . . . . .
H4 H 0.866(6) 0.439(5) 0.728(5) 0.081(18) Uiso 1 1 d . . . . .
O5 O 0.8884(2) 0.43658(16) 0.60421(17) 0.0209(4) Uani 1 1 d . . . . .
O6 O 0.8753(3) 0.3771(2) 0.4353(2) 0.0409(6) Uani 1 1 d . . . . .
O8 O 0.6913(2) 0.69935(16) 0.45248(17) 0.0203(4) Uani 1 1 d . . . . .
O9 O 0.4786(3) 0.72483(18) 0.30297(19) 0.0279(5) Uani 1 1 d . . . . .
H9 H 0.543(6) 0.711(4) 0.345(5) 0.072(17) Uiso 1 1 d . . . . .
O10 O 0.6369(2) 0.89866(17) 0.44366(18) 0.0233(4) Uani 1 1 d . . . . .
O11 O 0.7609(3) 0.86727(18) 0.67386(18) 0.0306(5) Uani 1 1 d . . . . .
O12 O 0.8750(3) 1.04242(18) 0.81148(19) 0.0268(5) Uani 1 1 d . . . . .
H12 H 0.914(4) 1.059(3) 0.771(3) 0.038(11) Uiso 1 1 d . . . . .
O13 O 0.9492(2) 1.06227(16) 0.65394(17) 0.0204(4) Uani 1 1 d . . . . .
O14 O 1.0897(3) 1.12409(19) 0.5761(2) 0.0348(6) Uani 1 1 d . . . . .
O16 O 1.1582(2) 0.80067(16) 0.76196(17) 0.0251(5) Uani 1 1 d . . . . .
C1 C 1.3233(4) 0.6743(2) 0.8739(3) 0.0240(6) Uani 1 1 d . . . . .
C2 C 1.4282(4) 0.6384(3) 0.9524(3) 0.0285(7) Uani 1 1 d . . . . .
C3 C 0.8897(3) 0.5624(2) 0.8257(3) 0.0229(6) Uani 1 1 d . U . . .
C4 C 0.8828(5) 0.6036(3) 0.9359(3) 0.0356(7) Uani 1 1 d . U . . .
C5 C 0.8396(3) 0.3643(2) 0.5068(2) 0.0205(6) Uani 1 1 d . . . . .
C6 C 0.7165(4) 0.2453(2) 0.4726(3) 0.0241(6) Uani 1 1 d . . . . .
C7 C 0.7048(3) 0.6159(2) 0.4698(2) 0.0198(6) Uani 1 1 d . . . . .
C8 C 0.5719(3) 0.4986(2) 0.3820(3) 0.0234(6) Uani 1 1 d . . . . .
C9 C 0.5218(3) 0.8320(2) 0.3566(3) 0.0218(6) Uani 1 1 d . U . . .
C10 C 0.4004(4) 0.8692(3) 0.2957(3) 0.0266(6) Uani 1 1 d . U . . .
C11 C 0.7933(3) 0.9338(3) 0.7649(2) 0.0224(6) Uani 1 1 d . . . . .
C12 C 0.7378(4) 0.8926(3) 0.8418(3) 0.0298(7) Uani 1 1 d . . . . .
C13 C 1.0469(3) 1.1364(2) 0.6471(2) 0.0197(5) Uani 1 1 d . U . . .
C14 C 1.1250(4) 1.2577(2) 0.7386(3) 0.0261(6) Uani 1 1 d . U . . .
C15 C 1.1432(3) 0.8785(2) 0.7346(2) 0.0186(5) Uani 1 1 d . . . . .
C16 C 1.2688(4) 0.9997(2) 0.8159(3) 0.0260(6) Uani 1 1 d . . . . .
F4 F 0.7605(11) 0.5298(5) 0.9299(7) 0.073(2) Uani 0.642(16) 1 d . U P A 1
F5 F 1.0058(10) 0.6181(9) 1.0185(5) 0.071(2) Uani 0.642(16) 1 d . U P A 1
F6 F 0.8718(11) 0.7014(5) 0.9568(7) 0.0546(17) Uani 0.642(16) 1 d . U P A 1
F13 F 0.2681(4) 0.8149(4) 0.2927(4) 0.0361(9) Uani 0.832(11) 1 d . U P B 1
F14 F 0.4452(5) 0.9781(3) 0.3445(5) 0.0558(13) Uani 0.832(11) 1 d . U P B 1
F15 F 0.3704(5) 0.8425(5) 0.1881(3) 0.0433(11) Uani 0.832(11) 1 d . U P B 1
F19 F 1.1049(9) 1.2571(5) 0.8301(5) 0.0433(16) Uani 0.625(19) 1 d . U P C 1
F20 F 1.2786(7) 1.2983(8) 0.7763(7) 0.0333(14) Uani 0.625(19) 1 d . U P C 1
F21 F 1.0762(9) 1.3255(5) 0.7064(6) 0.0439(18) Uani 0.625(19) 1 d . U P C 1
O7A O 0.822(4) 0.619(3) 0.536(3) 0.028(3) Uani 0.34(7) 1 d . . P D 1
O15 O 1.0439(7) 0.8688(4) 0.6450(7) 0.0251(13) Uani 0.77(3) 1 d . . P E 1
F4A F 0.837(2) 0.5246(8) 0.9692(10) 0.061(3) Uani 0.358(16) 1 d . U P A 2
F5A F 1.0290(12) 0.6668(12) 1.0207(9) 0.056(3) Uani 0.358(16) 1 d . U P A 2
F6A F 0.8110(19) 0.6625(15) 0.9321(12) 0.063(3) Uani 0.358(16) 1 d . U P A 2
F13A F 0.267(2) 0.8007(17) 0.2540(18) 0.034(3) Uani 0.168(11) 1 d . U P B 2
F14A F 0.423(2) 0.9671(14) 0.3802(14) 0.032(3) Uani 0.168(11) 1 d . U P B 2
F15A F 0.432(2) 0.905(2) 0.2294(18) 0.044(3) Uani 0.168(11) 1 d . U P B 2
F19A F 1.0552(15) 1.2747(7) 0.7959(12) 0.046(2) Uani 0.375(19) 1 d . U P C 2
F20A F 1.2675(13) 1.2935(13) 0.8011(11) 0.032(2) Uani 0.375(19) 1 d . U P C 2
F21A F 1.1107(12) 1.3291(7) 0.6802(9) 0.0308(18) Uani 0.375(19) 1 d . U P C 2
O7 O 0.803(2) 0.6135(14) 0.5508(18) 0.028(3) Uani 0.66(7) 1 d . . P D 2
O15A O 1.021(2) 0.8716(14) 0.6712(18) 0.0251(13) Uani 0.23(3) 1 d . . P E 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
Mn1 O2 2.246(2) . ?
Mn1 O3 2.215(2) . ?
Mn1 O5 2.1795(19) . ?
Mn1 O6 2.082(2) 2_766 ?
Mn1 O16 2.177(2) . ?
Mn1 O7A 2.09(3) . ?
Mn1 O7 2.102(16) . ?
Mn2 O8 2.184(2) . ?
Mn2 O10 2.220(2) . ?
Mn2 O11 2.231(2) . ?
Mn2 O13 2.176(2) . ?
Mn2 O14 2.082(2) 2_776 ?
Mn2 O15 2.107(5) . ?
Mn2 O15A 2.072(17) . ?
F1 C2 1.319(4) . ?
F2 C2 1.306(4) . ?
F3 C2 1.319(4) . ?
F7 C6 1.314(4) . ?
F8 C6 1.321(4) . ?
F9 C6 1.304(4) . ?
F10 C8 1.314(4) . ?
F11 C8 1.320(3) . ?
F12 C8 1.313(4) . ?
F16 C12 1.311(4) . ?
F17 C12 1.312(4) . ?
F18 C12 1.312(4) . ?
F22 C16 1.324(4) . ?
F23 C16 1.308(4) . ?
F24 C16 1.314(4) . ?
O1 C1 1.283(4) . ?
O2 C1 1.204(4) . ?
O3 C3 1.201(3) . ?
O4 C3 1.290(4) . ?
O5 C5 1.254(3) . ?
O6 Mn1 2.082(2) 2_766 ?
O6 C5 1.216(4) . ?
O8 C7 1.249(3) . ?
O9 C9 1.292(4) . ?
O10 C9 1.203(4) . ?
O11 C11 1.203(4) . ?
O12 C11 1.290(4) . ?
O13 C13 1.248(3) . ?
O14 Mn2 2.081(2) 2_776 ?
O14 C13 1.214(4) . ?
O16 C15 1.241(3) . ?
C1 C2 1.528(4) . ?
C3 C4 1.527(4) . ?
C4 F4 1.318(6) . ?
C4 F5 1.285(7) . ?
C4 F6 1.326(6) . ?
C4 F4A 1.303(9) . ?
C4 F5A 1.351(11) . ?
C4 F6A 1.235(12) . ?
C5 C6 1.544(4) . ?
C7 C8 1.543(4) . ?
C7 O7A 1.21(3) . ?
C7 O7 1.232(17) . ?
C9 C10 1.538(4) . ?
C10 F13 1.327(4) . ?
C10 F14 1.301(4) . ?
C10 F15 1.338(4) . ?
C10 F13A 1.216(19) . ?
C10 F14A 1.416(16) . ?
C10 F15A 1.251(14) . ?
C11 C12 1.537(4) . ?
C13 C14 1.533(4) . ?
C14 F19 1.365(6) . ?
C14 F20 1.351(7) . ?
C14 F21 1.272(6) . ?
C14 F19A 1.276(8) . ?
C14 F20A 1.260(12) . ?
C14 F21A 1.423(9) . ?
C15 C16 1.537(4) . ?
C15 O15 1.238(6) . ?
C15 O15A 1.210(18) . ?

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
O3 Mn1 O2 80.48(8) . . ?
O5 Mn1 O2 84.91(7) . . ?
O5 Mn1 O3 83.97(8) . . ?
O6 Mn1 O2 91.31(10) 2_766 . ?
O6 Mn1 O3 170.48(10) 2_766 . ?
O6 Mn1 O5 100.19(9) 2_766 . ?
O6 Mn1 O16 88.38(9) 2_766 . ?
O6 Mn1 O7A 91.1(8) 2_766 . ?
O6 Mn1 O7 100.4(9) 2_766 . ?
O16 Mn1 O2 82.40(8) . . ?
O16 Mn1 O3 85.79(8) . . ?
O16 Mn1 O5 164.85(8) . . ?
O7A Mn1 O2 175.0(8) . . ?
O7A Mn1 O3 97.5(8) . . ?
O7A Mn1 O5 90.3(9) . . ?
O7A Mn1 O16 102.1(9) . . ?
O7 Mn1 O2 166.9(8) . . ?
O7 Mn1 O3 88.3(8) . . ?
O7 Mn1 O5 87.3(5) . . ?
O7 Mn1 O16 103.6(4) . . ?
O8 Mn2 O10 83.50(8) . . ?
O8 Mn2 O11 85.36(8) . . ?
O10 Mn2 O11 91.50(8) . . ?
O13 Mn2 O8 165.97(8) . . ?
O13 Mn2 O10 88.63(8) . . ?
O13 Mn2 O11 83.25(8) . . ?
O14 Mn2 O8 89.02(8) 2_776 . ?
O14 Mn2 O10 89.42(9) 2_776 . ?
O14 Mn2 O11 174.16(8) 2_776 . ?
O14 Mn2 O13 102.54(8) 2_776 . ?
O14 Mn2 O15 88.6(3) 2_776 . ?
O15 Mn2 O8 97.96(13) . . ?
O15 Mn2 O10 177.5(3) . . ?
O15 Mn2 O11 90.6(3) . . ?
O15 Mn2 O13 90.34(15) . . ?
O15A Mn2 O8 98.4(5) . . ?
O15A Mn2 O10 168.1(7) . . ?
O15A Mn2 O11 77.0(7) . . ?
O15A Mn2 O13 87.0(5) . . ?
O15A Mn2 O14 102.4(7) . 2_776 ?
C1 O2 Mn1 133.55(19) . . ?
C3 O3 Mn1 131.4(2) . . ?
C5 O5 Mn1 124.66(18) . . ?
C5 O6 Mn1 161.1(3) . 2_766 ?
C7 O8 Mn2 130.68(18) . . ?
C9 O10 Mn2 131.40(19) . . ?
C11 O11 Mn2 133.3(2) . . ?
C13 O13 Mn2 124.67(18) . . ?
C13 O14 Mn2 173.2(2) . 2_776 ?
C15 O16 Mn1 126.25(19) . . ?
O1 C1 C2 110.9(3) . . ?
O2 C1 O1 127.6(3) . . ?
O2 C1 C2 121.5(3) . . ?
F1 C2 F3 108.0(3) . . ?
F1 C2 C1 109.6(3) . . ?
F2 C2 F1 107.9(3) . . ?
F2 C2 F3 109.0(3) . . ?
F2 C2 C1 111.5(3) . . ?
F3 C2 C1 110.7(3) . . ?
O3 C3 O4 127.5(3) . . ?
O3 C3 C4 119.4(3) . . ?
O4 C3 C4 113.1(3) . . ?
F4 C4 C3 110.6(4) . . ?
F4 C4 F6 106.8(5) . . ?
F5 C4 C3 109.6(4) . . ?
F5 C4 F4 110.0(5) . . ?
F5 C4 F6 108.4(5) . . ?
F6 C4 C3 111.3(4) . . ?
F4A C4 C3 115.0(5) . . ?
F4A C4 F5A 100.0(7) . . ?
F5A C4 C3 107.8(6) . . ?
F6A C4 C3 110.2(7) . . ?
F6A C4 F4A 113.6(8) . . ?
F6A C4 F5A 109.4(8) . . ?
O5 C5 C6 116.0(2) . . ?
O6 C5 O5 127.9(3) . . ?
O6 C5 C6 116.1(3) . . ?
F7 C6 F8 106.6(3) . . ?
F7 C6 C5 111.9(2) . . ?
F8 C6 C5 111.0(2) . . ?
F9 C6 F7 108.7(3) . . ?
F9 C6 F8 107.6(3) . . ?
F9 C6 C5 110.8(3) . . ?
O8 C7 C8 115.6(2) . . ?
O7A C7 O8 125.0(15) . . ?
O7A C7 C8 118.0(16) . . ?
O7 C7 O8 129.5(8) . . ?
O7 C7 C8 114.7(8) . . ?
F10 C8 F11 107.3(3) . . ?
F10 C8 C7 109.7(2) . . ?
F11 C8 C7 112.0(2) . . ?
F12 C8 F10 108.1(3) . . ?
F12 C8 F11 107.2(3) . . ?
F12 C8 C7 112.3(2) . . ?
O9 C9 C10 110.7(3) . . ?
O10 C9 O9 128.3(3) . . ?
O10 C9 C10 120.9(3) . . ?
F13 C10 C9 110.4(3) . . ?
F13 C10 F15 106.4(3) . . ?
F14 C10 C9 111.9(3) . . ?
F14 C10 F13 108.8(4) . . ?
F14 C10 F15 108.1(3) . . ?
F15 C10 C9 110.9(3) . . ?
F13A C10 C9 115.2(10) . . ?
F13A C10 F14A 107.0(12) . . ?
F13A C10 F15A 114.2(12) . . ?
F14A C10 C9 105.4(7) . . ?
F15A C10 C9 110.1(8) . . ?
F15A C10 F14A 103.8(10) . . ?
O11 C11 O12 127.9(3) . . ?
O11 C11 C12 120.6(3) . . ?
O12 C11 C12 111.6(3) . . ?
F16 C12 F17 108.3(3) . . ?
F16 C12 F18 109.5(3) . . ?
F16 C12 C11 111.1(3) . . ?
F17 C12 F18 107.4(3) . . ?
F17 C12 C11 110.9(3) . . ?
F18 C12 C11 109.6(3) . . ?
O13 C13 C14 117.3(3) . . ?
O14 C13 O13 127.6(3) . . ?
O14 C13 C14 115.0(3) . . ?
F19 C14 C13 110.4(3) . . ?
F20 C14 C13 108.5(5) . . ?
F20 C14 F19 105.8(4) . . ?
F21 C14 C13 114.2(4) . . ?
F21 C14 F19 107.7(4) . . ?
F21 C14 F20 109.9(6) . . ?
F19A C14 C13 113.8(5) . . ?
F19A C14 F21A 103.7(6) . . ?
F20A C14 C13 114.4(7) . . ?
F20A C14 F19A 112.0(7) . . ?
F20A C14 F21A 105.9(8) . . ?
F21A C14 C13 106.0(5) . . ?
O16 C15 C16 116.7(3) . . ?
O15 C15 O16 127.1(3) . . ?
O15 C15 C16 115.9(3) . . ?
O15A C15 O16 123.6(9) . . ?
O15A C15 C16 115.7(9) . . ?
F22 C16 C15 109.3(3) . . ?
F23 C16 F22 108.5(3) . . ?
F23 C16 F24 109.0(3) . . ?
F23 C16 C15 112.2(2) . . ?
F24 C16 F22 106.4(3) . . ?
F24 C16 C15 111.3(3) . . ?
C7 O7A Mn1 173(2) . . ?
C15 O15 Mn2 153.0(8) . . ?
C7 O7 Mn1 162(2) . . ?
C15 O15A Mn2 166.0(17) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_gunt21o05
_database_code_depnum_ccdc_archive 'CCDC 1508838'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             2015-07-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 F24 Fe3 O17'
_chemical_formula_sum            'C16 H F24 Fe3 O17'
_chemical_formula_weight         1088.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.7505(11)
_cell_length_b                   21.236(2)
_cell_length_c                   16.0879(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.358(2)
_cell_angle_gamma                90
_cell_volume                     3330.2(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.856
_cell_measurement_theta_min      2.299
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0677 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.9241.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_recrystallization_method 'crystallized from trifluoroacetic acid'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.0025
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (10 s exposure) covering -0.300° degrees in ω.
 The crystal to detector distance was 4.956 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         1.588
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Platform with a Apex I-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6265
_reflns_number_total             7688
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0710
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²+12.5704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1632
_refine_special_details          
'Several trifluoroacetyl groups are strongly disordered and were described by split positions. A description by anisotropic displacement parameters has not been possible with the TFA-group O50 O51 C52 C53 F54 F55 F56 and the refinement has been performed therefore by isotropic displacement parameters. Most likely as a result of this disorder, it was not possible to located the hydrogen-atom at the oxygen-atom O51/O51A . The hydrogen-atom has been omitted from the refinement.'
_olex2_refinement_description    
;
1. Restrained distances
 O51-C52 \\sim C52A-O51A
 with sigma of 0.001
2. Uiso/Uaniso restraints and constraints
Uiso(O50A) = Uiso(O50)
Uiso(C53A) = Uiso(C53)
Uiso(C52A) = Uiso(C52)
Uanis(C11) = Uanis(C11A)
Uanis(C10A) = Uanis(C10)
Uiso(F55A) = Uiso(F55) = Uiso(F54) = Uiso(F54A) = Uiso(F56A) = Uiso(F56)
Uiso(O51A) = Uiso(O51)
3. Rigid body (RIGU) restrains
 C3, C4, F5, F6, F7, F5A, F6A, F7A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O8, O9, F12, F13, F14, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, O9, F12A, F13A, F14A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F54, F55, F56, O50, O51, C52, C53, F54A, F55A, F56A, O50A, O51A, C52A, C53A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5A)=Sof(F6A)=Sof(F7A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F7)=FVAR(1)
 Sof(F54A)=Sof(F55A)=Sof(F56A)=Sof(O50A)=Sof(O51A)=Sof(C52A)=Sof(C53A)=1-FVAR(2)
 Sof(F54)=Sof(F55)=Sof(F56)=Sof(O50)=Sof(O51)=Sof(C52)=Sof(C53)=FVAR(2)
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(C10A)=Sof(C11A)=1-FVAR(3)
 Sof(F12)=Sof(F13)=Sof(F14)=Sof(C10)=Sof(C11)=FVAR(3)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.01033(7) 0.32932(3) 0.40576(4) 0.01225(16) Uani 1 1 d . . . . .
Fe2 Fe -0.01676(7) 0.25062(3) 0.22188(4) 0.01327(16) Uani 1 1 d . . . . .
Fe3 Fe 0.13088(7) 0.39023(3) 0.23257(4) 0.01569(17) Uani 1 1 d . . . . .
F19 F -0.4331(4) 0.2666(2) 0.4282(2) 0.0576(13) Uani 1 1 d . . . . .
F20 F -0.4311(4) 0.1977(2) 0.3315(3) 0.0579(13) Uani 1 1 d . . . . .
F21 F -0.4736(4) 0.2928(2) 0.3021(3) 0.0493(11) Uani 1 1 d . . . . .
F26 F 0.1971(5) 0.14058(18) 0.4942(2) 0.0471(11) Uani 1 1 d . . . . .
F27 F 0.1479(5) 0.08839(17) 0.3855(3) 0.0560(12) Uani 1 1 d . . . . .
F28 F 0.3187(4) 0.1500(2) 0.3871(3) 0.0661(15) Uani 1 1 d . . . . .
F33 F 0.4902(4) 0.2894(2) 0.1081(3) 0.0571(13) Uani 1 1 d . . . . .
F34 F 0.4331(4) 0.1990(2) 0.1533(3) 0.0489(11) Uani 1 1 d . . . . .
F35 F 0.3529(4) 0.23117(19) 0.0363(2) 0.0376(9) Uani 1 1 d . . . . .
F40 F 0.3973(4) 0.48335(16) 0.4429(3) 0.0446(10) Uani 1 1 d . . . . .
F41 F 0.5224(4) 0.4092(2) 0.3981(2) 0.0430(9) Uani 1 1 d . . . . .
F42 F 0.4252(3) 0.39963(17) 0.5149(2) 0.0331(8) Uani 1 1 d . . . . .
F47 F -0.2699(3) 0.10081(16) 0.0234(2) 0.0300(7) Uani 1 1 d . . . . .
F48 F -0.0999(4) 0.04158(15) 0.0600(2) 0.0363(9) Uani 1 1 d . . . . .
F49 F -0.2330(5) 0.0771(2) 0.1521(2) 0.0519(12) Uani 1 1 d . . . . .
O1 O -0.0946(4) 0.30102(17) 0.1258(2) 0.0238(8) Uani 1 1 d . . . . .
O2 O 0.0116(4) 0.39436(18) 0.1306(2) 0.0242(8) Uani 1 1 d . . . . .
O8 O 0.0166(4) 0.45844(17) 0.2788(2) 0.0280(9) Uani 1 1 d . U . . .
O9 O -0.0774(4) 0.41456(16) 0.3899(2) 0.0212(8) Uani 1 1 d . U . . .
O15 O -0.2055(4) 0.25159(19) 0.2684(2) 0.0261(9) Uani 1 1 d . . . . .
O16 O -0.1788(4) 0.29189(17) 0.3962(2) 0.0200(7) Uani 1 1 d . . . . .
O22 O 0.0566(4) 0.19060(16) 0.3081(2) 0.0232(8) Uani 1 1 d . . . . .
O23 O 0.0974(4) 0.24432(15) 0.4258(2) 0.0175(7) Uani 1 1 d . . . . .
O29 O 0.2719(4) 0.33503(17) 0.1738(2) 0.0216(8) Uani 1 1 d . . . . .
O30 O 0.1666(4) 0.24141(17) 0.1660(2) 0.0230(8) Uani 1 1 d . . . . .
O36 O 0.2816(4) 0.40429(18) 0.3169(2) 0.0244(8) Uani 1 1 d . . . . .
O37 O 0.1930(4) 0.36943(17) 0.4352(2) 0.0193(7) Uani 1 1 d . . . . .
O43 O -0.0804(4) 0.17430(16) 0.1611(2) 0.0170(7) Uani 1 1 d . . . . .
O44 O -0.0214(4) 0.16893(17) 0.0283(2) 0.0191(7) Uani 1 1 d . . . . .
O57 O 0.0429(3) 0.32369(15) 0.28614(19) 0.0135(7) Uani 1 1 d . . . . .
C3 C -0.0737(5) 0.3563(2) 0.1027(3) 0.0183(10) Uani 1 1 d . U . . .
C4 C -0.1666(6) 0.3793(3) 0.0299(3) 0.0259(10) Uani 1 1 d . U . . .
C17 C -0.2447(5) 0.2677(2) 0.3380(3) 0.0169(10) Uani 1 1 d . . . . .
C18 C -0.3978(6) 0.2556(3) 0.3516(4) 0.0271(12) Uani 1 1 d . . . . .
C24 C 0.1064(5) 0.1982(2) 0.3791(3) 0.0159(10) Uani 1 1 d . . . . .
C25 C 0.1938(6) 0.1429(3) 0.4121(3) 0.0234(11) Uani 1 1 d . . . . .
C31 C 0.2633(5) 0.2776(3) 0.1553(3) 0.0196(10) Uani 1 1 d . . . . .
C32 C 0.3889(6) 0.2484(3) 0.1124(4) 0.0294(13) Uani 1 1 d . . . . .
C38 C 0.2825(5) 0.3952(2) 0.3932(3) 0.0180(10) Uani 1 1 d . . . . .
C39 C 0.4099(5) 0.4217(2) 0.4396(3) 0.0219(11) Uani 1 1 d . . . . .
C45 C -0.0828(5) 0.1506(2) 0.0909(3) 0.0151(9) Uani 1 1 d . . . . .
C46 C -0.1735(6) 0.0917(3) 0.0822(3) 0.0225(11) Uani 1 1 d . . . . .
F5 F -0.1466(7) 0.4392(2) 0.0122(4) 0.0505(15) Uani 0.782(6) 1 d . U P A 1
F6 F -0.1397(6) 0.3477(3) -0.0379(3) 0.0452(14) Uani 0.782(6) 1 d . U P A 1
F7 F -0.2946(5) 0.3721(3) 0.0466(4) 0.0568(16) Uani 0.782(6) 1 d . U P A 1
F12 F -0.1165(9) 0.5625(4) 0.3107(6) 0.0339(17) Uani 0.82(2) 1 d . U P B 1
F13 F -0.2218(10) 0.5182(4) 0.4106(5) 0.053(2) Uani 0.82(2) 1 d . U P B 1
F14 F -0.2750(7) 0.4929(3) 0.2853(7) 0.057(2) Uani 0.82(2) 1 d . U P B 1
F54 F 0.4808(9) 0.5567(4) 0.2198(5) 0.0479(9) Uiso 0.577(9) 1 d . U P C 1
F55 F 0.3043(8) 0.5851(4) 0.1575(6) 0.0479(9) Uiso 0.577(9) 1 d . U P C 1
F56 F 0.4531(9) 0.5524(4) 0.0762(5) 0.0479(9) Uiso 0.577(9) 1 d . U P C 1
O50 O 0.2295(9) 0.4686(4) 0.1764(6) 0.0204(11) Uiso 0.577(9) 1 d . U P C 1
O51 O 0.4409(10) 0.4338(5) 0.1432(7) 0.0433(16) Uiso 0.577(9) 1 d D U P C 1
C10 C -0.0641(18) 0.4546(8) 0.3368(11) 0.0175(15) Uani 0.82(2) 1 d . U P B 1
C11 C -0.172(2) 0.5087(6) 0.3367(12) 0.0296(18) Uani 0.82(2) 1 d . U P B 1
C52 C 0.3500(13) 0.4763(6) 0.1600(9) 0.0291(16) Uiso 0.577(9) 1 d D U P C 1
C53 C 0.4036(13) 0.5442(6) 0.1520(8) 0.034(2) Uiso 0.577(9) 1 d . U P C 1
F5A F -0.0950(17) 0.3860(10) -0.0353(9) 0.033(3) Uani 0.218(6) 1 d . U P A 2
F6A F -0.2534(18) 0.3330(9) 0.0039(11) 0.038(3) Uani 0.218(6) 1 d . U P A 2
F7A F -0.228(2) 0.4276(9) 0.0479(10) 0.037(3) Uani 0.218(6) 1 d . U P A 2
F12A F -0.155(4) 0.563(2) 0.297(3) 0.032(6) Uani 0.18(2) 1 d . U P B 2
F13A F -0.164(4) 0.5358(16) 0.4229(18) 0.043(6) Uani 0.18(2) 1 d . U P B 2
F14A F -0.289(3) 0.4967(13) 0.334(3) 0.042(6) Uani 0.18(2) 1 d . U P B 2
F54A F 0.5153(12) 0.5489(5) 0.1969(7) 0.0479(9) Uiso 0.423(9) 1 d . U P C 2
F55A F 0.3357(12) 0.5748(5) 0.1279(8) 0.0479(9) Uiso 0.423(9) 1 d . U P C 2
F56A F 0.5131(13) 0.5341(5) 0.0785(6) 0.0479(9) Uiso 0.423(9) 1 d . U P C 2
O50A O 0.2514(12) 0.4597(6) 0.1695(8) 0.0204(11) Uiso 0.423(9) 1 d . U P C 2
O51A O 0.4639(14) 0.4217(6) 0.1560(9) 0.0433(16) Uiso 0.423(9) 1 d D U P C 2
C10A C -0.077(9) 0.462(4) 0.334(6) 0.0175(15) Uani 0.18(2) 1 d . U P B 2
C11A C -0.175(10) 0.519(3) 0.343(6) 0.0296(18) Uani 0.18(2) 1 d . U P B 2
C52A C 0.3721(16) 0.4659(7) 0.1543(13) 0.0291(16) Uiso 0.423(9) 1 d D U P C 2
C53A C 0.4352(18) 0.5304(8) 0.1393(11) 0.034(2) Uiso 0.423(9) 1 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 O9 2.016(3) . ?
Fe1 O16 2.011(4) . ?
Fe1 O23 2.017(3) . ?
Fe1 O37 2.021(3) . ?
Fe1 O44 2.003(3) 4_566 ?
Fe1 O57 1.962(3) . ?
Fe2 O1 2.014(4) . ?
Fe2 O15 2.003(4) . ?
Fe2 O22 2.003(4) . ?
Fe2 O30 2.030(4) . ?
Fe2 O43 1.984(3) . ?
Fe2 O57 1.946(3) . ?
Fe3 O2 1.991(4) . ?
Fe3 O8 1.983(4) . ?
Fe3 O29 2.054(4) . ?
Fe3 O36 1.999(4) . ?
Fe3 O57 1.874(3) . ?
Fe3 O50 2.134(9) . ?
Fe3 O50A 2.155(13) . ?
F19 C18 1.308(7) . ?
F20 C18 1.310(7) . ?
F21 C18 1.332(7) . ?
F26 C25 1.322(6) . ?
F27 C25 1.309(7) . ?
F28 C25 1.301(7) . ?
F33 C32 1.321(7) . ?
F34 C32 1.304(7) . ?
F35 C32 1.318(6) . ?
F40 C39 1.316(6) . ?
F41 C39 1.324(6) . ?
F42 C39 1.303(6) . ?
F47 C46 1.332(6) . ?
F48 C46 1.337(7) . ?
F49 C46 1.315(6) . ?
O1 C3 1.249(6) . ?
O2 C3 1.237(6) . ?
O8 C10 1.238(18) . ?
O8 C10A 1.29(9) . ?
O9 C10 1.214(16) . ?
O9 C10A 1.35(7) . ?
O15 C17 1.240(6) . ?
O16 C17 1.236(6) . ?
O22 C24 1.242(6) . ?
O23 C24 1.238(6) . ?
O29 C31 1.258(6) . ?
O30 C31 1.232(6) . ?
O36 C38 1.243(6) . ?
O37 C38 1.243(6) . ?
O43 C45 1.236(6) . ?
O44 Fe1 2.002(3) 4_565 ?
O44 C45 1.247(6) . ?
C3 C4 1.542(7) . ?
C4 F5 1.319(8) . ?
C4 F6 1.312(7) . ?
C4 F7 1.292(8) . ?
C4 F5A 1.283(17) . ?
C4 F6A 1.357(17) . ?
C4 F7A 1.226(17) . ?
C17 C18 1.535(7) . ?
C24 C25 1.539(7) . ?
C31 C32 1.549(7) . ?
C38 C39 1.541(7) . ?
C45 C46 1.537(7) . ?
F12 C11 1.335(19) . ?
F13 C11 1.312(18) . ?
F14 C11 1.33(2) . ?
F54 C53 1.337(15) . ?
F55 C53 1.304(15) . ?
F56 C53 1.334(15) . ?
O50 C52 1.222(16) . ?
O51 C52 1.297(9) . ?
C10 C11 1.557(16) . ?
C52 C53 1.540(18) . ?
F12A C11A 1.23(10) . ?
F13A C11A 1.33(9) . ?
F14A C11A 1.21(10) . ?
F54A C53A 1.26(2) . ?
F55A C53A 1.36(2) . ?
F56A C53A 1.25(2) . ?
O50A C52A 1.21(2) . ?
O51A C52A 1.297(9) . ?
C10A C11A 1.55(8) . ?
C52A C53A 1.52(2) . ?

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
O9 Fe1 O23 178.07(14) . . ?
O9 Fe1 O37 91.14(15) . . ?
O16 Fe1 O9 87.70(15) . . ?
O16 Fe1 O23 92.31(15) . . ?
O16 Fe1 O37 170.55(14) . . ?
O23 Fe1 O37 88.52(15) . . ?
O44 Fe1 O9 91.88(14) 4_566 . ?
O44 Fe1 O16 85.41(14) 4_566 . ?
O44 Fe1 O23 86.19(14) 4_566 . ?
O44 Fe1 O37 85.25(14) 4_566 . ?
O57 Fe1 O9 90.50(14) . . ?
O57 Fe1 O16 94.03(14) . . ?
O57 Fe1 O23 91.43(14) . . ?
O57 Fe1 O37 95.36(14) . . ?
O57 Fe1 O44 177.53(14) . 4_566 ?
O1 Fe2 O30 91.78(16) . . ?
O15 Fe2 O1 87.05(17) . . ?
O15 Fe2 O22 93.68(17) . . ?
O15 Fe2 O30 173.32(15) . . ?
O22 Fe2 O1 172.53(14) . . ?
O22 Fe2 O30 86.64(16) . . ?
O43 Fe2 O1 87.04(14) . . ?
O43 Fe2 O15 85.02(15) . . ?
O43 Fe2 O22 85.62(14) . . ?
O43 Fe2 O30 88.36(14) . . ?
O57 Fe2 O1 94.96(14) . . ?
O57 Fe2 O15 93.39(14) . . ?
O57 Fe2 O22 92.42(14) . . ?
O57 Fe2 O30 93.25(14) . . ?
O57 Fe2 O43 177.39(14) . . ?
O2 Fe3 O29 91.74(16) . . ?
O2 Fe3 O36 163.48(15) . . ?
O2 Fe3 O50 82.9(3) . . ?
O2 Fe3 O50A 84.0(4) . . ?
O8 Fe3 O2 87.38(17) . . ?
O8 Fe3 O29 167.85(15) . . ?
O8 Fe3 O36 92.69(17) . . ?
O8 Fe3 O50 81.5(2) . . ?
O8 Fe3 O50A 89.6(3) . . ?
O29 Fe3 O50 86.4(2) . . ?
O29 Fe3 O50A 78.2(3) . . ?
O36 Fe3 O29 84.72(16) . . ?
O36 Fe3 O50 80.7(3) . . ?
O36 Fe3 O50A 79.4(4) . . ?
O57 Fe3 O2 98.48(14) . . ?
O57 Fe3 O8 96.38(15) . . ?
O57 Fe3 O29 95.74(14) . . ?
O57 Fe3 O36 97.93(14) . . ?
O57 Fe3 O50 177.4(3) . . ?
O57 Fe3 O50A 173.6(3) . . ?
C3 O1 Fe2 131.9(3) . . ?
C3 O2 Fe3 130.2(3) . . ?
C10 O8 Fe3 127.4(7) . . ?
C10A O8 Fe3 135(3) . . ?
C10 O9 Fe1 131.7(8) . . ?
C10A O9 Fe1 138(4) . . ?
C17 O15 Fe2 130.3(3) . . ?
C17 O16 Fe1 133.0(3) . . ?
C24 O22 Fe2 132.8(3) . . ?
C24 O23 Fe1 130.2(3) . . ?
C31 O29 Fe3 128.4(3) . . ?
C31 O30 Fe2 133.4(4) . . ?
C38 O36 Fe3 129.4(3) . . ?
C38 O37 Fe1 133.1(3) . . ?
C45 O43 Fe2 141.4(3) . . ?
C45 O44 Fe1 152.9(3) . 4_565 ?
Fe2 O57 Fe1 121.10(16) . . ?
Fe3 O57 Fe1 119.47(16) . . ?
Fe3 O57 Fe2 119.43(16) . . ?
O1 C3 C4 115.3(5) . . ?
O2 C3 O1 128.2(5) . . ?
O2 C3 C4 116.5(5) . . ?
F5 C4 C3 112.5(5) . . ?
F6 C4 C3 110.1(5) . . ?
F6 C4 F5 106.2(6) . . ?
F7 C4 C3 111.0(5) . . ?
F7 C4 F5 107.9(6) . . ?
F7 C4 F6 109.0(6) . . ?
F5A C4 C3 109.6(8) . . ?
F5A C4 F6A 100.1(12) . . ?
F6A C4 C3 110.8(8) . . ?
F7A C4 C3 111.6(8) . . ?
F7A C4 F5A 112.3(13) . . ?
F7A C4 F6A 111.9(13) . . ?
O15 C17 C18 113.9(4) . . ?
O16 C17 O15 129.3(5) . . ?
O16 C17 C18 116.8(4) . . ?
F19 C18 F20 109.3(5) . . ?
F19 C18 F21 107.7(5) . . ?
F19 C18 C17 112.5(5) . . ?
F20 C18 F21 106.1(5) . . ?
F20 C18 C17 110.9(4) . . ?
F21 C18 C17 110.1(5) . . ?
O22 C24 C25 114.8(4) . . ?
O23 C24 O22 129.0(5) . . ?
O23 C24 C25 116.2(4) . . ?
F26 C25 C24 111.9(4) . . ?
F27 C25 F26 107.1(5) . . ?
F27 C25 C24 112.4(5) . . ?
F28 C25 F26 108.2(5) . . ?
F28 C25 F27 108.5(5) . . ?
F28 C25 C24 108.6(4) . . ?
O29 C31 C32 116.4(5) . . ?
O30 C31 O29 128.2(5) . . ?
O30 C31 C32 115.4(5) . . ?
F33 C32 C31 111.0(5) . . ?
F34 C32 F33 108.6(5) . . ?
F34 C32 F35 108.9(5) . . ?
F34 C32 C31 110.7(5) . . ?
F35 C32 F33 108.4(5) . . ?
F35 C32 C31 109.2(4) . . ?
O36 C38 C39 114.1(4) . . ?
O37 C38 O36 128.1(5) . . ?
O37 C38 C39 117.7(4) . . ?
F40 C39 F41 107.4(5) . . ?
F40 C39 C38 107.9(4) . . ?
F41 C39 C38 110.5(4) . . ?
F42 C39 F40 109.2(4) . . ?
F42 C39 F41 108.6(4) . . ?
F42 C39 C38 113.1(4) . . ?
O43 C45 O44 127.8(5) . . ?
O43 C45 C46 114.4(4) . . ?
O44 C45 C46 117.8(4) . . ?
F47 C46 F48 107.5(4) . . ?
F47 C46 C45 109.9(4) . . ?
F48 C46 C45 111.2(4) . . ?
F49 C46 F47 108.9(5) . . ?
F49 C46 F48 107.0(5) . . ?
F49 C46 C45 112.2(4) . . ?
C52 O50 Fe3 129.9(8) . . ?
O8 C10 C11 113.0(11) . . ?
O9 C10 O8 131.1(11) . . ?
O9 C10 C11 115.8(14) . . ?
F12 C11 C10 110.8(14) . . ?
F13 C11 F12 108.3(10) . . ?
F13 C11 F14 108.1(14) . . ?
F13 C11 C10 112.2(14) . . ?
F14 C11 F12 109.1(14) . . ?
F14 C11 C10 108.3(11) . . ?
O50 C52 O51 128.1(13) . . ?
O50 C52 C53 118.2(9) . . ?
O51 C52 C53 113.6(11) . . ?
F54 C53 C52 107.7(11) . . ?
F55 C53 F54 102.6(10) . . ?
F55 C53 F56 105.1(11) . . ?
F55 C53 C52 111.3(10) . . ?
F56 C53 F54 120.7(11) . . ?
F56 C53 C52 109.2(10) . . ?
C52A O50A Fe3 135.3(11) . . ?
O8 C10A O9 116(5) . . ?
O8 C10A C11A 124(6) . . ?
O9 C10A C11A 120(7) . . ?
F12A C11A F13A 112(6) . . ?
F12A C11A C10A 116(7) . . ?
F13A C11A C10A 106(7) . . ?
F14A C11A F12A 112(8) . . ?
F14A C11A F13A 106(7) . . ?
F14A C11A C10A 104(6) . . ?
O50A C52A O51A 126.1(17) . . ?
O50A C52A C53A 121.8(12) . . ?
O51A C52A C53A 111.9(15) . . ?
F54A C53A F55A 108.0(14) . . ?
F54A C53A C52A 114.1(15) . . ?
F55A C53A C52A 110.8(13) . . ?
F56A C53A F54A 100.2(14) . . ?
F56A C53A F55A 107.1(14) . . ?
F56A C53A C52A 115.8(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O9 C10 O8 -7(3) . . . . ?
Fe1 O9 C10 C11 168.3(9) . . . . ?
Fe1 O9 C10A O8 -13(12) . . . . ?
Fe1 O9 C10A C11A 174(4) . . . . ?
Fe1 O16 C17 O15 10.6(8) . . . . ?
Fe1 O16 C17 C18 -168.9(4) . . . . ?
Fe1 O23 C24 O22 -4.7(8) . . . . ?
Fe1 O23 C24 C25 173.8(3) . . . . ?
Fe1 O37 C38 O36 1.1(8) . . . . ?
Fe1 O37 C38 C39 178.9(3) . . . . ?
Fe1 O44 C45 O43 -163.9(5) 4_565 . . . ?
Fe1 O44 C45 C46 16.1(10) 4_565 . . . ?
Fe2 O1 C3 O2 6.2(8) . . . . ?
Fe2 O1 C3 C4 -173.9(3) . . . . ?
Fe2 O15 C17 O16 5.7(8) . . . . ?
Fe2 O15 C17 C18 -174.8(4) . . . . ?
Fe2 O22 C24 O23 18.6(8) . . . . ?
Fe2 O22 C24 C25 -160.0(4) . . . . ?
Fe2 O30 C31 O29 -4.2(8) . . . . ?
Fe2 O30 C31 C32 176.7(4) . . . . ?
Fe2 O43 C45 O44 10.1(9) . . . . ?
Fe2 O43 C45 C46 -169.9(4) . . . . ?
Fe3 O2 C3 O1 -10.4(8) . . . . ?
Fe3 O2 C3 C4 169.7(3) . . . . ?
Fe3 O8 C10 O9 16(3) . . . . ?
Fe3 O8 C10 C11 -159.8(9) . . . . ?
Fe3 O8 C10A O9 22(11) . . . . ?
Fe3 O8 C10A C11A -165(5) . . . . ?
Fe3 O29 C31 O30 2.2(8) . . . . ?
Fe3 O29 C31 C32 -178.7(3) . . . . ?
Fe3 O36 C38 O37 7.3(8) . . . . ?
Fe3 O36 C38 C39 -170.6(3) . . . . ?
Fe3 O50 C52 O51 28(2) . . . . ?
Fe3 O50 C52 C53 -156.4(9) . . . . ?
Fe3 O50A C52A O51A 18(3) . . . . ?
Fe3 O50A C52A C53A -155.3(13) . . . . ?
O1 C3 C4 F5 175.5(5) . . . . ?
O1 C3 C4 F6 -66.3(7) . . . . ?
O1 C3 C4 F7 54.5(7) . . . . ?
O1 C3 C4 F5A -110.6(11) . . . . ?
O1 C3 C4 F6A -1.1(11) . . . . ?
O1 C3 C4 F7A 124.4(12) . . . . ?
O2 Fe3 O57 Fe1 -136.85(19) . . . . ?
O2 Fe3 O57 Fe2 42.3(2) . . . . ?
O2 C3 C4 F5 -4.6(7) . . . . ?
O2 C3 C4 F6 113.6(6) . . . . ?
O2 C3 C4 F7 -125.7(6) . . . . ?
O2 C3 C4 F5A 69.3(12) . . . . ?
O2 C3 C4 F6A 178.8(10) . . . . ?
O2 C3 C4 F7A -55.8(13) . . . . ?
O8 Fe3 O57 Fe1 -48.6(2) . . . . ?
O8 Fe3 O57 Fe2 130.6(2) . . . . ?
O8 C10 C11 F12 -35(2) . . . . ?
O8 C10 C11 F13 -156.6(16) . . . . ?
O8 C10 C11 F14 84.1(19) . . . . ?
O8 C10A C11A F12A -2(13) . . . . ?
O8 C10A C11A F13A -127(9) . . . . ?
O8 C10A C11A F14A 121(9) . . . . ?
O9 C10 C11 F12 148.2(17) . . . . ?
O9 C10 C11 F13 27(2) . . . . ?
O9 C10 C11 F14 -92.2(19) . . . . ?
O9 C10A C11A F12A 170(8) . . . . ?
O9 C10A C11A F13A 46(10) . . . . ?
O9 C10A C11A F14A -66(10) . . . . ?
O15 C17 C18 F19 173.0(5) . . . . ?
O15 C17 C18 F20 50.2(7) . . . . ?
O15 C17 C18 F21 -66.9(6) . . . . ?
O16 C17 C18 F19 -7.4(7) . . . . ?
O16 C17 C18 F20 -130.2(5) . . . . ?
O16 C17 C18 F21 112.7(5) . . . . ?
O22 C24 C25 F26 -154.2(5) . . . . ?
O22 C24 C25 F27 -33.7(6) . . . . ?
O22 C24 C25 F28 86.4(6) . . . . ?
O23 C24 C25 F26 27.0(7) . . . . ?
O23 C24 C25 F27 147.6(5) . . . . ?
O23 C24 C25 F28 -92.4(6) . . . . ?
O29 Fe3 O57 Fe1 130.52(19) . . . . ?
O29 Fe3 O57 Fe2 -50.3(2) . . . . ?
O29 C31 C32 F33 4.5(7) . . . . ?
O29 C31 C32 F34 125.2(5) . . . . ?
O29 C31 C32 F35 -115.0(5) . . . . ?
O30 C31 C32 F33 -176.2(5) . . . . ?
O30 C31 C32 F34 -55.6(6) . . . . ?
O30 C31 C32 F35 64.3(6) . . . . ?
O36 Fe3 O57 Fe1 45.1(2) . . . . ?
O36 Fe3 O57 Fe2 -135.7(2) . . . . ?
O36 C38 C39 F40 74.0(6) . . . . ?
O36 C38 C39 F41 -43.1(6) . . . . ?
O36 C38 C39 F42 -165.1(5) . . . . ?
O37 C38 C39 F40 -104.1(5) . . . . ?
O37 C38 C39 F41 138.7(5) . . . . ?
O37 C38 C39 F42 16.8(7) . . . . ?
O43 C45 C46 F47 121.5(5) . . . . ?
O43 C45 C46 F48 -119.6(5) . . . . ?
O43 C45 C46 F49 0.2(7) . . . . ?
O44 C45 C46 F47 -58.5(6) . . . . ?
O44 C45 C46 F48 60.4(6) . . . . ?
O44 C45 C46 F49 -179.9(5) . . . . ?
O50 C52 C53 F54 106.1(14) . . . . ?
O50 C52 C53 F55 -5.6(18) . . . . ?
O50 C52 C53 F56 -121.2(13) . . . . ?
O51 C52 C53 F54 -77.5(14) . . . . ?
O51 C52 C53 F55 170.8(11) . . . . ?
O51 C52 C53 F56 55.2(15) . . . . ?
O50A C52A C53A F54A 109(2) . . . . ?
O50A C52A C53A F55A -13(2) . . . . ?
O50A C52A C53A F56A -135.1(19) . . . . ?
O51A C52A C53A F54A -65(2) . . . . ?
O51A C52A C53A F55A 172.8(15) . . . . ?
O51A C52A C53A F56A 51(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
