# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_knoks14
_database_code_depnum_ccdc_archive 'CCDC 1996869'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-04-14 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_vrf_PLAT430_knoks14             
;
PROBLEM: _B Short Inter D...A Contact  O12      ..O19'     .       2.84 Ang.  
                                                1-x,y,1/2-z  =      2_655 Check 
RESPONSE: The atoms are close due to hydrogen bonding. Due to disorder,
however, hydrogen atoms were not placed on atom pair O19/O19' (see alert
responses below).
;

_vrf_PLAT041_knoks14             
;
PROBLEM: _C Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT043_knoks14             
;
PROBLEM: _C Calculated and Reported Mol. Weight Differ by .. 5.03 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT068_knoks14             
;
PROBLEM: _C Reported F000 Differs from Calcd (or Missing).
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_FORMU01_knoks14             
;
PROBLEM: _G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_CELLZ01_knoks14             
;
PROBLEM: _G Difference between formula and atom_site contents detected.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT007_knoks14             
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 8 
RESPONSE: Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.
;

_vrf_PLAT301_knoks14             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 22% 
RESPONSE: Two metal sites were modeled as a disorder of Fe and Zn:
Fe2:Zn2, 0.513(3):0.487(3) and Fe3:Zn3, 0.487(3):0.513(3). The metal
ratio between the two sites was constrained to 1:1. Two CF3 groups
were modeled as disordered over two positions each: C4-F4-F5-F6,
0.58(3):0.42(3) and C8-F10-F11-F12, 0.687(7):0.313(7).
;

_vrf_PLAT302_knoks14             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-4, 6-8  ) .. 100% 
RESPONSE: Cocrystallized water solvent molecules O17, O18, and O19
were modeled as disordered over two positions each (0.653(6):0.347(6),
0.598(9):0.402(9), and 0.72(1):0.28(1), respectively).
;

_vrf_PLAT311_knoks14             
;
PROBLEM: _G Isolated Disordered Oxygen Atom (No H's ?) .. O17 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O17' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O19 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT860_knoks14             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 153 
RESPONSE: Positional and anisotropic displacement parameters,
respectively, for the two metal types of each site disorder were
constrained to be equivalent. Analogous bond lengths and angles
between the two positions of the disordered CF3 groups were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained to be similar and/or
constrained to be equivalent.
;

_audit_creation_date             2020-04-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 F18 Fe2 O16 Zn1, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 F18 Fe2 O19.50 Zn'
_chemical_formula_weight         988.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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                   33.6920(4)
_cell_length_b                   10.70450(10)
_cell_length_c                   16.4568(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.6740(10)
_cell_angle_gamma                90
_cell_volume                     5928.78(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19371
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.6430
_cell_measurement_theta_min      2.6340
_shelx_estimated_absorpt_T_max   0.251
_shelx_estimated_absorpt_T_min   0.168
_exptl_absorpt_coefficient_mu    10.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.181
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26971
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.758
_diffrn_reflns_theta_min         2.626
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  -4.00   0.50    0.30    --  -49.75 111.00-132.00  156
  2  ω    -71.00 -46.00   0.50    1.21    --  -84.25 111.00-132.00   50
  3  ω     -4.00  24.00   0.50    0.30    --  -49.75  19.00-180.00   56
  4  ω   -107.00 -73.00   0.50    0.30    --  -49.75-125.00-120.00   68
  5  ω   -120.00 -73.00   0.50    0.30    --  -49.75-125.00 -90.00   94
  6  ω   -121.00 -94.00   0.50    0.30    --  -49.75-125.00 -60.00   54
  7  ω   -119.00 -82.00   0.50    1.21    --  -84.25-111.00 133.00   74
  8  ω     -5.00  24.00   0.50    0.30    --  -49.75  19.00 150.00   58
  9  ω    -41.00 -12.00   0.50    1.21    --  -84.25  45.00 150.00   58
 10  ω     47.00  88.00   0.50    0.30    --   49.75-111.00 133.00   82
 11  ω     68.00 107.00   0.50    1.21    --  105.75-111.00 133.00   78
 12  ω     85.00 111.00   0.50    1.21    --  105.75-125.00  90.00   52
 13  ω     66.00 104.00   0.50    1.21    --  105.75 -94.00 150.00   76
 14  ω     62.00 102.00   0.50    1.21    --  105.75 -94.00  60.00   80
 15  ω     52.00  80.00   0.50    1.21    --  105.75 -61.00  30.00   56
 16  ω     38.00  76.00   0.50    1.21    --  105.75 -61.00  60.00   76
 17  ω     36.00  78.00   0.50    1.21    --  105.75-125.00  60.00   84
 18  ω     34.00  70.00   0.50    1.21    --  105.75-125.00  90.00   72
 19  ω     38.00  80.00   0.50    1.21    --  105.75 -61.00 -30.00   84
 20  ω     63.00  89.00   0.50    1.21    --  105.75 -94.00 -90.00   52
 21  ω     76.00 106.00   0.50    1.21    --  105.75-125.00 -90.00   60
 22  ω     79.00 104.00   0.50    1.21    --  105.75 -94.00-180.00   50
 23  ω     47.00 106.00   0.50    1.21    --  105.75 -94.00-150.00  118
 24  ω     46.00  79.00   0.50    1.21    --  105.75 -61.00-120.00   66
 25  ω     37.00  75.00   0.50    1.21    --  105.75 -94.00-180.00   76
 26  ω     34.00 105.00   0.50    1.21    --  105.75 -94.00 -60.00  142
 27  ω     37.00  79.00   0.50    1.21    --  105.75 -61.00 -60.00   84
 28  ω     98.00 175.00   0.50    1.21    --  105.75  15.00 -30.00  154
 29  ω    148.00 178.00   0.50    1.21    --  105.75  30.00  60.00   60
 30  ω    101.00 126.00   0.50    1.21    --  105.75  30.00  60.00   50
 31  ω    105.00 149.00   0.50    1.21    --  105.75 111.00-132.00   88
 32  ω    144.00 170.00   0.50    1.21    --  105.75  61.00-150.00   52
 33  ω    110.00 137.00   0.50    1.21    --  105.75  61.00-150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035866000
_diffrn_orient_matrix_UB_12      -0.1406699000
_diffrn_orient_matrix_UB_13      -0.0179281000
_diffrn_orient_matrix_UB_21      0.0410787000
_diffrn_orient_matrix_UB_22      -0.0023399000
_diffrn_orient_matrix_UB_23      0.0451969000
_diffrn_orient_matrix_UB_31      -0.0198768000
_diffrn_orient_matrix_UB_32      -0.0301361000
_diffrn_orient_matrix_UB_33      0.0801385000
_diffrn_oxdiff_digest_frames     
;
0197e62376e25d64e65005bfb30d62dbf000058b3a9
;
_diffrn_oxdiff_digest_hkl        
;
0167025de2229b91732ef18b8daa5aff759a96
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5851
_reflns_number_total             6185
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         6185
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0919P)²+25.3725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1371
_refine_special_details          
;
Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were
included in the molecular formula.

Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.

Two metal sites were modeled as a disorder of Fe and Zn: Fe2:Zn2,
0.513(3):0.487(3) and Fe3:Zn3, 0.487(3):0.513(3). The metal
ratio between the two sites was constrained to 1:1. Two CF3 groups
were modeled as disordered over two positions each: C4-F4-F5-F6,
0.58(3):0.42(3) and C8-F10-F11-F12, 0.687(7):0.313(7).

Cocrystallized water solvent molecules O17, O18, and O19 were
modeled as disordered over two positions each (0.653(6):0.347(6),
0.598(9):0.402(9), and 0.72(1):0.28(1), respectively).

Positional and anisotropic displacement parameters, respectively,
for the two metal types of each site disorder were constrained
to be equivalent. Analogous bond lengths and angles between
the two positions of the disordered CF3 groups were restrained
to be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and/or constrained to be
equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Fe2, Zn2}
{Fe3, Zn3}
3. Restrained distances
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
 C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C4'-F4' \\sim C4'-F5' \\sim C4'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 C7-C8 \\sim C7-C8'
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F10' \\sim C8'-F11' \\sim C8'-F12'
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10'-F11' \\sim F11'-F12' \\sim
F12'-F10'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C4 \\sim C4': within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C8 \\sim C8': within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
Uanis(Fe2) = Uanis(Zn2)
Uanis(Fe3) = Uanis(Zn3)
5. Rigid body (RIGU) restrains
 F4, F5, F6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4', F5', F6', C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8', F10', F11', F12'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Fe2)+Sof(Zn2)]+1*[Sof(Fe3)+Sof(Zn3)]=1 with esd of 0.0001
 Sof(O17')=1-FVAR(1)
 Sof(O17)=FVAR(1)
 Sof(O18')=1-FVAR(2)
 Sof(O18)=FVAR(2)
 Sof(O19')=0.5*(1-FVAR(4))
 Sof(O19)=0.5*FVAR(4)
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C4')=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(4)
 Sof(Zn2)=1-FVAR(5)
 Sof(Fe2)=FVAR(5)
 Sof(Zn3)=1-FVAR(6)
 Sof(Fe3)=FVAR(6)
 Sof(C8')=Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(7)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C8)=FVAR(7)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.62076(2) 0.86278(4) 0.48747(3) 0.01166(13) Uani 1 1 d . U . . .
Fe2 Fe 0.63428(2) 0.56337(4) 0.53375(3) 0.01587(14) Uani 0.513(3) 1 d . U . A 1
Fe3 Fe 0.59767(2) 0.64860(4) 0.34835(3) 0.01566(14) Uani 0.487(3) 1 d . U . A 1
Zn2 Zn 0.63428(2) 0.56337(4) 0.53375(3) 0.01587(14) Uani 0.487(3) 1 d . U . A 2
Zn3 Zn 0.59767(2) 0.64860(4) 0.34835(3) 0.01566(14) Uani 0.513(3) 1 d . U . A 2
F1 F 0.57417(8) 0.8970(2) 0.74263(14) 0.0396(6) Uani 1 1 d . U . . .
F2 F 0.53909(8) 0.7351(4) 0.72354(17) 0.0568(9) Uani 1 1 d . U . . .
F3 F 0.59588(9) 0.7206(3) 0.78543(13) 0.0522(8) Uani 1 1 d . U . . .
F7 F 0.51930(8) 0.3313(2) 0.53944(14) 0.0374(6) Uani 1 1 d . U . . .
F8 F 0.53650(9) 0.2470(2) 0.42903(16) 0.0427(7) Uani 1 1 d . U . . .
F9 F 0.49340(8) 0.3956(3) 0.4272(2) 0.0552(8) Uani 1 1 d . U . . .
F13 F 0.47829(6) 0.85552(19) 0.32055(12) 0.0225(4) Uani 1 1 d . U . . .
F14 F 0.50704(6) 1.0323(2) 0.34113(15) 0.0315(5) Uani 1 1 d . U . . .
F15 F 0.48356(6) 0.9315(2) 0.44064(12) 0.0259(4) Uani 1 1 d . U . . .
F16 F 0.69320(9) 0.8543(3) 0.21131(19) 0.0556(9) Uani 1 1 d . U . . .
F17 F 0.65494(8) 1.0124(4) 0.2082(2) 0.0674(11) Uani 1 1 d . U . . .
F18 F 0.70446(8) 1.0034(3) 0.29323(15) 0.0458(7) Uani 1 1 d . U . . .
F4 F 0.7578(3) 0.8575(17) 0.5633(6) 0.027(2) Uani 0.42(3) 1 d D U . B 1
F5 F 0.7600(3) 0.6764(9) 0.6168(12) 0.027(3) Uani 0.42(3) 1 d D U . B 1
F6 F 0.7369(6) 0.8316(16) 0.6829(7) 0.025(3) Uani 0.42(3) 1 d D U . B 1
F10 F 0.72631(16) 0.3575(6) 0.3740(3) 0.0563(16) Uani 0.687(7) 1 d D U . C 1
F11 F 0.67826(16) 0.2895(5) 0.2969(5) 0.077(2) Uani 0.687(7) 1 d D U . C 1
F12 F 0.71028(11) 0.4518(4) 0.2650(2) 0.0390(11) Uani 0.687(7) 1 d D U . C 1
F4' F 0.7507(3) 0.9036(10) 0.5826(7) 0.029(2) Uani 0.58(3) 1 d D U . B 2
F5' F 0.76493(16) 0.7092(11) 0.5870(6) 0.0259(17) Uani 0.58(3) 1 d D U . B 2
F6' F 0.7367(5) 0.7951(12) 0.6874(5) 0.0235(18) Uani 0.58(3) 1 d D U . B 2
O1 O 0.62693(7) 1.0500(2) 0.50910(15) 0.0214(5) Uani 1 1 d . U . . .
H1A H 0.651235 1.070334 0.506620 0.032 Uiso 1 1 d R . . . .
H1B H 0.618985 1.066774 0.556240 0.032 Uiso 1 1 d R . . . .
O2 O 0.65269(7) 0.4266(2) 0.61472(16) 0.0249(5) Uani 1 1 d . U . . .
H2A H 0.676301 0.404567 0.605367 0.037 Uiso 1 1 d R . . A .
H2B H 0.637321 0.363957 0.609468 0.037 Uiso 1 1 d R . . . .
O3 O 0.57745(8) 0.5882(2) 0.23181(14) 0.0227(5) Uani 1 1 d . U . . .
H3A H 0.591369 0.526789 0.217099 0.034 Uiso 1 1 d R . . A .
H3B H 0.553259 0.566129 0.233149 0.034 Uiso 1 1 d R . . . .
O4 O 0.59621(7) 0.8441(2) 0.59668(13) 0.0173(4) Uani 1 1 d . U . . .
O5 O 0.60558(7) 0.6420(2) 0.63218(14) 0.0191(5) Uani 1 1 d . U . . .
O6 O 0.67649(7) 0.8500(2) 0.54676(14) 0.0174(5) Uani 1 1 d . U . . .
O7 O 0.68673(7) 0.6453(2) 0.57070(15) 0.0205(5) Uani 1 1 d . U . . .
O8 O 0.58505(7) 0.4521(2) 0.51505(13) 0.0186(5) Uani 1 1 d . U . . .
O9 O 0.56144(7) 0.5058(2) 0.38969(13) 0.0183(4) Uani 1 1 d . U . . .
O10 O 0.66499(8) 0.4609(2) 0.44661(15) 0.0267(5) Uani 1 1 d . U . . .
O11 O 0.64364(7) 0.5346(3) 0.32481(14) 0.0245(5) Uani 1 1 d . U . . .
O12 O 0.54807(7) 0.7569(2) 0.34701(13) 0.0172(4) Uani 1 1 d . U . . .
O13 O 0.56618(6) 0.9086(2) 0.43605(13) 0.0173(4) Uani 1 1 d . U . . .
O14 O 0.62680(7) 0.7908(2) 0.28730(14) 0.0231(5) Uani 1 1 d . U . . .
O15 O 0.65138(7) 0.9144(2) 0.38785(13) 0.0178(4) Uani 1 1 d . U . . .
O16 O 0.61793(6) 0.69438(19) 0.45767(11) 0.0111(4) Uani 1 1 d . U . . .
C1 C 0.59460(8) 0.7518(3) 0.64284(17) 0.0139(6) Uani 1 1 d . U . . .
C2 C 0.57602(10) 0.7771(3) 0.72570(19) 0.0195(6) Uani 1 1 d . U . . .
C3 C 0.69616(8) 0.7572(3) 0.57058(16) 0.0130(6) Uani 1 1 d D U . . .
C5 C 0.56119(8) 0.4484(3) 0.45481(17) 0.0127(5) Uani 1 1 d . U . . .
C6 C 0.52696(10) 0.3536(3) 0.4619(2) 0.0220(7) Uani 1 1 d . U . . .
C7 C 0.66459(10) 0.4700(3) 0.3715(2) 0.0205(6) Uani 1 1 d D U . . .
C9 C 0.54302(9) 0.8547(3) 0.38661(17) 0.0125(6) Uani 1 1 d . U . . .
C10 C 0.50200(9) 0.9195(3) 0.37221(18) 0.0156(6) Uani 1 1 d . U . . .
C11 C 0.64878(9) 0.8742(3) 0.31763(19) 0.0143(6) Uani 1 1 d . U . . .
C12 C 0.67604(10) 0.9381(3) 0.2565(2) 0.0223(7) Uani 1 1 d . U . . .
C4 C 0.73824(19) 0.7793(8) 0.6098(6) 0.0135(16) Uani 0.42(3) 1 d D U . B 1
C8 C 0.69561(16) 0.3913(5) 0.3265(3) 0.0299(12) Uani 0.687(7) 1 d D U . C 1
C4' C 0.73791(16) 0.7926(7) 0.6069(5) 0.0164(13) Uani 0.58(3) 1 d D U . B 2
O17 O 0.70803(14) 1.1163(4) 0.5046(3) 0.0395(10) Uani 0.653(6) 1 d . U . D 1
O17' O 0.6918(3) 1.1867(9) 0.5057(6) 0.0395(10) Uani 0.347(6) 1 d . U . D 2
O18 O 0.7294(3) 0.3555(10) 0.5636(8) 0.0519(15) Uani 0.402(9) 1 d . U . E 1
O18' O 0.72909(19) 0.3533(6) 0.6114(5) 0.0519(15) Uani 0.598(9) 1 d . U . E 2
O19 O 0.500000 0.5061(16) 0.250000 0.0321(18) Uani 0.280(10) 2 d S TU P F 1
O19' O 0.5033(3) 0.5754(8) 0.2277(4) 0.0321(18) Uani 0.360(5) 1 d . U . F 2
O20 O 0.60458(7) 0.7812(2) 0.11841(14) 0.0216(5) Uani 1 1 d . U . . .
H20A H 0.580628 0.760007 0.107376 0.032 Uiso 1 1 d R . . . .
H20B H 0.605848 0.813087 0.165826 0.032 Uiso 1 1 d R . . . .
C8' C 0.6904(3) 0.3711(8) 0.3302(5) 0.033(2) Uani 0.313(7) 1 d D U . C 2
F10' F 0.6831(3) 0.3644(12) 0.2515(5) 0.063(4) Uani 0.313(7) 1 d D U . C 2
F11' F 0.7277(3) 0.4017(12) 0.3454(9) 0.057(3) Uani 0.313(7) 1 d D U . C 2
F12' F 0.6843(3) 0.2581(7) 0.3572(7) 0.046(2) Uani 0.313(7) 1 d D U . 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 2.044(2) . ?
Fe1 O4 2.023(2) . ?
Fe1 O6 2.080(2) . ?
Fe1 O13 2.048(2) . ?
Fe1 O15 2.053(2) . ?
Fe1 O16 1.869(2) . ?
Fe2 O2 2.056(3) . ?
Fe2 O5 2.101(2) . ?
Fe2 O7 2.040(2) . ?
Fe2 O8 2.053(2) . ?
Fe2 O10 2.114(2) . ?
Fe2 O16 1.943(2) . ?
Fe3 O3 2.107(2) . ?
Fe3 O9 2.090(2) . ?
Fe3 O11 2.023(2) . ?
Fe3 O12 2.033(2) . ?
Fe3 O14 2.093(2) . ?
Fe3 O16 1.956(2) . ?
Zn2 O2 2.056(3) . ?
Zn2 O5 2.101(2) . ?
Zn2 O7 2.040(2) . ?
Zn2 O8 2.053(2) . ?
Zn2 O10 2.114(2) . ?
Zn2 O16 1.943(2) . ?
Zn3 O3 2.107(2) . ?
Zn3 O9 2.090(2) . ?
Zn3 O11 2.023(2) . ?
Zn3 O12 2.033(2) . ?
Zn3 O14 2.093(2) . ?
Zn3 O16 1.956(2) . ?
F1 C2 1.315(4) . ?
F2 C2 1.322(4) . ?
F3 C2 1.311(4) . ?
F7 C6 1.336(4) . ?
F8 C6 1.309(4) . ?
F9 C6 1.321(4) . ?
F13 C10 1.329(4) . ?
F14 C10 1.326(4) . ?
F15 C10 1.318(4) . ?
F16 C12 1.316(5) . ?
F17 C12 1.311(4) . ?
F18 C12 1.310(4) . ?
F4 C4 1.329(7) . ?
F5 C4 1.324(6) . ?
F6 C4 1.330(6) . ?
F10 C8 1.317(6) . ?
F11 C8 1.319(6) . ?
F12 C8 1.317(5) . ?
F4' C4' 1.331(6) . ?
F5' C4' 1.327(6) . ?
F6' C4' 1.329(6) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8516 . ?
O2 H2A 0.8505 . ?
O2 H2B 0.8490 . ?
O3 H3A 0.8496 . ?
O3 H3B 0.8500 . ?
O4 C1 1.250(4) . ?
O5 C1 1.247(4) . ?
O6 C3 1.248(4) . ?
O7 C3 1.239(4) . ?
O8 C5 1.248(4) . ?
O9 C5 1.236(4) . ?
O10 C7 1.239(4) . ?
O11 C7 1.232(4) . ?
O12 C9 1.250(4) . ?
O13 C9 1.243(4) . ?
O14 C11 1.249(4) . ?
O15 C11 1.233(4) . ?
C1 C2 1.551(4) . ?
C3 C4 1.548(7) . ?
C3 C4' 1.549(6) . ?
C5 C6 1.545(4) . ?
C7 C8 1.556(6) . ?
C7 C8' 1.547(8) . ?
C9 C10 1.554(4) . ?
C11 C12 1.552(4) . ?
O19' O19' 0.777(14) 2_655 ?
O20 H20A 0.8495 . ?
O20 H20B 0.8512 . ?
C8' F10' 1.309(7) . ?
C8' F11' 1.311(7) . ?
C8' F12' 1.308(7) . ?

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 O6 84.29(9) . . ?
O1 Fe1 O13 85.37(10) . . ?
O1 Fe1 O15 79.88(10) . . ?
O4 Fe1 O1 89.12(9) . . ?
O4 Fe1 O6 88.54(9) . . ?
O4 Fe1 O13 89.66(9) . . ?
O4 Fe1 O15 167.81(9) . . ?
O13 Fe1 O6 169.53(9) . . ?
O13 Fe1 O15 94.62(9) . . ?
O15 Fe1 O6 85.19(9) . . ?
O16 Fe1 O1 173.98(10) . . ?
O16 Fe1 O4 96.88(9) . . ?
O16 Fe1 O6 95.37(9) . . ?
O16 Fe1 O13 95.09(9) . . ?
O16 Fe1 O15 94.10(9) . . ?
O2 Fe2 O5 85.49(10) . . ?
O2 Fe2 O10 85.85(10) . . ?
O5 Fe2 O10 171.26(10) . . ?
O7 Fe2 O2 83.21(10) . . ?
O7 Fe2 O5 91.24(10) . . ?
O7 Fe2 O8 167.52(10) . . ?
O7 Fe2 O10 88.89(10) . . ?
O8 Fe2 O2 84.32(10) . . ?
O8 Fe2 O5 87.15(9) . . ?
O8 Fe2 O10 90.85(10) . . ?
O16 Fe2 O2 178.81(10) . . ?
O16 Fe2 O5 94.64(9) . . ?
O16 Fe2 O7 95.60(9) . . ?
O16 Fe2 O8 96.86(9) . . ?
O16 Fe2 O10 94.04(9) . . ?
O9 Fe3 O3 84.43(9) . . ?
O9 Fe3 O14 169.18(9) . . ?
O11 Fe3 O3 81.87(10) . . ?
O11 Fe3 O9 94.88(10) . . ?
O11 Fe3 O12 167.94(9) . . ?
O11 Fe3 O14 88.09(11) . . ?
O12 Fe3 O3 86.23(9) . . ?
O12 Fe3 O9 85.88(9) . . ?
O12 Fe3 O14 89.07(10) . . ?
O14 Fe3 O3 85.70(9) . . ?
O16 Fe3 O3 176.44(9) . . ?
O16 Fe3 O9 93.90(8) . . ?
O16 Fe3 O11 95.15(9) . . ?
O16 Fe3 O12 96.80(8) . . ?
O16 Fe3 O14 96.20(9) . . ?
O2 Zn2 O5 85.49(10) . . ?
O2 Zn2 O10 85.85(10) . . ?
O5 Zn2 O10 171.26(10) . . ?
O7 Zn2 O2 83.21(10) . . ?
O7 Zn2 O5 91.24(10) . . ?
O7 Zn2 O8 167.52(10) . . ?
O7 Zn2 O10 88.89(10) . . ?
O8 Zn2 O2 84.32(10) . . ?
O8 Zn2 O5 87.15(9) . . ?
O8 Zn2 O10 90.85(10) . . ?
O16 Zn2 O2 178.81(10) . . ?
O16 Zn2 O5 94.64(9) . . ?
O16 Zn2 O7 95.60(9) . . ?
O16 Zn2 O8 96.86(9) . . ?
O16 Zn2 O10 94.04(9) . . ?
O9 Zn3 O3 84.43(9) . . ?
O9 Zn3 O14 169.18(9) . . ?
O11 Zn3 O3 81.87(10) . . ?
O11 Zn3 O9 94.88(10) . . ?
O11 Zn3 O12 167.94(9) . . ?
O11 Zn3 O14 88.09(11) . . ?
O12 Zn3 O3 86.23(9) . . ?
O12 Zn3 O9 85.88(9) . . ?
O12 Zn3 O14 89.07(10) . . ?
O14 Zn3 O3 85.70(9) . . ?
O16 Zn3 O3 176.44(9) . . ?
O16 Zn3 O9 93.90(8) . . ?
O16 Zn3 O11 95.15(9) . . ?
O16 Zn3 O12 96.80(8) . . ?
O16 Zn3 O14 96.20(9) . . ?
Fe1 O1 H1A 109.5 . . ?
Fe1 O1 H1B 109.4 . . ?
H1A O1 H1B 109.5 . . ?
Fe2 O2 H2A 109.7 . . ?
Fe2 O2 H2B 109.4 . . ?
Zn2 O2 H2A 109.7 . . ?
Zn2 O2 H2B 109.4 . . ?
H2A O2 H2B 109.5 . . ?
Fe3 O3 H3A 109.7 . . ?
Fe3 O3 H3B 109.4 . . ?
Zn3 O3 H3A 109.7 . . ?
Zn3 O3 H3B 109.4 . . ?
H3A O3 H3B 109.5 . . ?
C1 O4 Fe1 130.5(2) . . ?
C1 O5 Fe2 129.5(2) . . ?
C1 O5 Zn2 129.5(2) . . ?
C3 O6 Fe1 130.9(2) . . ?
C3 O7 Fe2 129.3(2) . . ?
C3 O7 Zn2 129.3(2) . . ?
C5 O8 Fe2 128.6(2) . . ?
C5 O8 Zn2 128.6(2) . . ?
C5 O9 Fe3 132.3(2) . . ?
C5 O9 Zn3 132.3(2) . . ?
C7 O10 Fe2 130.8(2) . . ?
C7 O10 Zn2 130.8(2) . . ?
C7 O11 Fe3 129.9(2) . . ?
C7 O11 Zn3 129.9(2) . . ?
C9 O12 Fe3 127.2(2) . . ?
C9 O12 Zn3 127.2(2) . . ?
C9 O13 Fe1 133.1(2) . . ?
C11 O14 Fe3 127.6(2) . . ?
C11 O14 Zn3 127.6(2) . . ?
C11 O15 Fe1 129.7(2) . . ?
Fe1 O16 Fe2 121.17(10) . . ?
Fe1 O16 Fe3 119.61(10) . . ?
Fe1 O16 Zn2 121.17(10) . . ?
Fe1 O16 Zn3 119.61(10) . . ?
Fe2 O16 Fe3 119.21(10) . . ?
Zn2 O16 Zn3 119.21(10) . . ?
O4 C1 C2 115.3(3) . . ?
O5 C1 O4 129.7(3) . . ?
O5 C1 C2 115.0(3) . . ?
F1 C2 F2 106.5(3) . . ?
F1 C2 C1 112.5(3) . . ?
F2 C2 C1 109.6(3) . . ?
F3 C2 F1 108.6(3) . . ?
F3 C2 F2 108.1(3) . . ?
F3 C2 C1 111.4(3) . . ?
O6 C3 C4 118.1(4) . . ?
O6 C3 C4' 112.7(4) . . ?
O7 C3 O6 129.7(3) . . ?
O7 C3 C4 112.1(4) . . ?
O7 C3 C4' 117.7(4) . . ?
O8 C5 C6 114.6(3) . . ?
O9 C5 O8 130.0(3) . . ?
O9 C5 C6 115.3(3) . . ?
F7 C6 C5 111.6(3) . . ?
F8 C6 F7 107.5(3) . . ?
F8 C6 F9 109.9(3) . . ?
F8 C6 C5 110.1(3) . . ?
F9 C6 F7 105.9(3) . . ?
F9 C6 C5 111.8(3) . . ?
O10 C7 C8 117.1(3) . . ?
O10 C7 C8' 113.9(4) . . ?
O11 C7 O10 130.2(3) . . ?
O11 C7 C8 112.6(3) . . ?
O11 C7 C8' 115.3(4) . . ?
O12 C9 C10 115.8(3) . . ?
O13 C9 O12 129.3(3) . . ?
O13 C9 C10 114.8(3) . . ?
F13 C10 C9 111.8(2) . . ?
F14 C10 F13 107.8(3) . . ?
F14 C10 C9 109.6(2) . . ?
F15 C10 F13 107.7(2) . . ?
F15 C10 F14 108.3(3) . . ?
F15 C10 C9 111.4(2) . . ?
O14 C11 C12 114.4(3) . . ?
O15 C11 O14 129.7(3) . . ?
O15 C11 C12 115.8(3) . . ?
F16 C12 C11 110.8(3) . . ?
F17 C12 F16 108.1(3) . . ?
F17 C12 C11 109.9(3) . . ?
F18 C12 F16 107.0(3) . . ?
F18 C12 F17 108.7(3) . . ?
F18 C12 C11 112.2(3) . . ?
F4 C4 F6 107.1(8) . . ?
F4 C4 C3 108.9(7) . . ?
F5 C4 F4 106.7(7) . . ?
F5 C4 F6 108.3(8) . . ?
F5 C4 C3 113.6(6) . . ?
F6 C4 C3 111.9(11) . . ?
F10 C8 F11 108.3(6) . . ?
F10 C8 C7 113.1(5) . . ?
F11 C8 C7 109.1(4) . . ?
F12 C8 F10 106.2(5) . . ?
F12 C8 F11 107.4(5) . . ?
F12 C8 C7 112.6(4) . . ?
F4' C4' C3 113.8(5) . . ?
F5' C4' F4' 106.9(5) . . ?
F5' C4' F6' 108.2(6) . . ?
F5' C4' C3 111.2(5) . . ?
F6' C4' F4' 107.8(6) . . ?
F6' C4' C3 108.7(8) . . ?
H20A O20 H20B 108.0 . . ?
F10' C8' C7 112.8(7) . . ?
F10' C8' F11' 109.8(9) . . ?
F11' C8' C7 107.3(8) . . ?
F12' C8' C7 112.5(7) . . ?
F12' C8' F10' 105.1(8) . . ?
F12' C8' F11' 109.3(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O17 0.85 1.98 2.827(5) 178.2 . yes
O1 H1A O17' 0.85 1.85 2.634(9) 152.4 . yes
O1 H1B O20 0.85 1.99 2.683(3) 137.2 6_576 yes
O2 H2A O18 0.85 2.02 2.858(10) 170.5 . yes
O2 H2A O18' 0.85 1.86 2.694(7) 166.5 . yes
O2 H2B O20 0.85 1.91 2.754(3) 169.6 6_566 yes
O3 H3A O5 0.85 2.35 3.131(3) 153.7 6_565 yes
O3 H3B O19 0.85 1.94 2.783(6) 172.5 . yes
O3 H3B O19' 0.85 2.04 2.835(9) 154.8 2_655 yes
O3 H3B O19' 0.85 1.68 2.499(9) 159.9 . yes
O20 H20A F13 0.85 2.57 3.115(3) 122.8 2_655 yes
O20 H20B O14 0.85 2.10 2.846(3) 145.7 . yes

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 O4 C1 O5 -5.1(5) . . . . ?
Fe1 O4 C1 C2 175.2(2) . . . . ?
Fe1 O6 C3 O7 -5.7(5) . . . . ?
Fe1 O6 C3 C4 177.2(4) . . . . ?
Fe1 O6 C3 C4' 176.0(3) . . . . ?
Fe1 O13 C9 O12 -6.9(5) . . . . ?
Fe1 O13 C9 C10 173.3(2) . . . . ?
Fe1 O15 C11 O14 0.1(5) . . . . ?
Fe1 O15 C11 C12 178.4(2) . . . . ?
Fe2 O5 C1 O4 3.1(5) . . . . ?
Fe2 O5 C1 C2 -177.1(2) . . . . ?
Fe2 O7 C3 O6 -1.3(5) . . . . ?
Fe2 O7 C3 C4 175.9(4) . . . . ?
Fe2 O8 C5 O9 3.3(5) . . . . ?
Fe2 O8 C5 C6 -179.3(2) . . . . ?
Fe2 O10 C7 O11 -6.9(6) . . . . ?
Fe2 O10 C7 C8 171.5(3) . . . . ?
Fe3 O9 C5 O8 -6.3(5) . . . . ?
Fe3 O9 C5 C6 176.3(2) . . . . ?
Fe3 O11 C7 O10 -4.2(6) . . . . ?
Fe3 O11 C7 C8 177.3(3) . . . . ?
Fe3 O12 C9 O13 -0.8(5) . . . . ?
Fe3 O12 C9 C10 179.00(19) . . . . ?
Fe3 O14 C11 O15 -20.2(5) . . . . ?
Fe3 O14 C11 C12 161.5(2) . . . . ?
Zn2 O5 C1 O4 3.1(5) . . . . ?
Zn2 O5 C1 C2 -177.1(2) . . . . ?
Zn2 O7 C3 O6 -1.3(5) . . . . ?
Zn2 O7 C3 C4' 176.9(3) . . . . ?
Zn2 O8 C5 O9 3.3(5) . . . . ?
Zn2 O8 C5 C6 -179.3(2) . . . . ?
Zn2 O10 C7 O11 -6.9(6) . . . . ?
Zn2 O10 C7 C8' -177.3(4) . . . . ?
Zn3 O9 C5 O8 -6.3(5) . . . . ?
Zn3 O9 C5 C6 176.3(2) . . . . ?
Zn3 O11 C7 O10 -4.2(6) . . . . ?
Zn3 O11 C7 C8' 166.1(5) . . . . ?
Zn3 O12 C9 O13 -0.8(5) . . . . ?
Zn3 O12 C9 C10 179.00(19) . . . . ?
Zn3 O14 C11 O15 -20.2(5) . . . . ?
Zn3 O14 C11 C12 161.5(2) . . . . ?
O4 Fe1 O16 Fe2 -45.97(13) . . . . ?
O4 Fe1 O16 Fe3 133.42(12) . . . . ?
O4 Fe1 O16 Zn2 -45.97(13) . . . . ?
O4 Fe1 O16 Zn3 133.42(12) . . . . ?
O4 C1 C2 F1 -16.2(4) . . . . ?
O4 C1 C2 F2 102.0(4) . . . . ?
O4 C1 C2 F3 -138.5(3) . . . . ?
O5 C1 C2 F1 164.0(3) . . . . ?
O5 C1 C2 F2 -77.7(4) . . . . ?
O5 C1 C2 F3 41.8(4) . . . . ?
O6 Fe1 O16 Fe2 43.20(13) . . . . ?
O6 Fe1 O16 Fe3 -137.41(12) . . . . ?
O6 Fe1 O16 Zn2 43.20(13) . . . . ?
O6 Fe1 O16 Zn3 -137.41(12) . . . . ?
O6 C3 C4 F4 -47.3(11) . . . . ?
O6 C3 C4 F5 -166.1(10) . . . . ?
O6 C3 C4 F6 70.9(12) . . . . ?
O6 C3 C4' F4' -21.4(9) . . . . ?
O6 C3 C4' F5' -142.2(6) . . . . ?
O6 C3 C4' F6' 98.8(9) . . . . ?
O7 C3 C4 F4 135.1(9) . . . . ?
O7 C3 C4 F5 16.4(11) . . . . ?
O7 C3 C4 F6 -106.6(11) . . . . ?
O7 C3 C4' F4' 160.2(8) . . . . ?
O7 C3 C4' F5' 39.3(8) . . . . ?
O7 C3 C4' F6' -79.7(9) . . . . ?
O8 C5 C6 F7 25.8(4) . . . . ?
O8 C5 C6 F8 -93.4(3) . . . . ?
O8 C5 C6 F9 144.2(3) . . . . ?
O9 C5 C6 F7 -156.4(3) . . . . ?
O9 C5 C6 F8 84.4(4) . . . . ?
O9 C5 C6 F9 -38.0(4) . . . . ?
O10 C7 C8 F10 -21.1(6) . . . . ?
O10 C7 C8 F11 99.5(6) . . . . ?
O10 C7 C8 F12 -141.5(4) . . . . ?
O10 C7 C8' F10' 166.1(8) . . . . ?
O10 C7 C8' F11' -72.8(9) . . . . ?
O10 C7 C8' F12' 47.4(9) . . . . ?
O11 C7 C8 F10 157.5(5) . . . . ?
O11 C7 C8 F11 -81.9(6) . . . . ?
O11 C7 C8 F12 37.2(5) . . . . ?
O11 C7 C8' F10' -5.8(10) . . . . ?
O11 C7 C8' F11' 115.3(8) . . . . ?
O11 C7 C8' F12' -124.5(7) . . . . ?
O12 C9 C10 F13 1.9(4) . . . . ?
O12 C9 C10 F14 -117.6(3) . . . . ?
O12 C9 C10 F15 122.5(3) . . . . ?
O13 Fe1 O16 Fe2 -136.24(12) . . . . ?
O13 Fe1 O16 Fe3 43.15(12) . . . . ?
O13 Fe1 O16 Zn2 -136.24(12) . . . . ?
O13 Fe1 O16 Zn3 43.15(12) . . . . ?
O13 C9 C10 F13 -178.3(3) . . . . ?
O13 C9 C10 F14 62.2(3) . . . . ?
O13 C9 C10 F15 -57.7(3) . . . . ?
O14 C11 C12 F16 -46.0(4) . . . . ?
O14 C11 C12 F17 73.4(4) . . . . ?
O14 C11 C12 F18 -165.6(3) . . . . ?
O15 Fe1 O16 Fe2 128.74(12) . . . . ?
O15 Fe1 O16 Fe3 -51.87(12) . . . . ?
O15 Fe1 O16 Zn2 128.74(12) . . . . ?
O15 Fe1 O16 Zn3 -51.87(12) . . . . ?
O15 C11 C12 F16 135.4(3) . . . . ?
O15 C11 C12 F17 -105.2(4) . . . . ?
O15 C11 C12 F18 15.8(4) . . . . ?

_olex2_submission_original_sample_id knoks14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.668
_oxdiff_exptl_absorpt_empirical_full_min 0.616
####################################################################### 
# 
# 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_knoks17
_database_code_depnum_ccdc_archive 'CCDC 1996871'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_vrf_PLAT007_knoks17             
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 6 
RESPONSE: Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.
;

_vrf_PLAT301_knoks17             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 14% 
RESPONSE: Each metal site was modeled as a disorder of Fe and Ni:
Fe1:Ni1, 0.917(3):0.083(3), Fe2:Ni2, 0.782(3):0.218(3), Fe3:Ni3,
0.302(3):0.698(3). The total metal ratio was constrained to 2Fe:1Ni.
CF3 group C2-F1-F2-F3 is modeled as disordered over two
positions (0.59(1):0.41(1)).
;

_vrf_PLAT302_knoks17             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  4-9 ) .. 100% 
RESPONSE: One cocrystallized water and two acetone solvent molecules
were modeled as disordered over two positions (0.557(5):0.443(5)).
The common disorder ratio is due to their adjacency.
;

_vrf_PLAT860_knoks17             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 280 
RESPONSE: Positional and anisotropic displacement parameters,
respectively, for the two metal types of each site disorder were
constrained to be equivalent. Analogous bond lengths and angles
between the two positions of the disordered CF3 groups were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained to be similar and/or
constrained to be equivalent.
;

_audit_creation_date             2020-04-23
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 F18 Fe2 Ni1 O16, 4(C3 H6 O), H2 O'
_chemical_formula_sum            'C24 H32 F18 Fe2 Ni O21'
_chemical_formula_weight         1168.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.56550(10)
_cell_length_b                   11.5802(2)
_cell_length_c                   19.90320(10)
_cell_angle_alpha                92.6340(10)
_cell_angle_beta                 97.2410(10)
_cell_angle_gamma                111.9130(10)
_cell_volume                     2229.74(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18978
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1320
_cell_measurement_theta_min      4.5140
_shelx_estimated_absorpt_T_max   0.703
_shelx_estimated_absorpt_T_min   0.166
_exptl_absorpt_coefficient_mu    7.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.059
_diffrn_reflns_theta_min         4.136
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00   4.00   0.50    0.14    --  -49.75  38.00  90.00   52
  2  ω    -31.00  21.00   0.50    0.14    --  -49.75  38.00  30.00  104
  3  ω    -46.00 -21.00   0.50    0.57    --  -84.25  96.00 -95.00   50
  4  ω    -72.00   8.00   0.50    0.14    --  -49.75  96.00 -95.00  160
  5  ω     -5.00  58.00   0.50    0.14    --   49.75 -96.00 155.00  126
  6  ω     43.00  71.00   0.50    0.57    --  105.75 -96.00 155.00   56
  7  ω     88.00 114.00   0.50    0.57    --  105.75 -77.00 150.00   52
  8  ω     72.00 106.00   0.50    0.57    --  105.75 -94.00  90.00   68
  9  ω     65.00 104.00   0.50    0.57    --  105.75 -94.00  60.00   78
 10  ω     76.00 106.00   0.50    0.57    --  105.75 -94.00   0.00   60
 11  ω     59.00 106.00   0.50    0.57    --  105.75 -94.00 -90.00   94
 12  ω     81.00 106.00   0.50    0.57    --  105.75 -94.00-150.00   50
 13  ω     38.00  94.00   0.50    0.57    --  105.75 -77.00 -90.00  112
 14  ω     41.00  72.00   0.50    0.57    --  105.75 -61.00 -90.00   62
 15  ω     46.00  76.00   0.50    0.57    --  105.75 -94.00-150.00   60
 16  ω     47.00  79.00   0.50    0.57    --  105.75 -61.00-150.00   64
 17  ω    103.00 175.00   0.50    0.57    --  105.75  15.00-120.00  144
 18  ω    106.00 167.00   0.50    0.57    --  105.75  96.00 -95.00  122
 19  ω    124.00 166.00   0.50    0.57    --  105.75  15.00  30.00   84
 20  ω    153.00 178.00   0.50    0.57    --  105.75  30.00 120.00   50
 21  ω    105.00 141.00   0.50    0.57    --  105.75  30.00 120.00   72
 22  ω    102.00 174.00   0.50    0.57    --  105.75  15.00   0.00  144
 23  ω     92.00 121.00   0.50    0.57    --  105.75  61.00-150.00   58
 24  ω     96.00 147.00   0.50    0.57    --  105.75  61.00-120.00  102
 25  ω    115.00 143.00   0.50    0.57    --  105.75  15.00-180.00   56
 26  ω     99.00 175.00   0.50    0.57    --  105.75  45.00-180.00  152
 27  ω    105.00 173.00   0.50    0.57    --  105.75  15.00 -90.00  136
 28  ω    101.00 126.00   0.50    0.57    --  105.75  15.00 -30.00   50
 29  ω     43.00  69.00   0.50    0.57    --  105.75 -61.00 -30.00   52
 30  ω     47.00 105.00   0.50    0.57    --  105.75 -94.00 -30.00  116
 31  ω     52.00 111.00   0.50    0.57    --  105.75-125.00  30.00  118
 32  ω     44.00  73.00   0.50    0.57    --  105.75-125.00 120.00   58
 33  ω     47.00 109.00   0.50    0.57    --  105.75-125.00 150.00  124
 34  ω     69.00 107.00   0.50    0.57    --  105.75-104.00 174.71   76
 35  ω     35.00  61.00   0.50    0.57    --  105.75 -77.00 150.00   52
 36  ω     43.00  88.00   0.50    0.57    --  105.75-125.00  90.00   90
 37  ω     34.00 104.00   0.50    0.57    --  105.75 -94.00  30.00  140
 38  ω     34.00  71.00   0.50    0.57    --  105.75 -61.00  60.00   74
 39  ω     35.00  60.00   0.50    0.57    --  105.75 -94.00   0.00   50
 40  ω     34.00  68.00   0.50    0.57    --  105.75 -61.00  30.00   68
 41  ω    -22.00   3.00   0.50    0.14    --   49.75 -19.00 150.00   50
 42  ω    -20.00  13.00   0.50    0.14    --   49.75 -19.00  60.00   66
 43  ω     -3.00  22.00   0.50    0.14    --  -49.75  19.00-150.00   50
 44  ω    -21.00  59.00   0.50    0.14    --   49.75 -57.00-180.00  160
 45  ω     34.00  76.00   0.50    0.57    --  105.75 -61.00-180.00   84
 46  ω     41.00 106.00   0.50    0.57    --  105.75 -94.00-180.00  130
 47  ω     45.00  82.00   0.50    0.57    --  105.75-125.00-180.00   74
 48  ω    -21.00  42.00   0.50    0.14    --   49.75 -38.00-150.00  126
 49  ω   -113.00 -80.00   0.50    0.14    --  -49.75-125.00 -60.00   66
 50  ω   -153.00-116.00   0.50    0.57    --  -84.25 -45.00   0.00   74
 51  ω   -124.00 -90.00   0.50    0.57    --  -84.25 -96.00 155.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0968565000
_diffrn_orient_matrix_UB_12      0.0805487000
_diffrn_orient_matrix_UB_13      0.0636276000
_diffrn_orient_matrix_UB_21      -0.1255337000
_diffrn_orient_matrix_UB_22      -0.0197708000
_diffrn_orient_matrix_UB_23      0.0365695000
_diffrn_orient_matrix_UB_31      0.0128525000
_diffrn_orient_matrix_UB_32      -0.1178767000
_diffrn_orient_matrix_UB_33      0.0276566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8318
_reflns_number_total             9354
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         9354
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      1.047
_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)+(0.0980P)²+0.6801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1444
_refine_special_details          
;
Each metal site was modeled as a disorder of Fe and Ni:
Fe1:Ni1, 0.917(3):0.083(3), Fe2:Ni2, 0.782(3):0.218(3),
Fe3:Ni3, 0.302(3):0.698(3). The total metal ratio was
constrained to 2Fe:1Ni. CF3 group C2-F1-F2-F3 is
modeled as disordered over two positions (0.59(1):0.41(1)).

One cocrystallized water and two acetone solvent
molecules were modeled as disordered over two positions
(0.557(5):0.443(5)). The common disorder ratio is due to
their adjacency.

Positional and anisotropic displacement parameters,
respectively, for the two metal types of each site disorder
were constrained to be equivalent. Analogous bond lengths
and angles between the two positions of the disordered CF3
groups were restrained to be similar. Anisotropic
displacement parameters for proximal atoms were
restrained to be similar and/or constrained to be equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{Ni1, Fe1}
{Ni2, Fe2}
{Ni3, Fe3}
3. Restrained distances
 C1-C2 \\sim C1-C2'
 with sigma of 0.01
 C2-F1 \\sim C2-F2 \\sim C2-F3 \\sim C2'-F1' \\sim C2'-F2' \\sim C2'-F3'
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1'-F2' \\sim F2'-F3' \\sim F3'-F1'
 with sigma of 0.02
 C19-O19 \\sim C19'-O19' \\sim C22-O21 \\sim C22'-O21'
 with sigma of 0.01
 C19-C20 \\sim C19-C21 \\sim C19'-C20' \\sim C19'-C21' \\sim C22-C23 \\sim
C22-C24 \\sim C22'-C23' ~
 C22'-C24'
 with sigma of 0.01
 O19-C20 \\sim O19-C21 \\sim O19'-C20' \\sim O19'-C21' \\sim O21-C23 \\sim
O21-C24 \\sim O21'-C23' ~
 O21'-C24'
 with sigma of 0.02
 C20-C21 \\sim C20'-C21' \\sim C23-C24 \\sim C23'-C24'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1A
Uanis(Ni1) = Uanis(Fe1)
Uanis(Ni2) = Uanis(Fe2)
Uanis(Ni3) = Uanis(Fe3)
5. Rigid body (RIGU) restrains
 F1, F2, F3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1', F2', F3', C2'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19', C19', C20', C21'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21', C22', C23', C24'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Ni1)+Sof(Fe1)]+1*[Sof(Ni2)+Sof(Fe2)]+1*[Sof(Ni3)+Sof(Fe3)]=2 with esd
 of 0.0001
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C2')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C2)=FVAR(1)
 Sof(O19')=Sof(C19')=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21')=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(O20')=Sof(H20I)=Sof(H20J)=Sof(O21')=
 Sof(C22')=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O19)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(O20)=Sof(H20G)=Sof(H20H)=Sof(O21)=Sof(C22)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(Ni1)=1-FVAR(3)
 Sof(Fe1)=FVAR(3)
 Sof(Ni2)=1-FVAR(4)
 Sof(Fe2)=FVAR(4)
 Sof(Ni3)=1-FVAR(5)
 Sof(Fe3)=FVAR(5)
7.a Riding coordinates:
 O1(H1A,H1B), O20(H20G,H20H), O20'(H20I,H20J)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20'(H20D,H20E,H20F),
 C21'(H21D,H21E,H21F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23'(H23D,H23E,
 H23F), C24'(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.57604(4) 0.49064(4) 0.67572(2) 0.02091(12) Uani 0.083(3) 1 d . U P A 2
Ni2 Ni 0.43617(4) 0.55968(4) 0.80221(2) 0.02034(12) Uani 0.218(3) 1 d . U P A 2
Ni3 Ni 0.75936(4) 0.57699(4) 0.83063(2) 0.01993(12) Uani 0.698(3) 1 d . U P A 2
Fe1 Fe 0.57604(4) 0.49064(4) 0.67572(2) 0.02091(12) Uani 0.917(3) 1 d . U P A 1
Fe2 Fe 0.43617(4) 0.55968(4) 0.80221(2) 0.02034(12) Uani 0.782(3) 1 d . U P A 1
Fe3 Fe 0.75936(4) 0.57699(4) 0.83063(2) 0.01993(12) Uani 0.302(3) 1 d . U P A 1
F1 F 0.1427(6) 0.1692(5) 0.6199(2) 0.070(2) Uani 0.587(12) 1 d D . P B 1
F1' F 0.1239(12) 0.1602(7) 0.7451(4) 0.086(4) Uani 0.413(12) 1 d D . P B 2
F2 F 0.2113(6) 0.1167(4) 0.7117(5) 0.085(3) Uani 0.587(12) 1 d D U P B 1
F2' F 0.0737(9) 0.2091(7) 0.6494(7) 0.108(6) Uani 0.413(12) 1 d D . P B 2
F3 F 0.0644(5) 0.2003(5) 0.7060(4) 0.079(3) Uani 0.587(12) 1 d D . P B 1
F3' F 0.2031(9) 0.1139(6) 0.6622(6) 0.081(4) Uani 0.413(12) 1 d D U P B 2
F4 F 0.3726(3) 0.7330(2) 0.56152(10) 0.0543(6) Uani 1 1 d . . . . .
F5 F 0.5052(3) 0.8723(2) 0.63964(17) 0.0727(8) Uani 1 1 d . . . . .
F6 F 0.2899(3) 0.7865(3) 0.64393(13) 0.0621(7) Uani 1 1 d . . . . .
F7 F 0.40210(18) 0.33506(19) 0.99290(9) 0.0365(4) Uani 1 1 d . . . . .
F8 F 0.4601(3) 0.22031(18) 0.92549(11) 0.0597(7) Uani 1 1 d . . . . .
F9 F 0.6079(2) 0.3415(2) 1.00726(10) 0.0431(5) Uani 1 1 d . . . . .
F10 F 0.6237(2) 0.92792(19) 0.94890(12) 0.0464(5) Uani 1 1 d . . . . .
F11 F 0.7355(3) 0.99257(18) 0.86657(11) 0.0530(6) Uani 1 1 d . . . . .
F12 F 0.8346(2) 0.94900(17) 0.95687(10) 0.0415(4) Uani 1 1 d . . . . .
F13 F 0.8546(2) 0.22117(19) 0.78267(10) 0.0434(5) Uani 1 1 d . . . . .
F14 F 0.6347(3) 0.1344(2) 0.76700(16) 0.0602(7) Uani 1 1 d . . . . .
F15 F 0.7434(3) 0.1727(2) 0.68140(10) 0.0518(6) Uani 1 1 d . . . . .
F16 F 1.08880(19) 0.84138(19) 0.71249(10) 0.0419(5) Uani 1 1 d . . . . .
F17 F 0.9244(3) 0.9002(2) 0.6787(2) 0.0797(10) Uani 1 1 d . . . . .
F18 F 0.9733(3) 0.7762(3) 0.61330(11) 0.0717(9) Uani 1 1 d . . . . .
O1 O 0.5665(2) 0.43501(19) 0.57539(10) 0.0286(4) Uani 1 1 d . . . . .
H1A H 0.626887 0.487075 0.555659 0.043 Uiso 1 1 d R U . A .
H1B H 0.517757 0.368685 0.549479 0.043 Uiso 1 1 d R U . . .
O2 O 0.2678(2) 0.5757(2) 0.83819(11) 0.0266(4) Uani 1 1 d . . . . .
H2A H 0.257(5) 0.639(5) 0.844(2) 0.050(13) Uiso 1 1 d . . . . .
H2B H 0.215(4) 0.525(4) 0.860(2) 0.036(10) Uiso 1 1 d . . . . .
O3 O 0.9415(2) 0.6150(2) 0.89543(10) 0.0239(4) Uani 1 1 d . . . . .
H3A H 1.008(5) 0.666(4) 0.883(2) 0.040(11) Uiso 1 1 d . . . . .
H3B H 0.963(4) 0.560(4) 0.900(2) 0.031(10) Uiso 1 1 d . . . . .
O4 O 0.3869(2) 0.34730(18) 0.66645(10) 0.0271(4) Uani 1 1 d . . . . .
O5 O 0.2906(2) 0.39578(18) 0.75315(10) 0.0263(4) Uani 1 1 d . . . . .
O6 O 0.4885(2) 0.61002(19) 0.64007(10) 0.0260(4) Uani 1 1 d . . . . .
O7 O 0.3946(2) 0.66104(18) 0.72715(9) 0.0256(4) Uani 1 1 d . . . . .
O8 O 0.4444(2) 0.45763(18) 0.88334(9) 0.0246(4) Uani 1 1 d . . . . .
O9 O 0.66632(19) 0.47502(18) 0.90363(9) 0.0244(4) Uani 1 1 d . . . . .
O10 O 0.54562(19) 0.72819(17) 0.85768(9) 0.0234(4) Uani 1 1 d . . . . .
O11 O 0.7655(2) 0.73988(18) 0.87812(10) 0.0255(4) Uani 1 1 d . . . . .
O12 O 0.78338(19) 0.41669(18) 0.79776(9) 0.0247(4) Uani 1 1 d . . . . .
O13 O 0.6564(2) 0.3579(2) 0.69313(10) 0.0294(4) Uani 1 1 d . . . . .
O14 O 0.8824(2) 0.69002(19) 0.76828(10) 0.0269(4) Uani 1 1 d . . . . .
O15 O 0.7600(2) 0.62343(19) 0.66319(10) 0.0284(4) Uani 1 1 d . . . . .
O16 O 0.58712(19) 0.54122(16) 0.76835(9) 0.0214(4) Uani 1 1 d . . . . .
C1 C 0.2964(3) 0.3288(2) 0.70397(13) 0.0236(5) Uani 1 1 d D . . . .
C2 C 0.1751(5) 0.2013(5) 0.6847(3) 0.0344(19) Uani 0.587(12) 1 d D U P B 1
C2' C 0.1736(7) 0.2012(6) 0.6909(4) 0.032(3) Uani 0.413(12) 1 d D U P B 2
C3 C 0.4283(3) 0.6670(2) 0.66914(14) 0.0242(5) Uani 1 1 d . . . . .
C4 C 0.3965(4) 0.7653(3) 0.62806(16) 0.0351(7) Uani 1 1 d . . . . .
C5 C 0.5434(3) 0.4337(2) 0.91082(12) 0.0202(5) Uani 1 1 d . . . . .
C6 C 0.5036(3) 0.3318(3) 0.96049(14) 0.0267(5) Uani 1 1 d . . . . .
C7 C 0.6711(3) 0.7787(2) 0.88006(13) 0.0215(5) Uani 1 1 d . . . . .
C8 C 0.7172(3) 0.9135(3) 0.91399(14) 0.0278(6) Uani 1 1 d . . . . .
C9 C 0.7271(3) 0.3445(2) 0.74521(13) 0.0225(5) Uani 1 1 d . . . . .
C10 C 0.7410(3) 0.2166(3) 0.74334(15) 0.0300(6) Uani 1 1 d . . . . .
C11 C 0.8578(3) 0.6939(2) 0.70637(14) 0.0230(5) Uani 1 1 d . . . . .
C12 C 0.9626(3) 0.8048(3) 0.67722(17) 0.0368(7) Uani 1 1 d . . . . .
O17 O 0.1930(2) 0.77421(19) 0.86592(12) 0.0327(5) Uani 1 1 d . . . . .
C13 C 0.2317(3) 0.8838(3) 0.85395(15) 0.0281(6) Uani 1 1 d . . . . .
C14 C 0.1515(4) 0.9615(3) 0.86996(18) 0.0375(7) Uani 1 1 d . . . . .
H14A H 0.068084 0.909903 0.885447 0.056 Uiso 1 1 calc R U . . .
H14B H 0.128904 0.997032 0.829763 0.056 Uiso 1 1 calc R U . . .
H14C H 0.206116 1.027461 0.904938 0.056 Uiso 1 1 calc R U . . .
C15 C 0.3603(3) 0.9428(3) 0.82382(18) 0.0353(7) Uani 1 1 d . . . . .
H15A H 0.426821 1.008878 0.855573 0.053 Uiso 1 1 calc R U . . .
H15B H 0.339409 0.976333 0.782573 0.053 Uiso 1 1 calc R U . . .
H15C H 0.397512 0.880979 0.813896 0.053 Uiso 1 1 calc R U . . .
O18 O 1.0615(2) 0.44352(19) 0.91158(11) 0.0308(4) Uani 1 1 d . . . . .
C16 C 1.0083(3) 0.3379(3) 0.92833(14) 0.0265(5) Uani 1 1 d . . . . .
C17 C 0.8700(3) 0.2947(3) 0.95081(15) 0.0291(6) Uani 1 1 d . . . . .
H17A H 0.847744 0.365823 0.961864 0.044 Uiso 1 1 calc R U . . .
H17B H 0.871604 0.250302 0.990249 0.044 Uiso 1 1 calc R U . . .
H17C H 0.801524 0.240352 0.914784 0.044 Uiso 1 1 calc R U . . .
C18 C 1.0799(4) 0.2488(3) 0.9263(2) 0.0480(9) Uani 1 1 d . . . . .
H18A H 1.162640 0.285595 0.906605 0.072 Uiso 1 1 calc R U . . .
H18B H 1.019992 0.172715 0.899167 0.072 Uiso 1 1 calc R U . . .
H18C H 1.103301 0.230671 0.971674 0.072 Uiso 1 1 calc R U . . .
O19 O 0.8249(9) 0.5268(13) 0.4038(6) 0.047(2) Uani 0.557(5) 1 d D U P C 1
C19 C 0.9441(8) 0.5579(11) 0.3943(5) 0.038(2) Uani 0.557(5) 1 d D U P C 1
C20 C 0.9754(13) 0.5077(14) 0.3311(6) 0.059(3) Uani 0.557(5) 1 d D U P C 1
H20A H 0.899907 0.431450 0.312612 0.088 Uiso 0.557(5) 1 calc R U P C 1
H20B H 1.058012 0.491383 0.341427 0.088 Uiso 0.557(5) 1 calc R U P C 1
H20C H 0.988455 0.567903 0.298344 0.088 Uiso 0.557(5) 1 calc R U P C 1
C21 C 1.0618(8) 0.6482(9) 0.4432(4) 0.057(2) Uani 0.557(5) 1 d D U P C 1
H21A H 1.027365 0.690417 0.474571 0.086 Uiso 0.557(5) 1 calc R U P C 1
H21B H 1.123555 0.708423 0.418767 0.086 Uiso 0.557(5) 1 calc R U P C 1
H21C H 1.110195 0.603931 0.467927 0.086 Uiso 0.557(5) 1 calc R U P C 1
O19' O 0.8384(10) 0.511(2) 0.3933(8) 0.057(4) Uani 0.443(5) 1 d D U P C 2
C19' C 0.9517(9) 0.5313(12) 0.3780(5) 0.026(2) Uani 0.443(5) 1 d D U P C 2
C20' C 0.9651(14) 0.4946(13) 0.3074(4) 0.032(2) Uani 0.443(5) 1 d D U P C 2
H20D H 0.895516 0.413413 0.291648 0.048 Uiso 0.443(5) 1 calc R U P C 2
H20E H 1.054832 0.492226 0.306928 0.048 Uiso 0.443(5) 1 calc R U P C 2
H20F H 0.953580 0.554594 0.277979 0.048 Uiso 0.443(5) 1 calc R U P C 2
C21' C 1.0786(8) 0.5837(10) 0.4300(4) 0.0432(19) Uani 0.443(5) 1 d D U P C 2
H21D H 1.149685 0.647442 0.411618 0.065 Uiso 0.443(5) 1 calc R U P C 2
H21E H 1.109602 0.518218 0.441949 0.065 Uiso 0.443(5) 1 calc R U P C 2
H21F H 1.058394 0.619282 0.469770 0.065 Uiso 0.443(5) 1 calc R U P C 2
O20 O 0.6849(4) 0.6041(4) 0.49313(19) 0.0340(10) Uani 0.557(5) 1 d . . P C 1
H20G H 0.714664 0.683296 0.500315 0.051 Uiso 0.557(5) 1 d R U P C 1
H20H H 0.732514 0.577326 0.469985 0.051 Uiso 0.557(5) 1 d R U P C 1
O20' O 0.7801(6) 0.5738(5) 0.5176(3) 0.0408(14) Uani 0.443(5) 1 d . . P C 2
H20I H 0.774528 0.539147 0.478150 0.061 Uiso 0.443(5) 1 d R U P C 2
H20J H 0.759938 0.637017 0.510150 0.061 Uiso 0.443(5) 1 d R U P C 2
O21 O 0.2174(9) 0.1394(6) 0.4837(4) 0.093(3) Uani 0.557(5) 1 d D . P C 1
C22 C 0.2683(9) 0.0666(7) 0.5039(4) 0.059(2) Uani 0.557(5) 1 d D U P C 1
C23 C 0.4009(16) 0.1094(13) 0.5518(12) 0.062(3) Uani 0.557(5) 1 d D U P C 1
H23A H 0.455679 0.194499 0.546075 0.092 Uiso 0.557(5) 1 calc R U P C 1
H23B H 0.450372 0.057217 0.542572 0.092 Uiso 0.557(5) 1 calc R U P C 1
H23C H 0.382004 0.103871 0.597775 0.092 Uiso 0.557(5) 1 calc R U P C 1
C24 C 0.1950(15) -0.0703(7) 0.4852(7) 0.107(5) Uani 0.557(5) 1 d D . P C 1
H24A H 0.129101 -0.104129 0.515299 0.161 Uiso 0.557(5) 1 calc R U P C 1
H24B H 0.260596 -0.109746 0.488945 0.161 Uiso 0.557(5) 1 calc R U P C 1
H24C H 0.147964 -0.085325 0.439162 0.161 Uiso 0.557(5) 1 calc R U P C 1
O21' O 0.3307(6) 0.2359(5) 0.5087(3) 0.0434(15) Uani 0.443(5) 1 d D . P C 2
C22' C 0.3152(10) 0.1292(7) 0.5175(5) 0.048(2) Uani 0.443(5) 1 d D U P C 2
C23' C 0.423(2) 0.0987(16) 0.5602(17) 0.063(4) Uani 0.443(5) 1 d D U P C 2
H23D H 0.483534 0.083755 0.531808 0.094 Uiso 0.443(5) 1 calc R U P C 2
H23E H 0.379530 0.025163 0.582199 0.094 Uiso 0.443(5) 1 calc R U P C 2
H23F H 0.475390 0.167550 0.593951 0.094 Uiso 0.443(5) 1 calc R U P C 2
C24' C 0.1850(13) 0.0231(9) 0.4865(7) 0.080(4) Uani 0.443(5) 1 d D U P C 2
H24D H 0.117585 0.055349 0.468540 0.120 Uiso 0.443(5) 1 calc R U P C 2
H24E H 0.150069 -0.031184 0.520590 0.120 Uiso 0.443(5) 1 calc R U P C 2
H24F H 0.203860 -0.023087 0.450369 0.120 Uiso 0.443(5) 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
Ni1 O1 2.048(2) . ?
Ni1 O4 2.046(2) . ?
Ni1 O6 2.0366(18) . ?
Ni1 O13 2.0385(19) . ?
Ni1 O15 2.032(2) . ?
Ni1 O16 1.8844(18) . ?
Ni2 O2 2.066(2) . ?
Ni2 O5 2.048(2) . ?
Ni2 O7 2.0454(18) . ?
Ni2 O8 2.0565(17) . ?
Ni2 O10 2.040(2) . ?
Ni2 O16 1.8856(19) . ?
Ni3 O3 2.0621(19) . ?
Ni3 O9 2.0305(18) . ?
Ni3 O11 2.046(2) . ?
Ni3 O12 2.0542(19) . ?
Ni3 O14 2.0566(18) . ?
Ni3 O16 1.9599(18) . ?
Fe1 O1 2.048(2) . ?
Fe1 O4 2.046(2) . ?
Fe1 O6 2.0366(18) . ?
Fe1 O13 2.0385(19) . ?
Fe1 O15 2.032(2) . ?
Fe1 O16 1.8844(18) . ?
Fe2 O2 2.066(2) . ?
Fe2 O5 2.048(2) . ?
Fe2 O7 2.0454(18) . ?
Fe2 O8 2.0565(17) . ?
Fe2 O10 2.040(2) . ?
Fe2 O16 1.8856(19) . ?
Fe3 O3 2.0621(19) . ?
Fe3 O9 2.0305(18) . ?
Fe3 O11 2.046(2) . ?
Fe3 O12 2.0542(19) . ?
Fe3 O14 2.0566(18) . ?
Fe3 O16 1.9599(18) . ?
F1 C2 1.292(6) . ?
F1' C2' 1.291(6) . ?
F2 C2 1.293(6) . ?
F2' C2' 1.290(7) . ?
F3 C2 1.290(6) . ?
F3' C2' 1.293(6) . ?
F4 C4 1.326(4) . ?
F5 C4 1.324(4) . ?
F6 C4 1.311(4) . ?
F7 C6 1.331(3) . ?
F8 C6 1.325(4) . ?
F9 C6 1.316(3) . ?
F10 C8 1.331(4) . ?
F11 C8 1.327(3) . ?
F12 C8 1.326(3) . ?
F13 C10 1.330(4) . ?
F14 C10 1.328(4) . ?
F15 C10 1.318(4) . ?
F16 C12 1.329(4) . ?
F17 C12 1.310(4) . ?
F18 C12 1.329(4) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8500 . ?
O2 H2A 0.79(5) . ?
O2 H2B 0.83(4) . ?
O3 H3A 0.82(5) . ?
O3 H3B 0.76(4) . ?
O4 C1 1.249(3) . ?
O5 C1 1.242(3) . ?
O6 C3 1.243(3) . ?
O7 C3 1.248(3) . ?
O8 C5 1.247(3) . ?
O9 C5 1.235(3) . ?
O10 C7 1.243(3) . ?
O11 C7 1.242(3) . ?
O12 C9 1.240(3) . ?
O13 C9 1.249(3) . ?
O14 C11 1.233(3) . ?
O15 C11 1.247(3) . ?
C1 C2 1.543(6) . ?
C1 C2' 1.544(7) . ?
C3 C4 1.542(4) . ?
C5 C6 1.545(3) . ?
C7 C8 1.543(4) . ?
C9 C10 1.542(4) . ?
C11 C12 1.543(4) . ?
O17 C13 1.225(4) . ?
C13 C14 1.497(4) . ?
C13 C15 1.490(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O18 C16 1.223(3) . ?
C16 C17 1.492(4) . ?
C16 C18 1.492(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O19 C19 1.216(7) . ?
C19 C20 1.488(7) . ?
C19 C21 1.489(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O19' C19' 1.213(7) . ?
C19' C20' 1.489(7) . ?
C19' C21' 1.491(7) . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
O20 H20G 0.8500 . ?
O20 H20H 0.8501 . ?
O20' H20I 0.8500 . ?
O20' H20J 0.8499 . ?
O21 C22 1.215(7) . ?
C22 C23 1.490(7) . ?
C22 C24 1.486(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O21' C22' 1.208(7) . ?
C22' C23' 1.493(7) . ?
C22' C24' 1.496(7) . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?

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
O4 Ni1 O1 84.06(8) . . ?
O6 Ni1 O1 85.69(8) . . ?
O6 Ni1 O4 91.39(8) . . ?
O6 Ni1 O13 169.43(8) . . ?
O13 Ni1 O1 83.86(8) . . ?
O13 Ni1 O4 86.00(9) . . ?
O15 Ni1 O1 83.71(8) . . ?
O15 Ni1 O4 167.72(8) . . ?
O15 Ni1 O6 86.61(8) . . ?
O15 Ni1 O13 93.78(9) . . ?
O16 Ni1 O1 179.15(8) . . ?
O16 Ni1 O4 96.32(8) . . ?
O16 Ni1 O6 95.05(8) . . ?
O16 Ni1 O13 95.41(8) . . ?
O16 Ni1 O15 95.92(8) . . ?
O5 Ni2 O2 82.91(9) . . ?
O5 Ni2 O8 85.54(8) . . ?
O7 Ni2 O2 84.32(8) . . ?
O7 Ni2 O5 92.08(8) . . ?
O7 Ni2 O8 169.26(8) . . ?
O8 Ni2 O2 85.00(8) . . ?
O10 Ni2 O2 84.83(8) . . ?
O10 Ni2 O5 167.71(8) . . ?
O10 Ni2 O7 85.89(8) . . ?
O10 Ni2 O8 94.21(8) . . ?
O16 Ni2 O2 178.62(9) . . ?
O16 Ni2 O5 95.72(8) . . ?
O16 Ni2 O7 95.87(8) . . ?
O16 Ni2 O8 94.79(7) . . ?
O16 Ni2 O10 96.55(8) . . ?
O9 Ni3 O3 85.61(8) . . ?
O9 Ni3 O11 92.30(8) . . ?
O9 Ni3 O12 84.72(8) . . ?
O9 Ni3 O14 170.62(8) . . ?
O11 Ni3 O3 84.05(8) . . ?
O11 Ni3 O12 168.94(8) . . ?
O11 Ni3 O14 85.37(8) . . ?
O12 Ni3 O3 85.11(8) . . ?
O12 Ni3 O14 95.86(8) . . ?
O14 Ni3 O3 85.11(8) . . ?
O16 Ni3 O3 179.50(8) . . ?
O16 Ni3 O9 94.85(7) . . ?
O16 Ni3 O11 96.13(8) . . ?
O16 Ni3 O12 94.74(8) . . ?
O16 Ni3 O14 94.43(7) . . ?
O4 Fe1 O1 84.06(8) . . ?
O6 Fe1 O1 85.69(8) . . ?
O6 Fe1 O4 91.39(8) . . ?
O6 Fe1 O13 169.43(8) . . ?
O13 Fe1 O1 83.86(8) . . ?
O13 Fe1 O4 86.00(9) . . ?
O15 Fe1 O1 83.71(8) . . ?
O15 Fe1 O4 167.72(8) . . ?
O15 Fe1 O6 86.61(8) . . ?
O15 Fe1 O13 93.78(9) . . ?
O16 Fe1 O1 179.15(8) . . ?
O16 Fe1 O4 96.32(8) . . ?
O16 Fe1 O6 95.05(8) . . ?
O16 Fe1 O13 95.41(8) . . ?
O16 Fe1 O15 95.92(8) . . ?
O5 Fe2 O2 82.91(9) . . ?
O5 Fe2 O8 85.54(8) . . ?
O7 Fe2 O2 84.32(8) . . ?
O7 Fe2 O5 92.08(8) . . ?
O7 Fe2 O8 169.26(8) . . ?
O8 Fe2 O2 85.00(8) . . ?
O10 Fe2 O2 84.83(8) . . ?
O10 Fe2 O5 167.71(8) . . ?
O10 Fe2 O7 85.89(8) . . ?
O10 Fe2 O8 94.21(8) . . ?
O16 Fe2 O2 178.62(9) . . ?
O16 Fe2 O5 95.72(8) . . ?
O16 Fe2 O7 95.87(8) . . ?
O16 Fe2 O8 94.79(7) . . ?
O16 Fe2 O10 96.55(8) . . ?
O9 Fe3 O3 85.61(8) . . ?
O9 Fe3 O11 92.30(8) . . ?
O9 Fe3 O12 84.72(8) . . ?
O9 Fe3 O14 170.62(8) . . ?
O11 Fe3 O3 84.05(8) . . ?
O11 Fe3 O12 168.94(8) . . ?
O11 Fe3 O14 85.37(8) . . ?
O12 Fe3 O3 85.11(8) . . ?
O12 Fe3 O14 95.86(8) . . ?
O14 Fe3 O3 85.11(8) . . ?
O16 Fe3 O3 179.50(8) . . ?
O16 Fe3 O9 94.85(7) . . ?
O16 Fe3 O11 96.13(8) . . ?
O16 Fe3 O12 94.74(8) . . ?
O16 Fe3 O14 94.43(7) . . ?
Ni1 O1 H1A 113.9 . . ?
Ni1 O1 H1B 133.7 . . ?
Fe1 O1 H1A 113.9 . . ?
Fe1 O1 H1B 133.7 . . ?
H1A O1 H1B 112.3 . . ?
Ni2 O2 H2A 124(4) . . ?
Ni2 O2 H2B 126(3) . . ?
Fe2 O2 H2A 124(4) . . ?
Fe2 O2 H2B 126(3) . . ?
H2A O2 H2B 107(4) . . ?
Ni3 O3 H3A 113(3) . . ?
Ni3 O3 H3B 116(3) . . ?
Fe3 O3 H3A 113(3) . . ?
Fe3 O3 H3B 116(3) . . ?
H3A O3 H3B 103(4) . . ?
C1 O4 Ni1 128.69(19) . . ?
C1 O4 Fe1 128.69(19) . . ?
C1 O5 Ni2 129.82(18) . . ?
C1 O5 Fe2 129.82(18) . . ?
C3 O6 Ni1 130.38(17) . . ?
C3 O6 Fe1 130.38(17) . . ?
C3 O7 Ni2 128.07(18) . . ?
C3 O7 Fe2 128.07(18) . . ?
C5 O8 Ni2 128.72(17) . . ?
C5 O8 Fe2 128.72(17) . . ?
C5 O9 Ni3 129.56(16) . . ?
C5 O9 Fe3 129.56(16) . . ?
C7 O10 Ni2 129.99(18) . . ?
C7 O10 Fe2 129.99(18) . . ?
C7 O11 Ni3 129.24(18) . . ?
C7 O11 Fe3 129.24(18) . . ?
C9 O12 Ni3 129.53(17) . . ?
C9 O12 Fe3 129.53(17) . . ?
C9 O13 Ni1 130.09(19) . . ?
C9 O13 Fe1 130.09(19) . . ?
C11 O14 Ni3 128.90(18) . . ?
C11 O14 Fe3 128.90(18) . . ?
C11 O15 Ni1 130.18(17) . . ?
C11 O15 Fe1 130.18(17) . . ?
Ni1 O16 Ni2 121.27(9) . . ?
Ni1 O16 Ni3 119.44(10) . . ?
Ni2 O16 Ni3 119.29(9) . . ?
Fe1 O16 Fe2 121.27(9) . . ?
Fe1 O16 Fe3 119.44(10) . . ?
Fe2 O16 Fe3 119.29(9) . . ?
O4 C1 C2 112.8(3) . . ?
O4 C1 C2' 116.8(4) . . ?
O5 C1 O4 130.2(3) . . ?
O5 C1 C2 117.0(3) . . ?
O5 C1 C2' 112.9(3) . . ?
F1 C2 F2 107.3(6) . . ?
F1 C2 C1 113.6(4) . . ?
F2 C2 C1 108.0(4) . . ?
F3 C2 F1 106.4(6) . . ?
F3 C2 F2 109.5(6) . . ?
F3 C2 C1 111.9(4) . . ?
F1' C2' F3' 106.9(7) . . ?
F1' C2' C1 114.0(6) . . ?
F2' C2' F1' 106.8(8) . . ?
F2' C2' F3' 105.2(8) . . ?
F2' C2' C1 110.1(6) . . ?
F3' C2' C1 113.2(6) . . ?
O6 C3 O7 130.4(2) . . ?
O6 C3 C4 114.6(2) . . ?
O7 C3 C4 114.9(2) . . ?
F4 C4 C3 112.3(3) . . ?
F5 C4 F4 106.7(3) . . ?
F5 C4 C3 109.1(3) . . ?
F6 C4 F4 107.3(3) . . ?
F6 C4 F5 107.9(3) . . ?
F6 C4 C3 113.3(2) . . ?
O8 C5 C6 114.1(2) . . ?
O9 C5 O8 131.0(2) . . ?
O9 C5 C6 114.9(2) . . ?
F7 C6 C5 112.2(2) . . ?
F8 C6 F7 107.6(3) . . ?
F8 C6 C5 108.9(2) . . ?
F9 C6 F7 107.1(2) . . ?
F9 C6 F8 108.1(2) . . ?
F9 C6 C5 112.7(2) . . ?
O10 C7 C8 114.4(2) . . ?
O11 C7 O10 130.7(3) . . ?
O11 C7 C8 114.9(2) . . ?
F10 C8 C7 112.3(2) . . ?
F11 C8 F10 107.3(2) . . ?
F11 C8 C7 109.6(2) . . ?
F12 C8 F10 106.9(2) . . ?
F12 C8 F11 107.7(3) . . ?
F12 C8 C7 112.8(2) . . ?
O12 C9 O13 129.8(2) . . ?
O12 C9 C10 116.4(2) . . ?
O13 C9 C10 113.7(2) . . ?
F13 C10 C9 112.2(3) . . ?
F14 C10 F13 106.7(2) . . ?
F14 C10 C9 109.2(2) . . ?
F15 C10 F13 107.6(3) . . ?
F15 C10 F14 108.3(3) . . ?
F15 C10 C9 112.6(2) . . ?
O14 C11 O15 130.4(2) . . ?
O14 C11 C12 115.5(2) . . ?
O15 C11 C12 114.2(2) . . ?
F16 C12 F18 106.3(3) . . ?
F16 C12 C11 112.0(2) . . ?
F17 C12 F16 108.1(3) . . ?
F17 C12 F18 108.2(3) . . ?
F17 C12 C11 109.9(3) . . ?
F18 C12 C11 112.2(3) . . ?
O17 C13 C14 120.6(3) . . ?
O17 C13 C15 120.7(3) . . ?
C15 C13 C14 118.8(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O18 C16 C17 120.8(3) . . ?
O18 C16 C18 120.7(3) . . ?
C18 C16 C17 118.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O19 C19 C20 119.7(7) . . ?
O19 C19 C21 122.3(8) . . ?
C20 C19 C21 118.0(7) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O19' C19' C20' 120.1(8) . . ?
O19' C19' C21' 121.2(8) . . ?
C20' C19' C21' 118.6(7) . . ?
C19' C20' H20D 109.5 . . ?
C19' C20' H20E 109.5 . . ?
C19' C20' H20F 109.5 . . ?
H20D C20' H20E 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C19' C21' H21D 109.5 . . ?
C19' C21' H21E 109.5 . . ?
C19' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
H20G O20 H20H 114.3 . . ?
H20I O20' H20J 104.3 . . ?
O21 C22 C23 121.8(8) . . ?
O21 C22 C24 120.8(7) . . ?
C24 C22 C23 117.3(8) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O21' C22' C23' 121.6(9) . . ?
O21' C22' C24' 120.6(7) . . ?
C23' C22' C24' 117.8(9) . . ?
C22' C23' H23D 109.5 . . ?
C22' C23' H23E 109.5 . . ?
C22' C23' H23F 109.5 . . ?
H23D C23' H23E 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C22' C24' H24D 109.5 . . ?
C22' C24' H24E 109.5 . . ?
C22' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O20 0.85 1.87 2.657(4) 153.9 . yes
O1 H1A O20' 0.85 1.84 2.667(6) 165.8 . yes
O1 H1B O21' 0.85 2.03 2.807(6) 150.7 . yes
O2 H2A O17 0.79(5) 1.97(5) 2.750(3) 167(5) . yes
O2 H2B O18 0.83(4) 1.99(4) 2.783(3) 162(4) 1_455 yes
O3 H3A O17 0.82(5) 1.96(5) 2.764(3) 167(4) 1_655 yes
O3 H3B O18 0.76(4) 1.99(4) 2.736(3) 167(4) . yes
O20 H20G O21 0.85 1.90 2.752(8) 179.6 2_666 yes
O20 H20H O19 0.85 1.93 2.767(11) 169.6 . yes
O20' H20I O19' 0.85 1.95 2.751(15) 156.4 . yes
O20' H20J O21' 0.85 2.06 2.895(8) 168.0 2_666 yes

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
Ni1 O4 C1 O5 6.6(4) . . . . ?
Ni1 O4 C1 C2' -170.3(3) . . . . ?
Ni1 O6 C3 O7 -6.0(5) . . . . ?
Ni1 O6 C3 C4 170.7(2) . . . . ?
Ni1 O13 C9 O12 -10.6(4) . . . . ?
Ni1 O13 C9 C10 167.38(19) . . . . ?
Ni1 O15 C11 O14 14.0(5) . . . . ?
Ni1 O15 C11 C12 -164.7(2) . . . . ?
Ni2 O5 C1 O4 -7.3(4) . . . . ?
Ni2 O5 C1 C2' 169.6(3) . . . . ?
Ni2 O7 C3 O6 4.1(5) . . . . ?
Ni2 O7 C3 C4 -172.6(2) . . . . ?
Ni2 O8 C5 O9 10.0(4) . . . . ?
Ni2 O8 C5 C6 -167.74(17) . . . . ?
Ni2 O10 C7 O11 -3.8(4) . . . . ?
Ni2 O10 C7 C8 174.25(16) . . . . ?
Ni3 O9 C5 O8 -13.2(4) . . . . ?
Ni3 O9 C5 C6 164.55(18) . . . . ?
Ni3 O11 C7 O10 4.8(4) . . . . ?
Ni3 O11 C7 C8 -173.19(16) . . . . ?
Ni3 O12 C9 O13 11.9(4) . . . . ?
Ni3 O12 C9 C10 -166.04(18) . . . . ?
Ni3 O14 C11 O15 -8.6(4) . . . . ?
Ni3 O14 C11 C12 170.08(19) . . . . ?
Fe1 O4 C1 O5 6.6(4) . . . . ?
Fe1 O4 C1 C2 -173.0(3) . . . . ?
Fe1 O6 C3 O7 -6.0(5) . . . . ?
Fe1 O6 C3 C4 170.7(2) . . . . ?
Fe1 O13 C9 O12 -10.6(4) . . . . ?
Fe1 O13 C9 C10 167.38(19) . . . . ?
Fe1 O15 C11 O14 14.0(5) . . . . ?
Fe1 O15 C11 C12 -164.7(2) . . . . ?
Fe2 O5 C1 O4 -7.3(4) . . . . ?
Fe2 O5 C1 C2 172.2(3) . . . . ?
Fe2 O7 C3 O6 4.1(5) . . . . ?
Fe2 O7 C3 C4 -172.6(2) . . . . ?
Fe2 O8 C5 O9 10.0(4) . . . . ?
Fe2 O8 C5 C6 -167.74(17) . . . . ?
Fe2 O10 C7 O11 -3.8(4) . . . . ?
Fe2 O10 C7 C8 174.25(16) . . . . ?
Fe3 O9 C5 O8 -13.2(4) . . . . ?
Fe3 O9 C5 C6 164.55(18) . . . . ?
Fe3 O11 C7 O10 4.8(4) . . . . ?
Fe3 O11 C7 C8 -173.19(16) . . . . ?
Fe3 O12 C9 O13 11.9(4) . . . . ?
Fe3 O12 C9 C10 -166.04(18) . . . . ?
Fe3 O14 C11 O15 -8.6(4) . . . . ?
Fe3 O14 C11 C12 170.08(19) . . . . ?
O4 Ni1 O16 Ni2 -45.78(11) . . . . ?
O4 Ni1 O16 Ni3 134.83(10) . . . . ?
O4 Fe1 O16 Fe2 -45.78(11) . . . . ?
O4 Fe1 O16 Fe3 134.83(10) . . . . ?
O4 C1 C2 F1 -37.0(6) . . . . ?
O4 C1 C2 F2 81.9(7) . . . . ?
O4 C1 C2 F3 -157.5(6) . . . . ?
O4 C1 C2' F1' 147.4(8) . . . . ?
O4 C1 C2' F2' -92.6(9) . . . . ?
O4 C1 C2' F3' 24.9(9) . . . . ?
O5 Ni2 O16 Ni1 45.17(11) . . . . ?
O5 Ni2 O16 Ni3 -135.44(10) . . . . ?
O5 Fe2 O16 Fe1 45.17(11) . . . . ?
O5 Fe2 O16 Fe3 -135.44(10) . . . . ?
O5 C1 C2 F1 143.5(5) . . . . ?
O5 C1 C2 F2 -97.7(6) . . . . ?
O5 C1 C2 F3 22.9(7) . . . . ?
O5 C1 C2' F1' -29.9(9) . . . . ?
O5 C1 C2' F2' 90.1(9) . . . . ?
O5 C1 C2' F3' -152.5(8) . . . . ?
O6 Ni1 O16 Ni2 46.18(11) . . . . ?
O6 Ni1 O16 Ni3 -133.21(10) . . . . ?
O6 Fe1 O16 Fe2 46.18(11) . . . . ?
O6 Fe1 O16 Fe3 -133.21(10) . . . . ?
O6 C3 C4 F4 31.9(4) . . . . ?
O6 C3 C4 F5 -86.1(4) . . . . ?
O6 C3 C4 F6 153.7(3) . . . . ?
O7 Ni2 O16 Ni1 -47.52(12) . . . . ?
O7 Ni2 O16 Ni3 131.87(10) . . . . ?
O7 Fe2 O16 Fe1 -47.52(12) . . . . ?
O7 Fe2 O16 Fe3 131.87(10) . . . . ?
O7 C3 C4 F4 -150.8(3) . . . . ?
O7 C3 C4 F5 91.2(3) . . . . ?
O7 C3 C4 F6 -29.0(4) . . . . ?
O8 Ni2 O16 Ni1 131.16(11) . . . . ?
O8 Ni2 O16 Ni3 -49.45(11) . . . . ?
O8 Fe2 O16 Fe1 131.16(11) . . . . ?
O8 Fe2 O16 Fe3 -49.45(11) . . . . ?
O8 C5 C6 F7 -33.8(3) . . . . ?
O8 C5 C6 F8 85.2(3) . . . . ?
O8 C5 C6 F9 -154.9(2) . . . . ?
O9 C5 C6 F7 148.1(2) . . . . ?
O9 C5 C6 F8 -92.9(3) . . . . ?
O9 C5 C6 F9 27.0(3) . . . . ?
O10 Ni2 O16 Ni1 -134.03(10) . . . . ?
O10 Ni2 O16 Ni3 45.35(10) . . . . ?
O10 Fe2 O16 Fe1 -134.03(10) . . . . ?
O10 Fe2 O16 Fe3 45.35(10) . . . . ?
O10 C7 C8 F10 37.2(3) . . . . ?
O10 C7 C8 F11 -82.0(3) . . . . ?
O10 C7 C8 F12 158.1(2) . . . . ?
O11 C7 C8 F10 -144.5(2) . . . . ?
O11 C7 C8 F11 96.4(3) . . . . ?
O11 C7 C8 F12 -23.6(3) . . . . ?
O12 C9 C10 F13 -27.0(4) . . . . ?
O12 C9 C10 F14 91.1(3) . . . . ?
O12 C9 C10 F15 -148.6(3) . . . . ?
O13 Ni1 O16 Ni2 -132.34(11) . . . . ?
O13 Ni1 O16 Ni3 48.27(11) . . . . ?
O13 Fe1 O16 Fe2 -132.34(11) . . . . ?
O13 Fe1 O16 Fe3 48.27(11) . . . . ?
O13 C9 C10 F13 154.8(2) . . . . ?
O13 C9 C10 F14 -87.1(3) . . . . ?
O13 C9 C10 F15 33.2(4) . . . . ?
O14 C11 C12 F16 30.2(4) . . . . ?
O14 C11 C12 F17 -89.9(3) . . . . ?
O14 C11 C12 F18 149.6(3) . . . . ?
O15 Ni1 O16 Ni2 133.28(11) . . . . ?
O15 Ni1 O16 Ni3 -46.11(11) . . . . ?
O15 Fe1 O16 Fe2 133.28(11) . . . . ?
O15 Fe1 O16 Fe3 -46.11(11) . . . . ?
O15 C11 C12 F16 -150.9(3) . . . . ?
O15 C11 C12 F17 88.9(4) . . . . ?
O15 C11 C12 F18 -31.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.728
_oxdiff_exptl_absorpt_empirical_full_min 0.401
####################################################################### 
# 
# 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_knoks16
_database_code_depnum_ccdc_archive 'CCDC 1996873'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-04-14 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_vrf_PLAT041_knoks16             
;
PROBLEM: _C Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT043_knoks16             
;
PROBLEM: _C Calculated and Reported Mol. Weight Differ by .. 5.03 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT068_knoks16             
;
PROBLEM: _C Reported F000 Differs from Calcd (or Missing).
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_FORMU01_knoks16             
;
PROBLEM: _G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_CELLZ01_knoks16             
;
PROBLEM: _G Difference between formula and atom_site contents detected.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT007_knoks16             
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 8 
RESPONSE: Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.
;

_vrf_PLAT301_knoks16             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 16% 
RESPONSE: Two CF3 groups were modeled as disordered over two
positions each: C4-F4-F5-F6, 0.65(2):0.35(2) and C8-F10-F11-F12,
0.730(6):0.270(6).
;

_vrf_PLAT302_knoks16             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-4, 6-8  ) .. 100% 
RESPONSE: Cocrystallized water solvent molecules O17, O18, and O19
were modeled as disordered over two positions each (0.586(6):0.414(6),
0.557(9):0.443(9), and 0.850(8):0.150(8), respectively).
;

_vrf_PLAT311_knoks16             
;
PROBLEM: _G Isolated Disordered Oxygen Atom (No H's ?) .. O17 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O17' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O19 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT860_knoks16             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 153 
RESPONSE: Analogous bond lengths and angles between the two
positions of the disordered CF3 groups were restrained to be
similar. Anisotropic displacement parameters for proximal atoms
were restrained to be similar and/or constrained to be equivalent.
;

_audit_creation_date             2020-04-02
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 F18 Fe3 O16, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 F18 Fe3 O19.50'
_chemical_formula_weight         978.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   33.7504(3)
_cell_length_b                   10.71550(10)
_cell_length_c                   16.4299(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.8530(10)
_cell_angle_gamma                90
_cell_volume                     5934.55(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    17034
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      77.1590
_cell_measurement_theta_min      2.6180
_shelx_estimated_absorpt_T_max   0.321
_shelx_estimated_absorpt_T_min   0.168
_exptl_absorpt_coefficient_mu    13.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.109
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26694
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.792
_diffrn_reflns_theta_min         2.622
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     60.00 121.00   0.50    0.41    --   49.87  23.00  74.00  122
  2  ω    107.00 156.00   0.50    1.63    --  105.75  30.00 120.00   98
  3  ω     92.00 153.00   0.50    1.63    --  105.75  61.00  90.00  122
  4  ω    101.00 161.00   0.50    1.63    --  105.75  23.00  74.00  120
  5  ω    107.00 133.00   0.50    1.63    --  105.75  15.00   0.00   52
  6  ω     99.00 176.00   0.50    1.63    --  105.75  45.00 -60.00  154
  7  ω    102.00 173.00   0.50    1.63    --  105.75  61.00   0.00  142
  8  ω     95.00 140.00   0.50    1.63    --  105.75 125.00 120.00   90
  9  ω    153.00 178.00   0.50    1.63    --  105.75 125.00 120.00   50
 10  ω    -19.00   6.00   0.50    0.41    --   49.87 -23.00 -91.00   50
 11  ω    -21.00  13.00   0.50    0.41    --   49.87 -19.00  90.00   68
 12  ω    -19.00  11.00   0.50    0.41    --   49.87 -19.00 120.00   60
 13  ω    -21.00   8.00   0.50    0.41    --   49.87 -19.00 150.00   58
 14  ω     53.00  96.00   0.50    1.63    --  105.75 -94.00 120.00   86
 15  ω     34.00 106.00   0.50    1.63    --  105.75 -94.00 150.00  144
 16  ω     40.00  71.00   0.50    1.63    --  105.75 -94.00  90.00   62
 17  ω     55.00  99.00   0.50    1.63    --  105.75 -94.00-150.00   88
 18  ω     39.00  65.00   0.50    1.63    --  105.75 -94.00-180.00   52
 19  ω     36.00  62.00   0.50    1.63    --  105.75 -61.00-180.00   52
 20  ω     37.00  63.00   0.50    1.63    --  105.75 -61.00-150.00   52
 21  ω     51.00  80.00   0.50    1.63    --  105.75 -61.00 -60.00   58
 22  ω     48.00  78.00   0.50    1.63    --  105.75 -61.00   0.00   60
 23  ω     37.00  64.00   0.50    1.63    --  105.75 -61.00 150.00   54
 24  ω     45.00  73.00   0.50    1.63    --  105.75 -61.00  90.00   56
 25  ω     -4.00  24.00   0.50    0.41    --  -49.87  19.00 -60.00   56
 26  ω    -33.00   8.00   0.50    0.41    --  -49.87  38.00-180.00   82
 27  ω     -5.00  20.00   0.50    0.41    --  -49.87  19.00-150.00   50
 28  ω    -12.00  23.00   0.50    0.41    --  -49.87  23.00  74.00   70
 29  ω    -44.00 -19.00   0.50    1.63    --  -84.25  45.00  30.00   50
 30  ω    -41.00 -12.00   0.50    1.63    --  -84.25  45.00-120.00   58
 31  ω    -98.00 -50.00   0.50    0.41    --  -49.87 -23.00 -91.00   96
 32  ω   -141.00-116.00   0.50    1.63    --  -84.25 -23.00 -91.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0432460000
_diffrn_orient_matrix_UB_12      0.0428577000
_diffrn_orient_matrix_UB_13      -0.0070959000
_diffrn_orient_matrix_UB_21      0.0065026000
_diffrn_orient_matrix_UB_22      -0.0065662000
_diffrn_orient_matrix_UB_23      0.0933466000
_diffrn_orient_matrix_UB_31      0.0132380000
_diffrn_orient_matrix_UB_32      -0.1371623000
_diffrn_orient_matrix_UB_33      -0.0066446000
_diffrn_oxdiff_digest_frames     
;
01c0e8682fc596e2f56ef3b6ce392f3df2000517da8
;
_diffrn_oxdiff_digest_hkl        
;
01b6c31fbb17fffa75c514e5eb53b59b8d76d5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5776
_reflns_number_total             6218
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.761
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     590
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+13.2079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1347
_refine_special_details          
;
Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were
included in the molecular formula.

Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.

Two CF3 groups were modeled as disordered over two positions
each: C4-F4-F5-F6, 0.65(2):0.35(2) and C8-F10-F11-F12,
0.730(6):0.270(6).

Cocrystallized water solvent molecules O17, O18, and O19 were
modeled as disordered over two positions each (0.586(6):0.414(6),
0.557(9):0.443(9), and 0.850(8):0.150(8), respectively).

Analogous bond lengths and angles between the two positions
of the disordered CF3 groups were restrained to be similar.
Anisotropic displacement parameters for proximal atoms were
restrained to be similar and/or constrained to be equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
 C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C4'-F4' \\sim C4'-F5' \\sim C4'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 C7-C8 \\sim C7-C8'
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F11' \\sim C8'-F12' \\sim C8'-F10'
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F11'-F12' \\sim F12'-F10' \\sim
F10'-F11'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
F11 \\sim F12': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
4. Rigid body (RIGU) restrains
 F10, F11, F12, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10', F11', F12', C8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4', F5', F6', C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C4')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(1)
 Sof(F10')=Sof(F11')=Sof(F12')=Sof(C8')=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C8)=FVAR(2)
 Sof(O17')=1-FVAR(3)
 Sof(O17)=FVAR(3)
 Sof(O18')=1-FVAR(4)
 Sof(O18)=FVAR(4)
 Sof(O19')=0.5*(1-FVAR(6))
 Sof(O19)=0.5*FVAR(6)
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.62089(2) 0.86060(4) 0.48753(3) 0.01641(13) Uani 1 1 d . U . . .
Fe2 Fe 0.63457(2) 0.56115(4) 0.53326(3) 0.02021(14) Uani 1 1 d . U . . .
Fe3 Fe 0.59800(2) 0.64525(4) 0.34932(3) 0.01992(14) Uani 1 1 d . U . . .
F1 F 0.57393(8) 0.8972(2) 0.74216(14) 0.0427(6) Uani 1 1 d . U . . .
F2 F 0.53955(7) 0.7329(3) 0.72446(17) 0.0618(8) Uani 1 1 d . U . . .
F3 F 0.59643(8) 0.7230(3) 0.78655(14) 0.0533(7) Uani 1 1 d . U . . .
F7 F 0.51855(8) 0.3307(2) 0.53910(15) 0.0458(6) Uani 1 1 d . U . . .
F8 F 0.53514(8) 0.2459(2) 0.42795(15) 0.0430(6) Uani 1 1 d . U . . .
F9 F 0.49280(7) 0.3965(3) 0.4268(2) 0.0619(8) Uani 1 1 d . U . . .
F13 F 0.47836(6) 0.85444(19) 0.32050(12) 0.0282(4) Uani 1 1 d . U . . .
F14 F 0.50743(6) 1.03135(19) 0.34047(14) 0.0347(5) Uani 1 1 d . U . . .
F15 F 0.48384(6) 0.9313(2) 0.44094(12) 0.0299(4) Uani 1 1 d . U . . .
F16 F 0.69326(9) 0.8548(3) 0.21100(17) 0.0555(8) Uani 1 1 d . U . . .
F17 F 0.65472(8) 1.0123(3) 0.2090(2) 0.0688(10) Uani 1 1 d . U . . .
F18 F 0.70423(7) 1.0029(3) 0.29394(15) 0.0479(6) Uani 1 1 d . U . . .
F4 F 0.7572(3) 0.8590(16) 0.5624(6) 0.027(2) Uani 0.35(2) 1 d D U . A 1
F5 F 0.7604(3) 0.6804(9) 0.6191(10) 0.028(2) Uani 0.35(2) 1 d D U . A 1
F6 F 0.7366(6) 0.8380(14) 0.6821(8) 0.029(2) Uani 0.35(2) 1 d D U . A 1
F10 F 0.72652(12) 0.3512(4) 0.3745(3) 0.0519(11) Uani 0.730(6) 1 d D U . B 1
F11 F 0.67857(13) 0.2872(4) 0.2945(4) 0.0748(17) Uani 0.730(6) 1 d D U . B 1
F12 F 0.71105(9) 0.4489(3) 0.26561(18) 0.0400(9) Uani 0.730(6) 1 d D U . B 1
F4' F 0.7506(2) 0.9052(8) 0.5814(5) 0.0330(15) Uani 0.65(2) 1 d D U . A 2
F5' F 0.76521(14) 0.7108(8) 0.5888(5) 0.0321(14) Uani 0.65(2) 1 d D U . A 2
F6' F 0.7368(3) 0.8003(9) 0.6875(4) 0.0292(14) Uani 0.65(2) 1 d D U . A 2
F10' F 0.6834(3) 0.3595(11) 0.2512(5) 0.058(3) Uani 0.270(6) 1 d D U . B 2
F11' F 0.7276(3) 0.3982(11) 0.3457(8) 0.056(3) Uani 0.270(6) 1 d D U . B 2
F12' F 0.6842(3) 0.2551(7) 0.3577(7) 0.046(2) Uani 0.270(6) 1 d D U . B 2
O1 O 0.62665(7) 1.04733(19) 0.50981(14) 0.0234(4) Uani 1 1 d . U . . .
H1A H 0.650955 1.067670 0.507343 0.035 Uiso 1 1 d R . . . .
H1B H 0.618705 1.064110 0.556973 0.035 Uiso 1 1 d R . . . .
O2 O 0.65326(7) 0.4243(2) 0.61640(18) 0.0341(6) Uani 1 1 d . U . . .
H2A H 0.676875 0.402328 0.607058 0.051 Uiso 1 1 d R . . . .
H2B H 0.637895 0.361738 0.611158 0.051 Uiso 1 1 d R . . . .
O3 O 0.57737(8) 0.5854(2) 0.23146(15) 0.0309(5) Uani 1 1 d . U . . .
H3A H 0.591305 0.523988 0.216771 0.046 Uiso 1 1 d R . . . .
H3B H 0.553195 0.563308 0.232821 0.046 Uiso 1 1 d R . . . .
O4 O 0.59645(6) 0.84201(19) 0.59673(13) 0.0207(4) Uani 1 1 d . U . . .
O5 O 0.60540(7) 0.64061(19) 0.63303(14) 0.0232(5) Uani 1 1 d . U . . .
O6 O 0.67630(6) 0.84917(19) 0.54612(13) 0.0209(4) Uani 1 1 d . U . . .
O7 O 0.68759(7) 0.6457(2) 0.57111(16) 0.0262(5) Uani 1 1 d . U . . .
O8 O 0.58468(6) 0.44841(19) 0.51477(12) 0.0193(4) Uani 1 1 d . U . . .
O9 O 0.56113(6) 0.50462(19) 0.38947(12) 0.0202(4) Uani 1 1 d . U . . .
O10 O 0.66581(8) 0.4590(2) 0.44677(16) 0.0318(5) Uani 1 1 d . U . . .
O11 O 0.64398(7) 0.5305(2) 0.32359(16) 0.0293(5) Uani 1 1 d . U . . .
O12 O 0.54830(7) 0.7569(2) 0.34659(13) 0.0238(5) Uani 1 1 d . U . . .
O13 O 0.56627(6) 0.90687(19) 0.43732(13) 0.0208(4) Uani 1 1 d . U . . .
O14 O 0.62782(7) 0.7864(2) 0.28732(14) 0.0295(5) Uani 1 1 d . U . . .
O15 O 0.65082(6) 0.91339(19) 0.38761(13) 0.0203(4) Uani 1 1 d . U . . .
O16 O 0.61791(5) 0.69282(17) 0.45726(11) 0.0136(4) Uani 1 1 d . U . . .
C1 C 0.59463(8) 0.7500(3) 0.64369(18) 0.0177(5) Uani 1 1 d . U . . .
C2 C 0.57590(9) 0.7770(3) 0.72576(19) 0.0223(6) Uani 1 1 d . U . . .
C3 C 0.69642(8) 0.7582(3) 0.57055(17) 0.0168(5) Uani 1 1 d D U . . .
C5 C 0.56075(8) 0.4458(2) 0.45491(16) 0.0137(5) Uani 1 1 d . U . . .
C6 C 0.52629(10) 0.3533(3) 0.4610(2) 0.0254(7) Uani 1 1 d . U . . .
C7 C 0.66536(9) 0.4663(3) 0.3707(2) 0.0248(6) Uani 1 1 d D U . . .
C9 C 0.54297(9) 0.8534(3) 0.38651(17) 0.0173(5) Uani 1 1 d . U . . .
C10 C 0.50263(9) 0.9183(3) 0.37209(17) 0.0201(6) Uani 1 1 d . U . . .
C11 C 0.64906(9) 0.8719(3) 0.31711(19) 0.0191(6) Uani 1 1 d . U . . .
C12 C 0.67592(10) 0.9371(3) 0.2571(2) 0.0260(7) Uani 1 1 d . U . . .
C4 C 0.7381(2) 0.7820(9) 0.6101(6) 0.018(2) Uani 0.35(2) 1 d D U . A 1
C8 C 0.69623(14) 0.3876(4) 0.3266(3) 0.0303(11) Uani 0.730(6) 1 d D U . B 1
C4' C 0.73801(14) 0.7945(6) 0.6067(4) 0.0191(12) Uani 0.65(2) 1 d D U . A 2
C8' C 0.6906(3) 0.3674(8) 0.3299(6) 0.036(2) Uani 0.270(6) 1 d D U . B 2
O17 O 0.70821(15) 1.1167(5) 0.5062(3) 0.0417(10) Uani 0.586(6) 1 d . U . C 1
O17' O 0.6910(2) 1.1802(7) 0.5045(5) 0.0417(10) Uani 0.414(6) 1 d . U . C 2
O18 O 0.7329(3) 0.3643(11) 0.5643(7) 0.0683(16) Uani 0.443(9) 1 d . U . D 1
O18' O 0.7287(2) 0.3567(8) 0.6091(6) 0.0683(16) Uani 0.557(9) 1 d . U . D 2
O19 O 0.500000 0.503(2) 0.250000 0.0233(11) Uani 0.150(8) 2 d S TU P E 1
O19' O 0.50446(15) 0.5716(5) 0.2242(3) 0.0233(11) Uani 0.425(4) 1 d . U . E 2
O20 O 0.60448(7) 0.7805(2) 0.11757(13) 0.0251(5) Uani 1 1 d . U . . .
H20A H 0.580521 0.759348 0.106536 0.038 Uiso 1 1 d R . . . .
H20B H 0.605751 0.812428 0.164996 0.038 Uiso 1 1 d R . . . .


_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 2.042(2) . ?
Fe1 O4 2.022(2) . ?
Fe1 O6 2.064(2) . ?
Fe1 O13 2.043(2) . ?
Fe1 O15 2.050(2) . ?
Fe1 O16 1.8668(19) . ?
Fe2 O2 2.080(3) . ?
Fe2 O5 2.131(2) . ?
Fe2 O7 2.074(2) . ?
Fe2 O8 2.082(2) . ?
Fe2 O10 2.116(2) . ?
Fe2 O16 1.948(2) . ?
Fe3 O3 2.124(3) . ?
Fe3 O9 2.082(2) . ?
Fe3 O11 2.040(2) . ?
Fe3 O12 2.059(2) . ?
Fe3 O14 2.107(2) . ?
Fe3 O16 1.9334(19) . ?
F1 C2 1.318(4) . ?
F2 C2 1.314(4) . ?
F3 C2 1.321(4) . ?
F7 C6 1.344(4) . ?
F8 C6 1.313(4) . ?
F9 C6 1.320(4) . ?
F13 C10 1.337(3) . ?
F14 C10 1.331(4) . ?
F15 C10 1.331(3) . ?
F16 C12 1.318(4) . ?
F17 C12 1.314(4) . ?
F18 C12 1.311(4) . ?
F4 C4 1.327(7) . ?
F5 C4 1.328(7) . ?
F6 C4 1.330(7) . ?
F10 C8 1.318(5) . ?
F11 C8 1.326(5) . ?
F12 C8 1.317(5) . ?
F4' C4' 1.333(5) . ?
F5' C4' 1.327(5) . ?
F6' C4' 1.332(5) . ?
F10' C8' 1.307(7) . ?
F11' C8' 1.307(7) . ?
F12' C8' 1.308(7) . ?
O1 H1A 0.8515 . ?
O1 H1B 0.8517 . ?
O2 H2A 0.8523 . ?
O2 H2B 0.8498 . ?
O3 H3A 0.8510 . ?
O3 H3B 0.8512 . ?
O4 C1 1.255(4) . ?
O5 C1 1.243(4) . ?
O6 C3 1.243(4) . ?
O7 C3 1.241(4) . ?
O8 C5 1.242(3) . ?
O9 C5 1.247(3) . ?
O10 C7 1.252(4) . ?
O11 C7 1.240(4) . ?
O12 C9 1.242(4) . ?
O13 C9 1.256(4) . ?
O14 C11 1.248(4) . ?
O15 C11 1.239(4) . ?
C1 C2 1.545(4) . ?
C3 C4 1.543(8) . ?
C3 C4' 1.546(5) . ?
C5 C6 1.535(4) . ?
C7 C8 1.548(5) . ?
C7 C8' 1.534(8) . ?
C9 C10 1.537(4) . ?
C11 C12 1.541(4) . ?
O19' O19' 0.913(10) 2_655 ?
O20 H20A 0.8506 . ?
O20 H20B 0.8502 . ?

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 O6 84.17(9) . . ?
O1 Fe1 O13 84.87(9) . . ?
O1 Fe1 O15 80.02(9) . . ?
O4 Fe1 O1 88.68(9) . . ?
O4 Fe1 O6 88.88(9) . . ?
O4 Fe1 O13 89.00(9) . . ?
O4 Fe1 O15 167.76(8) . . ?
O13 Fe1 O6 168.88(8) . . ?
O13 Fe1 O15 94.61(9) . . ?
O15 Fe1 O6 85.34(9) . . ?
O16 Fe1 O1 174.29(9) . . ?
O16 Fe1 O4 97.04(8) . . ?
O16 Fe1 O6 95.89(8) . . ?
O16 Fe1 O13 95.20(8) . . ?
O16 Fe1 O15 94.28(8) . . ?
O2 Fe2 O5 85.02(10) . . ?
O2 Fe2 O8 84.47(9) . . ?
O2 Fe2 O10 86.08(11) . . ?
O7 Fe2 O2 83.22(9) . . ?
O7 Fe2 O5 91.12(9) . . ?
O7 Fe2 O8 167.64(9) . . ?
O7 Fe2 O10 88.62(10) . . ?
O8 Fe2 O5 86.72(9) . . ?
O8 Fe2 O10 91.62(9) . . ?
O10 Fe2 O5 171.06(10) . . ?
O16 Fe2 O2 178.36(9) . . ?
O16 Fe2 O5 94.24(8) . . ?
O16 Fe2 O7 95.33(9) . . ?
O16 Fe2 O8 96.96(8) . . ?
O16 Fe2 O10 94.68(9) . . ?
O9 Fe3 O3 84.06(9) . . ?
O9 Fe3 O14 168.50(9) . . ?
O11 Fe3 O3 81.23(10) . . ?
O11 Fe3 O9 95.87(9) . . ?
O11 Fe3 O12 166.59(10) . . ?
O11 Fe3 O14 86.89(10) . . ?
O12 Fe3 O3 85.75(9) . . ?
O12 Fe3 O9 85.90(9) . . ?
O12 Fe3 O14 88.88(10) . . ?
O14 Fe3 O3 85.33(9) . . ?
O16 Fe3 O3 177.53(9) . . ?
O16 Fe3 O9 94.93(8) . . ?
O16 Fe3 O11 96.65(9) . . ?
O16 Fe3 O12 96.44(8) . . ?
O16 Fe3 O14 95.83(8) . . ?
Fe1 O1 H1A 109.0 . . ?
Fe1 O1 H1B 109.8 . . ?
H1A O1 H1B 109.7 . . ?
Fe2 O2 H2A 109.4 . . ?
Fe2 O2 H2B 109.0 . . ?
H2A O2 H2B 109.6 . . ?
Fe3 O3 H3A 109.4 . . ?
Fe3 O3 H3B 109.3 . . ?
H3A O3 H3B 109.6 . . ?
C1 O4 Fe1 131.13(19) . . ?
C1 O5 Fe2 129.4(2) . . ?
C3 O6 Fe1 131.67(19) . . ?
C3 O7 Fe2 128.7(2) . . ?
C5 O8 Fe2 128.18(19) . . ?
C5 O9 Fe3 132.14(19) . . ?
C7 O10 Fe2 131.0(2) . . ?
C7 O11 Fe3 129.1(2) . . ?
C9 O12 Fe3 127.7(2) . . ?
C9 O13 Fe1 132.8(2) . . ?
C11 O14 Fe3 128.0(2) . . ?
C11 O15 Fe1 130.31(19) . . ?
Fe1 O16 Fe2 121.11(10) . . ?
Fe1 O16 Fe3 120.66(10) . . ?
Fe3 O16 Fe2 118.23(9) . . ?
O4 C1 C2 115.1(3) . . ?
O5 C1 O4 129.1(3) . . ?
O5 C1 C2 115.8(3) . . ?
F1 C2 F3 107.7(3) . . ?
F1 C2 C1 112.9(3) . . ?
F2 C2 F1 107.4(3) . . ?
F2 C2 F3 108.0(3) . . ?
F2 C2 C1 109.9(3) . . ?
F3 C2 C1 110.9(2) . . ?
O6 C3 C4 118.6(4) . . ?
O6 C3 C4' 113.4(3) . . ?
O7 C3 O6 129.5(3) . . ?
O7 C3 C4 111.8(4) . . ?
O7 C3 C4' 117.1(3) . . ?
O8 C5 O9 129.6(3) . . ?
O8 C5 C6 115.4(3) . . ?
O9 C5 C6 115.0(3) . . ?
F7 C6 C5 111.2(3) . . ?
F8 C6 F7 107.2(3) . . ?
F8 C6 F9 109.8(3) . . ?
F8 C6 C5 110.5(3) . . ?
F9 C6 F7 105.4(3) . . ?
F9 C6 C5 112.4(3) . . ?
O10 C7 C8 117.3(3) . . ?
O10 C7 C8' 114.4(5) . . ?
O11 C7 O10 129.5(3) . . ?
O11 C7 C8 113.2(3) . . ?
O11 C7 C8' 115.4(5) . . ?
O12 C9 O13 128.9(3) . . ?
O12 C9 C10 116.5(3) . . ?
O13 C9 C10 114.6(2) . . ?
F13 C10 C9 112.1(2) . . ?
F14 C10 F13 107.5(2) . . ?
F14 C10 F15 108.0(3) . . ?
F14 C10 C9 110.4(2) . . ?
F15 C10 F13 106.8(2) . . ?
F15 C10 C9 111.9(2) . . ?
O14 C11 C12 115.3(3) . . ?
O15 C11 O14 129.0(3) . . ?
O15 C11 C12 115.7(3) . . ?
F16 C12 C11 110.9(3) . . ?
F17 C12 F16 108.0(3) . . ?
F17 C12 C11 110.0(3) . . ?
F18 C12 F16 106.9(3) . . ?
F18 C12 F17 108.1(3) . . ?
F18 C12 C11 112.7(3) . . ?
F4 C4 F5 106.7(7) . . ?
F4 C4 F6 106.7(8) . . ?
F4 C4 C3 108.2(7) . . ?
F5 C4 F6 108.6(8) . . ?
F5 C4 C3 114.3(7) . . ?
F6 C4 C3 112.0(11) . . ?
F10 C8 F11 108.4(5) . . ?
F10 C8 C7 113.7(4) . . ?
F11 C8 C7 109.2(4) . . ?
F12 C8 F10 106.8(4) . . ?
F12 C8 F11 106.4(5) . . ?
F12 C8 C7 112.0(3) . . ?
F4' C4' C3 113.6(4) . . ?
F5' C4' F4' 107.3(5) . . ?
F5' C4' F6' 107.9(5) . . ?
F5' C4' C3 111.7(4) . . ?
F6' C4' F4' 107.2(5) . . ?
F6' C4' C3 108.8(6) . . ?
F10' C8' C7 113.4(8) . . ?
F11' C8' F10' 109.9(9) . . ?
F11' C8' C7 106.5(8) . . ?
F12' C8' F10' 105.1(8) . . ?
F12' C8' F11' 109.7(9) . . ?
F12' C8' C7 112.3(7) . . ?
H20A O20 H20B 107.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O17 0.85 2.00 2.855(5) 177.8 . yes
O1 H1A O17' 0.85 1.81 2.603(7) 153.2 . yes
O1 H1B O20 0.85 2.01 2.689(3) 136.0 6_576 yes
O2 H2A O18 0.85 2.09 2.933(10) 169.8 . yes
O2 H2A O18' 0.85 1.82 2.657(7) 168.6 . yes
O2 H2B O20 0.85 1.90 2.745(3) 171.0 6_566 yes
O3 H3A O5 0.85 2.30 3.087(3) 153.7 6_565 yes
O3 H3B O19 0.85 1.94 2.789(8) 172.3 . yes
O3 H3B O19' 0.85 2.10 2.895(6) 154.3 2_655 yes
O3 H3B O19' 0.85 1.65 2.462(6) 159.7 . yes
O20 H20A F13 0.85 2.58 3.125(3) 122.8 2_655 yes
O20 H20B O14 0.85 2.13 2.861(3) 144.4 . yes

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 O4 C1 O5 -5.3(5) . . . . ?
Fe1 O4 C1 C2 175.48(19) . . . . ?
Fe1 O6 C3 O7 -5.1(5) . . . . ?
Fe1 O6 C3 C4 177.9(5) . . . . ?
Fe1 O6 C3 C4' 176.3(3) . . . . ?
Fe1 O13 C9 O12 -5.9(5) . . . . ?
Fe1 O13 C9 C10 174.64(19) . . . . ?
Fe1 O15 C11 O14 1.1(5) . . . . ?
Fe1 O15 C11 C12 179.1(2) . . . . ?
Fe2 O5 C1 O4 3.6(5) . . . . ?
Fe2 O5 C1 C2 -177.15(19) . . . . ?
Fe2 O7 C3 O6 -1.4(5) . . . . ?
Fe2 O7 C3 C4 175.8(4) . . . . ?
Fe2 O7 C3 C4' 177.2(3) . . . . ?
Fe2 O8 C5 O9 3.7(5) . . . . ?
Fe2 O8 C5 C6 -178.66(19) . . . . ?
Fe2 O10 C7 O11 -5.9(5) . . . . ?
Fe2 O10 C7 C8 172.4(3) . . . . ?
Fe2 O10 C7 C8' -175.8(5) . . . . ?
Fe3 O9 C5 O8 -5.7(5) . . . . ?
Fe3 O9 C5 C6 176.6(2) . . . . ?
Fe3 O11 C7 O10 -3.8(5) . . . . ?
Fe3 O11 C7 C8 177.8(2) . . . . ?
Fe3 O11 C7 C8' 166.0(5) . . . . ?
Fe3 O12 C9 O13 0.6(5) . . . . ?
Fe3 O12 C9 C10 -179.97(18) . . . . ?
Fe3 O14 C11 O15 -18.5(5) . . . . ?
Fe3 O14 C11 C12 163.5(2) . . . . ?
O4 Fe1 O16 Fe2 -46.39(12) . . . . ?
O4 Fe1 O16 Fe3 133.46(11) . . . . ?
O4 C1 C2 F1 -16.1(4) . . . . ?
O4 C1 C2 F2 103.8(3) . . . . ?
O4 C1 C2 F3 -137.0(3) . . . . ?
O5 C1 C2 F1 164.6(3) . . . . ?
O5 C1 C2 F2 -75.6(4) . . . . ?
O5 C1 C2 F3 43.7(4) . . . . ?
O6 Fe1 O16 Fe2 43.20(12) . . . . ?
O6 Fe1 O16 Fe3 -136.95(11) . . . . ?
O6 C3 C4 F4 -48.3(11) . . . . ?
O6 C3 C4 F5 -167.0(9) . . . . ?
O6 C3 C4 F6 69.1(12) . . . . ?
O6 C3 C4' F4' -21.8(7) . . . . ?
O6 C3 C4' F5' -143.4(5) . . . . ?
O6 C3 C4' F6' 97.5(7) . . . . ?
O7 C3 C4 F4 134.2(9) . . . . ?
O7 C3 C4 F5 15.5(11) . . . . ?
O7 C3 C4 F6 -108.4(11) . . . . ?
O7 C3 C4' F4' 159.4(6) . . . . ?
O7 C3 C4' F5' 37.8(7) . . . . ?
O7 C3 C4' F6' -81.2(7) . . . . ?
O8 C5 C6 F7 25.9(4) . . . . ?
O8 C5 C6 F8 -93.0(3) . . . . ?
O8 C5 C6 F9 143.9(3) . . . . ?
O9 C5 C6 F7 -156.0(3) . . . . ?
O9 C5 C6 F8 85.0(3) . . . . ?
O9 C5 C6 F9 -38.1(4) . . . . ?
O10 C7 C8 F10 -19.0(6) . . . . ?
O10 C7 C8 F11 102.2(5) . . . . ?
O10 C7 C8 F12 -140.2(4) . . . . ?
O10 C7 C8' F10' 166.6(8) . . . . ?
O10 C7 C8' F11' -72.4(9) . . . . ?
O10 C7 C8' F12' 47.6(9) . . . . ?
O11 C7 C8 F10 159.6(4) . . . . ?
O11 C7 C8 F11 -79.2(5) . . . . ?
O11 C7 C8 F12 38.4(5) . . . . ?
O11 C7 C8' F10' -4.8(10) . . . . ?
O11 C7 C8' F11' 116.2(8) . . . . ?
O11 C7 C8' F12' -123.7(7) . . . . ?
O12 C9 C10 F13 3.5(4) . . . . ?
O12 C9 C10 F14 -116.4(3) . . . . ?
O12 C9 C10 F15 123.4(3) . . . . ?
O13 Fe1 O16 Fe2 -136.03(11) . . . . ?
O13 Fe1 O16 Fe3 43.83(12) . . . . ?
O13 C9 C10 F13 -177.1(2) . . . . ?
O13 C9 C10 F14 63.1(3) . . . . ?
O13 C9 C10 F15 -57.1(3) . . . . ?
O14 C11 C12 F16 -44.2(4) . . . . ?
O14 C11 C12 F17 75.2(4) . . . . ?
O14 C11 C12 F18 -164.0(3) . . . . ?
O15 Fe1 O16 Fe2 128.94(11) . . . . ?
O15 Fe1 O16 Fe3 -51.21(12) . . . . ?
O15 C11 C12 F16 137.5(3) . . . . ?
O15 C11 C12 F17 -103.1(4) . . . . ?
O15 C11 C12 F18 17.6(4) . . . . ?

_olex2_submission_original_sample_id knoks16
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.672
####################################################################### 
# 
# 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_knoks12mo
_database_code_depnum_ccdc_archive 'CCDC 1996872'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-04-14 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_vrf_PLAT041_knoks12mo           
;
PROBLEM: _C Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT043_knoks12mo           
;
PROBLEM: _C Calculated and Reported Mol. Weight Differ by .. 4.95 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT068_knoks12mo           
;
PROBLEM: _C Reported F000 Differs from Calcd (or Missing).
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_FORMU01_knoks12mo           
;
PROBLEM: _G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data. 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_CELLZ01_knoks12mo           
;
PROBLEM: _G Difference between formula and atom_site contents detected. 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT007_knoks12mo           
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 8 
RESPONSE: Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.
;

_vrf_PLAT042_knoks12mo           
;
PROBLEM: _G Calc. and Reported MoietyFormula Strings  Differ 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT301_knoks12mo           
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 22% 
RESPONSE: Each metal site was modeled as a disorder of Fe and Cu:
Fe1:Cu1, 0.907(3):0.093(3), Fe2:Cu2, 0.595(3):0.405(3), Fe3:Cu3,
0.498(3):0.502(3). The total metal ratio was constrained to 2Fe:1Cu.
Two CF3 groups were modeled as disordered over two and four
positions each, respectively: C4-F4-F5-F6, 0.54(2):0.48(2) and
C8-F10-F11-F12, 0.475(3):0.238(8):0.158(3):0.129(3).
;

_vrf_PLAT302_knoks12mo           
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-3, 5-8 ) .. 100% 
RESPONSE: Cocrystallized water solvent molecules O17, O18, and O19
were modeled as disordered over two positions each (0.683(4):0.317(4),
0.69(1):0.31(1), and 0.95(1):0.05(1), respectively).
;

_vrf_PLAT311_knoks12mo           
;
PROBLEM: _G Isolated Disordered Oxygen Atom (No H's ?) ..... O17 
         _G Isolated Disordered Oxygen Atom (No H's ?) ..... O18' 
         _G Isolated Disordered Oxygen Atom (No H's ?) ..... O19 
         _G Isolated Disordered Oxygen Atom (No H's ?) ..... O17' 
         _G Isolated Disordered Oxygen Atom (No H's ?) ..... O18 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT860_knoks12mo           
;
PROBLEM: _G Number of Least-Squares Restraints ............. 519 
RESPONSE: Positional and anisotropic displacement parameters,
respectively, for the two metal types of each site disorder were
constrained to be equivalent. Analogous bond lengths and angles
between the two positions of the disordered CF3 groups were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained to be similar and/or
constrained to be equivalent.
;

_audit_creation_date             2020-04-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Cu1 F18 Fe2 O16, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 Cu F18 Fe2 O19.50'
_chemical_formula_weight         986.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
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'
Cu Cu 0.3201 1.2651 '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                   33.6407(8)
_cell_length_b                   10.6483(3)
_cell_length_c                   16.5280(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.306(2)
_cell_angle_gamma                90
_cell_volume                     5910.7(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    21331
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.3180
_cell_measurement_theta_min      2.6170
_shelx_estimated_absorpt_T_max   0.762
_shelx_estimated_absorpt_T_min   0.570
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red-orange
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.153
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32063
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         33.171
_diffrn_reflns_theta_min         2.469
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00   6.00   0.50    3.52    --  -12.20  83.00 -75.00   80
  2  ω    -59.00   0.00   0.50    3.52    --  -12.20 -38.00 120.00  118
  3  ω    -39.00  21.00   0.50    3.52    --   10.95 -83.00 164.00  120
  4  ω    -42.00 -17.00   0.50    3.52    --  -12.20 -83.00 164.00   50
  5  ω    -19.00  43.00   0.50    3.52    --   10.95 -99.00  60.00  124
  6  ω    -23.00  40.00   0.50    3.52    --   10.95 -99.00 -60.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143712000
_diffrn_orient_matrix_UB_12      -0.0418398000
_diffrn_orient_matrix_UB_13      0.0178577000
_diffrn_orient_matrix_UB_21      -0.0154478000
_diffrn_orient_matrix_UB_22      -0.0408195000
_diffrn_orient_matrix_UB_23      0.0110544000
_diffrn_orient_matrix_UB_31      0.0008829000
_diffrn_orient_matrix_UB_32      -0.0320272000
_diffrn_orient_matrix_UB_33      -0.0374890000
_diffrn_oxdiff_digest_frames     
;
0169c4662de78dfbc0b470ebd54fcc273100027a225
;
_diffrn_oxdiff_digest_hkl        
;
01090b1ff4100f1db79b3b52b9387a100181a5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8563
_reflns_number_total             9615
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_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       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9615
_refine_ls_number_restraints     519
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.137
_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)+(0.0212P)²+27.5714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0957
_refine_special_details          
;
Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were
included in the molecular formula.

Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.

Each metal site was modeled as a disorder of Fe and Cu:
Fe1:Cu1, 0.907(3):0.093(3), Fe2:Cu2, 0.595(3):0.405(3), Fe3:Cu3,
0.498(3):0.502(3). The total metal ratio was constrained to 2Fe:1Cu.
Two CF3 groups were modeled as disordered over two and four
positions each, respectively: C4-F4-F5-F6, 0.54(2):0.48(2) and
C8-F10-F11-F12, 0.475(3):0.238(8):0.158(3):0.129(3).

Cocrystallized water solvent molecules O17, O18, and O19 were
modeled as disordered over two positions each (0.683(4):0.317(4),
0.69(1):0.31(1), and 0.95(1):0.05(1), respectively).

Positional and anisotropic displacement parameters, respectively,
for the two metal types of each site disorder were constrained
to be equivalent. Analogous bond lengths and angles between
the two positions of the disordered CF3 groups were restrained
to be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and/or constrained to be
equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Fe1, Cu1}
{Fe2, Cu2}
{Fe3, Cu3}
3. Restrained distances
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
 C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C4'-F4' \\sim C4'-F5' \\sim C4'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 C7-C8 \\sim C7-C8' \\sim C7-C8" \\sim C7-C8Z
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F11' \\sim C8'-F12' \\sim C8'-F10'
\\sim C8"-F10" \\sim C8"-
 F11" \\sim C8"-F12" \\sim C8Z-F10Z \\sim C8Z-F11Z \\sim C8Z-F12Z
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F11'-F12' \\sim F12'-F10' \\sim
F10'-F11' \\sim F10"-F11" ~
 F11"-F12" \\sim F12"-F10" \\sim F10Z-F11Z \\sim F11Z-F12Z \\sim F12Z-F10Z
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
F12 \\sim F12Z: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
Uanis(Fe1) = Uanis(Cu1)
Uanis(Fe2) = Uanis(Cu2)
Uanis(Fe3) = Uanis(Cu3)
5. Rigid body (RIGU) restrains
 F4, F5, F6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4', F5', F6', C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8', F10', F11', F12'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8", F10", F11", F12"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8Z, F10Z, F11Z, F12Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Fe1)+Sof(Cu1)]+1*[Sof(Fe2)+Sof(Cu2)]+1*[Sof(Fe3)+Sof(Cu3)]=2 with esd
 of 0.0001
 1*[Sof(C8)+Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(C8')+Sof(F12')+Sof(F10')+
 Sof(F11')]+1*[Sof(C8")+Sof(F10")+Sof(F11")+Sof(F12")]+1*[Sof(C8Z)+Sof(F10Z)+
 Sof(F11Z)+Sof(F12Z)]=1 with esd of 0.0001
 Sof(C4')=Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(C4)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(O17')=1-FVAR(2)
 Sof(O17)=FVAR(2)
 Sof(O18')=1-FVAR(3)
 Sof(O18)=FVAR(3)
 Sof(O19')=0.5*(1-FVAR(5))
 Sof(O19)=0.5*FVAR(5)
 Sof(Cu1)=1-FVAR(5)
 Sof(Fe1)=FVAR(5)
 Sof(Cu2)=1-FVAR(6)
 Sof(Fe2)=FVAR(6)
 Sof(Cu3)=1-FVAR(7)
 Sof(Fe3)=FVAR(7)
 Sof(C8)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(8)
 Sof(C8')=Sof(F12')=Sof(F10')=Sof(F11')=FVAR(9)
 Sof(C8")=Sof(F10")=Sof(F11")=Sof(F12")=FVAR(10)
 Sof(C8Z)=Sof(F10Z)=Sof(F11Z)=Sof(F12Z)=FVAR(11)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.62091(2) 0.86401(3) 0.48477(2) 0.01643(8) Uani 0.907(3) 1 d . U . A 1
Fe2 Fe 0.63245(2) 0.56397(3) 0.52957(2) 0.01614(7) Uani 0.595(3) 1 d . U . A 1
Fe3 Fe 0.59666(2) 0.65074(3) 0.34755(2) 0.01485(7) Uani 0.498(3) 1 d . U . A 1
Cu1 Cu 0.62091(2) 0.86401(3) 0.48477(2) 0.01643(8) Uani 0.093(3) 1 d . U . A 5
Cu2 Cu 0.63245(2) 0.56397(3) 0.52957(2) 0.01614(7) Uani 0.405(3) 1 d . U . A 5
Cu3 Cu 0.59666(2) 0.65074(3) 0.34755(2) 0.01485(7) Uani 0.502(3) 1 d . U . A 5
F1 F 0.57547(6) 0.91093(18) 0.73775(11) 0.0332(4) Uani 1 1 d . U . . .
F2 F 0.53942(6) 0.7471(2) 0.72296(15) 0.0487(6) Uani 1 1 d . U . . .
F3 F 0.59743(8) 0.7341(3) 0.78317(13) 0.0657(8) Uani 1 1 d . U . . .
F7 F 0.51890(6) 0.3318(2) 0.54188(12) 0.0431(5) Uani 1 1 d . U . . .
F8 F 0.53735(8) 0.2369(2) 0.43745(14) 0.0555(6) Uani 1 1 d . U . . .
F9 F 0.49296(7) 0.3818(3) 0.4270(2) 0.0848(10) Uani 1 1 d . U . . .
F13 F 0.47758(4) 0.85401(15) 0.31902(9) 0.0212(3) Uani 1 1 d . U . . .
F14 F 0.50741(5) 1.03172(16) 0.33667(11) 0.0305(4) Uani 1 1 d . U . . .
F15 F 0.48426(5) 0.93512(17) 0.43754(10) 0.0272(3) Uani 1 1 d . U . . .
F16 F 0.69485(7) 0.8623(3) 0.21618(15) 0.0588(7) Uani 1 1 d . U . . .
F17 F 0.65601(7) 1.0206(3) 0.20751(15) 0.0653(8) Uani 1 1 d . U . . .
F18 F 0.70437(6) 1.0156(2) 0.29640(12) 0.0499(6) Uani 1 1 d . U . . .
C4 C 0.73785(16) 0.7683(6) 0.6079(4) 0.0185(16) Uani 0.540(19) 1 d D U . B 1
F4 F 0.75806(17) 0.8491(9) 0.5645(3) 0.0300(14) Uani 0.540(19) 1 d D U . B 1
F5 F 0.75878(17) 0.6628(6) 0.6147(6) 0.0301(15) Uani 0.540(19) 1 d D U . B 1
F6 F 0.7355(5) 0.8173(10) 0.6818(5) 0.0304(18) Uani 0.540(19) 1 d D U . B 1
C4' C 0.73746(16) 0.7842(7) 0.6062(5) 0.0166(17) Uani 0.460(19) 1 d D U . B 2
F4' F 0.7508(2) 0.8967(9) 0.5846(6) 0.0291(18) Uani 0.460(19) 1 d D U . B 2
F5' F 0.76434(14) 0.7002(9) 0.5854(6) 0.0254(17) Uani 0.460(19) 1 d D U . B 2
F6' F 0.7375(5) 0.7834(12) 0.6871(5) 0.0274(19) Uani 0.460(19) 1 d D U . B 2
C8 C 0.69319(17) 0.4025(6) 0.3118(4) 0.0274(14) Uani 0.476(3) 1 d D U . C 1
F10 F 0.72319(14) 0.3443(5) 0.3546(3) 0.0408(11) Uani 0.476(3) 1 d D U . C 1
F11 F 0.67578(16) 0.3136(6) 0.2638(4) 0.0433(15) Uani 0.476(3) 1 d D U . C 1
F12 F 0.7110(3) 0.4800(8) 0.2608(5) 0.0322(17) Uani 0.476(3) 1 d D U . C 1
C8' C 0.6967(5) 0.3956(17) 0.3293(10) 0.028(3) Uani 0.129(3) 1 d D U . C 2
F12' F 0.6978(7) 0.428(2) 0.2518(11) 0.034(4) Uani 0.129(3) 1 d D U . C 2
F10' F 0.7324(8) 0.411(3) 0.3668(15) 0.027(4) Uani 0.129(3) 1 d D U . C 2
F11' F 0.6865(9) 0.275(2) 0.3341(16) 0.030(5) Uani 0.129(3) 1 d D U . C 2
C8" C 0.6890(3) 0.3754(9) 0.3253(5) 0.026(2) Uani 0.238(3) 1 d D U . C 3
F10" F 0.7255(3) 0.4197(12) 0.3391(7) 0.035(2) Uani 0.238(3) 1 d D U . C 3
F11" F 0.6855(4) 0.2637(10) 0.3586(7) 0.033(2) Uani 0.238(3) 1 d D U . C 3
F12" F 0.6794(3) 0.3727(11) 0.2468(5) 0.032(2) Uani 0.238(3) 1 d D U . C 3
C8Z C 0.6983(4) 0.4070(16) 0.3262(11) 0.028(3) Uani 0.158(3) 1 d D U . C 4
F10Z F 0.7288(7) 0.397(3) 0.3812(13) 0.034(4) Uani 0.158(3) 1 d D U . C 4
F11Z F 0.6843(6) 0.2918(16) 0.3105(13) 0.034(3) Uani 0.158(3) 1 d D U . C 4
F12Z F 0.7122(10) 0.453(2) 0.2582(14) 0.030(4) Uani 0.158(3) 1 d D U . C 4
O1 O 0.62796(5) 1.05060(17) 0.50765(11) 0.0202(4) Uani 1 1 d . U . . .
H1A H 0.652254 1.070936 0.505183 0.030 Uiso 1 1 d R . . A .
H1B H 0.620004 1.067376 0.554813 0.030 Uiso 1 1 d R . . . .
O2 O 0.65099(5) 0.42773(17) 0.60824(11) 0.0195(3) Uani 1 1 d . U . . .
H2A H 0.674608 0.405714 0.598901 0.029 Uiso 1 1 d R . . A .
H2B H 0.635628 0.365124 0.602991 0.029 Uiso 1 1 d R . . . .
O3 O 0.57536(5) 0.59683(17) 0.23254(10) 0.0180(3) Uani 1 1 d . U . . .
H3A H 0.589282 0.535371 0.217830 0.027 Uiso 1 1 d R . . A .
H3B H 0.551162 0.574691 0.233880 0.027 Uiso 1 1 d R . . . .
O4 O 0.59598(5) 0.84896(17) 0.59280(11) 0.0195(3) Uani 1 1 d . U . . .
O5 O 0.60429(6) 0.64667(19) 0.63128(13) 0.0266(4) Uani 1 1 d . U . . .
O6 O 0.67640(5) 0.84628(18) 0.54685(11) 0.0211(4) Uani 1 1 d . U . . .
O7 O 0.68543(5) 0.63849(17) 0.56501(11) 0.0208(4) Uani 1 1 d . U . . .
O8 O 0.58371(5) 0.45694(17) 0.51496(10) 0.0187(3) Uani 1 1 d . U . . .
O9 O 0.56065(6) 0.4930(2) 0.38675(11) 0.0272(4) Uani 1 1 d . U . . .
O10 O 0.66214(7) 0.4551(3) 0.43881(14) 0.0422(6) Uani 1 1 d . U . . .
O11 O 0.64245(5) 0.54551(18) 0.32099(10) 0.0198(3) Uani 1 1 d . U . . .
O12 O 0.54731(5) 0.75156(16) 0.34872(10) 0.0152(3) Uani 1 1 d . U . . .
O13 O 0.56714(5) 0.91135(17) 0.43093(11) 0.0197(4) Uani 1 1 d . U . . .
O14 O 0.62465(6) 0.8070(2) 0.28510(12) 0.0296(5) Uani 1 1 d . U . . .
O15 O 0.65309(5) 0.91531(17) 0.38936(10) 0.0175(3) Uani 1 1 d . U . . .
O16 O 0.61680(5) 0.69355(15) 0.45528(9) 0.0120(3) Uani 1 1 d . U . . .
C1 C 0.59416(7) 0.7580(2) 0.64025(16) 0.0190(5) Uani 1 1 d . U . . .
C2 C 0.57661(8) 0.7887(3) 0.72248(17) 0.0251(5) Uani 1 1 d . U . . .
C3 C 0.69550(7) 0.7507(2) 0.56850(13) 0.0156(4) Uani 1 1 d D U . . .
C5 C 0.56020(7) 0.4433(2) 0.45452(14) 0.0182(4) Uani 1 1 d . U . . .
C6 C 0.52683(9) 0.3465(3) 0.46481(18) 0.0295(6) Uani 1 1 d . U . . .
C7 C 0.66297(8) 0.4726(3) 0.36459(17) 0.0243(5) Uani 1 1 d D U . . .
C9 C 0.54300(7) 0.8533(2) 0.38442(14) 0.0145(4) Uani 1 1 d . U . . .
C10 C 0.50236(7) 0.9197(2) 0.36911(14) 0.0164(4) Uani 1 1 d . U . . .
C11 C 0.64857(7) 0.8838(2) 0.31694(15) 0.0182(4) Uani 1 1 d . U . . .
C12 C 0.67651(8) 0.9482(3) 0.25865(16) 0.0250(5) Uani 1 1 d . U . . .
O17 O 0.70991(9) 1.1135(3) 0.5057(2) 0.0319(6) Uani 0.683(4) 1 d . U . D 1
O17' O 0.6928(2) 1.1886(7) 0.4961(5) 0.0319(6) Uani 0.317(4) 1 d . U . D 2
O18 O 0.7265(2) 0.3584(8) 0.5602(6) 0.0356(8) Uani 0.312(6) 1 d . U . E 1
O18' O 0.72855(10) 0.3461(3) 0.6068(3) 0.0356(8) Uani 0.688(6) 1 d . U . E 2
O19 O 0.500000 0.5075(4) 0.250000 0.0304(10) Uani 0.953(12) 2 d S TU P F 1
O19' O 0.506(3) 0.573(10) 0.240(8) 0.0304(10) Uani 0.024(6) 1 d . U . F 2
O20 O 0.60530(5) 0.78548(17) 0.11904(10) 0.0199(3) Uani 1 1 d . U . . .
H20A H 0.581336 0.764335 0.108005 0.030 Uiso 1 1 d R . . . .
H20B H 0.606566 0.817425 0.166465 0.030 Uiso 1 1 d R . . . .


_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 2.0338(18) . ?
Fe1 O4 2.0224(18) . ?
Fe1 O6 2.0863(18) . ?
Fe1 O13 2.0327(17) . ?
Fe1 O15 2.0381(18) . ?
Fe1 O16 1.8824(16) . ?
Fe2 O2 2.0224(17) . ?
Fe2 O5 2.164(2) . ?
Fe2 O7 2.0070(18) . ?
Fe2 O8 2.0001(17) . ?
Fe2 O10 2.183(3) . ?
Fe2 O16 1.9012(16) . ?
Fe3 O3 2.0735(17) . ?
Fe3 O9 2.191(2) . ?
Fe3 O11 1.9745(18) . ?
Fe3 O12 1.9783(17) . ?
Fe3 O14 2.198(2) . ?
Fe3 O16 1.9230(15) . ?
Cu1 O1 2.0338(18) . ?
Cu1 O4 2.0224(18) . ?
Cu1 O6 2.0863(18) . ?
Cu1 O13 2.0327(17) . ?
Cu1 O15 2.0381(18) . ?
Cu1 O16 1.8824(16) . ?
Cu2 O2 2.0224(17) . ?
Cu2 O5 2.164(2) . ?
Cu2 O7 2.0070(18) . ?
Cu2 O8 2.0001(17) . ?
Cu2 O10 2.183(3) . ?
Cu2 O16 1.9012(16) . ?
Cu3 O3 2.0735(17) . ?
Cu3 O9 2.191(2) . ?
Cu3 O11 1.9745(18) . ?
Cu3 O12 1.9783(17) . ?
Cu3 O14 2.198(2) . ?
Cu3 O16 1.9230(15) . ?
F1 C2 1.326(4) . ?
F2 C2 1.328(3) . ?
F3 C2 1.325(3) . ?
F7 C6 1.326(4) . ?
F8 C6 1.307(4) . ?
F9 C6 1.322(4) . ?
F13 C10 1.338(3) . ?
F14 C10 1.322(3) . ?
F15 C10 1.325(3) . ?
F16 C12 1.327(4) . ?
F17 C12 1.310(3) . ?
F18 C12 1.310(3) . ?
C4 F4 1.332(6) . ?
C4 F5 1.326(6) . ?
C4 F6 1.334(6) . ?
C4 C3 1.544(6) . ?
C4' F4' 1.335(6) . ?
C4' F5' 1.331(6) . ?
C4' F6' 1.336(6) . ?
C4' C3 1.552(6) . ?
C8 F10 1.349(6) . ?
C8 F11 1.347(6) . ?
C8 F12 1.346(6) . ?
C8 C7 1.567(6) . ?
C8' F12' 1.330(8) . ?
C8' F10' 1.330(7) . ?
C8' F11' 1.330(8) . ?
C8' C7 1.541(9) . ?
C8" F10" 1.323(7) . ?
C8" F11" 1.319(7) . ?
C8" F12" 1.320(7) . ?
C8" C7 1.525(8) . ?
C8Z F10Z 1.336(7) . ?
C8Z F11Z 1.335(7) . ?
C8Z F12Z 1.335(7) . ?
C8Z C7 1.546(9) . ?
O1 H1A 0.8486 . ?
O1 H1B 0.8575 . ?
O2 H2A 0.8511 . ?
O2 H2B 0.8449 . ?
O3 H3A 0.8484 . ?
O3 H3B 0.8491 . ?
O4 C1 1.250(3) . ?
O5 C1 1.245(3) . ?
O6 C3 1.245(3) . ?
O7 C3 1.242(3) . ?
O8 C5 1.246(3) . ?
O9 C5 1.240(3) . ?
O10 C7 1.243(3) . ?
O11 C7 1.241(3) . ?
O12 C9 1.246(3) . ?
O13 C9 1.249(3) . ?
O14 C11 1.242(3) . ?
O15 C11 1.244(3) . ?
C1 C2 1.548(4) . ?
C5 C6 1.541(4) . ?
C9 C10 1.547(3) . ?
C11 C12 1.545(4) . ?
O19' O19' 0.51(19) 2_655 ?
O20 H20A 0.8466 . ?
O20 H20B 0.8533 . ?

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 O6 84.58(7) . . ?
O1 Fe1 O15 79.67(7) . . ?
O4 Fe1 O1 87.89(7) . . ?
O4 Fe1 O6 87.91(7) . . ?
O4 Fe1 O13 90.13(7) . . ?
O4 Fe1 O15 165.98(7) . . ?
O13 Fe1 O1 86.01(7) . . ?
O13 Fe1 O6 170.45(7) . . ?
O13 Fe1 O15 95.37(7) . . ?
O15 Fe1 O6 84.53(7) . . ?
O16 Fe1 O1 174.96(8) . . ?
O16 Fe1 O4 97.13(7) . . ?
O16 Fe1 O6 95.18(7) . . ?
O16 Fe1 O13 94.33(7) . . ?
O16 Fe1 O15 95.30(7) . . ?
O2 Fe2 O5 85.70(7) . . ?
O2 Fe2 O10 85.68(8) . . ?
O5 Fe2 O10 171.19(8) . . ?
O7 Fe2 O2 81.97(7) . . ?
O7 Fe2 O5 91.92(8) . . ?
O7 Fe2 O10 88.67(9) . . ?
O8 Fe2 O2 83.64(7) . . ?
O8 Fe2 O5 86.16(8) . . ?
O8 Fe2 O7 165.58(7) . . ?
O8 Fe2 O10 91.08(9) . . ?
O16 Fe2 O2 178.12(7) . . ?
O16 Fe2 O5 95.11(7) . . ?
O16 Fe2 O7 96.30(7) . . ?
O16 Fe2 O8 98.11(7) . . ?
O16 Fe2 O10 93.57(8) . . ?
O3 Fe3 O9 83.75(7) . . ?
O3 Fe3 O14 85.06(7) . . ?
O9 Fe3 O14 168.05(7) . . ?
O11 Fe3 O3 82.64(7) . . ?
O11 Fe3 O9 94.72(8) . . ?
O11 Fe3 O12 167.44(7) . . ?
O11 Fe3 O14 87.96(8) . . ?
O12 Fe3 O3 85.03(7) . . ?
O12 Fe3 O9 86.25(7) . . ?
O12 Fe3 O14 88.64(8) . . ?
O16 Fe3 O3 177.63(7) . . ?
O16 Fe3 O9 94.55(7) . . ?
O16 Fe3 O11 95.89(7) . . ?
O16 Fe3 O12 96.51(7) . . ?
O16 Fe3 O14 96.76(7) . . ?
O1 Cu1 O6 84.58(7) . . ?
O1 Cu1 O15 79.67(7) . . ?
O4 Cu1 O1 87.89(7) . . ?
O4 Cu1 O6 87.91(7) . . ?
O4 Cu1 O13 90.13(7) . . ?
O4 Cu1 O15 165.98(7) . . ?
O13 Cu1 O1 86.01(7) . . ?
O13 Cu1 O6 170.45(7) . . ?
O13 Cu1 O15 95.37(7) . . ?
O15 Cu1 O6 84.53(7) . . ?
O16 Cu1 O1 174.96(8) . . ?
O16 Cu1 O4 97.13(7) . . ?
O16 Cu1 O6 95.18(7) . . ?
O16 Cu1 O13 94.33(7) . . ?
O16 Cu1 O15 95.30(7) . . ?
O2 Cu2 O5 85.70(7) . . ?
O2 Cu2 O10 85.68(8) . . ?
O5 Cu2 O10 171.19(8) . . ?
O7 Cu2 O2 81.97(7) . . ?
O7 Cu2 O5 91.92(8) . . ?
O7 Cu2 O10 88.67(9) . . ?
O8 Cu2 O2 83.64(7) . . ?
O8 Cu2 O5 86.16(8) . . ?
O8 Cu2 O7 165.58(7) . . ?
O8 Cu2 O10 91.08(9) . . ?
O16 Cu2 O2 178.12(7) . . ?
O16 Cu2 O5 95.11(7) . . ?
O16 Cu2 O7 96.30(7) . . ?
O16 Cu2 O8 98.11(7) . . ?
O16 Cu2 O10 93.57(8) . . ?
O3 Cu3 O9 83.75(7) . . ?
O3 Cu3 O14 85.06(7) . . ?
O9 Cu3 O14 168.05(7) . . ?
O11 Cu3 O3 82.64(7) . . ?
O11 Cu3 O9 94.72(8) . . ?
O11 Cu3 O12 167.44(7) . . ?
O11 Cu3 O14 87.96(8) . . ?
O12 Cu3 O3 85.03(7) . . ?
O12 Cu3 O9 86.25(7) . . ?
O12 Cu3 O14 88.64(8) . . ?
O16 Cu3 O3 177.63(7) . . ?
O16 Cu3 O9 94.55(7) . . ?
O16 Cu3 O11 95.89(7) . . ?
O16 Cu3 O12 96.51(7) . . ?
O16 Cu3 O14 96.76(7) . . ?
F4 C4 F6 107.5(6) . . ?
F4 C4 C3 109.7(5) . . ?
F5 C4 F4 107.9(5) . . ?
F5 C4 F6 108.3(6) . . ?
F5 C4 C3 113.9(5) . . ?
F6 C4 C3 109.3(8) . . ?
F4' C4' F6' 107.0(7) . . ?
F4' C4' C3 114.3(5) . . ?
F5' C4' F4' 106.8(5) . . ?
F5' C4' F6' 107.0(7) . . ?
F5' C4' C3 111.0(5) . . ?
F6' C4' C3 110.4(10) . . ?
F10 C8 C7 114.7(5) . . ?
F11 C8 F10 105.8(5) . . ?
F11 C8 C7 112.9(5) . . ?
F12 C8 F10 105.2(6) . . ?
F12 C8 F11 104.8(6) . . ?
F12 C8 C7 112.6(6) . . ?
F12' C8' F10' 109.9(11) . . ?
F12' C8' F11' 109.4(11) . . ?
F12' C8' C7 106.6(14) . . ?
F10' C8' F11' 108.8(11) . . ?
F10' C8' C7 115(2) . . ?
F11' C8' C7 107(2) . . ?
F10" C8" C7 103.6(8) . . ?
F11" C8" F10" 110.7(8) . . ?
F11" C8" F12" 111.6(8) . . ?
F11" C8" C7 111.6(9) . . ?
F12" C8" F10" 110.5(8) . . ?
F12" C8" C7 108.6(7) . . ?
F10Z C8Z C7 109.6(18) . . ?
F11Z C8Z F10Z 108.0(11) . . ?
F11Z C8Z F12Z 108.2(10) . . ?
F11Z C8Z C7 102.9(13) . . ?
F12Z C8Z F10Z 108.0(11) . . ?
F12Z C8Z C7 120(2) . . ?
Fe1 O1 H1A 110.0 . . ?
Fe1 O1 H1B 109.5 . . ?
Cu1 O1 H1A 110.0 . . ?
Cu1 O1 H1B 109.5 . . ?
H1A O1 H1B 110.0 . . ?
Fe2 O2 H2A 109.7 . . ?
Fe2 O2 H2B 109.6 . . ?
Cu2 O2 H2A 109.7 . . ?
Cu2 O2 H2B 109.6 . . ?
H2A O2 H2B 109.6 . . ?
Fe3 O3 H3A 108.0 . . ?
Fe3 O3 H3B 109.5 . . ?
Cu3 O3 H3A 108.0 . . ?
Cu3 O3 H3B 109.5 . . ?
H3A O3 H3B 109.8 . . ?
C1 O4 Fe1 130.78(17) . . ?
C1 O4 Cu1 130.78(17) . . ?
C1 O5 Fe2 127.97(19) . . ?
C1 O5 Cu2 127.97(19) . . ?
C3 O6 Fe1 130.36(17) . . ?
C3 O6 Cu1 130.36(17) . . ?
C3 O7 Fe2 128.98(16) . . ?
C3 O7 Cu2 128.98(16) . . ?
C5 O8 Fe2 129.88(17) . . ?
C5 O8 Cu2 129.88(17) . . ?
C5 O9 Fe3 129.07(19) . . ?
C5 O9 Cu3 129.07(19) . . ?
C7 O10 Fe2 129.5(2) . . ?
C7 O10 Cu2 129.5(2) . . ?
C7 O11 Fe3 129.84(18) . . ?
C7 O11 Cu3 129.84(18) . . ?
C9 O12 Fe3 126.65(15) . . ?
C9 O12 Cu3 126.65(15) . . ?
C9 O13 Fe1 132.64(16) . . ?
C9 O13 Cu1 132.64(16) . . ?
C11 O14 Fe3 125.70(18) . . ?
C11 O14 Cu3 125.70(18) . . ?
C11 O15 Fe1 129.15(16) . . ?
C11 O15 Cu1 129.15(16) . . ?
Fe1 O16 Fe2 121.28(8) . . ?
Fe1 O16 Fe3 119.01(8) . . ?
Fe2 O16 Fe3 119.71(8) . . ?
Cu1 O16 Cu2 121.28(8) . . ?
Cu1 O16 Cu3 119.01(8) . . ?
Cu2 O16 Cu3 119.71(8) . . ?
O4 C1 C2 115.0(2) . . ?
O5 C1 O4 129.8(3) . . ?
O5 C1 C2 115.3(2) . . ?
F1 C2 F2 106.8(2) . . ?
F1 C2 C1 113.0(2) . . ?
F2 C2 C1 110.0(2) . . ?
F3 C2 F1 107.9(3) . . ?
F3 C2 F2 107.8(3) . . ?
F3 C2 C1 111.1(2) . . ?
O6 C3 C4 118.1(3) . . ?
O6 C3 C4' 111.7(3) . . ?
O7 C3 C4 112.3(3) . . ?
O7 C3 C4' 118.6(3) . . ?
O7 C3 O6 129.6(2) . . ?
O8 C5 C6 115.0(2) . . ?
O9 C5 O8 129.4(3) . . ?
O9 C5 C6 115.6(2) . . ?
F7 C6 C5 111.9(2) . . ?
F8 C6 F7 107.5(3) . . ?
F8 C6 F9 109.5(3) . . ?
F8 C6 C5 110.2(2) . . ?
F9 C6 F7 105.8(3) . . ?
F9 C6 C5 111.8(3) . . ?
O10 C7 C8 122.0(3) . . ?
O10 C7 C8' 110.6(7) . . ?
O10 C7 C8" 111.4(4) . . ?
O10 C7 C8Z 113.5(8) . . ?
O11 C7 C8 109.4(3) . . ?
O11 C7 C8' 120.7(7) . . ?
O11 C7 C8" 119.4(4) . . ?
O11 C7 C8Z 117.3(8) . . ?
O11 C7 O10 128.6(3) . . ?
O12 C9 O13 129.2(2) . . ?
O12 C9 C10 116.5(2) . . ?
O13 C9 C10 114.3(2) . . ?
F13 C10 C9 112.04(19) . . ?
F14 C10 F13 108.1(2) . . ?
F14 C10 F15 108.1(2) . . ?
F14 C10 C9 110.20(19) . . ?
F15 C10 F13 107.00(19) . . ?
F15 C10 C9 111.23(19) . . ?
O14 C11 O15 128.7(2) . . ?
O14 C11 C12 115.5(2) . . ?
O15 C11 C12 115.8(2) . . ?
F16 C12 C11 110.0(3) . . ?
F17 C12 F16 107.9(3) . . ?
F17 C12 C11 110.3(2) . . ?
F18 C12 F16 106.7(2) . . ?
F18 C12 F17 108.7(3) . . ?
F18 C12 C11 113.0(2) . . ?
H20A O20 H20B 107.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O17 0.85 1.99 2.839(3) 176.6 . yes
O1 H1A O17' 0.85 1.86 2.646(7) 152.4 . yes
O1 H1B O20 0.86 1.97 2.679(2) 139.1 6_576 yes
O2 H2A O18 0.85 1.96 2.803(8) 171.4 . yes
O2 H2A O18' 0.85 1.92 2.751(4) 165.3 . yes
O2 H2B O20 0.84 1.93 2.753(3) 165.5 6_566 yes
O3 H3A O5 0.85 2.48 3.265(3) 154.5 6_565 yes
O3 H3B O19 0.85 1.90 2.739(2) 170.9 . yes
O3 H3B O19' 0.85 1.98 2.80(8) 161.0 2_655 yes
O3 H3B O19' 0.85 1.54 2.37(9) 164.3 . yes
O20 H20A F13 0.85 2.56 3.112(2) 123.5 2_655 yes
O20 H20B O14 0.85 2.02 2.794(3) 149.9 . yes

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 O4 C1 O5 -7.0(4) . . . . ?
Fe1 O4 C1 C2 173.09(16) . . . . ?
Fe1 O6 C3 C4 175.1(3) . . . . ?
Fe1 O6 C3 O7 -6.6(4) . . . . ?
Fe1 O13 C9 O12 -10.0(4) . . . . ?
Fe1 O13 C9 C10 170.77(16) . . . . ?
Fe1 O15 C11 O14 -4.7(4) . . . . ?
Fe1 O15 C11 C12 175.58(16) . . . . ?
Fe2 O5 C1 O4 3.2(4) . . . . ?
Fe2 O5 C1 C2 -176.90(16) . . . . ?
Fe2 O7 C3 C4 173.8(3) . . . . ?
Fe2 O7 C3 O6 -4.6(4) . . . . ?
Fe2 O8 C5 O9 -0.2(4) . . . . ?
Fe2 O8 C5 C6 176.99(18) . . . . ?
Fe2 O10 C7 C8 166.4(3) . . . . ?
Fe2 O10 C7 O11 -11.8(5) . . . . ?
Fe3 O9 C5 O8 -11.5(4) . . . . ?
Fe3 O9 C5 C6 171.30(18) . . . . ?
Fe3 O11 C7 C8 174.7(3) . . . . ?
Fe3 O11 C7 O10 -6.9(5) . . . . ?
Fe3 O12 C9 O13 -4.9(4) . . . . ?
Fe3 O12 C9 C10 174.37(15) . . . . ?
Fe3 O14 C11 O15 -23.7(4) . . . . ?
Fe3 O14 C11 C12 156.11(18) . . . . ?
Cu1 O4 C1 O5 -7.0(4) . . . . ?
Cu1 O4 C1 C2 173.09(16) . . . . ?
Cu1 O6 C3 O7 -6.6(4) . . . . ?
Cu1 O13 C9 O12 -10.0(4) . . . . ?
Cu1 O13 C9 C10 170.77(16) . . . . ?
Cu1 O15 C11 O14 -4.7(4) . . . . ?
Cu1 O15 C11 C12 175.58(16) . . . . ?
Cu2 O5 C1 O4 3.2(4) . . . . ?
Cu2 O5 C1 C2 -176.90(16) . . . . ?
Cu2 O7 C3 O6 -4.6(4) . . . . ?
Cu2 O8 C5 O9 -0.2(4) . . . . ?
Cu2 O8 C5 C6 176.99(18) . . . . ?
Cu2 O10 C7 O11 -11.8(5) . . . . ?
Cu3 O9 C5 O8 -11.5(4) . . . . ?
Cu3 O9 C5 C6 171.30(18) . . . . ?
Cu3 O11 C7 O10 -6.9(5) . . . . ?
Cu3 O12 C9 O13 -4.9(4) . . . . ?
Cu3 O12 C9 C10 174.37(15) . . . . ?
Cu3 O14 C11 O15 -23.7(4) . . . . ?
Cu3 O14 C11 C12 156.11(18) . . . . ?
F4 C4 C3 O6 -46.6(7) . . . . ?
F4 C4 C3 O7 134.9(5) . . . . ?
F5 C4 C3 O6 -167.6(6) . . . . ?
F5 C4 C3 O7 13.8(8) . . . . ?
F6 C4 C3 O6 71.1(8) . . . . ?
F6 C4 C3 O7 -107.5(7) . . . . ?
F4' C4' C3 O6 -21.8(9) . . . . ?
F4' C4' C3 O7 159.3(7) . . . . ?
F5' C4' C3 O6 -142.7(6) . . . . ?
F5' C4' C3 O7 38.4(8) . . . . ?
F6' C4' C3 O6 98.8(8) . . . . ?
F6' C4' C3 O7 -80.1(8) . . . . ?
F10 C8 C7 O10 -13.7(7) . . . . ?
F10 C8 C7 O11 164.8(5) . . . . ?
F11 C8 C7 O10 107.6(6) . . . . ?
F11 C8 C7 O11 -73.9(6) . . . . ?
F12 C8 C7 O10 -134.0(6) . . . . ?
F12 C8 C7 O11 44.5(6) . . . . ?
F12' C8' C7 O10 -174.4(12) . . . . ?
F12' C8' C7 O11 1.8(16) . . . . ?
F10' C8' C7 O10 -52.4(15) . . . . ?
F10' C8' C7 O11 123.8(12) . . . . ?
F11' C8' C7 O10 68.5(14) . . . . ?
F11' C8' C7 O11 -115.3(12) . . . . ?
F10" C8" C7 O10 -81.8(7) . . . . ?
F10" C8" C7 O11 106.6(7) . . . . ?
F11" C8" C7 O10 37.3(9) . . . . ?
F11" C8" C7 O11 -134.3(7) . . . . ?
F12" C8" C7 O10 160.7(7) . . . . ?
F12" C8" C7 O11 -10.9(10) . . . . ?
F10Z C8Z C7 O10 -28.8(14) . . . . ?
F10Z C8Z C7 O11 143.2(11) . . . . ?
F11Z C8Z C7 O10 86.0(12) . . . . ?
F11Z C8Z C7 O11 -102.0(13) . . . . ?
F12Z C8Z C7 O10 -154.2(13) . . . . ?
F12Z C8Z C7 O11 17.8(16) . . . . ?
O4 Fe1 O16 Fe2 -46.97(10) . . . . ?
O4 Fe1 O16 Fe3 133.43(9) . . . . ?
O4 Cu1 O16 Cu2 -46.97(10) . . . . ?
O4 Cu1 O16 Cu3 133.43(9) . . . . ?
O4 C1 C2 F1 -15.8(3) . . . . ?
O4 C1 C2 F2 103.4(3) . . . . ?
O4 C1 C2 F3 -137.2(3) . . . . ?
O5 C1 C2 F1 164.3(2) . . . . ?
O5 C1 C2 F2 -76.5(3) . . . . ?
O5 C1 C2 F3 42.9(3) . . . . ?
O6 Fe1 O16 Fe2 41.57(10) . . . . ?
O6 Fe1 O16 Fe3 -138.04(9) . . . . ?
O6 Cu1 O16 Cu2 41.57(10) . . . . ?
O6 Cu1 O16 Cu3 -138.04(9) . . . . ?
O8 C5 C6 F7 25.3(4) . . . . ?
O8 C5 C6 F8 -94.3(3) . . . . ?
O8 C5 C6 F9 143.7(3) . . . . ?
O9 C5 C6 F7 -157.1(3) . . . . ?
O9 C5 C6 F8 83.3(3) . . . . ?
O9 C5 C6 F9 -38.7(4) . . . . ?
O12 C9 C10 F13 0.6(3) . . . . ?
O12 C9 C10 F14 -119.8(2) . . . . ?
O12 C9 C10 F15 120.4(2) . . . . ?
O13 Fe1 O16 Fe2 -137.64(10) . . . . ?
O13 Fe1 O16 Fe3 42.75(10) . . . . ?
O13 Cu1 O16 Cu2 -137.64(10) . . . . ?
O13 Cu1 O16 Cu3 42.75(10) . . . . ?
O13 C9 C10 F13 -180.0(2) . . . . ?
O13 C9 C10 F14 59.6(3) . . . . ?
O13 C9 C10 F15 -60.3(3) . . . . ?
O14 C11 C12 F16 -52.6(3) . . . . ?
O14 C11 C12 F17 66.4(3) . . . . ?
O14 C11 C12 F18 -171.8(3) . . . . ?
O15 Fe1 O16 Fe2 126.54(10) . . . . ?
O15 Fe1 O16 Fe3 -53.06(10) . . . . ?
O15 Cu1 O16 Cu2 126.54(10) . . . . ?
O15 Cu1 O16 Cu3 -53.06(10) . . . . ?
O15 C11 C12 F16 127.2(3) . . . . ?
O15 C11 C12 F17 -113.8(3) . . . . ?
O15 C11 C12 F18 8.0(4) . . . . ?

_olex2_submission_original_sample_id knoks12mo
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.817
####################################################################### 
# 
# 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_knoks11
_database_code_depnum_ccdc_archive 'CCDC 1996870'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2020-04-14 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

_vrf_PLAT041_knoks11             
;
PROBLEM: _C Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT043_knoks11             
;
PROBLEM: _C Calculated and Reported Mol. Weight Differ by .. 5.03 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT068_knoks11             
;
PROBLEM: _C Reported F000 Differs from Calcd (or Missing).
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_FORMU01_knoks11             
;
PROBLEM: _G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_CELLZ01_knoks11             
;
PROBLEM: _G Difference between formula and atom_site contents detected.
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT007_knoks11             
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 8 
RESPONSE: Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.
;

_vrf_PLAT301_knoks11             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 22% 
RESPONSE: Each metal site was modeled as a disorder of Fe and Co:
Fe1:Co1, 0.914(3):0.086(3), Fe2:Co2, 0.489(3):0.511(3), Fe3:Co3,
0.597(3):0.403(3). The total metal ratio was constrained to 2Fe:1Co.
Two CF3 groups were modeled as disordered over two positions each:
C4-F4-F5-F6, 0.59(4):0.41(4) and C8-F10-F11-F12, 0.659(8):0.341(8).
;

_vrf_PLAT302_knoks11             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-4, 6-8  ) .. 100% 
RESPONSE: Cocrystallized water solvent molecules O17, O18, and O19
were modeled as disordered over two positions each (0.677(6):0.323(6),
0.61(1):0.39(1), and 0.71(1):0.29(1), respectively).
;

_vrf_PLAT311_knoks11             
;
PROBLEM: _G Isolated Disordered Oxygen Atom (No H's ?) .. O17 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O17' 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O18 
         _G Isolated Disordered Oxygen Atom (No H's ?) .. O19 
RESPONSE: Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were included in
the molecular formula.
;

_vrf_PLAT860_knoks11             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 153 
RESPONSE: Positional and anisotropic displacement parameters,
respectively, for the two metal types of each site disorder were
constrained to be equivalent. Analogous bond lengths and angles
between the two positions of the disordered CF3 groups were
restrained to be similar. Anisotropic displacement parameters
for proximal atoms were restrained to be similar and/or
constrained to be equivalent.
;

_audit_creation_date             2020-03-31
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Co1 F18 Fe2 O16, 2.5(O), H2 O'
_chemical_formula_sum            'C12 H13 Co F18 Fe2 O19.50'
_chemical_formula_weight         981.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   33.6911(3)
_cell_length_b                   10.7211(2)
_cell_length_c                   16.4167(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.6060(10)
_cell_angle_gamma                90
_cell_volume                     5923.67(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    18236
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3960
_cell_measurement_theta_min      2.6450
_shelx_estimated_absorpt_T_max   0.387
_shelx_estimated_absorpt_T_min   0.102
_exptl_absorpt_coefficient_mu    13.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27273
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.885
_diffrn_reflns_theta_min         2.626
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00 -26.00   0.50    0.91    --  -49.87  98.00-100.00  104
  2  ω    -10.00  21.00   0.50    0.91    --  -49.87  98.00-100.00   62
  3  ω     24.00  76.00   0.50    0.91    --   49.87 -98.00 152.00  104
  4  ω   -121.00 -78.00   0.50    0.91    --  -49.87-125.00 -90.00   86
  5  ω   -120.00 -78.00   0.50    0.91    --  -49.87-125.00 -60.00   84
  6  ω     -5.00  21.00   0.50    0.91    --  -49.87  19.00 -30.00   52
  7  ω     -5.00  24.00   0.50    0.91    --  -49.87  19.00   0.00   58
  8  ω    -20.00   5.00   0.50    0.91    --   49.87 -19.00-120.00   50
  9  ω    -22.00   3.00   0.50    0.91    --   49.87 -19.00  90.00   50
 10  ω    -70.00 -45.00   0.50    3.63    --  -84.25  98.00-100.00   50
 11  ω    -44.00 -13.00   0.50    3.63    --  -84.25  45.00 120.00   62
 12  ω   -141.00-115.00   0.50    3.63    --  -84.25 -98.00 152.00   52
 13  ω     53.00 106.00   0.50    3.63    --  105.75 -98.00 152.00  106
 14  ω    106.00 174.00   0.50    3.63    --  105.75  98.00-100.00  136
 15  ω     38.00  64.00   0.50    3.63    --  105.75-125.00 -30.00   52
 16  ω     43.00  73.00   0.50    3.63    --  105.75 -61.00-120.00   60
 17  ω     35.00  79.00   0.50    3.63    --  105.75 -61.00-180.00   88
 18  ω     95.00 139.00   0.50    3.63    --  105.75 125.00  90.00   88
 19  ω     40.00  79.00   0.50    3.63    --  105.75 -61.00  30.00   78
 20  ω     72.00 125.00   0.50    3.63    --  105.75 -77.00-180.00  106
 21  ω    148.00 178.00   0.50    3.63    --  105.75  45.00-120.00   60
 22  ω     34.00  59.00   0.50    3.63    --  105.75 -77.00-180.00   50
 23  ω     97.00 138.00   0.50    3.63    --  105.75  45.00-120.00   82
 24  ω     37.00  78.00   0.50    3.63    --  105.75 -61.00   0.00   82
 25  ω    106.00 171.00   0.50    3.63    --  105.75  15.00-120.00  130
 26  ω     96.00 158.00   0.50    3.63    --  105.75 125.00-180.00  124
 27  ω     34.00  74.00   0.50    3.63    --  105.75 -94.00-180.00   80
 28  ω     71.00 127.00   0.50    3.63    --  105.75 -77.00 150.00  112
 29  ω     34.00  72.00   0.50    3.63    --  105.75 -61.00  60.00   76
 30  ω     45.00 101.00   0.50    3.63    --  105.75 -94.00 -30.00  112
 31  ω     50.00  76.00   0.50    3.63    --  105.75 -61.00 150.00   52
 32  ω     55.00  80.00   0.50    3.63    --  105.75 -94.00-120.00   50
 33  ω     50.00  75.00   0.50    3.63    --  105.75 -61.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002271000
_diffrn_orient_matrix_UB_12      -0.1217967000
_diffrn_orient_matrix_UB_13      -0.0497439000
_diffrn_orient_matrix_UB_21      0.0282888000
_diffrn_orient_matrix_UB_22      -0.0596089000
_diffrn_orient_matrix_UB_23      0.0653829000
_diffrn_orient_matrix_UB_31      -0.0359719000
_diffrn_orient_matrix_UB_32      -0.0475975000
_diffrn_orient_matrix_UB_33      0.0455715000
_diffrn_oxdiff_digest_frames     
;
0128e9885f50e78007bd94469a29227ec400034ebf6
;
_diffrn_oxdiff_digest_hkl        
;
0161b7b4ab8072f2e2e2c4e0621c07a5078296
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5847
_reflns_number_total             6194
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0545
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1159P)²+7.5669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1516
_refine_special_details          
;
Hydrogen atoms on disordered cocrystallized water solvent
molecules were not included in the atom list, but were
included in the molecular formula.

Due to disorder in most of the hydrogen-bonding acceptors,
positions of the donor hydrogen atoms were based on the
difference Fourier map, but given idealized riding models.

Each metal site was modeled as a disorder of Fe and Co:
Fe1:Co1, 0.914(3):0.086(3), Fe2:Co2, 0.489(3):0.511(3), Fe3:Co3,
0.597(3):0.403(3). The total metal ratio was constrained to 2Fe:1Co.
Two CF3 groups were modeled as disordered over two positions each:
C4-F4-F5-F6, 0.59(4):0.41(4) and C8-F10-F11-F12, 0.659(8):0.341(8).

Cocrystallized water solvent molecules O17, O18, and O19 were
modeled as disordered over two positions each (0.677(6):0.323(6),
0.61(1):0.39(1), and 0.71(1):0.29(1), respectively).

Positional and anisotropic displacement parameters, respectively,
for the two metal types of each site disorder were constrained
to be equivalent. Analogous bond lengths and angles between
the two positions of the disordered CF3 groups were restrained
to be similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and/or constrained to be
equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Fe1, Co1}
{Fe2, Co2}
{Fe3, Co3}
3. Restrained distances
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
 C4-F4 \\sim C4-F5 \\sim C4-F6 \\sim C4'-F4' \\sim C4'-F5' \\sim C4'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 C7-C8 \\sim C7-C8'
 with sigma of 0.01
 C8-F10 \\sim C8-F11 \\sim C8-F12 \\sim C8'-F11' \\sim C8'-F12' \\sim C8'-F10'
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F11'-F12' \\sim F12'-F10' \\sim
F10'-F11'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C4': within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C8': within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
F11 \\sim F12': within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O17) = Uanis(O17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
Uanis(Fe1) = Uanis(Co1)
Uanis(Fe2) = Uanis(Co2)
Uanis(Fe3) = Uanis(Co3)
5. Rigid body (RIGU) restrains
 F10, F11, F12, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10', F11', F12', C8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4', F5', F6', C4'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Fe1)+Sof(Co1)]+1*[Sof(Fe2)+Sof(Co2)]+1*[Sof(Fe3)+Sof(Co3)]=2 with esd
 of 0.0001
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C4')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=FVAR(1)
 Sof(F10')=Sof(F11')=Sof(F12')=Sof(C8')=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C8)=FVAR(2)
 Sof(O17')=1-FVAR(3)
 Sof(O17)=FVAR(3)
 Sof(O18')=1-FVAR(4)
 Sof(O18)=FVAR(4)
 Sof(O19')=0.5*(1-FVAR(6))
 Sof(O19)=0.5*FVAR(6)
 Sof(Co1)=1-FVAR(6)
 Sof(Fe1)=FVAR(6)
 Sof(Co2)=1-FVAR(7)
 Sof(Fe2)=FVAR(7)
 Sof(Co3)=1-FVAR(8)
 Sof(Fe3)=FVAR(8)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.62089(2) 0.86298(4) 0.48744(3) 0.01441(14) Uani 0.914(3) 1 d . . . A 1
Fe2 Fe 0.63411(2) 0.56472(4) 0.53320(3) 0.01712(15) Uani 0.489(3) 1 d . . . A 1
Fe3 Fe 0.59777(2) 0.64839(4) 0.34978(3) 0.01692(15) Uani 0.597(3) 1 d . . . A 1
Co1 Co 0.62089(2) 0.86298(4) 0.48744(3) 0.01441(14) Uani 0.086(3) 1 d . . . A 5
Co2 Co 0.63411(2) 0.56472(4) 0.53320(3) 0.01712(15) Uani 0.511(3) 1 d . . . A 5
Co3 Co 0.59777(2) 0.64839(4) 0.34978(3) 0.01692(15) Uani 0.403(3) 1 d . . . A 5
F1 F 0.57442(8) 0.8965(2) 0.74365(15) 0.0440(6) Uani 1 1 d . . . . .
F2 F 0.53921(7) 0.7355(3) 0.72383(17) 0.0607(9) Uani 1 1 d . . . . .
F3 F 0.59592(9) 0.7202(3) 0.78603(14) 0.0566(8) Uani 1 1 d . . . . .
F7 F 0.51920(7) 0.3318(2) 0.53906(14) 0.0389(6) Uani 1 1 d . . . . .
F8 F 0.53651(8) 0.2480(2) 0.42864(15) 0.0435(6) Uani 1 1 d . . . . .
F9 F 0.49356(7) 0.3958(3) 0.4264(2) 0.0570(8) Uani 1 1 d . . . . .
F13 F 0.47835(5) 0.85506(19) 0.32064(12) 0.0252(4) Uani 1 1 d . . . . .
F14 F 0.50693(6) 1.0323(2) 0.34170(14) 0.0334(5) Uani 1 1 d . . . . .
F15 F 0.48346(5) 0.9304(2) 0.44128(12) 0.0280(4) Uani 1 1 d . . . . .
F16 F 0.69316(9) 0.8526(3) 0.21032(18) 0.0563(8) Uani 1 1 d . . . . .
F17 F 0.65475(8) 1.0109(4) 0.2079(2) 0.0701(11) Uani 1 1 d . . . . .
F18 F 0.70452(7) 1.0018(3) 0.29209(15) 0.0490(7) Uani 1 1 d . . . . .
F4 F 0.7578(3) 0.858(2) 0.5642(7) 0.028(3) Uani 0.41(4) 1 d D U . B 1
F5 F 0.7600(3) 0.6761(11) 0.6171(15) 0.031(3) Uani 0.41(4) 1 d D U . B 1
F6 F 0.7364(8) 0.830(2) 0.6834(9) 0.030(3) Uani 0.41(4) 1 d D U . B 1
F10 F 0.72564(16) 0.3555(6) 0.3757(3) 0.0516(15) Uani 0.659(8) 1 d D U . C 1
F11 F 0.67808(15) 0.2883(5) 0.2983(5) 0.073(2) Uani 0.659(8) 1 d D U . C 1
F12 F 0.71024(11) 0.4500(4) 0.2660(2) 0.0402(12) Uani 0.659(8) 1 d D U . C 1
F4' F 0.7509(3) 0.9037(12) 0.5833(8) 0.033(2) Uani 0.59(4) 1 d D U . B 2
F5' F 0.76466(16) 0.7097(13) 0.5875(7) 0.029(2) Uani 0.59(4) 1 d D U . B 2
F6' F 0.7369(6) 0.7966(14) 0.6879(5) 0.030(2) Uani 0.59(4) 1 d D U . B 2
F10' F 0.6843(4) 0.3683(12) 0.2522(4) 0.079(5) Uani 0.341(8) 1 d D U . C 2
F11' F 0.7283(3) 0.4004(11) 0.3478(9) 0.063(3) Uani 0.341(8) 1 d D U . C 2
F12' F 0.6842(3) 0.2582(6) 0.3564(7) 0.053(2) Uani 0.341(8) 1 d D U . C 2
O1 O 0.62695(7) 1.0503(2) 0.50908(15) 0.0235(5) Uani 1 1 d . . . . .
H1A H 0.651249 1.070629 0.506609 0.035 Uiso 1 1 d R . . A .
H1B H 0.618999 1.067069 0.556239 0.035 Uiso 1 1 d R . . . .
O2 O 0.65239(7) 0.4275(2) 0.61554(17) 0.0283(5) Uani 1 1 d . . . . .
H2A H 0.675999 0.405493 0.606197 0.042 Uiso 1 1 d R . . A .
H2B H 0.637019 0.364894 0.610297 0.042 Uiso 1 1 d R . . . .
O3 O 0.57729(7) 0.5885(2) 0.23174(14) 0.0254(5) Uani 1 1 d . . . . .
H3A H 0.591206 0.527038 0.217031 0.038 Uiso 1 1 d R . . A .
H3B H 0.553096 0.566357 0.233091 0.038 Uiso 1 1 d R . . . .
O4 O 0.59631(6) 0.8443(2) 0.59702(13) 0.0192(4) Uani 1 1 d . . . . .
O5 O 0.60571(7) 0.6422(2) 0.63221(14) 0.0217(5) Uani 1 1 d . . . . .
O6 O 0.67674(6) 0.8507(2) 0.54633(14) 0.0198(4) Uani 1 1 d . . . . .
O7 O 0.68661(6) 0.6464(2) 0.57101(15) 0.0227(5) Uani 1 1 d . . . . .
O8 O 0.58505(6) 0.4525(2) 0.51478(13) 0.0208(4) Uani 1 1 d . . . . .
O9 O 0.56147(6) 0.5068(2) 0.38944(13) 0.0201(4) Uani 1 1 d . . . . .
O10 O 0.66487(7) 0.4620(2) 0.44790(15) 0.0277(5) Uani 1 1 d . . . . .
O11 O 0.64333(7) 0.5335(2) 0.32495(15) 0.0263(5) Uani 1 1 d . . . . .
O12 O 0.54819(6) 0.7574(2) 0.34754(12) 0.0188(4) Uani 1 1 d . . . . .
O13 O 0.56623(6) 0.9091(2) 0.43674(14) 0.0198(4) Uani 1 1 d . . . . .
O14 O 0.62735(7) 0.7879(2) 0.28765(14) 0.0242(5) Uani 1 1 d . . . . .
O15 O 0.65125(6) 0.9142(2) 0.38754(13) 0.0194(4) Uani 1 1 d . . . . .
O16 O 0.61781(5) 0.69439(18) 0.45770(11) 0.0132(4) Uani 1 1 d . . . . .
C1 C 0.59468(8) 0.7518(3) 0.64337(18) 0.0172(6) Uani 1 1 d . . . . .
C2 C 0.57595(9) 0.7769(3) 0.72588(19) 0.0225(6) Uani 1 1 d . . . . .
C3 C 0.69602(8) 0.7582(3) 0.57063(16) 0.0152(5) Uani 1 1 d D . . . .
C5 C 0.56128(8) 0.4486(3) 0.45482(17) 0.0153(5) Uani 1 1 d . . . . .
C6 C 0.52700(10) 0.3540(3) 0.4613(2) 0.0246(7) Uani 1 1 d . . . . .
C7 C 0.66449(9) 0.4689(3) 0.3727(2) 0.0228(6) Uani 1 1 d D . . . .
C9 C 0.54300(8) 0.8549(3) 0.38708(18) 0.0155(5) Uani 1 1 d . . . . .
C10 C 0.50194(9) 0.9194(3) 0.37292(19) 0.0186(6) Uani 1 1 d . . . . .
C11 C 0.64887(8) 0.8728(3) 0.3171(2) 0.0175(6) Uani 1 1 d . . . . .
C12 C 0.67589(10) 0.9372(3) 0.2557(2) 0.0241(7) Uani 1 1 d . . . . .
C4 C 0.73825(19) 0.7788(9) 0.6099(6) 0.015(2) Uani 0.41(4) 1 d D U . B 1
C8 C 0.69546(16) 0.3903(5) 0.3277(3) 0.0307(12) Uani 0.659(8) 1 d D U . C 1
C4' C 0.73783(16) 0.7936(8) 0.6071(5) 0.0196(17) Uani 0.59(4) 1 d D U . B 2
C8' C 0.6910(3) 0.3719(8) 0.3314(5) 0.032(2) Uani 0.341(8) 1 d D U . C 2
O17 O 0.70823(13) 1.1169(4) 0.5053(3) 0.0438(10) Uani 0.677(6) 1 d . . . D 1
O17' O 0.6918(3) 1.1852(9) 0.5058(7) 0.0438(10) Uani 0.323(6) 1 d . . . D 2
O18 O 0.7299(3) 0.3563(11) 0.5629(9) 0.0569(17) Uani 0.389(9) 1 d . . . E 1
O18' O 0.72844(18) 0.3531(6) 0.6096(5) 0.0569(17) Uani 0.611(9) 1 d . . . E 2
O19 O 0.500000 0.5075(15) 0.250000 0.037(2) Uani 0.295(10) 2 d S T P F 1
O19' O 0.5035(3) 0.5780(8) 0.2291(5) 0.037(2) Uani 0.353(5) 1 d . . . F 2
O20 O 0.60449(7) 0.7801(2) 0.11801(14) 0.0247(5) Uani 1 1 d . . . . .
H20A H 0.580531 0.758948 0.106977 0.037 Uiso 1 1 d R . . . .
H20B H 0.605761 0.812038 0.165437 0.037 Uiso 1 1 d R . . . .


_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 2.048(2) . ?
Fe1 O4 2.024(2) . ?
Fe1 O6 2.080(2) . ?
Fe1 O13 2.047(2) . ?
Fe1 O15 2.047(2) . ?
Fe1 O16 1.874(2) . ?
Fe2 O2 2.072(3) . ?
Fe2 O5 2.095(2) . ?
Fe2 O7 2.044(2) . ?
Fe2 O8 2.056(2) . ?
Fe2 O10 2.093(2) . ?
Fe2 O16 1.926(2) . ?
Fe3 O3 2.127(2) . ?
Fe3 O9 2.073(2) . ?
Fe3 O11 2.024(2) . ?
Fe3 O12 2.038(2) . ?
Fe3 O14 2.089(2) . ?
Fe3 O16 1.9311(19) . ?
Co1 O1 2.048(2) . ?
Co1 O4 2.024(2) . ?
Co1 O6 2.080(2) . ?
Co1 O13 2.047(2) . ?
Co1 O15 2.047(2) . ?
Co1 O16 1.874(2) . ?
Co2 O2 2.072(3) . ?
Co2 O5 2.095(2) . ?
Co2 O7 2.044(2) . ?
Co2 O8 2.056(2) . ?
Co2 O10 2.093(2) . ?
Co2 O16 1.926(2) . ?
Co3 O3 2.127(2) . ?
Co3 O9 2.073(2) . ?
Co3 O11 2.024(2) . ?
Co3 O12 2.038(2) . ?
Co3 O14 2.089(2) . ?
Co3 O16 1.9311(19) . ?
F1 C2 1.317(4) . ?
F2 C2 1.314(4) . ?
F3 C2 1.318(4) . ?
F7 C6 1.336(4) . ?
F8 C6 1.303(4) . ?
F9 C6 1.319(4) . ?
F13 C10 1.335(3) . ?
F14 C10 1.328(4) . ?
F15 C10 1.313(4) . ?
F16 C12 1.324(4) . ?
F17 C12 1.302(4) . ?
F18 C12 1.310(4) . ?
F4 C4 1.326(7) . ?
F5 C4 1.325(7) . ?
F6 C4 1.328(7) . ?
F10 C8 1.312(6) . ?
F11 C8 1.321(5) . ?
F12 C8 1.316(6) . ?
F4' C4' 1.324(6) . ?
F5' C4' 1.325(6) . ?
F6' C4' 1.329(6) . ?
F10' C8' 1.311(7) . ?
F11' C8' 1.308(7) . ?
F12' C8' 1.309(7) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8499 . ?
O2 H2A 0.8503 . ?
O2 H2B 0.8497 . ?
O3 H3A 0.8501 . ?
O3 H3B 0.8501 . ?
O4 C1 1.253(4) . ?
O5 C1 1.249(4) . ?
O6 C3 1.242(4) . ?
O7 C3 1.240(4) . ?
O8 C5 1.241(4) . ?
O9 C5 1.242(4) . ?
O10 C7 1.237(4) . ?
O11 C7 1.245(4) . ?
O12 C9 1.247(4) . ?
O13 C9 1.248(4) . ?
O14 C11 1.247(4) . ?
O15 C11 1.237(4) . ?
C1 C2 1.544(4) . ?
C3 C4 1.551(7) . ?
C3 C4' 1.552(6) . ?
C5 C6 1.544(4) . ?
C7 C8 1.553(5) . ?
C7 C8' 1.546(8) . ?
C9 C10 1.555(4) . ?
C11 C12 1.551(4) . ?
O19' O19' 0.736(16) 2_655 ?
O20 H20A 0.8500 . ?
O20 H20B 0.8499 . ?

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 O6 84.27(9) . . ?
O4 Fe1 O1 89.10(9) . . ?
O4 Fe1 O6 88.77(9) . . ?
O4 Fe1 O13 89.34(9) . . ?
O4 Fe1 O15 167.97(9) . . ?
O13 Fe1 O1 85.08(9) . . ?
O13 Fe1 O6 169.22(9) . . ?
O13 Fe1 O15 94.73(9) . . ?
O15 Fe1 O1 80.01(9) . . ?
O15 Fe1 O6 85.11(9) . . ?
O16 Fe1 O1 174.23(9) . . ?
O16 Fe1 O4 96.68(9) . . ?
O16 Fe1 O6 95.65(8) . . ?
O16 Fe1 O13 95.11(9) . . ?
O16 Fe1 O15 94.23(9) . . ?
O2 Fe2 O5 84.72(10) . . ?
O2 Fe2 O10 85.49(10) . . ?
O7 Fe2 O2 83.02(9) . . ?
O7 Fe2 O5 90.81(10) . . ?
O7 Fe2 O8 166.89(9) . . ?
O7 Fe2 O10 88.89(10) . . ?
O8 Fe2 O2 83.88(9) . . ?
O8 Fe2 O5 87.34(9) . . ?
O8 Fe2 O10 90.73(10) . . ?
O10 Fe2 O5 170.17(10) . . ?
O16 Fe2 O2 178.93(9) . . ?
O16 Fe2 O5 94.94(8) . . ?
O16 Fe2 O7 95.97(9) . . ?
O16 Fe2 O8 97.12(8) . . ?
O16 Fe2 O10 94.86(9) . . ?
O9 Fe3 O3 83.88(9) . . ?
O9 Fe3 O14 168.29(9) . . ?
O11 Fe3 O3 81.39(10) . . ?
O11 Fe3 O9 94.66(10) . . ?
O11 Fe3 O12 166.91(9) . . ?
O11 Fe3 O14 87.40(10) . . ?
O12 Fe3 O3 85.69(9) . . ?
O12 Fe3 O9 86.03(9) . . ?
O12 Fe3 O14 89.39(9) . . ?
O14 Fe3 O3 85.04(9) . . ?
O16 Fe3 O3 176.96(9) . . ?
O16 Fe3 O9 94.90(8) . . ?
O16 Fe3 O11 95.95(9) . . ?
O16 Fe3 O12 97.02(8) . . ?
O16 Fe3 O14 96.35(9) . . ?
O1 Co1 O6 84.27(9) . . ?
O4 Co1 O1 89.10(9) . . ?
O4 Co1 O6 88.77(9) . . ?
O4 Co1 O13 89.34(9) . . ?
O4 Co1 O15 167.97(9) . . ?
O13 Co1 O1 85.08(9) . . ?
O13 Co1 O6 169.22(9) . . ?
O13 Co1 O15 94.73(9) . . ?
O15 Co1 O1 80.01(9) . . ?
O15 Co1 O6 85.11(9) . . ?
O16 Co1 O1 174.23(9) . . ?
O16 Co1 O4 96.68(9) . . ?
O16 Co1 O6 95.65(8) . . ?
O16 Co1 O13 95.11(9) . . ?
O16 Co1 O15 94.23(9) . . ?
O2 Co2 O5 84.72(10) . . ?
O2 Co2 O10 85.49(10) . . ?
O7 Co2 O2 83.02(9) . . ?
O7 Co2 O5 90.81(10) . . ?
O7 Co2 O8 166.89(9) . . ?
O7 Co2 O10 88.89(10) . . ?
O8 Co2 O2 83.88(9) . . ?
O8 Co2 O5 87.34(9) . . ?
O8 Co2 O10 90.73(10) . . ?
O10 Co2 O5 170.17(10) . . ?
O16 Co2 O2 178.93(9) . . ?
O16 Co2 O5 94.94(8) . . ?
O16 Co2 O7 95.97(9) . . ?
O16 Co2 O8 97.12(8) . . ?
O16 Co2 O10 94.86(9) . . ?
O9 Co3 O3 83.88(9) . . ?
O9 Co3 O14 168.29(9) . . ?
O11 Co3 O3 81.39(10) . . ?
O11 Co3 O9 94.66(10) . . ?
O11 Co3 O12 166.91(9) . . ?
O11 Co3 O14 87.40(10) . . ?
O12 Co3 O3 85.69(9) . . ?
O12 Co3 O9 86.03(9) . . ?
O12 Co3 O14 89.39(9) . . ?
O14 Co3 O3 85.04(9) . . ?
O16 Co3 O3 176.96(9) . . ?
O16 Co3 O9 94.90(8) . . ?
O16 Co3 O11 95.95(9) . . ?
O16 Co3 O12 97.02(8) . . ?
O16 Co3 O14 96.35(9) . . ?
Fe1 O1 H1A 109.4 . . ?
Fe1 O1 H1B 109.4 . . ?
Co1 O1 H1A 109.4 . . ?
Co1 O1 H1B 109.4 . . ?
H1A O1 H1B 109.5 . . ?
Fe2 O2 H2A 109.4 . . ?
Fe2 O2 H2B 109.5 . . ?
Co2 O2 H2A 109.4 . . ?
Co2 O2 H2B 109.5 . . ?
H2A O2 H2B 109.5 . . ?
Fe3 O3 H3A 109.4 . . ?
Fe3 O3 H3B 109.4 . . ?
Co3 O3 H3A 109.4 . . ?
Co3 O3 H3B 109.4 . . ?
H3A O3 H3B 109.5 . . ?
C1 O4 Fe1 130.5(2) . . ?
C1 O4 Co1 130.5(2) . . ?
C1 O5 Fe2 129.5(2) . . ?
C1 O5 Co2 129.5(2) . . ?
C3 O6 Fe1 130.43(19) . . ?
C3 O6 Co1 130.43(19) . . ?
C3 O7 Fe2 129.1(2) . . ?
C3 O7 Co2 129.1(2) . . ?
C5 O8 Fe2 128.4(2) . . ?
C5 O8 Co2 128.4(2) . . ?
C5 O9 Fe3 131.73(19) . . ?
C5 O9 Co3 131.73(19) . . ?
C7 O10 Fe2 130.8(2) . . ?
C7 O10 Co2 130.8(2) . . ?
C7 O11 Fe3 129.0(2) . . ?
C7 O11 Co3 129.0(2) . . ?
C9 O12 Fe3 127.3(2) . . ?
C9 O12 Co3 127.3(2) . . ?
C9 O13 Fe1 132.8(2) . . ?
C9 O13 Co1 132.8(2) . . ?
C11 O14 Fe3 127.9(2) . . ?
C11 O14 Co3 127.9(2) . . ?
C11 O15 Fe1 129.7(2) . . ?
C11 O15 Co1 129.7(2) . . ?
Fe1 O16 Fe2 121.19(10) . . ?
Fe1 O16 Fe3 119.88(10) . . ?
Fe2 O16 Fe3 118.93(10) . . ?
Co1 O16 Co2 121.19(10) . . ?
Co1 O16 Co3 119.88(10) . . ?
Co2 O16 Co3 118.93(10) . . ?
O4 C1 C2 115.2(3) . . ?
O5 C1 O4 129.4(3) . . ?
O5 C1 C2 115.4(3) . . ?
F1 C2 F3 107.9(3) . . ?
F1 C2 C1 112.7(3) . . ?
F2 C2 F1 106.7(3) . . ?
F2 C2 F3 108.2(3) . . ?
F2 C2 C1 109.9(3) . . ?
F3 C2 C1 111.2(2) . . ?
O6 C3 C4 118.4(4) . . ?
O6 C3 C4' 112.4(4) . . ?
O7 C3 O6 130.1(3) . . ?
O7 C3 C4 111.5(4) . . ?
O7 C3 C4' 117.5(4) . . ?
O8 C5 O9 129.8(3) . . ?
O8 C5 C6 115.1(3) . . ?
O9 C5 C6 115.0(3) . . ?
F7 C6 C5 111.3(3) . . ?
F8 C6 F7 107.5(3) . . ?
F8 C6 F9 109.8(3) . . ?
F8 C6 C5 110.2(3) . . ?
F9 C6 F7 105.9(3) . . ?
F9 C6 C5 112.0(3) . . ?
O10 C7 O11 129.8(3) . . ?
O10 C7 C8 117.7(3) . . ?
O10 C7 C8' 114.6(4) . . ?
O11 C7 C8 112.4(3) . . ?
O11 C7 C8' 115.1(4) . . ?
O12 C9 O13 129.2(3) . . ?
O12 C9 C10 116.1(3) . . ?
O13 C9 C10 114.7(3) . . ?
F13 C10 C9 111.4(2) . . ?
F14 C10 F13 107.8(3) . . ?
F14 C10 C9 109.6(2) . . ?
F15 C10 F13 107.7(2) . . ?
F15 C10 F14 108.7(3) . . ?
F15 C10 C9 111.4(2) . . ?
O14 C11 C12 114.9(3) . . ?
O15 C11 O14 129.5(3) . . ?
O15 C11 C12 115.7(3) . . ?
F16 C12 C11 110.3(3) . . ?
F17 C12 F16 108.6(3) . . ?
F17 C12 F18 109.0(3) . . ?
F17 C12 C11 109.9(3) . . ?
F18 C12 F16 106.6(3) . . ?
F18 C12 C11 112.4(3) . . ?
F4 C4 F6 107.2(8) . . ?
F4 C4 C3 109.0(7) . . ?
F5 C4 F4 107.1(7) . . ?
F5 C4 F6 108.0(9) . . ?
F5 C4 C3 114.3(7) . . ?
F6 C4 C3 110.9(14) . . ?
F10 C8 F11 107.6(6) . . ?
F10 C8 F12 106.9(5) . . ?
F10 C8 C7 112.8(5) . . ?
F11 C8 C7 109.0(4) . . ?
F12 C8 F11 107.4(5) . . ?
F12 C8 C7 112.8(4) . . ?
F4' C4' F5' 107.1(6) . . ?
F4' C4' F6' 107.1(6) . . ?
F4' C4' C3 114.3(5) . . ?
F5' C4' F6' 107.8(7) . . ?
F5' C4' C3 111.0(5) . . ?
F6' C4' C3 109.2(10) . . ?
F10' C8' C7 112.2(7) . . ?
F11' C8' F10' 109.4(9) . . ?
F11' C8' F12' 109.5(8) . . ?
F11' C8' C7 108.8(8) . . ?
F12' C8' F10' 104.9(8) . . ?
F12' C8' C7 112.1(7) . . ?
H20A O20 H20B 108.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O17 0.85 1.98 2.833(5) 177.9 . yes
O1 H1A O17' 0.85 1.84 2.623(9) 152.8 . yes
O1 H1B O20 0.85 2.00 2.683(3) 136.9 6_576 yes
O2 H2A O18 0.85 2.05 2.891(11) 170.1 . yes
O2 H2A O18' 0.85 1.85 2.689(7) 167.8 . yes
O2 H2B O20 0.85 1.91 2.751(3) 170.2 6_566 yes
O3 H3A O5 0.85 2.35 3.138(3) 153.9 6_565 yes
O3 H3B O19 0.85 1.93 2.774(6) 172.6 . yes
O3 H3B O19' 0.85 2.04 2.829(9) 154.6 2_655 yes
O3 H3B O19' 0.85 1.67 2.485(10) 159.2 . yes
O20 H20A F13 0.85 2.57 3.116(3) 122.6 2_655 yes
O20 H20B O14 0.85 2.12 2.857(3) 145.0 . yes

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 O4 C1 O5 -5.1(5) . . . . ?
Fe1 O4 C1 C2 175.53(19) . . . . ?
Fe1 O6 C3 O7 -4.6(5) . . . . ?
Fe1 O6 C3 C4 177.5(5) . . . . ?
Fe1 O13 C9 O12 -6.8(5) . . . . ?
Fe1 O13 C9 C10 173.49(19) . . . . ?
Fe1 O15 C11 O14 -0.3(5) . . . . ?
Fe1 O15 C11 C12 178.3(2) . . . . ?
Fe2 O5 C1 O4 2.9(5) . . . . ?
Fe2 O5 C1 C2 -177.74(19) . . . . ?
Fe2 O7 C3 O6 -1.3(5) . . . . ?
Fe2 O7 C3 C4 176.6(4) . . . . ?
Fe2 O8 C5 O9 3.2(5) . . . . ?
Fe2 O8 C5 C6 -179.1(2) . . . . ?
Fe2 O10 C7 O11 -5.9(5) . . . . ?
Fe2 O10 C7 C8 171.7(3) . . . . ?
Fe3 O9 C5 O8 -5.8(5) . . . . ?
Fe3 O9 C5 C6 176.5(2) . . . . ?
Fe3 O11 C7 O10 -4.2(5) . . . . ?
Fe3 O11 C7 C8 178.1(3) . . . . ?
Fe3 O12 C9 O13 0.0(5) . . . . ?
Fe3 O12 C9 C10 179.78(18) . . . . ?
Fe3 O14 C11 O15 -18.3(5) . . . . ?
Fe3 O14 C11 C12 163.1(2) . . . . ?
Co1 O4 C1 O5 -5.1(5) . . . . ?
Co1 O4 C1 C2 175.53(19) . . . . ?
Co1 O6 C3 O7 -4.6(5) . . . . ?
Co1 O13 C9 O12 -6.8(5) . . . . ?
Co1 O13 C9 C10 173.49(19) . . . . ?
Co1 O15 C11 O14 -0.3(5) . . . . ?
Co1 O15 C11 C12 178.3(2) . . . . ?
Co2 O5 C1 O4 2.9(5) . . . . ?
Co2 O5 C1 C2 -177.74(19) . . . . ?
Co2 O7 C3 O6 -1.3(5) . . . . ?
Co2 O8 C5 O9 3.2(5) . . . . ?
Co2 O8 C5 C6 -179.1(2) . . . . ?
Co2 O10 C7 O11 -5.9(5) . . . . ?
Co3 O9 C5 O8 -5.8(5) . . . . ?
Co3 O9 C5 C6 176.5(2) . . . . ?
Co3 O11 C7 O10 -4.2(5) . . . . ?
Co3 O12 C9 O13 0.0(5) . . . . ?
Co3 O12 C9 C10 179.78(18) . . . . ?
Co3 O14 C11 O15 -18.3(5) . . . . ?
Co3 O14 C11 C12 163.1(2) . . . . ?
O4 Fe1 O16 Fe2 -46.28(12) . . . . ?
O4 Fe1 O16 Fe3 133.45(11) . . . . ?
O4 Co1 O16 Co2 -46.28(12) . . . . ?
O4 Co1 O16 Co3 133.45(11) . . . . ?
O4 C1 C2 F1 -17.1(4) . . . . ?
O4 C1 C2 F2 101.8(3) . . . . ?
O4 C1 C2 F3 -138.4(3) . . . . ?
O5 C1 C2 F1 163.4(3) . . . . ?
O5 C1 C2 F2 -77.7(4) . . . . ?
O5 C1 C2 F3 42.1(4) . . . . ?
O6 Fe1 O16 Fe2 43.14(12) . . . . ?
O6 Fe1 O16 Fe3 -137.12(11) . . . . ?
O6 Co1 O16 Co2 43.14(12) . . . . ?
O6 Co1 O16 Co3 -137.12(11) . . . . ?
O6 C3 C4 F4 -45.6(13) . . . . ?
O6 C3 C4 F5 -165.5(12) . . . . ?
O6 C3 C4 F6 72.2(15) . . . . ?
O6 C3 C4' F4' -20.7(10) . . . . ?
O6 C3 C4' F5' -142.0(7) . . . . ?
O6 C3 C4' F6' 99.2(10) . . . . ?
O7 C3 C4 F4 136.2(11) . . . . ?
O7 C3 C4 F5 16.3(13) . . . . ?
O7 C3 C4 F6 -106.0(14) . . . . ?
O7 C3 C4' F4' 160.4(9) . . . . ?
O7 C3 C4' F5' 39.1(9) . . . . ?
O7 C3 C4' F6' -79.6(11) . . . . ?
O8 C5 C6 F7 26.0(4) . . . . ?
O8 C5 C6 F8 -93.1(3) . . . . ?
O8 C5 C6 F9 144.4(3) . . . . ?
O9 C5 C6 F7 -155.9(3) . . . . ?
O9 C5 C6 F8 84.9(4) . . . . ?
O9 C5 C6 F9 -37.6(4) . . . . ?
O10 C7 C8 F10 -19.4(6) . . . . ?
O10 C7 C8 F11 100.2(6) . . . . ?
O10 C7 C8 F12 -140.6(4) . . . . ?
O10 C7 C8' F10' 168.7(8) . . . . ?
O10 C7 C8' F11' -70.2(9) . . . . ?
O10 C7 C8' F12' 51.0(9) . . . . ?
O11 C7 C8 F10 158.7(5) . . . . ?
O11 C7 C8 F11 -81.8(6) . . . . ?
O11 C7 C8 F12 37.4(5) . . . . ?
O11 C7 C8' F10' -4.8(9) . . . . ?
O11 C7 C8' F11' 116.3(8) . . . . ?
O11 C7 C8' F12' -122.5(7) . . . . ?
O12 C9 C10 F13 1.6(4) . . . . ?
O12 C9 C10 F14 -117.6(3) . . . . ?
O12 C9 C10 F15 122.0(3) . . . . ?
O13 Fe1 O16 Fe2 -136.22(11) . . . . ?
O13 Fe1 O16 Fe3 43.52(12) . . . . ?
O13 Co1 O16 Co2 -136.22(11) . . . . ?
O13 Co1 O16 Co3 43.52(12) . . . . ?
O13 C9 C10 F13 -178.6(2) . . . . ?
O13 C9 C10 F14 62.2(3) . . . . ?
O13 C9 C10 F15 -58.3(3) . . . . ?
O14 C11 C12 F16 -45.1(4) . . . . ?
O14 C11 C12 F17 74.6(4) . . . . ?
O14 C11 C12 F18 -163.9(3) . . . . ?
O15 Fe1 O16 Fe2 128.64(11) . . . . ?
O15 Fe1 O16 Fe3 -51.63(12) . . . . ?
O15 Co1 O16 Co2 128.64(11) . . . . ?
O15 Co1 O16 Co3 -51.63(12) . . . . ?
O15 C11 C12 F16 136.1(3) . . . . ?
O15 C11 C12 F17 -104.2(4) . . . . ?
O15 C11 C12 F18 17.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.433
_oxdiff_exptl_absorpt_empirical_full_min 0.503
