# 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_HTB
_database_code_depnum_ccdc_archive 'CCDC 2002319'
loop_
_audit_author_name
_audit_author_address
'Jerome Lhoste'
;IMMM
France
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'F16 Fe3.28 O2.60 V2.72'
_chemical_formula_weight         667.31
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
fe 11.76950 4.76110 7.35730 0.30720 3.52220 15.35350 2.30450 76.88050 1.03690
-3.33000 0.49000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
v 9.43141 6.39535 7.74190 0.38335 2.15343 15.19080 0.01687 63.96900 0.65657
-0.38710 2.69940
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
f 3.63220 5.27756 3.51057 14.73530 1.26064 0.44226 0.94071 47.34370 0.65340
0.09200 0.07250
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 4.75800 7.83100 3.63700 30.05000 0.00000 0.00000 0.00000 0.00000 1.59400
0.06300 0.04400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
x-y,x,z+1/2
-y,x-y,z
-x,-y,z+1/2
-x+y,-x,z
y,-x+y,z+1/2
-x,-y,-z
-x+y,-x,-z+1/2
y,-x+y,-z
x,y,-z+1/2
x-y,x,-z
-y,x-y,-z+1/2

_cell_length_a                   7.3908(3)
_cell_length_b                   7.3908(3)
_cell_length_c                   7.5568(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.000
_cell_volume                     357.48(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_exptl_crystal_colour            green
_exptl_crystal_description       powder
_pd_spec_size_axial              ? # perpendicular to 
# equatorial plane
_pd_spec_size_equat              ? # parallel to 
# scattering vector
# in transmission
_pd_spec_size_thick              ? # parallel to 
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; ?
;
_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   ? # options are 'cylinder' 
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      296
_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           'Co K\a'
_diffrn_source_target            Co

_diffrn_radiation_wavelength     1.789010
_diffrn_measurement_device_type  'Panalytical XPERT-PRO'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector
_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        8676
_pd_meas_2theta_range_min        5.02136
_pd_meas_2theta_range_max        149.99161
_pd_meas_2theta_range_inc        0.016711

#=============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     ?
_pd_proc_ls_background_function  ?
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        3.1420
_pd_proc_ls_prof_wR_factor       4.2170
_pd_proc_ls_prof_wR_expected     3.2124

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       54.4476
_pd_proc_ls_prof_cwR_factor      26.8331
_pd_proc_ls_prof_cwR_expected    20.4410

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            1.7232
_pd_proc_ls_prof_echi2           1.8380
_refine_ls_goodness_of_fit_all   1.3557

#  Items related to LS refinement

_refine_ls_R_I_factor            8.6297
_refine_ls_number_reflns         366
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        4.9794
_pd_proc_2theta_range_max        149.9497
_pd_proc_2theta_range_inc        0.016711
_pd_proc_wavelength              1.789010

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Fe1 0.50000 0.00000 0.00000 0.0211(11) 0.54600 Uiso Fe
V1 0.50000 0.00000 0.00000 0.0211(11) 0.45400 Uiso V
F1 0.505(5) -0.017(4) 0.25000 0.059(3) 1.00000 Uiso F
F2 0.210(13) -0.206(13) -0.001(5) 0.059(3) 0.83333 Uiso F
O2 0.210(13) -0.206(13) -0.001(5) 0.059(3) 0.16667 Uiso O
Ow 0.00000 0.00000 0.75000 0.059(3) 0.30000 Uiso O

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#=============================================================================

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 

_geom_special_details            ?

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 F1 1.895(3) 1_555 ?
Fe1 F1 1.895(3) 4_654 ?
Fe1 F2 1.91(7) 1_555 ?
Fe1 F2 1.94(12) 5_655 ?
Fe1 F2 1.91(7) 7_655 ?
Fe1 F2 1.94(12) 11_555 ?
Fe1 O2 1.91(7) 1_555 ?
Fe1 O2 1.94(12) 5_655 ?
Fe1 O2 1.91(7) 7_655 ?
Fe1 O2 1.94(12) 11_555 ?
V1 F1 1.895(3) 1_555 ?
V1 F1 1.895(3) 4_654 ?
V1 F2 1.91(7) 1_555 ?
V1 F2 1.94(12) 5_655 ?
V1 F2 1.91(7) 7_655 ?
V1 F2 1.94(12) 11_555 ?
V1 O2 1.91(7) 1_555 ?
V1 O2 1.94(12) 5_655 ?
V1 O2 1.91(7) 7_655 ?
V1 O2 1.94(12) 11_555 ?
F1 Fe1 1.895(3) 1_555 ?
F1 Fe1 1.895(3) 4_655 ?
F1 V1 1.895(3) 1_555 ?
F1 V1 1.895(3) 4_655 ?
F2 Fe1 1.91(7) 1_555 ?
F2 Fe1 1.94(7) 3_545 ?
F2 V1 1.91(7) 1_555 ?
F2 V1 1.94(7) 3_545 ?
O2 Fe1 1.91(7) 1_555 ?
O2 Fe1 1.94(7) 3_545 ?
O2 V1 1.91(7) 1_555 ?
O2 V1 1.94(7) 3_545 ?

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
F1 Fe1 F1 180.0(3) 1_555 4_654 ?
F1 Fe1 F2 90(3) 1_555 1_555 ?
F1 Fe1 F2 86(5) 1_555 5_655 ?
F1 Fe1 F2 90(3) 1_555 7_655 ?
F1 Fe1 F2 94(5) 1_555 11_555 ?
F1 Fe1 O2 90(3) 1_555 1_555 ?
F1 Fe1 O2 86(5) 1_555 5_655 ?
F1 Fe1 O2 90(3) 1_555 7_655 ?
F1 Fe1 O2 94(5) 1_555 11_555 ?
F1 Fe1 F2 90(3) 4_654 1_555 ?
F1 Fe1 F2 94(5) 4_654 5_655 ?
F1 Fe1 F2 90(3) 4_654 7_655 ?
F1 Fe1 F2 86(5) 4_654 11_555 ?
F1 Fe1 O2 90(3) 4_654 1_555 ?
F1 Fe1 O2 94(5) 4_654 5_655 ?
F1 Fe1 O2 90(3) 4_654 7_655 ?
F1 Fe1 O2 86(5) 4_654 11_555 ?
F2 Fe1 F2 92(8) 1_555 5_655 ?
F2 Fe1 F2 180(7) 1_555 7_655 ?
F2 Fe1 F2 88(6) 1_555 11_555 ?
F2 Fe1 O2 92(8) 1_555 5_655 ?
F2 Fe1 O2 180(7) 1_555 7_655 ?
F2 Fe1 O2 88(6) 1_555 11_555 ?
F2 Fe1 F2 88(6) 5_655 7_655 ?
F2 Fe1 F2 180(11) 5_655 11_555 ?
F2 Fe1 O2 92(8) 5_655 1_555 ?
F2 Fe1 O2 88(6) 5_655 7_655 ?
F2 Fe1 O2 180(11) 5_655 11_555 ?
F2 Fe1 F2 92(8) 7_655 11_555 ?
F2 Fe1 O2 180(7) 7_655 1_555 ?
F2 Fe1 O2 88(6) 7_655 5_655 ?
F2 Fe1 O2 92(8) 7_655 11_555 ?
F2 Fe1 O2 88(6) 11_555 1_555 ?
F2 Fe1 O2 180(11) 11_555 5_655 ?
F2 Fe1 O2 92(8) 11_555 7_655 ?
O2 Fe1 O2 92(8) 1_555 5_655 ?
O2 Fe1 O2 180(7) 1_555 7_655 ?
O2 Fe1 O2 88(6) 1_555 11_555 ?
O2 Fe1 O2 88(6) 5_655 7_655 ?
O2 Fe1 O2 180(11) 5_655 11_555 ?
O2 Fe1 O2 92(8) 7_655 11_555 ?
F1 V1 F1 180.0(3) 1_555 4_654 ?
F1 V1 F2 90(3) 1_555 1_555 ?
F1 V1 F2 86(5) 1_555 5_655 ?
F1 V1 F2 90(3) 1_555 7_655 ?
F1 V1 F2 94(5) 1_555 11_555 ?
F1 V1 O2 90(3) 1_555 1_555 ?
F1 V1 O2 86(5) 1_555 5_655 ?
F1 V1 O2 90(3) 1_555 7_655 ?
F1 V1 O2 94(5) 1_555 11_555 ?
F1 V1 F2 90(3) 4_654 1_555 ?
F1 V1 F2 94(5) 4_654 5_655 ?
F1 V1 F2 90(3) 4_654 7_655 ?
F1 V1 F2 86(5) 4_654 11_555 ?
F1 V1 O2 90(3) 4_654 1_555 ?
F1 V1 O2 94(5) 4_654 5_655 ?
F1 V1 O2 90(3) 4_654 7_655 ?
F1 V1 O2 86(5) 4_654 11_555 ?
F2 V1 F2 92(8) 1_555 5_655 ?
F2 V1 F2 180(7) 1_555 7_655 ?
F2 V1 F2 88(6) 1_555 11_555 ?
F2 V1 O2 92(8) 1_555 5_655 ?
F2 V1 O2 180(7) 1_555 7_655 ?
F2 V1 O2 88(6) 1_555 11_555 ?
F2 V1 F2 88(6) 5_655 7_655 ?
F2 V1 F2 180(11) 5_655 11_555 ?
F2 V1 O2 92(8) 5_655 1_555 ?
F2 V1 O2 88(6) 5_655 7_655 ?
F2 V1 O2 180(11) 5_655 11_555 ?
F2 V1 F2 92(8) 7_655 11_555 ?
F2 V1 O2 180(7) 7_655 1_555 ?
F2 V1 O2 88(6) 7_655 5_655 ?
F2 V1 O2 92(8) 7_655 11_555 ?
F2 V1 O2 88(6) 11_555 1_555 ?
F2 V1 O2 180(11) 11_555 5_655 ?
F2 V1 O2 92(8) 11_555 7_655 ?
O2 V1 O2 92(8) 1_555 5_655 ?
O2 V1 O2 180(7) 1_555 7_655 ?
O2 V1 O2 88(6) 1_555 11_555 ?
O2 V1 O2 88(6) 5_655 7_655 ?
O2 V1 O2 180(11) 5_655 11_555 ?
O2 V1 O2 92(8) 7_655 11_555 ?
Fe1 F1 Fe1 171.06(13) 1_555 4_655 ?
Fe1 F1 V1 171.06(13) 1_555 4_655 ?
Fe1 F1 V1 171.06(13) 4_655 1_555 ?
V1 F1 V1 171.06(13) 1_555 4_655 ?
Fe1 F2 Fe1 148(3) 1_555 3_545 ?
Fe1 F2 V1 148(3) 1_555 3_545 ?
Fe1 F2 V1 148(3) 3_545 1_555 ?
V1 F2 V1 148(3) 1_555 3_545 ?
Fe1 O2 Fe1 148(3) 1_555 3_545 ?
Fe1 O2 V1 148(3) 1_555 3_545 ?
Fe1 O2 V1 148(3) 3_545 1_555 ?
V1 O2 V1 148(3) 1_555 3_545 ?
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_FeV2
_database_code_depnum_ccdc_archive 'CCDC 2002320'
loop_
_audit_author_name
_audit_author_address
'Jerome Lhoste'
;IMMM
France
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'F8 Fe1.64 O2 V1.36'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'F8 Fe1.64 O2 V1.36'
_chemical_formula_weight         344.9
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and 
# natural products

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
fe+2 11.04240 4.65380 7.37400 0.30530 4.13460 12.05460 0.43990 31.28090 1.00970
-1.17900 3.20400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
v+3 9.43141 6.39535 7.74190 0.38335 2.15343 15.19080 0.01687 63.96900 0.65657
0.03500 2.11000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
fe+3 11.17640 4.61470 7.38630 0.30050 3.39480 11.67290 0.07240 38.55660 0.97070
-1.17900 3.20400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
f 3.53920 10.28250 2.64120 4.29440 1.51700 0.26150 1.02430 26.14760 0.27760
0.06900 0.05300
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y,-z
-x,-y,-z
x,-y,z
x+1/2,y+1/2,z
-x+1/2,y+1/2,-z
-x+1/2,-y+1/2,-z
x+1/2,-y+1/2,z

_cell_length_a                   7.5835(3)
_cell_length_b                   7.4814(3)
_cell_length_c                   7.5269(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 119.925(3)
_cell_angle_gamma                90.0000
_cell_volume                     370.11(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to 
# equatorial plane
_pd_spec_size_equat              ? # parallel to 
# scattering vector
# in transmission
_pd_spec_size_thick              ? # parallel to 
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
; ?
;
_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   ? # options are 'cylinder' 
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions
_exptl_crystal_colour            'dark green'
_exptl_crystal_description       powder

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54060

_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'Panalytical XPERT-PRO'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector
_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        7660
_pd_meas_2theta_range_min        10.00036
_pd_meas_2theta_range_max        137.99196
_pd_meas_2theta_range_inc        0.016711

#=============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     ?
_pd_proc_ls_background_function  ?
_pd_proc_ls_pref_orient_corr     
; ?
;

#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        1.7719
_pd_proc_ls_prof_wR_factor       2.3892
_pd_proc_ls_prof_wR_expected     1.6675

#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       25.1453
_pd_proc_ls_prof_cwR_factor      13.6934
_pd_proc_ls_prof_cwR_expected    9.5570

#  The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            2.0530
_pd_proc_ls_prof_echi2           2.1760
_refine_ls_goodness_of_fit_all   1.4751

#  Items related to LS refinement

_refine_ls_R_I_factor            3.9346
_refine_ls_number_reflns         406
_refine_ls_number_parameters     84
_refine_ls_number_restraints     0

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        9.8781
_pd_proc_2theta_range_max        137.8697
_pd_proc_2theta_range_inc        0.016711
_pd_proc_wavelength              1.540600

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Fe1 0.00000 0.50000 0.00000 0.0408(13) 1.00000 Uiso Fe
V1 0.25000 0.25000 0.50000 0.0210(6) 0.68000 Uiso V
Fe2 0.25000 0.25000 0.50000 0.0210(6) 0.32000 Uiso Fe
O1 0.2088(10) 0.00000 -0.0183(14) 0.0494(11) 1.00000 Uiso O
F1 0.00000 0.2144(9) 0.50000 0.0494(11) 1.00000 Uiso F
F2 0.2412(10) 0.00000 0.4253(9) 0.0494(11) 1.00000 Uiso F
F3 0.1008(10) 0.3027(4) 0.2160(4) 0.0494(11) 1.00000 Uiso F

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#=============================================================================

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 

_geom_special_details            ?

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 2.143(9) 5_455 ?
Fe1 O1 2.143(9) 6_555 ?
Fe1 F3 2.041(3) 1_555 ?
Fe1 F3 2.041(3) 2_555 ?
Fe1 F3 2.041(3) 3_565 ?
Fe1 F3 2.041(3) 4_565 ?
V1 F1 1.9145(9) 1_555 ?
V1 F1 1.9145(9) 7_556 ?
V1 F2 1.945(2) 1_555 ?
V1 F2 1.945(2) 6_556 ?
V1 F3 1.895(3) 1_555 ?
V1 F3 1.895(3) 7_556 ?
Fe2 F1 1.9145(9) 1_555 ?
Fe2 F1 1.9145(9) 7_556 ?
Fe2 F2 1.945(2) 1_555 ?
Fe2 F2 1.945(2) 6_556 ?
Fe2 F3 1.895(3) 1_555 ?
Fe2 F3 1.895(3) 7_556 ?
O1 Fe1 2.143(9) 5_545 ?
F1 V1 1.9145(9) 1_555 ?
F1 V1 1.9145(9) 2_556 ?
F1 Fe2 1.9145(9) 1_555 ?
F1 Fe2 1.9145(9) 2_556 ?
F2 V1 1.945(2) 1_555 ?
F2 V1 1.945(2) 4_555 ?
F2 Fe2 1.945(2) 1_555 ?
F2 Fe2 1.945(2) 4_555 ?
F3 Fe1 2.041(3) 1_555 ?
F3 V1 1.895(3) 1_555 ?
F3 Fe2 1.895(3) 1_555 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 180.0(8) 5_455 6_555 ?
O1 Fe1 F3 90.9(4) 5_455 1_555 ?
O1 Fe1 F3 89.1(5) 5_455 2_555 ?
O1 Fe1 F3 89.1(5) 5_455 3_565 ?
O1 Fe1 F3 90.9(4) 5_455 4_565 ?
O1 Fe1 F3 89.1(5) 6_555 1_555 ?
O1 Fe1 F3 90.9(4) 6_555 2_555 ?
O1 Fe1 F3 90.9(4) 6_555 3_565 ?
O1 Fe1 F3 89.1(5) 6_555 4_565 ?
F3 Fe1 F3 87.37(18) 1_555 2_555 ?
F3 Fe1 F3 180.0(3) 1_555 3_565 ?
F3 Fe1 F3 92.6(2) 1_555 4_565 ?
F3 Fe1 F3 92.6(2) 2_555 3_565 ?
F3 Fe1 F3 180.0(3) 2_555 4_565 ?
F3 Fe1 F3 87.37(18) 3_565 4_565 ?
F1 V1 F1 179.97(9) 1_555 7_556 ?
F1 V1 F2 88.6(3) 1_555 1_555 ?
F1 V1 F2 91.4(3) 1_555 6_556 ?
F1 V1 F3 89.7(3) 1_555 1_555 ?
F1 V1 F3 90.3(3) 1_555 7_556 ?
F1 V1 F2 91.4(3) 7_556 1_555 ?
F1 V1 F2 88.6(3) 7_556 6_556 ?
F1 V1 F3 90.3(3) 7_556 1_555 ?
F1 V1 F3 89.7(3) 7_556 7_556 ?
F2 V1 F2 180.00(19) 1_555 6_556 ?
F2 V1 F3 87.64(19) 1_555 1_555 ?
F2 V1 F3 92.4(3) 1_555 7_556 ?
F2 V1 F3 92.4(3) 6_556 1_555 ?
F2 V1 F3 87.64(19) 6_556 7_556 ?
F3 V1 F3 180.0(2) 1_555 7_556 ?
F1 Fe2 F1 179.97(9) 1_555 7_556 ?
F1 Fe2 F2 88.6(3) 1_555 1_555 ?
F1 Fe2 F2 91.4(3) 1_555 6_556 ?
F1 Fe2 F3 89.7(3) 1_555 1_555 ?
F1 Fe2 F3 90.3(3) 1_555 7_556 ?
F1 Fe2 F2 91.4(3) 7_556 1_555 ?
F1 Fe2 F2 88.6(3) 7_556 6_556 ?
F1 Fe2 F3 90.3(3) 7_556 1_555 ?
F1 Fe2 F3 89.7(3) 7_556 7_556 ?
F2 Fe2 F2 180.00(19) 1_555 6_556 ?
F2 Fe2 F3 87.64(19) 1_555 1_555 ?
F2 Fe2 F3 92.4(3) 1_555 7_556 ?
F2 Fe2 F3 92.4(3) 6_556 1_555 ?
F2 Fe2 F3 87.64(19) 6_556 7_556 ?
F3 Fe2 F3 180.0(2) 1_555 7_556 ?
V1 F1 V1 164.01(4) 1_555 2_556 ?
V1 F1 Fe2 164.01(4) 1_555 2_556 ?
V1 F1 Fe2 164.01(4) 2_556 1_555 ?
Fe2 F1 Fe2 164.01(4) 1_555 2_556 ?
V1 F2 V1 148.24(8) 1_555 4_555 ?
V1 F2 Fe2 148.24(8) 1_555 4_555 ?
V1 F2 Fe2 148.24(8) 4_555 1_555 ?
Fe2 F2 Fe2 148.24(8) 1_555 4_555 ?
Fe1 F3 V1 145.53(11) 1_555 1_555 ?
Fe1 F3 Fe2 145.53(11) 1_555 1_555 ?
_chemical_properties_physical    Air-sensitive
