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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C2-m
_audit_block_doi                 10.5517/cc1j7d49
_database_code_depnum_ccdc_archive 'CCDC 1407280'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Potassium iron Vanadium Sulfur
;
_chemical_name_common            'Potassium iron Vanadium Sulfur'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(Fe S8 V4), 2(K0.50) '
_chemical_formula_sum            ' Fe2 K S16 V8'
_chemical_formula_weight         1071.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.465(5)
_cell_length_b                   3.2929(11)
_cell_length_c                   8.473(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.824(12)
_cell_angle_gamma                90
_cell_volume                     473.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5646
_cell_measurement_theta_min      2.402
_cell_measurement_theta_max      27.463

_exptl_crystal_description       polyhedra
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.759
_exptl_crystal_F_000             511
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    7.215
_shelx_estimated_absorpt_T_min   0.680
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   .
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            7878
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.402
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             638
_reflns_number_gt                612
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SHELXL-2014 (Sheldrick, 2014)'
_computing_cell_refinement       'SHELXL-2014 (Sheldrick, 2014)'
_computing_data_reduction        'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+1.1975P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         638
_refine_ls_number_parameters     46
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0161
_refine_ls_wR_factor_ref         0.0427
_refine_ls_wR_factor_gt          0.0423
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.0000 0.0000 0.0000 0.0235(4) Uani 0.5 4 d S T P . .
V1 V 0.28978(2) 0.5000 0.14231(5) 0.01556(14) Uani 0.5 2 d S T P . .
Fe1 Fe 0.28978(2) 0.5000 0.14231(5) 0.01556(14) Uani 0.5 2 d S T P . .
V2 V 0.0000 0.5000 0.5000 0.01343(16) Uani 1 4 d S T P . .
V3 V 0.14927(3) 0.0000 0.48986(5) 0.01126(13) Uani 1 2 d S T P . .
S1 S 0.16100(4) 0.5000 0.00184(7) 0.01202(16) Uani 1 2 d S T P . .
S2 S 0.08517(4) 0.5000 0.31567(7) 0.01166(15) Uani 1 2 d S T P . .
S3 S 0.42648(3) 0.5000 0.32375(7) 0.01060(15) Uani 1 2 d S T P . .
S4 S 0.23997(3) -0.5000 0.65716(7) 0.01006(15) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K 0.0161(8) 0.0390(11) 0.0151(8) 0.000 0.0029(6) 0.000
V1 0.0144(2) 0.0180(2) 0.0142(2) 0.000 0.00321(16) 0.000
Fe1 0.0144(2) 0.0180(2) 0.0142(2) 0.000 0.00321(16) 0.000
V2 0.0110(3) 0.0193(3) 0.0095(3) 0.000 0.0015(2) 0.000
V3 0.0105(2) 0.0129(2) 0.0104(2) 0.000 0.00256(16) 0.000
S1 0.0119(3) 0.0116(3) 0.0124(3) 0.000 0.0026(2) 0.000
S2 0.0123(3) 0.0118(3) 0.0112(3) 0.000 0.0034(2) 0.000
S3 0.0103(3) 0.0098(3) 0.0115(3) 0.000 0.0022(2) 0.000
S4 0.0102(3) 0.0093(3) 0.0109(3) 0.000 0.0031(2) 0.000

_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
K S2 3.1899(9) . ?
K S2 3.1899(9) 5 ?
K S2 3.1899(9) 5_565 ?
K S2 3.1899(9) 1_545 ?
K S1 3.2553(9) 5 ?
K S1 3.2553(9) 5_565 ?
K S1 3.2553(9) 1_545 ?
K S1 3.2553(9) . ?
K K 3.2929(11) 1_545 ?
K K 3.2929(11) 1_565 ?
K S3 3.2949(11) 7 ?
K S3 3.2949(11) 3_445 ?
V1 S1 2.2794(10) . ?
V1 S1 2.3330(7) 7 ?
V1 S1 2.3330(7) 7_565 ?
V1 S4 2.5078(8) 7_556 ?
V1 S4 2.5078(8) 7_546 ?
V1 S3 2.5117(10) . ?
V1 Fe1 2.9759(10) 7 ?
V1 V1 2.9759(10) 7 ?
V1 V1 2.9759(10) 7_565 ?
V1 V3 3.0431(12) 7_556 ?
V2 S3 2.3819(7) 7_566 ?
V2 S3 2.3819(7) 3_445 ?
V2 S3 2.3819(7) 7_556 ?
V2 S3 2.3819(7) 3_455 ?
V2 S2 2.4003(8) 5_566 ?
V2 S2 2.4004(8) . ?
V2 V3 3.1019(8) . ?
V2 V3 3.1020(8) 1_565 ?
V2 V3 3.1020(8) 5_556 ?
V2 V3 3.1020(8) 5_566 ?
V3 S3 2.2897(9) 7_556 ?
V3 S2 2.3136(7) 1_545 ?
V3 S2 2.3136(7) . ?
V3 S4 2.4811(7) 1_565 ?
V3 S4 2.4812(7) . ?
V3 S4 2.5387(9) 7_546 ?
V3 V1 3.0431(12) 7_556 ?
V3 V2 3.1019(8) 1_545 ?
S1 V1 2.3330(7) 7 ?
S1 V1 2.3330(7) 7_565 ?
S1 K 3.2553(9) 1_565 ?
S2 V3 2.3136(7) 1_565 ?
S2 K 3.1899(9) 1_565 ?
S3 V3 2.2897(9) 7_556 ?
S3 V2 2.3819(7) 3 ?
S3 V2 2.3819(7) 3_545 ?
S3 K 3.2949(11) 3 ?
S4 V3 2.4811(7) 1_545 ?
S4 V1 2.5078(8) 7_556 ?
S4 V1 2.5078(8) 7_546 ?
S4 V3 2.5386(9) 7_546 ?

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
S2 K S2 180.0 . 5 ?
S2 K S2 117.85(3) . 5_565 ?
S2 K S2 62.15(3) 5 5_565 ?
S2 K S2 62.15(3) . 1_545 ?
S2 K S2 117.85(3) 5 1_545 ?
S2 K S2 180.00(2) 5_565 1_545 ?
S2 K S1 119.62(2) . 5 ?
S2 K S1 60.38(2) 5 5 ?
S2 K S1 91.60(2) 5_565 5 ?
S2 K S1 88.40(2) 1_545 5 ?
S2 K S1 88.40(2) . 5_565 ?
S2 K S1 91.60(2) 5 5_565 ?
S2 K S1 60.38(2) 5_565 5_565 ?
S2 K S1 119.62(2) 1_545 5_565 ?
S1 K S1 60.77(2) 5 5_565 ?
S2 K S1 91.60(2) . 1_545 ?
S2 K S1 88.40(2) 5 1_545 ?
S2 K S1 119.62(2) 5_565 1_545 ?
S2 K S1 60.38(2) 1_545 1_545 ?
S1 K S1 119.23(2) 5 1_545 ?
S1 K S1 180.000(11) 5_565 1_545 ?
S2 K S1 60.38(2) . . ?
S2 K S1 119.62(2) 5 . ?
S2 K S1 88.40(2) 5_565 . ?
S2 K S1 91.60(2) 1_545 . ?
S1 K S1 180.0 5 . ?
S1 K S1 119.23(3) 5_565 . ?
S1 K S1 60.77(3) 1_545 . ?
S2 K S3 120.11(2) . 7 ?
S2 K S3 59.89(2) 5 7 ?
S2 K S3 59.89(2) 5_565 7 ?
S2 K S3 120.11(2) 1_545 7 ?
S1 K S3 120.268(18) 5 7 ?
S1 K S3 120.268(17) 5_565 7 ?
S1 K S3 59.732(18) 1_545 7 ?
S1 K S3 59.732(18) . 7 ?
S2 K S3 59.89(2) . 3_445 ?
S2 K S3 120.11(2) 5 3_445 ?
S2 K S3 120.11(2) 5_565 3_445 ?
S2 K S3 59.89(2) 1_545 3_445 ?
S1 K S3 59.732(18) 5 3_445 ?
S1 K S3 59.732(18) 5_565 3_445 ?
S1 K S3 120.268(17) 1_545 3_445 ?
S1 K S3 120.268(18) . 3_445 ?
K K S3 90.0 1_545 3_445 ?
K K S3 90.0 1_565 3_445 ?
S3 K S3 180.00(2) 7 3_445 ?
S1 V1 S1 99.65(3) . 7 ?
S1 V1 S1 99.65(3) . 7_565 ?
S1 V1 S1 89.78(3) 7 7_565 ?
S1 V1 S4 90.89(3) . 7_556 ?
S1 V1 S4 168.48(3) 7 7_556 ?
S1 V1 S4 93.05(3) 7_565 7_556 ?
S1 V1 S4 90.89(3) . 7_546 ?
S1 V1 S4 93.05(3) 7 7_546 ?
S1 V1 S4 168.48(3) 7_565 7_546 ?
S4 V1 S4 82.07(3) 7_556 7_546 ?
S1 V1 S3 174.00(3) . . ?
S1 V1 S3 84.56(3) 7 . ?
S1 V1 S3 84.56(3) 7_565 . ?
S4 V1 S3 84.60(3) 7_556 . ?
S4 V1 S3 84.60(3) 7_546 . ?
S3 V2 S3 180.0 7_566 3_445 ?
S3 V2 S3 87.46(3) 7_566 7_556 ?
S3 V2 S3 92.54(3) 3_445 7_556 ?
S3 V2 S3 92.54(3) 7_566 3_455 ?
S3 V2 S3 87.46(3) 3_445 3_455 ?
S3 V2 S3 180.0 7_556 3_455 ?
S3 V2 S2 85.25(3) 7_566 5_566 ?
S3 V2 S2 94.75(3) 3_445 5_566 ?
S3 V2 S2 85.25(3) 7_556 5_566 ?
S3 V2 S2 94.75(3) 3_455 5_566 ?
S3 V2 S2 94.75(3) 7_566 . ?
S3 V2 S2 85.25(3) 3_445 . ?
S3 V2 S2 94.75(3) 7_556 . ?
S3 V2 S2 85.25(3) 3_455 . ?
S2 V2 S2 180.0 5_566 . ?
S3 V3 S2 99.71(3) 7_556 1_545 ?
S3 V3 S2 99.71(3) 7_556 . ?
S2 V3 S2 90.74(4) 1_545 . ?
S3 V3 S4 90.07(3) 7_556 1_565 ?
S2 V3 S4 169.19(3) 1_545 1_565 ?
S2 V3 S4 92.16(3) . 1_565 ?
S3 V3 S4 90.07(3) 7_556 . ?
S2 V3 S4 92.17(3) 1_545 . ?
S2 V3 S4 169.18(3) . . ?
S4 V3 S4 83.15(3) 1_565 . ?
S3 V3 S4 166.41(3) 7_556 7_546 ?
S2 V3 S4 89.79(3) 1_545 7_546 ?
S2 V3 S4 89.79(3) . 7_546 ?
S4 V3 S4 79.81(3) 1_565 7_546 ?
S4 V3 S4 79.81(3) . 7_546 ?

_refine_diff_density_max         0.611
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.090

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL KFe2V8S16 in C2/m
CELL 0.71073  17.46490   3.29290   8.47270  90.0000 103.8238  90.0000
ZERR    4.00   0.00520   0.00110   0.00290   0.0000   0.0120   0.0000
LATT 7
SYMM -X, Y, -Z
SFAC S  K  V  Fe
UNIT 16  1  8  2
L.S. 4
ACTA
BOND
FMAP 2
PLAN 2
EADP V1 Fe1
EXYZ V1 Fe1
SIZE 0.01 0.053 0.058
TEMP 22.290
WGHT    0.020900    1.197500
EXTI    0.002996
FVAR       0.11838
K     2    0.000000    0.000000    0.000000    10.12500    0.01613    0.03896 =
         0.01514    0.00000    0.00292    0.00000
V1    3    0.289782    0.500000    0.142312    10.25000    0.01437    0.01800 =
         0.01421    0.00000    0.00321    0.00000
FE1   4    0.289782    0.500000    0.142312    10.25000    0.01437    0.01800 =
         0.01421    0.00000    0.00321    0.00000
V2    3    0.000000    0.500000    0.500000    10.25000    0.01102    0.01931 =
         0.00948    0.00000    0.00149    0.00000
V3    3    0.149274    0.000000    0.489857    10.50000    0.01051    0.01292 =
         0.01038    0.00000    0.00256    0.00000
S1    1    0.161004    0.500000    0.001835    10.50000    0.01189    0.01158 =
         0.01242    0.00000    0.00258    0.00000
S2    1    0.085169    0.500000    0.315670    10.50000    0.01226    0.01180 =
         0.01121    0.00000    0.00337    0.00000
S3    1    0.426476    0.500000    0.323755    10.50000    0.01027    0.00985 =
         0.01150    0.00000    0.00222    0.00000
S4    1    0.239969   -0.500000    0.657161    10.50000    0.01024    0.00933 =
         0.01091    0.00000    0.00315    0.00000
HKLF 4

REM  KFe2V8S16 in C2/m
REM R1 =  0.0161 for     612 Fo > 4sig(Fo)  and  0.0171 for all     638 data
REM     46 parameters refined using      0 restraints

END

WGHT      0.0209      1.1975

REM Highest difference peak  0.611,  deepest hole -0.579,  1-sigma level  0.090
Q1    1   0.1710  0.0000  0.5059  10.50000  0.05    0.61
Q2    1   0.0161  0.0000 -0.0382  10.50000  0.05    0.28
;
_shelx_res_checksum              43796

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1432650'
_audit_update_record             
;
2015-10-22 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Fe1 S8 V4'
_chemical_formula_sum            'Fe1 S8 V4'
_chemical_formula_weight         516.09
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.9000(11)
_cell_length_b                   6.6425(11)
_cell_length_c                   8.0327(11)
_cell_angle_alpha                90
_cell_angle_beta                 91.202(5)
_cell_angle_gamma                90
_cell_volume                     421.43(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.067
_exptl_crystal_F_000             492
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    7.852
_shelx_estimated_absorpt_T_min   .
_shelx_estimated_absorpt_T_max   .
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.48
_exptl_absorpt_process_details   SADABS
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2867
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.580
_diffrn_reflns_theta_max         25.640
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             430
_reflns_number_gt                367
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²+4.3343P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         430
_refine_ls_number_parameters     44
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.0000 0.0064(4) Uani 0.888(5) 4 d S T P . .
V1 V 0.5000 0.28256(17) 0.5000 0.0098(3) Uani 1 2 d S T P . .
V2 V 0.74367(14) 0.5000 0.26982(14) 0.0141(4) Uani 1 2 d S T P . .
S1 S 0.7224(2) 0.5000 0.5564(2) 0.0100(4) Uani 1 2 d S T P . .
S2 S 0.53708(14) 0.74930(17) 0.20827(13) 0.0106(3) Uani 1 1 d . . . . .
S3 S 0.80286(19) 0.5000 -0.0254(2) 0.0103(4) Uani 1 2 d S T P . .
Fe2 Fe 0.7500 0.7500 0.7500 0.034(7) Uani 0.056(2) 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0057(8) 0.0070(8) 0.0065(8) 0.000 0.0000(5) 0.000
V1 0.0108(6) 0.0062(6) 0.0122(6) 0.000 -0.0023(4) 0.000
V2 0.0115(6) 0.0186(8) 0.0122(6) 0.000 -0.0033(4) 0.000
S1 0.0101(8) 0.0083(8) 0.0116(8) 0.000 -0.0014(6) 0.000
S2 0.0125(6) 0.0078(6) 0.0116(6) -0.0003(4) 0.0013(5) -0.0006(4)
S3 0.0089(8) 0.0078(8) 0.0141(9) 0.000 0.0007(6) 0.000
Fe2 0.034(13) 0.037(15) 0.031(12) 0.015(10) -0.020(10) -0.020(10)

_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 S2 2.3678(11) 5_665 ?
Fe1 S2 2.3678(11) 6_565 ?
Fe1 S2 2.3678(11) 2_655 ?
Fe1 S2 2.3678(11) . ?
Fe1 S3 2.4055(16) . ?
Fe1 S3 2.4055(16) 5_665 ?
V1 S1 2.3121(14) . ?
V1 S1 2.3121(14) 5_666 ?
V1 S2 2.3772(11) 6_565 ?
V1 S2 2.3772(11) 5_666 ?
V1 S3 2.4447(13) 3_445 ?
V1 S3 2.4447(13) 7_655 ?
V2 S1 2.3114(19) . ?
V2 S2 2.3699(14) 6_565 ?
V2 S2 2.3699(14) . ?
V2 S2 2.4065(14) 7_665 ?
V2 S2 2.4065(14) 4_645 ?
V2 S3 2.427(2) . ?
V2 V1 3.0594(12) 5_666 ?
S1 Fe2 2.2825(11) . ?
S1 Fe2 2.2825(11) 4_646 ?
S1 V1 2.3121(14) 5_666 ?
S2 Fe2 2.2995(12) 2_656 ?
S2 V1 2.3771(11) 5_666 ?
S2 V2 2.4065(14) 7_665 ?
S3 V1 2.4447(13) 3_554 ?
S3 V1 2.4447(13) 7_655 ?
S3 Fe2 2.4811(12) 4_645 ?
S3 Fe2 2.4811(12) 1_554 ?
Fe2 S1 2.2825(11) 7_666 ?
Fe2 S2 2.2996(12) 8_565 ?
Fe2 S2 2.2996(12) 2_656 ?
Fe2 S3 2.4811(12) 7_665 ?
Fe2 S3 2.4811(12) 1_556 ?

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
S2 Fe1 S2 91.24(5) 5_665 6_565 ?
S2 Fe1 S2 88.76(5) 5_665 2_655 ?
S2 Fe1 S2 180.0 6_565 2_655 ?
S2 Fe1 S2 180.0 5_665 . ?
S2 Fe1 S2 88.76(5) 6_565 . ?
S2 Fe1 S2 91.24(5) 2_655 . ?
S2 Fe1 S3 92.79(4) 5_665 . ?
S2 Fe1 S3 87.21(4) 6_565 . ?
S2 Fe1 S3 92.79(4) 2_655 . ?
S2 Fe1 S3 87.21(4) . . ?
S2 Fe1 S3 87.21(4) 5_665 5_665 ?
S2 Fe1 S3 92.79(4) 6_565 5_665 ?
S2 Fe1 S3 87.21(4) 2_655 5_665 ?
S2 Fe1 S3 92.79(4) . 5_665 ?
S3 Fe1 S3 180.0 . 5_665 ?
S1 V1 S1 102.68(7) . 5_666 ?
S1 V1 S2 98.04(5) . 6_565 ?
S1 V1 S2 88.36(5) 5_666 6_565 ?
S1 V1 S2 88.36(5) . 5_666 ?
S1 V1 S2 98.04(5) 5_666 5_666 ?
S2 V1 S2 169.78(8) 6_565 5_666 ?
S1 V1 S3 167.47(5) . 3_445 ?
S1 V1 S3 89.03(4) 5_666 3_445 ?
S2 V1 S3 86.61(5) 6_565 3_445 ?
S2 V1 S3 85.55(5) 5_666 3_445 ?
S1 V1 S3 89.03(4) . 7_655 ?
S1 V1 S3 167.47(5) 5_666 7_655 ?
S2 V1 S3 85.55(5) 6_565 7_655 ?
S2 V1 S3 86.61(5) 5_666 7_655 ?
S3 V1 S3 79.70(7) 3_445 7_655 ?
S1 V2 S2 98.26(5) . 6_565 ?
S1 V2 S2 98.26(5) . . ?
S2 V2 S2 88.65(7) 6_565 . ?
S1 V2 S2 89.68(5) . 7_665 ?
S2 V2 S2 171.98(6) 6_565 7_665 ?
S2 V2 S2 91.33(4) . 7_665 ?
S1 V2 S2 89.68(5) . 4_645 ?
S2 V2 S2 91.33(4) 6_565 4_645 ?
S2 V2 S2 171.98(6) . 4_645 ?
S2 V2 S2 87.58(7) 7_665 4_645 ?
S1 V2 S3 173.05(7) . . ?
S2 V2 S3 86.68(5) 6_565 . ?
S2 V2 S3 86.68(5) . . ?
S2 V2 S3 85.32(5) 7_665 . ?
S2 V2 S3 85.32(5) 4_645 . ?
S1 Fe2 S1 180.0 7_666 . ?
S1 Fe2 S2 91.01(5) 7_666 8_565 ?
S1 Fe2 S2 88.99(5) . 8_565 ?
S1 Fe2 S2 88.99(5) 7_666 2_656 ?
S1 Fe2 S2 91.01(5) . 2_656 ?
S2 Fe2 S2 180.0 8_565 2_656 ?
S1 Fe2 S3 91.19(4) 7_666 7_665 ?
S1 Fe2 S3 88.81(4) . 7_665 ?
S2 Fe2 S3 92.53(4) 8_565 7_665 ?
S2 Fe2 S3 87.47(4) 2_656 7_665 ?
S1 Fe2 S3 88.81(4) 7_666 1_556 ?
S1 Fe2 S3 91.19(4) . 1_556 ?
S2 Fe2 S3 87.47(4) 8_565 1_556 ?
S2 Fe2 S3 92.53(4) 2_656 1_556 ?
S3 Fe2 S3 180.0 7_665 1_556 ?

_refine_diff_density_max         0.619
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.167

_shelx_res_file                  
;

    I2-m.res created by SHELXL-2014/7


TITL I2-m_a.res in I2/m
CELL  0.71073   7.9000   6.6425   8.0327   90.000   91.202   90.000
ZERR    1.000   0.0011   0.0011   0.0011    0.000    0.005    0.000
LATT  2
SYMM -X, Y, -Z
SFAC  S  V FE
UNIT  16 8 2
L.S. 10
LIST 4
ACTA
FMAP 2
PLAN 2
WGHT    0.015700    4.334301
FVAR       0.11829   0.88782
FE1   3    0.500000    0.500000    0.000000    20.25000    0.00565    0.00696 =
         0.00651    0.00000    0.00002    0.00000
V1    2    0.500000    0.282565    0.500000    10.50000    0.01083    0.00622 =
         0.01224    0.00000   -0.00227    0.00000
V2    2    0.743673    0.500000    0.269823    10.50000    0.01145    0.01864 =
         0.01220    0.00000   -0.00327    0.00000
S1    1    0.722439    0.500000    0.556380    10.50000    0.01011    0.00832 =
         0.01161    0.00000   -0.00137    0.00000
S2    1    0.537084    0.749302    0.208270    11.00000    0.01252    0.00777 =
         0.01164   -0.00028    0.00132   -0.00063
S3    1    0.802855    0.500000   -0.025381    10.50000    0.00895    0.00783 =
         0.01415    0.00000    0.00069    0.00000
FE2   3    0.750000    0.750000    0.750000   -20.25000    0.03415    0.03714 =
         0.03088    0.01458   -0.01996   -0.01953
HKLF 4

REM  I2-m_a.res in I2/m
REM R1 =  0.0308 for     367 Fo > 4sig(Fo)  and  0.0412 for all     430 data
REM     44 parameters refined using      0 restraints

END

WGHT      0.0157      4.3343

REM Highest difference peak  0.619,  deepest hole -0.771,  1-sigma level  0.167
Q1    1   0.6659  0.6776  0.0426  11.00000  0.05    0.62
Q2    1   0.7143  0.7243  0.6376  11.00000  0.05    0.54
;
_shelx_res_checksum              8540
