# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Spencer, Elinor'
_publ_contact_author_email       elinor.c.spencer@gmail.com

_publ_section_title              
;
Re-determination of the Structure of an Anionic Oxovanadium Arsenate Framework
;
_publ_author_name                E.Spencer

# Attachment '- Soghomonian_CIF.cif'

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 776172'
#TrackingRef '- Soghomonian_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As6 O51 V15'
_chemical_formula_sum            'As6 O51 V15'
_chemical_formula_weight         2029.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Im-3m
_symmetry_space_group_name_Hall  '-I 4 2 3'

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

_cell_length_a                   16.62170(10)
_cell_length_b                   16.62170(10)
_cell_length_c                   16.62170(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4592.26(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6774
_cell_measurement_theta_min      3.8534
_cell_measurement_theta_max      24.9980

_exptl_crystal_description       Cube
_exptl_crystal_colour            'Dark green'
_exptl_crystal_size_max          0.0832
_exptl_crystal_size_mid          0.0801
_exptl_crystal_size_min          0.0720
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1902
_exptl_absorpt_coefficient_mu    3.657
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Atlas CCD'
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.2265
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <2%
_diffrn_reflns_number            27190
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.88
_diffrn_reflns_theta_max         25.11
_reflns_number_total             437
_reflns_number_gt                336
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_structure_solution    
'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement  
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_molecular_graphics    'CrystalMaker v2.0'
_computing_publication_material  
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         437
_refine_ls_number_parameters     33
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2214
_refine_ls_wR_factor_gt          0.2160
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.5000 0.0000 0.2500 0.0432(9) Uani 1 8 d S . .
V1 V 0.5000 0.1473(3) 0.5000 0.0403(14) Uani 0.50 8 d SP . .
V2 V 0.61271(13) 0.0758(2) 0.38729(13) 0.0503(11) Uani 0.50 2 d SP . .
O1 O 0.5838(4) 0.0000 0.3064(3) 0.0546(17) Uani 1 2 d S . .
O2 O 0.5000 0.2426(14) 0.5000 0.069(9) Uani 0.50 8 d SP . .
O3 O 0.6579(6) 0.1487(8) 0.3421(6) 0.059(3) Uani 0.50 2 d SP . .
O4 O 0.6080(6) 0.1106(6) 0.5000 0.041(3) Uani 0.50 2 d SP . .

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
As1 0.0488(10) 0.0488(10) 0.0320(11) 0.000 0.000 0.000
V1 0.044(2) 0.032(3) 0.044(2) 0.000 0.000 0.000
V2 0.0438(12) 0.063(2) 0.0438(12) -0.0007(10) 0.0012(13) 0.0007(10)
O1 0.052(4) 0.073(4) 0.039(3) 0.000 -0.004(3) 0.000
O2 0.087(14) 0.035(14) 0.087(14) 0.000 0.000 0.000
O3 0.056(5) 0.067(8) 0.056(5) 0.017(5) -0.012(6) -0.017(5)
O4 0.037(6) 0.039(6) 0.048(7) 0.000 0.000 -0.008(5)

_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
As1 O1 1.678(6) 74 ?
As1 O1 1.678(6) . ?
As1 O1 1.678(6) 76_545 ?
As1 O1 1.678(6) 3_655 ?
V1 O2 1.58(2) . ?
V1 O4 1.896(11) 8_556 ?
V1 O4 1.896(11) 54_655 ?
V1 O4 1.896(11) 10_655 ?
V1 O4 1.896(11) . ?
V1 V2 2.903(4) 54_655 ?
V1 V2 2.903(4) . ?
V1 V2 2.903(4) 51_556 ?
V1 V2 2.903(4) 9_656 ?
V2 O3 1.612(13) . ?
V2 O1 1.905(5) . ?
V2 O1 1.905(5) 71_656 ?
V2 O4 1.962(4) . ?
V2 O4 1.962(4) 8_556 ?
V2 V2 2.520(7) 57 ?
O1 V2 1.905(5) 57 ?
O4 V2 1.962(4) 51_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
O1 As1 O1 108.18(19) 74 . ?
O1 As1 O1 112.1(4) 74 76_545 ?
O1 As1 O1 108.18(19) . 76_545 ?
O1 As1 O1 108.18(19) 74 3_655 ?
O1 As1 O1 112.1(4) . 3_655 ?
O1 As1 O1 108.18(19) 76_545 3_655 ?
O2 V1 O4 108.8(3) . 8_556 ?
O2 V1 O4 108.8(3) . 54_655 ?
O4 V1 O4 84.1(2) 8_556 54_655 ?
O2 V1 O4 108.8(3) . 10_655 ?
O4 V1 O4 142.5(7) 8_556 10_655 ?
O4 V1 O4 84.1(2) 54_655 10_655 ?
O2 V1 O4 108.8(3) . . ?
O4 V1 O4 84.1(2) 8_556 . ?
O4 V1 O4 142.5(7) 54_655 . ?
O4 V1 O4 84.1(2) 10_655 . ?
O2 V1 V2 114.15(12) . 54_655 ?
O4 V1 V2 42.05(9) 8_556 54_655 ?
O4 V1 V2 42.05(9) 54_655 54_655 ?
O4 V1 V2 118.6(3) 10_655 54_655 ?
O4 V1 V2 118.6(3) . 54_655 ?
O2 V1 V2 114.15(12) . . ?
O4 V1 V2 42.05(9) 8_556 . ?
O4 V1 V2 118.6(3) 54_655 . ?
O4 V1 V2 118.6(3) 10_655 . ?
O4 V1 V2 42.05(9) . . ?
V2 V1 V2 80.36(9) 54_655 . ?
O2 V1 V2 114.15(12) . 51_556 ?
O4 V1 V2 118.6(3) 8_556 51_556 ?
O4 V1 V2 118.6(3) 54_655 51_556 ?
O4 V1 V2 42.05(9) 10_655 51_556 ?
O4 V1 V2 42.05(9) . 51_556 ?
V2 V1 V2 131.7(2) 54_655 51_556 ?
V2 V1 V2 80.36(9) . 51_556 ?
O2 V1 V2 114.15(12) . 9_656 ?
O4 V1 V2 118.6(3) 8_556 9_656 ?
O4 V1 V2 42.05(9) 54_655 9_656 ?
O4 V1 V2 42.05(9) 10_655 9_656 ?
O4 V1 V2 118.6(3) . 9_656 ?
V2 V1 V2 80.36(9) 54_655 9_656 ?
V2 V1 V2 131.7(2) . 9_656 ?
V2 V1 V2 80.36(9) 51_556 9_656 ?
O3 V2 O1 106.6(4) . . ?
O3 V2 O1 106.6(4) . 71_656 ?
O1 V2 O1 85.3(3) . 71_656 ?
O3 V2 O4 104.0(5) . . ?
O1 V2 O4 149.2(4) . . ?
O1 V2 O4 89.0(4) 71_656 . ?
O3 V2 O4 104.0(5) . 8_556 ?
O1 V2 O4 89.0(4) . 8_556 ?
O1 V2 O4 149.2(4) 71_656 8_556 ?
O4 V2 O4 80.6(6) . 8_556 ?
O3 V2 V2 138.7(5) . 57 ?
O1 V2 V2 48.57(14) . 57 ?
O1 V2 V2 48.57(14) 71_656 57 ?
O4 V2 V2 107.1(3) . 57 ?
O4 V2 V2 107.1(3) 8_556 57 ?
O3 V2 V1 107.1(5) . . ?
O1 V2 V1 124.3(2) . . ?
O1 V2 V1 124.3(2) 71_656 . ?
O4 V2 V1 40.3(3) . . ?
O4 V2 V1 40.3(3) 8_556 . ?
V2 V2 V1 114.15(12) 57 . ?
As1 O1 V2 127.2(2) . . ?
As1 O1 V2 127.2(2) . 57 ?
V2 O1 V2 82.9(3) . 57 ?
V1 O4 V2 97.6(3) . . ?
V1 O4 V2 97.6(3) . 51_556 ?
V2 O4 V2 145.4(6) . 51_556 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.11
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.835
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.205