Supplementary Material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2001
data_VAs-1
_database_code_CSD 160407
_journal_coden_Cambridge 1145
_publ_requested_journal 'Journal of Materials Chemistry'
loop_
_publ_author_name
'Chen, Xiangming'
'Li, Yafeng'
'Liu, Qingsheng'
'Mai, Zhenghong'
'Zhao, Yongnan'
_publ_contact_author_name 'Dr Yongnan Zhao'
_publ_contact_author_address
;
Dr Yongnan Zhao
Institute of Physics & Center for Condensed Matter Physics
Chinese Academy of Sciences
PO Box 603-79
Beijing
100080
CHINA
;
_publ_contact_author_email 'ZHAOYN@263.NET'
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'H18 As2 O35 V10'
_chemical_formula_weight 1237.38
_chemical_melting_point ?
_chemical_compound_source ?
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'
'H' 'H' 0.0000 0.0000
'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 I-43m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+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, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+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'
'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'
'-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'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
_cell_length_a 16.708(2)
_cell_length_b 16.708(2)
_cell_length_c 16.708(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4664.4(9)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 27
_cell_measurement_theta_min 5.73
_cell_measurement_theta_max 12.29
_exptl_crystal_description cube
_exptl_crystal_colour dark-green
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.762
_exptl_crystal_density_method ?
_exptl_crystal_F_000 2376
_exptl_absorpt_coefficient_mu 3.395
_exptl_absorpt_correction_type 'Semi-empirical from psi scan '
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Siemens P4 '
_diffrn_measurement_method 'w scan'
_diffrn_standards_number 3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 2915
_diffrn_reflns_av_R_equivalents 0.0486
_diffrn_reflns_av_sigmaI/netI 0.0742
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.72
_diffrn_reflns_theta_max 25.06
_reflns_number_total 633
_reflns_number_observed 440
_reflns_observed_criterion >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed
criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0006(4)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.54(19)
_refine_ls_number_reflns 633
_refine_ls_number_parameters 71
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1099
_refine_ls_R_factor_obs 0.0569
_refine_ls_wR_factor_all 0.1392
_refine_ls_wR_factor_obs 0.0775
_refine_ls_goodness_of_fit_all 1.133
_refine_ls_goodness_of_fit_obs 1.199
_refine_ls_restrained_S_all 1.133
_refine_ls_restrained_S_obs 1.199
_refine_ls_shift/esd_max 0.093
_refine_ls_shift/esd_mean 0.013
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
As As 0.5000 0.0000 0.2500 0.017(2) Uani 1 d S .
V1 V 0.3875(5) 0.0768(6) 0.3875(5) 0.020(4) Uani 1 d S .
V2 V 0.5000 0.1473(9) 0.5000 0.022(4) Uani 1 d S .
V3 V 0.6125(8) 0.0715(6) 0.3875(8) 0.023(7) Uani 1 d S .
O1 O 0.3444(8) 0.1522(8) 0.3444(9) 0.029(6) Uani 1 d S .
O2 O 0.5000 0.2443(10) 0.5000 0.035(8) Uani 1 d S .
O3 O 0.6705(12) 0.1322(12) 0.3295(13) 0.030(8) Uani 1 d S .
O4 O 0.4171(9) 0.0043(12) 0.30636(9) 0.021(4) Uani 1 d . .
O5 O 0.6077(10) 0.1097(15) 0.4903(10) 0.041(8) Uani 1 d . .
O6 O 0.5000 0.0000 0.5000 0.106(7) Uani 1 d S .
OW1 O 0.7343(12) 0.2657(12) 0.4757(11) 0.175(11) Uani 1 d S .
OW2 O 0.7583(13) 0.2417(13) 0.3450(13) 0.066(13) Uani 1 d S .
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
As 0.018(2) 0.015(2) 0.018(2) -0.003(2) 0.006(5) 0.002(2)
V1 0.020(6) 0.023(7) 0.018(6) 0.004(4) -0.002(6) 0.001(4)
V2 0.025(6) 0.012(9) 0.028(6) 0.000 -0.005(16) 0.000
V3 0.028(10) 0.018(12) 0.025(10) 0.001(10) 0.006(10) -0.002(10)
O1 0.025(10) 0.025(12) 0.036(10) 0.000 0.004(12) 0.000
O2 0.042(13) 0.042(12) 0.023(13) -0.009(10) 0.009(14) -0.009(10)
O3 0.047(12) 0.027(11) 0.015(12) 0.002(12) -0.004(12) -0.004(12)
O4 0.018(9) 0.033(10) 0.013(8) -0.011(15) 0.010(7) 0.003(14)
O5 0.047(12) 0.039(12) 0.037(12) -0.010(16) -0.017(12) 0.011(16)
O6 0.076(14) 0.165(18) 0.070(19) -0.008(11) -0.035(16) 0.008(16)
OW1 0.087(19) 0.351(11) 0.087(14) 0.000 0.000 0.000
OW2 0.087(21) 0.087(21) 0.024(20) -0.006(17) 0.006(17) -0.033(29)
_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
As O4 1.676(6) 40_545 ?
As O4 1.676(6) 39 ?
As O4 1.676(6) . ?
As O4 1.676(6) 2_655 ?
V1 O1 1.620(5) . ?
V1 O4 1.884(6) 21 ?
V1 O4 1.884(6) . ?
V1 O5 2.116(6) 23_656 ?
V1 O5 2.116(6) 3_656 ?
V2 O2 1.600(8) . ?
V2 O5 1.913(9) 3_656 ?
V2 O5 1.913(9) 23_656 ?
V2 O5 1.913(9) 21 ?
V2 O5 1.913(9) . ?
V3 O3 1.706(9) . ?
V3 O5 1.834(9) . ?
V3 O5 1.834(9) 23_656 ?
V3 O4 1.921(9) 2_655 ?
V3 O4 1.921(9) 24_655 ?
O4 V3 1.921(9) 2_655 ?
O5 V1 2.116(6) 3_656 ?
O6 V2 2.461(6) 2_655 ?
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 As O4 110.6(5) 40_545 39 ?
O4 As O4 108.9(5) 40_545 . ?
O4 As O4 108.9(5) 39 . ?
O4 As O4 108.9(5) 40_545 2_655 ?
O4 As O4 108.9(5) 39 2_655 ?
O4 As O4 110.6(5) . 2_655 ?
O1 V1 O4 109.1(6) . 21 ?
O1 V1 O4 109.1(6) . . ?
O4 V1 O4 87.2(7) 21 . ?
O1 V1 O5 100.6(8) . 23_656 ?
O4 V1 O5 150.3(7) 21 23_656 ?
O4 V1 O5 85.9(9) . 23_656 ?
O1 V1 O5 100.5(6) . 3_656 ?
O4 V1 O5 85.9(10) 21 3_656 ?
O4 V1 O5 150.3(7) . 3_656 ?
O5 V1 O5 85.9(7) 23_656 3_656 ?
O2 V2 O5 106.4(9) . 3_656 ?
O2 V2 O5 106.4(9) . 23_656 ?
O5 V2 O5 96.6(10) 3_656 23_656 ?
O2 V2 O5 106.4(9) . 21 ?
O5 V2 O5 74.1(8) 3_656 21 ?
O5 V2 O5 147.2(8) 23_656 21 ?
O2 V2 O5 106.4(9) . . ?
O5 V2 O5 147.2(8) 3_656 . ?
O5 V2 O5 74.1(7) 23_656 . ?
O5 V2 O5 96.6(10) 21 . ?
O2 V2 O6 180.0 . . ?
O5 V2 O6 73.6(9) 3_656 . ?
O5 V2 O6 73.6(9) 23_656 . ?
O5 V2 O6 73.6(9) 21 . ?
O5 V2 O6 73.6(9) . . ?
O3 V3 O5 105.0(10) . . ?
O3 V3 O5 105.0(10) . 23_656 ?
O5 V3 O5 79.3(11) . 23_656 ?
O3 V3 O4 103.9(8) . 2_655 ?
O5 V3 O4 150.7(7) . 2_655 ?
O5 V3 O4 89.0(11) 23_656 2_655 ?
O3 V3 O4 103.9(8) . 24_655 ?
O5 V3 O4 89.0(11) . 24_655 ?
O5 V3 O4 150.8(7) 23_656 24_655 ?
O4 V3 O4 88.5(6) 2_655 24_655 ?
As O4 V3 128.5(6) . 2_655 ?
As O4 V1 129.5(5) . . ?
V3 O4 V1 82.1(7) 2_655 . ?
V3 O5 V2 103.0(11) . . ?
V3 O5 V1 142.1(5) . 3_656 ?
V2 O5 V1 88.7(5) . 3_656 ?
V2 O6 V2 180.0 2_655 . ?
_refine_diff_density_max 1.235
_refine_diff_density_min -2.490
_refine_diff_density_rms 0.474
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