 
data_Ag3(TiO)3(SeO3)4F2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Ag3 F O15 Se4 Ti3' 
_chemical_formula_weight          1042.15 
 
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' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ti'  'Ti'   0.2776   0.4457 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Se'  'Se'  -0.0929   2.2259 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ag'  'Ag'  -0.8971   1.1015 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal
_symmetry_space_group_name_H-M    P6(3)
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 
_cell_length_a                    12.8975(4) 
_cell_length_b                    12.8975(4) 
_cell_length_c                    5.2180(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      751.70(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     5830  
_cell_measurement_theta_min       3.6409 
_cell_measurement_theta_max       26.2701 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             colorless  
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.02 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     4.604 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              944 
_exptl_absorpt_coefficient_mu     15.123 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.73370 
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    ? 
 
_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_type   SuperNova 
_diffrn_measurement_method        SuperNova 
_diffrn_detector_area_resol_mean  10.3503 
_diffrn_reflns_number             11687 
_diffrn_reflns_av_R_equivalents   0.0500 
_diffrn_reflns_av_sigmaI/netI     0.0218 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -6 
_diffrn_reflns_limit_l_max        6 
_diffrn_reflns_theta_min          4.31 
_diffrn_reflns_theta_max          26.33 
_reflns_number_total              1025 
_reflns_number_gt                 1008 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0539P)²+14.1150P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0019(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.03(3) 
_refine_ls_number_reflns          1025 
_refine_ls_number_parameters      80 
_refine_ls_number_restraints      19 
_refine_ls_R_factor_all           0.0367 
_refine_ls_R_factor_gt            0.0360 
_refine_ls_wR_factor_ref          0.1005 
_refine_ls_wR_factor_gt           0.0999 
_refine_ls_goodness_of_fit_ref    1.078 
_refine_ls_restrained_S_all       1.076 
_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 
Ag1 Ag 0.19223(8) 0.25027(8) 0.6919(2) 0.0303(3) Uani 1 1 d . . . 
Ti1 Ti 0.39568(13) -0.05045(13) 0.6743(4) 0.0076(3) Uani 1 1 d . . . 
Se1 Se 0.44557(7) 0.22830(7) 0.6640(2) 0.0079(3) Uani 1 1 d . . . 
Se2 Se 0.3333 -0.3333 0.6205(3) 0.0132(4) Uani 1 3 d S . . 
F1 F 0.0000 0.0000 0.926(2) 0.0040(13) Uani 1 3 d SU . . 
O1 O 0.3892(8) 0.2334(7) 0.9542(13) 0.0138(15) Uani 1 1 d . . . 
O2 O 0.3706(7) 0.2748(6) 0.4658(13) 0.0113(14) Uani 1 1 d U . . 
O3 O 0.3600(6) 0.0769(6) 0.5976(13) 0.0107(15) Uani 1 1 d U . . 
O4 O 0.3975(6) -0.1980(6) 0.7680(14) 0.0134(15) Uani 1 1 d . . . 
O5 O 0.5235(6) 0.0418(7) 0.8617(14) 0.0109(14) Uani 1 1 d . . . 
 
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 
Ag1 0.0297(5) 0.0294(5) 0.0389(6) -0.0041(5) -0.0015(4) 0.0200(4) 
Ti1 0.0076(7) 0.0066(7) 0.0086(8) 0.0009(8) 0.0002(8) 0.0035(6) 
Se1 0.0091(4) 0.0078(4) 0.0073(4) 0.0003(4) 0.0001(4) 0.0046(3) 
Se2 0.0134(5) 0.0134(5) 0.0127(9) 0.000 0.000 0.0067(3) 
F1 0.0012(13) 0.0012(13) 0.010(2) 0.000 0.000 0.0006(7) 
O1 0.027(4) 0.008(3) 0.003(3) 0.001(3) 0.004(3) 0.006(3) 
O2 0.0114(17) 0.0113(17) 0.0111(17) 0.0005(10) -0.0003(10) 0.0056(11) 
O3 0.011(3) 0.006(3) 0.017(3) -0.001(2) -0.002(2) 0.006(2) 
O4 0.009(3) 0.012(3) 0.017(4) 0.001(3) 0.003(3) 0.003(3) 
O5 0.007(3) 0.012(3) 0.009(3) -0.004(3) 0.002(3) 0.002(3) 
 
_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 
Ag1 O1 2.411(7) 6_554 ? 
Ag1 O2 2.461(7) . ? 
Ag1 O3 2.490(7) 6 ? 
Ti1 O5 1.769(7) . ? 
Ti1 O5 1.909(8) 4_654 ? 
Ti1 O3 1.956(7) . ? 
Ti1 O4 1.976(8) . ? 
Ti1 O2 2.043(7) 5 ? 
Ti1 O1 2.169(7) 5_554 ? 
Se1 O1 1.695(7) . ? 
Se1 O2 1.716(7) . ? 
Se1 O3 1.731(7) . ? 
Se2 O4 1.697(7) 2_545 ? 
Se2 O4 1.697(7) 3_655 ? 
Se2 O4 1.697(7) . ? 
O1 Ti1 2.169(7) 6 ? 
O1 Ag1 2.411(7) 5 ? 
O2 Ti1 2.043(7) 6_554 ? 
O3 Ag1 2.490(7) 5_554 ? 
O5 Ti1 1.909(8) 4_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 
O1 Ag1 O2 100.1(2) 6_554 . ? 
O1 Ag1 O3 103.1(3) 6_554 6 ? 
O2 Ag1 O3 101.0(2) . 6 ? 
O5 Ti1 O5 97.76(15) . 4_654 ? 
O5 Ti1 O3 94.6(3) . . ? 
O5 Ti1 O3 97.3(3) 4_654 . ? 
O5 Ti1 O4 93.2(3) . . ? 
O5 Ti1 O4 89.9(3) 4_654 . ? 
O3 Ti1 O4 168.6(3) . . ? 
O5 Ti1 O2 95.9(3) . 5 ? 
O5 Ti1 O2 165.7(3) 4_654 5 ? 
O3 Ti1 O2 85.8(3) . 5 ? 
O4 Ti1 O2 85.1(3) . 5 ? 
O5 Ti1 O1 175.8(3) . 5_554 ? 
O5 Ti1 O1 84.9(3) 4_654 5_554 ? 
O3 Ti1 O1 81.9(3) . 5_554 ? 
O4 Ti1 O1 90.0(3) . 5_554 ? 
O2 Ti1 O1 81.7(3) 5 5_554 ? 
O1 Se1 O2 101.4(4) . . ? 
O1 Se1 O3 100.3(4) . . ? 
O2 Se1 O3 96.9(3) . . ? 
O4 Se2 O4 101.0(3) 2_545 3_655 ? 
O4 Se2 O4 101.0(3) 2_545 . ? 
O4 Se2 O4 101.0(3) 3_655 . ? 
Se1 O1 Ti1 124.5(4) . 6 ? 
Se1 O1 Ag1 123.7(4) . 5 ? 
Ti1 O1 Ag1 111.5(3) 6 5 ? 
Se1 O2 Ti1 125.3(4) . 6_554 ? 
Se1 O2 Ag1 108.7(3) . . ? 
Ti1 O2 Ag1 120.9(3) 6_554 . ? 
Se1 O3 Ti1 128.4(4) . . ? 
Se1 O3 Ag1 106.9(3) . 5_554 ? 
Ti1 O3 Ag1 116.9(3) . 5_554 ? 
Se2 O4 Ti1 130.1(4) . . ? 
Ti1 O5 Ti1 144.1(4) . 4_655 ? 
 
_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              26.33 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    2.979 
_refine_diff_density_min   -1.435 
_refine_diff_density_rms    0.279 

#===end
 
data_Ag2Zr(SeO3)2F2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          Ag2F2O6Se2Zr 
_chemical_formula_sum 
 'Ag2 F2 O6 Se2 Zr' 
_chemical_formula_weight          598.88 
 
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' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Se'  'Se'  -0.0929   2.2259 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zr'  'Zr'  -2.9673   0.5597 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ag'  'Ag'  -0.8971   1.1015 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Cmca 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y+1/2, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x, -y, -z' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, -y+1, z+1/2' 
 '-x+1/2, y+1, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x, y-1/2, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x, y, z' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, y, -z-1/2' 
 'x+1/2, -y, z-1/2' 
 '-x+1/2, y+1/2, z' 
 
_cell_length_a                    7.3640(5) 
_cell_length_b                    31.451(2) 
_cell_length_c                    6.2719(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1452.62(19) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     1906 
_cell_measurement_theta_min       3.3740 
_cell_measurement_theta_max       27.4239 
 
_exptl_crystal_description        brick
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.477 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2144 
_exptl_absorpt_coefficient_mu     16.802 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.21069 
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details    ? 
 
_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_type   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        SuperNova 
_diffrn_detector_area_resol_mean  10.3503 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5486 
_diffrn_reflns_av_R_equivalents   0.0476 
_diffrn_reflns_av_sigmaI/netI     0.0364 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -39 
_diffrn_reflns_limit_k_max        40 
_diffrn_reflns_limit_l_min        -7 
_diffrn_reflns_limit_l_max        7 
_diffrn_reflns_theta_min          3.50 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              895 
_reflns_number_gt                 758 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0127P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    no 
_refine_ls_hydrogen_treatment     no
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00035(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          895 
_refine_ls_number_parameters      71 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0335 
_refine_ls_R_factor_gt            0.0237 
_refine_ls_wR_factor_ref          0.0477 
_refine_ls_wR_factor_gt           0.0433 
_refine_ls_goodness_of_fit_ref    1.097 
_refine_ls_restrained_S_all       1.097 
_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 
Ag1 Ag 0.2500 0.26792(2) 0.2500 0.02599(18) Uani 1 2 d S . . 
Ag2 Ag 0.27953(8) 0.5000 0.0000 0.02626(19) Uani 1 2 d S . . 
Zr1 Zr 0.2500 0.38066(2) 0.2500 0.00790(17) Uani 1 2 d S . . 
Se1 Se 0.5000 0.31930(2) -0.13020(11) 0.01319(19) Uani 1 2 d S . . 
Se2 Se 0.0000 0.42475(2) -0.16232(11) 0.01103(18) Uani 1 2 d S . . 
F1 F 0.0000 0.35451(12) 0.1148(6) 0.0137(9) Uani 1 2 d S . . 
F2 F 0.5000 0.40696(12) 0.1221(6) 0.0136(9) Uani 1 2 d S . . 
O1 O 0.5000 0.26652(16) -0.0910(9) 0.0256(13) Uani 1 2 d S . . 
O2 O 0.3176(4) 0.33229(11) 0.0231(6) 0.0177(8) Uani 1 1 d . . . 
O3 O 0.1817(4) 0.42538(10) 0.0083(5) 0.0135(8) Uani 1 1 d . . . 
O4 O 0.0000 0.47570(15) -0.2324(7) 0.0161(11) Uani 1 2 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 
Ag1 0.0233(3) 0.0196(3) 0.0351(4) 0.000 0.0005(3) 0.000 
Ag2 0.0200(3) 0.0221(4) 0.0367(4) -0.0145(3) 0.000 0.000 
Zr1 0.0063(3) 0.0089(3) 0.0085(4) 0.000 -0.0002(2) 0.000 
Se1 0.0105(4) 0.0154(4) 0.0137(4) -0.0026(3) 0.000 0.000 
Se2 0.0098(3) 0.0121(4) 0.0112(4) 0.0014(3) 0.000 0.000 
F1 0.015(2) 0.011(2) 0.015(2) -0.0025(17) 0.000 0.000 
F2 0.010(2) 0.017(2) 0.013(2) 0.0021(17) 0.000 0.000 
O1 0.023(3) 0.015(3) 0.040(4) -0.008(3) 0.000 0.000 
O2 0.0083(17) 0.022(2) 0.023(2) -0.0099(16) 0.0028(14) -0.0013(15) 
O3 0.0121(17) 0.0147(19) 0.014(2) 0.0047(15) -0.0020(14) -0.0016(15) 
O4 0.017(3) 0.014(3) 0.017(3) 0.008(2) 0.000 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 
Ag1 O1 2.357(3) 13 ? 
Ag1 O1 2.357(3) 2_655 ? 
Ag1 O2 2.524(4) 7_545 ? 
Ag1 O2 2.524(4) . ? 
Ag1 O1 2.822(4) . ? 
Ag1 Ag1 3.3324(5) 13 ? 
Ag1 Ag1 3.3324(5) 13_556 ? 
Ag1 F1 3.395(3) . ? 
Ag2 O3 2.456(3) 4_565 ? 
Ag2 O3 2.456(3) . ? 
Ag2 O4 2.457(3) 14 ? 
Ag2 O4 2.457(3) 6 ? 
Ag2 O4 2.636(3) . ? 
Ag2 Ag2 3.1660(3) 6_554 ? 
Ag2 Ag2 3.1660(3) 6 ? 
Ag2 Ag2 3.2471(12) 9_665 ? 
Ag2 F2 3.433(3) . ? 
Zr1 O3 2.128(3) 7_545 ? 
Zr1 O3 2.128(3) . ? 
Zr1 O2 2.142(3) . ? 
Zr1 O2 2.142(3) 7_545 ? 
Zr1 F2 2.172(2) . ? 
Zr1 F2 2.172(2) 14_456 ? 
Zr1 F1 2.188(2) . ? 
Zr1 F1 2.188(2) 14_556 ? 
Se1 O1 1.678(5) . ? 
Se1 O2 1.702(3) 12_655 ? 
Se1 O2 1.702(3) . ? 
Se2 O4 1.662(5) . ? 
Se2 O3 1.713(3) . ? 
Se2 O3 1.713(3) 12 ? 
F1 Zr1 2.188(2) 14_456 ? 
F2 Zr1 2.172(2) 14_556 ? 
O1 Ag1 2.357(3) 13 ? 
O1 Ag1 2.357(3) 2_654 ? 
O4 Ag2 2.457(3) 14_455 ? 
O4 Ag2 2.457(3) 6_554 ? 
 
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 Ag1 O1 125.3(2) 13 2_655 ? 
O1 Ag1 O2 116.95(12) 13 7_545 ? 
O1 Ag1 O2 106.50(16) 2_655 7_545 ? 
O1 Ag1 O2 106.50(16) 13 . ? 
O1 Ag1 O2 116.95(12) 2_655 . ? 
O2 Ag1 O2 73.34(15) 7_545 . ? 
O1 Ag1 O1 100.47(7) 13 . ? 
O1 Ag1 O1 78.70(7) 2_655 . ? 
O2 Ag1 O1 124.63(13) 7_545 . ? 
O2 Ag1 O1 57.10(13) . . ? 
O1 Ag1 Ag1 56.39(12) 13 13 ? 
O1 Ag1 Ag1 104.05(14) 2_655 13 ? 
O2 Ag1 Ag1 143.30(8) 7_545 13 ? 
O2 Ag1 Ag1 74.98(8) . 13 ? 
O1 Ag1 Ag1 44.08(8) . 13 ? 
O1 Ag1 Ag1 104.05(14) 13 13_556 ? 
O1 Ag1 Ag1 56.39(12) 2_655 13_556 ? 
O2 Ag1 Ag1 74.98(8) 7_545 13_556 ? 
O2 Ag1 Ag1 143.30(8) . 13_556 ? 
O1 Ag1 Ag1 135.06(9) . 13_556 ? 
Ag1 Ag1 Ag1 140.46(4) 13 13_556 ? 
O1 Ag1 F1 80.76(12) 13 . ? 
O1 Ag1 F1 153.87(13) 2_655 . ? 
O2 Ag1 F1 52.45(10) 7_545 . ? 
O2 Ag1 F1 47.36(9) . . ? 
O1 Ag1 F1 100.19(11) . . ? 
Ag1 Ag1 F1 92.08(6) 13 . ? 
Ag1 Ag1 F1 120.43(6) 13_556 . ? 
O3 Ag2 O3 145.87(15) 4_565 . ? 
O3 Ag2 O4 118.47(14) 4_565 14 ? 
O3 Ag2 O4 84.90(13) . 14 ? 
O3 Ag2 O4 84.90(13) 4_565 6 ? 
O3 Ag2 O4 118.47(14) . 6 ? 
O4 Ag2 O4 97.28(14) 14 6 ? 
O3 Ag2 O4 92.07(13) 4_565 . ? 
O3 Ag2 O4 60.36(13) . . ? 
O4 Ag2 O4 92.76(7) 14 . ? 
O4 Ag2 O4 169.77(16) 6 . ? 
O3 Ag2 Ag2 86.48(8) 4_565 6_554 ? 
O3 Ag2 Ag2 88.90(8) . 6_554 ? 
O4 Ag2 Ag2 54.14(9) 14 6_554 ? 
O4 Ag2 Ag2 140.12(10) 6 6_554 ? 
O4 Ag2 Ag2 49.07(9) . 6_554 ? 
O3 Ag2 Ag2 88.90(8) 4_565 6 ? 
O3 Ag2 Ag2 86.48(8) . 6 ? 
O4 Ag2 Ag2 140.12(10) 14 6 ? 
O4 Ag2 Ag2 54.14(9) 6 6 ? 
O4 Ag2 Ag2 116.14(9) . 6 ? 
Ag2 Ag2 Ag2 164.21(4) 6_554 6 ? 
O3 Ag2 Ag2 107.06(8) 4_565 9_665 ? 
O3 Ag2 Ag2 107.06(8) . 9_665 ? 
O4 Ag2 Ag2 48.64(7) 14 9_665 ? 
O4 Ag2 Ag2 48.64(7) 6 9_665 ? 
O4 Ag2 Ag2 141.35(8) . 9_665 ? 
Ag2 Ag2 Ag2 97.90(2) 6_554 9_665 ? 
Ag2 Ag2 Ag2 97.90(2) 6 9_665 ? 
O3 Ag2 F2 163.37(9) 4_565 . ? 
O3 Ag2 F2 47.11(8) . . ? 
O4 Ag2 F2 64.83(13) 14 . ? 
O4 Ag2 F2 78.48(12) 6 . ? 
O4 Ag2 F2 104.22(11) . . ? 
Ag2 Ag2 F2 106.61(6) 6_554 . ? 
Ag2 Ag2 F2 81.03(6) 6 . ? 
Ag2 Ag2 F2 61.78(3) 9_665 . ? 
O3 Zr1 O3 97.26(18) 7_545 . ? 
O3 Zr1 O2 152.60(13) 7_545 . ? 
O3 Zr1 O2 92.93(14) . . ? 
O3 Zr1 O2 92.93(14) 7_545 7_545 ? 
O3 Zr1 O2 152.60(13) . 7_545 ? 
O2 Zr1 O2 89.5(2) . 7_545 ? 
O3 Zr1 F2 79.11(14) 7_545 . ? 
O3 Zr1 F2 71.68(12) . . ? 
O2 Zr1 F2 80.11(14) . . ? 
O2 Zr1 F2 135.47(13) 7_545 . ? 
O3 Zr1 F2 71.68(12) 7_545 14_456 ? 
O3 Zr1 F2 79.11(14) . 14_456 ? 
O2 Zr1 F2 135.47(13) . 14_456 ? 
O2 Zr1 F2 80.11(14) 7_545 14_456 ? 
F2 Zr1 F2 135.23(19) . 14_456 ? 
O3 Zr1 F1 136.35(12) 7_545 . ? 
O3 Zr1 F1 76.90(13) . . ? 
O2 Zr1 F1 70.78(12) . . ? 
O2 Zr1 F1 78.17(14) 7_545 . ? 
F2 Zr1 F1 135.51(13) . . ? 
F2 Zr1 F1 64.72(12) 14_456 . ? 
O3 Zr1 F1 76.90(13) 7_545 14_556 ? 
O3 Zr1 F1 136.35(12) . 14_556 ? 
O2 Zr1 F1 78.17(14) . 14_556 ? 
O2 Zr1 F1 70.78(12) 7_545 14_556 ? 
F2 Zr1 F1 64.72(12) . 14_556 ? 
F2 Zr1 F1 135.51(13) 14_456 14_556 ? 
F1 Zr1 F1 135.82(18) . 14_556 ? 
O1 Se1 O2 98.90(17) . 12_655 ? 
O1 Se1 O2 98.90(17) . . ? 
O2 Se1 O2 104.2(2) 12_655 . ? 
O4 Se2 O3 98.86(15) . . ? 
O4 Se2 O3 98.86(15) . 12 ? 
O3 Se2 O3 102.7(2) . 12 ? 
Zr1 F1 Zr1 114.62(16) . 14_456 ? 
Zr1 F1 Ag1 75.43(7) . . ? 
Zr1 F1 Ag1 131.39(14) 14_456 . ? 
Zr1 F2 Zr1 115.92(17) . 14_556 ? 
Zr1 F2 Ag2 90.35(6) . . ? 
Zr1 F2 Ag2 143.89(13) 14_556 . ? 
Se1 O1 Ag1 113.11(19) . 13 ? 
Se1 O1 Ag1 113.11(19) . 2_654 ? 
Ag1 O1 Ag1 102.7(2) 13 2_654 ? 
Se1 O1 Ag1 95.49(18) . . ? 
Ag1 O1 Ag1 79.53(7) 13 . ? 
Ag1 O1 Ag1 146.8(2) 2_654 . ? 
Se1 O2 Zr1 136.84(19) . . ? 
Se1 O2 Ag1 106.35(16) . . ? 
Zr1 O2 Ag1 98.59(13) . . ? 
Se2 O3 Zr1 128.45(17) . . ? 
Se2 O3 Ag2 103.12(14) . . ? 
Zr1 O3 Ag2 125.27(14) . . ? 
Se2 O4 Ag2 118.73(18) . 14_455 ? 
Se2 O4 Ag2 118.73(18) . 6_554 ? 
Ag2 O4 Ag2 82.72(14) 14_455 6_554 ? 
Se2 O4 Ag2 97.66(14) . . ? 
Ag2 O4 Ag2 143.5(2) 14_455 . ? 
Ag2 O4 Ag2 76.79(5) 6_554 . ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    1.047 
_refine_diff_density_min   -0.940 
_refine_diff_density_rms    0.212 

#===end


 
data_AgNbO(SeO3)2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Ag Nb O7 Se2' 
_chemical_formula_weight          470.70 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Ag'  'Ag'  -0.8971   1.1015 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Nb'  'Nb'  -2.0727   0.6215 
 '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' 
 'Se'  'Se'  -0.0929   2.2259 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Cmcm 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, 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' 
 '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, y, z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, y+1/2, -z-1/2' 
 '-x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    10.813(5) 
_cell_length_b                    7.792(4) 
_cell_length_c                    7.363(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      620.4(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     3201 
_cell_measurement_theta_min       2.6142 
_cell_measurement_theta_max       27.4391 
 
_exptl_crystal_description        brick 
_exptl_crystal_colour             Colorless 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.040 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              848 
_exptl_absorpt_coefficient_mu     16.724 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.7178
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    ? 
 
_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_type   SuperNova
_diffrn_measurement_method        SuperNova 
_diffrn_detector_area_resol_mean  28.5714 
_diffrn_reflns_number             2488 
_diffrn_reflns_av_R_equivalents   0.0417 
_diffrn_reflns_av_sigmaI/netI     0.0246 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          27.44 
_reflns_number_total              399 
_reflns_number_gt                 393 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0299P)²+7.1312P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none  
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0015(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          399 
_refine_ls_number_parameters      35 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0301 
_refine_ls_R_factor_gt            0.0294 
_refine_ls_wR_factor_ref          0.0726 
_refine_ls_wR_factor_gt           0.0723 
_refine_ls_goodness_of_fit_ref    1.185 
_refine_ls_restrained_S_all       1.247 
_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 
Ag1 Ag 0.0000 0.5000 0.0000 0.0335(4) Uani 1 4 d S . . 
Nb1 Nb 0.0000 0.0000 0.5000 0.0235(3) Uani 1 4 d SU . . 
Se1 Se -0.20814(7) 0.26075(8) 0.2500 0.0106(3) Uani 1 2 d S . . 
O1 O -0.1468(5) 0.4553(6) 0.2500 0.0217(12) Uani 1 2 d S . . 
O2 O -0.1297(3) 0.1683(5) 0.4320(5) 0.0177(8) Uani 1 1 d . . . 
O3 O 0.0000 0.0873(9) 0.7500 0.0164(14) Uani 1 4 d SU . . 
 
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 
Ag1 0.0260(6) 0.0470(7) 0.0275(6) 0.0217(4) 0.000 0.000 
Nb1 0.0088(5) 0.0202(5) 0.0416(7) 0.0216(4) 0.000 0.000 
Se1 0.0119(5) 0.0107(4) 0.0092(4) 0.000 0.000 0.0037(2) 
O1 0.027(3) 0.014(2) 0.025(3) 0.000 0.000 0.001(2) 
O2 0.0216(19) 0.0216(18) 0.0100(18) 0.0011(15) 0.0003(14) 0.0113(15) 
O3 0.009(3) 0.011(3) 0.029(3) 0.000 0.000 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 
Ag1 O1 2.455(4) . ? 
Ag1 O1 2.455(4) 11 ? 
Ag1 O1 2.455(4) 3_565 ? 
Ag1 O1 2.455(4) 9_565 ? 
Nb1 O3 1.963(3) 9_556 ? 
Nb1 O3 1.963(3) . ? 
Nb1 O2 1.984(3) 11 ? 
Nb1 O2 1.984(3) 3_556 ? 
Nb1 O2 1.984(3) 9_556 ? 
Nb1 O2 1.984(3) . ? 
Se1 O1 1.655(5) . ? 
Se1 O2 1.742(3) . ? 
Se1 O2 1.742(3) 10_556 ? 
O1 Ag1 2.455(4) 2_565 ? 
O3 Nb1 1.963(3) 2 ? 
 
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 Ag1 O1 80.5(2) . 11 ? 
O1 Ag1 O1 99.5(2) . 3_565 ? 
O1 Ag1 O1 180.0 11 3_565 ? 
O1 Ag1 O1 180.0 . 9_565 ? 
O1 Ag1 O1 99.5(2) 11 9_565 ? 
O1 Ag1 O1 80.5(2) 3_565 9_565 ? 
O3 Nb1 O3 180.0 9_556 . ? 
O3 Nb1 O2 89.58(17) 9_556 11 ? 
O3 Nb1 O2 90.42(17) . 11 ? 
O3 Nb1 O2 90.42(17) 9_556 3_556 ? 
O3 Nb1 O2 89.58(17) . 3_556 ? 
O2 Nb1 O2 180.0(2) 11 3_556 ? 
O3 Nb1 O2 90.42(17) 9_556 9_556 ? 
O3 Nb1 O2 89.58(17) . 9_556 ? 
O2 Nb1 O2 90.0(2) 11 9_556 ? 
O2 Nb1 O2 90.0(2) 3_556 9_556 ? 
O3 Nb1 O2 89.58(17) 9_556 . ? 
O3 Nb1 O2 90.42(17) . . ? 
O2 Nb1 O2 90.0(2) 11 . ? 
O2 Nb1 O2 90.0(2) 3_556 . ? 
O2 Nb1 O2 180.00(14) 9_556 . ? 
O1 Se1 O2 100.59(18) . . ? 
O1 Se1 O2 100.59(18) . 10_556 ? 
O2 Se1 O2 100.6(2) . 10_556 ? 
Se1 O1 Ag1 112.89(17) . 2_565 ? 
Se1 O1 Ag1 112.89(17) . . ? 
Ag1 O1 Ag1 97.1(2) 2_565 . ? 
Se1 O2 Nb1 144.2(2) . . ? 
Nb1 O3 Nb1 139.4(4) . 2 ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              27.44 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.891 
_refine_diff_density_min   -1.668 
_refine_diff_density_rms    0.188 


#===end

 
data_AgTaO(SeO3)2
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Ag O7 Se2 Ta' 
_chemical_formula_weight          558.74 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Ag'  'Ag'  -0.8971   1.1015 
 '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' 
 'Se'  'Se'  -0.0929   2.2259 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ta'  'Ta'  -0.7052   6.5227 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Cmcm 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, 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' 
 '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, y, z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, y+1/2, -z-1/2' 
 '-x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    10.7921(11) 
_cell_length_b                    7.8283(7) 
_cell_length_c                    7.2717(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      614.34(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     1009  
_cell_measurement_theta_min       3.3715 
_cell_measurement_theta_max       26.3070 
 
_exptl_crystal_description       brick 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     6.041 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              976 
_exptl_absorpt_coefficient_mu     32.821 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.029 
_exptl_absorpt_correction_T_max   0.161 
_exptl_absorpt_process_details    ? 
 
_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_type   SuperNova 
_diffrn_measurement_method        SuperNova 
_diffrn_detector_area_resol_mean  10.3503 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             1996 
_diffrn_reflns_av_R_equivalents   0.0595 
_diffrn_reflns_av_sigmaI/netI     0.0391 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          3.78 
_diffrn_reflns_theta_max          26.33 
_reflns_number_total              361 
_reflns_number_gt                 323 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0336P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    no 
_refine_ls_hydrogen_treatment     no 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          361 
_refine_ls_number_parameters      34 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0340 
_refine_ls_R_factor_gt            0.0292 
_refine_ls_wR_factor_ref          0.0727 
_refine_ls_wR_factor_gt           0.0689 
_refine_ls_goodness_of_fit_ref    1.132 
_refine_ls_restrained_S_all       1.122 
_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 
Ag1 Ag 0.0000 0.5000 0.0000 0.0258(4) Uani 1 4 d S . . 
NB1 Ta 0.0000 0.0000 0.5000 0.0060(3) Uani 1 4 d S . . 
Se1 Se -0.20927(13) 0.25986(12) 0.2500 0.0078(3) Uani 1 2 d S . . 
O1 O -0.1486(8) 0.4524(10) 0.2500 0.0182(19) Uani 1 2 d S . . 
O2 O -0.1308(5) 0.1686(8) 0.4341(8) 0.0147(12) Uani 1 1 d . . . 
O3 O 0.0000 0.0832(14) 0.7500 0.010(2) Uani 1 4 d SU . . 
 
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 
Ag1 0.0243(9) 0.0338(10) 0.0192(8) 0.0135(6) 0.000 0.000 
NB1 0.0089(4) 0.0056(4) 0.0036(4) 0.0017(2) 0.000 0.000 
Se1 0.0113(7) 0.0071(6) 0.0048(6) 0.000 0.000 0.0036(4) 
O1 0.033(5) 0.007(4) 0.015(4) 0.000 0.000 -0.008(4) 
O2 0.020(3) 0.015(3) 0.009(3) 0.002(3) 0.002(3) 0.011(3) 
O3 0.011(3) 0.011(3) 0.009(3) 0.000 0.000 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 
Ag1 O1 2.453(6) 3_565 ? 
Ag1 O1 2.453(6) 11 ? 
Ag1 O1 2.453(6) . ? 
Ag1 O1 2.453(6) 9_565 ? 
NB1 O3 1.931(4) 9_556 ? 
NB1 O3 1.931(4) . ? 
NB1 O2 1.992(5) 3_556 ? 
NB1 O2 1.992(5) . ? 
NB1 O2 1.992(5) 11 ? 
NB1 O2 1.992(5) 9_556 ? 
Se1 O1 1.643(8) . ? 
Se1 O2 1.737(6) . ? 
Se1 O2 1.737(6) 10_556 ? 
O1 Ag1 2.453(6) 2_565 ? 
O3 NB1 1.931(4) 2 ? 
 
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 Ag1 O1 180.0(4) 3_565 11 ? 
O1 Ag1 O1 98.3(3) 3_565 . ? 
O1 Ag1 O1 81.7(3) 11 . ? 
O1 Ag1 O1 81.7(3) 3_565 9_565 ? 
O1 Ag1 O1 98.3(3) 11 9_565 ? 
O1 Ag1 O1 180.0(4) . 9_565 ? 
O3 NB1 O3 180.000(1) 9_556 . ? 
O3 NB1 O2 90.2(3) 9_556 3_556 ? 
O3 NB1 O2 89.8(3) . 3_556 ? 
O3 NB1 O2 89.8(3) 9_556 . ? 
O3 NB1 O2 90.2(3) . . ? 
O2 NB1 O2 89.7(3) 3_556 . ? 
O3 NB1 O2 89.8(3) 9_556 11 ? 
O3 NB1 O2 90.2(3) . 11 ? 
O2 NB1 O2 180.0 3_556 11 ? 
O2 NB1 O2 90.3(3) . 11 ? 
O3 NB1 O2 90.2(3) 9_556 9_556 ? 
O3 NB1 O2 89.8(3) . 9_556 ? 
O2 NB1 O2 90.3(3) 3_556 9_556 ? 
O2 NB1 O2 180.0(3) . 9_556 ? 
O2 NB1 O2 89.7(3) 11 9_556 ? 
O1 Se1 O2 100.5(3) . . ? 
O1 Se1 O2 100.5(3) . 10_556 ? 
O2 Se1 O2 100.8(4) . 10_556 ? 
Se1 O1 Ag1 113.6(3) . 2_565 ? 
Se1 O1 Ag1 113.6(3) . . ? 
Ag1 O1 Ag1 95.7(3) 2_565 . ? 
Se1 O2 NB1 143.5(3) . . ? 
NB1 O3 NB1 140.6(6) . 2 ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              26.33 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    1.830 
_refine_diff_density_min   -3.224 
_refine_diff_density_rms    0.444 


#===end