 
data_shelx 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'O14 P2 Pb2 Te2 Zn3' 
_chemical_formula_weight          1151.63 
 
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' 
 'P'  'P'   0.1023   0.0942 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Te'  'Te'  -0.5308   1.6751 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pb'  'Pb'  -3.3944  10.1111 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    5.2722(7) 
_cell_length_b                    7.9432(10) 
_cell_length_c                    15.213(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.058(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      637.09(15) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     572(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        Prism 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     6.003 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1000 
_exptl_absorpt_coefficient_mu     36.722 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       572(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   'Rigaku' 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4190 
_diffrn_reflns_av_R_equivalents   0.0486 
_diffrn_reflns_av_sigmaI/netI     0.0505 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        6 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.68 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              1446 
_reflns_number_gt                 1339 
_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)+(0.0344P)²+14.6023P] 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        0.0076(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1446 
_refine_ls_number_parameters      107 
_refine_ls_number_restraints      33 
_refine_ls_R_factor_all           0.0407 
_refine_ls_R_factor_gt            0.0368 
_refine_ls_wR_factor_ref          0.0850 
_refine_ls_wR_factor_gt           0.0823 
_refine_ls_goodness_of_fit_ref    1.037 
_refine_ls_restrained_S_all       1.166 
_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 
Pb1 Pb 0.50373(8) 0.44021(6) 0.80153(3) 0.0123(2) Uani 1 1 d U . . 
Te1 Te 0.51682(13) 0.22237(9) 0.01167(5) 0.0077(2) Uani 1 1 d . . . 
Zn1 Zn 0.9904(2) 0.10971(17) 0.88514(9) 0.0085(3) Uani 1 1 d U . . 
Zn2 Zn 0.0000 0.0000 0.5000 0.0308(6) Uani 1 2 d SU . . 
P1 P 0.9641(5) 0.2379(4) 0.69198(19) 0.0073(5) Uani 1 1 d U . . 
O1 O 0.8143(14) 0.1969(11) 0.7781(5) 0.0116(12) Uani 1 1 d U . . 
O2 O 0.2479(15) 0.2481(12) 0.7105(6) 0.0163(18) Uani 1 1 d U . . 
O3 O 0.9063(17) 0.0991(12) 0.6257(6) 0.0194(19) Uani 1 1 d U . . 
O4 O 0.1491(16) -0.0942(12) 0.8398(6) 0.0182(19) Uani 1 1 d U . . 
O5 O 0.7082(17) 0.3897(12) 0.9498(6) 0.0173(17) Uani 1 1 d U . . 
O6 O 0.7057(16) 0.0481(10) 0.9600(6) 0.0150(17) Uani 1 1 d U . . 
O7 O 0.2520(19) 0.2599(13) 0.9294(8) 0.029(2) Uani 1 1 d U . . 
 
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 
Pb1 0.0106(3) 0.0140(3) 0.0122(3) -0.00221(18) -0.00233(17) 0.00237(16) 
Te1 0.0035(3) 0.0122(4) 0.0075(4) -0.0005(3) -0.0009(3) -0.0007(3) 
Zn1 0.0043(6) 0.0128(7) 0.0082(6) -0.0008(5) -0.0001(4) -0.0020(4) 
Zn2 0.0219(11) 0.0470(13) 0.0234(11) -0.0203(10) -0.0144(9) 0.0250(10) 
P1 0.0044(11) 0.0099(14) 0.0076(11) -0.0005(10) -0.0022(9) -0.0026(9) 
O1 0.002(3) 0.021(4) 0.0109(18) 0.001(2) 0.0006(13) 0.003(2) 
O2 0.004(3) 0.027(4) 0.017(4) -0.006(3) -0.005(3) 0.002(3) 
O3 0.014(4) 0.023(4) 0.021(4) -0.016(3) 0.000(3) 0.000(4) 
O4 0.011(4) 0.018(4) 0.026(5) -0.010(4) 0.003(3) 0.000(3) 
O5 0.021(5) 0.026(5) 0.005(2) 0.000(2) 0.000(2) -0.015(4) 
O6 0.015(4) 0.012(4) 0.018(3) 0.002(3) 0.011(3) 0.001(3) 
O7 0.023(5) 0.023(5) 0.043(6) 0.012(4) -0.026(4) -0.006(4) 
 
_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 
Pb1 O2 2.461(8) . ? 
Pb1 O5 2.532(9) . ? 
Pb1 O1 2.558(8) . ? 
Pb1 O3 2.738(10) 2_656 ? 
Te1 O6 1.878(8) 1_554 ? 
Te1 O7 1.898(9) 1_554 ? 
Te1 O5 1.916(9) 1_554 ? 
Te1 O6 2.485(8) 3_656 ? 
Zn1 O7 1.944(10) 1_655 ? 
Zn1 O4 1.949(9) 1_655 ? 
Zn1 O6 1.948(9) . ? 
Zn1 O1 1.997(8) . ? 
Zn2 O5 1.927(8) 2_646 ? 
Zn2 O5 1.927(8) 4_465 ? 
Zn2 O3 2.127(9) 3_656 ? 
Zn2 O3 2.127(9) 1_455 ? 
P1 O3 1.525(9) . ? 
P1 O2 1.525(8) 1_655 ? 
P1 O4 1.539(9) 2_656 ? 
P1 O1 1.565(9) . ? 
O2 P1 1.525(8) 1_455 ? 
O3 Zn2 2.127(9) 1_655 ? 
O3 Pb1 2.738(9) 2_646 ? 
O4 P1 1.539(9) 2_646 ? 
O4 Zn1 1.949(9) 1_455 ? 
O5 Te1 1.916(9) 1_556 ? 
O5 Zn2 1.927(8) 2_656 ? 
O6 Te1 1.878(8) 1_556 ? 
O6 Te1 2.485(8) 3_656 ? 
O7 Te1 1.898(9) 1_556 ? 
O7 Zn1 1.944(9) 1_455 ? 
 
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 
O2 Pb1 O5 129.5(3) . . ? 
O2 Pb1 O1 78.7(3) . . ? 
O5 Pb1 O1 74.5(3) . . ? 
O2 Pb1 O3 94.6(3) . 2_656 ? 
O5 Pb1 O3 92.8(3) . 2_656 ? 
O1 Pb1 O3 155.6(3) . 2_656 ? 
O6 Te1 O7 103.3(5) 1_554 1_554 ? 
O6 Te1 O5 91.5(4) 1_554 1_554 ? 
O7 Te1 O5 87.4(4) 1_554 1_554 ? 
O6 Te1 O6 71.7(4) 1_554 3_656 ? 
O7 Te1 O6 84.4(4) 1_554 3_656 ? 
O5 Te1 O6 159.0(3) 1_554 3_656 ? 
O7 Zn1 O4 109.1(4) 1_655 1_655 ? 
O7 Zn1 O6 119.9(5) 1_655 . ? 
O4 Zn1 O6 109.2(4) 1_655 . ? 
O7 Zn1 O1 113.5(4) 1_655 . ? 
O4 Zn1 O1 101.5(4) 1_655 . ? 
O6 Zn1 O1 101.9(4) . . ? 
O5 Zn2 O5 180.0(5) 2_646 4_465 ? 
O5 Zn2 O3 90.1(4) 2_646 3_656 ? 
O5 Zn2 O3 89.9(4) 4_465 3_656 ? 
O5 Zn2 O3 89.9(4) 2_646 1_455 ? 
O5 Zn2 O3 90.1(4) 4_465 1_455 ? 
O3 Zn2 O3 180.0(2) 3_656 1_455 ? 
O3 P1 O2 110.9(5) . 1_655 ? 
O3 P1 O4 110.0(6) . 2_656 ? 
O2 P1 O4 113.1(5) 1_655 2_656 ? 
O3 P1 O1 107.6(5) . . ? 
O2 P1 O1 110.6(5) 1_655 . ? 
O4 P1 O1 104.3(5) 2_656 . ? 
P1 O1 Zn1 121.4(4) . . ? 
P1 O1 Pb1 106.5(4) . . ? 
Zn1 O1 Pb1 116.5(4) . . ? 
P1 O2 Pb1 132.4(5) 1_455 . ? 
P1 O3 Zn2 144.7(6) . 1_655 ? 
P1 O3 Pb1 102.9(5) . 2_646 ? 
Zn2 O3 Pb1 112.2(4) 1_655 2_646 ? 
P1 O4 Zn1 131.7(5) 2_646 1_455 ? 
Te1 O5 Zn2 122.8(5) 1_556 2_656 ? 
Te1 O5 Pb1 108.9(4) 1_556 . ? 
Zn2 O5 Pb1 128.3(4) 2_656 . ? 
Te1 O6 Zn1 117.9(4) 1_556 . ? 
Te1 O6 Te1 108.3(4) 1_556 3_656 ? 
Zn1 O6 Te1 133.1(4) . 3_656 ? 
Te1 O7 Zn1 130.8(5) 1_556 1_455 ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    4.734 
_refine_diff_density_min   -3.898 
_refine_diff_density_rms    0.458 
