 
data_plumbotell_c
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         'alpha lead tellurite'
_chemical_name_common             'plumbotellurite'
_chemical_melting_point           ?
_chemical_formula_moiety          'O9 Pb3 Te3'
_chemical_formula_sum
 'O4.50 Pb1.50 Te1.50' 
_chemical_formula_weight          574.18

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'
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 2/c'
_space_group_name_Hall            '-C 2yc'
 
_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+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+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    26.442(5)
_cell_length_b                    4.6010(9)
_cell_length_c                    17.890(4)
_cell_angle_alpha                 90
_cell_angle_beta                  107.01(3)
_cell_angle_gamma                 90
_cell_volume                      2081.3(8)
_cell_formula_units_Z             16
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     438
_cell_measurement_theta_min       2.27
_cell_measurement_theta_max       20
 
_exptl_crystal_description        'clear fragment'
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     7.330          
_exptl_crystal_F_000              3792
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.050
_exptl_crystal_size_mid           0.020
_exptl_crystal_size_min           0.020
_exptl_absorpt_coefficient_mu     56.686
_shelx_estimated_absorpt_T_min    0.164
_shelx_estimated_absorpt_T_max    0.397
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.2989
_exptl_absorpt_correction_T_max   0.4346
_exptl_absorpt_process_details    'SADABS (Bruker, 2001)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            'synchrotron'
_diffrn_source                    'synchrotron'
_diffrn_measurement_device_type   'Dectris EigerX 16M'
_diffrn_measurement_method        'φ scan'
_diffrn_detector_area_resol_mean  49.972
_diffrn_reflns_number             18440
_diffrn_reflns_av_unetI/netI      0.0184
_diffrn_reflns_av_R_equivalents   0.0292
_diffrn_reflns_limit_h_min        -36
_diffrn_reflns_limit_h_max        36
_diffrn_reflns_limit_k_min        -5
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          1.611
_diffrn_reflns_theta_max          32.347
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.823
_diffrn_measured_fraction_theta_full  0.981
_diffrn_reflns_Laue_measured_fraction_max    0.823
_diffrn_reflns_Laue_measured_fraction_full   0.981
_diffrn_reflns_point_group_measured_fraction_max   0.823
_diffrn_reflns_point_group_measured_fraction_full  0.981
_reflns_number_total              3060
_reflns_number_gt                 2967
_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        'local program'
_computing_cell_refinement        'XDS (Kabsch, 2010)'
_computing_data_reduction         'XPREP (Bruker, 2001)'
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0324P)²+15.9897P] 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          3060
_refine_ls_number_parameters      136
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0205
_refine_ls_R_factor_gt            0.0197
_refine_ls_wR_factor_ref          0.0540
_refine_ls_wR_factor_gt           0.0531
_refine_ls_goodness_of_fit_ref    1.082
_refine_ls_restrained_S_all       1.082
_refine_ls_shift/su_max           0.003
_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
Pb01 Pb 0.56660(2) -0.22260(4) 0.54352(2) 0.01293(5) Uani 1 1 d . . . . .
Pb02 Pb 0.31633(2) 1.20984(4) 0.26343(2) 0.01283(5) Uani 1 1 d . . . . .
Pb03 Pb 0.33788(2) 0.24946(4) 0.58579(2) 0.01374(6) Uani 1 1 d . . . . .
Te01 Te 0.29313(2) 0.69347(7) 0.40713(2) 0.01197(7) Uani 1 1 d . . . . .
Te02 Te 0.43091(2) 0.25348(6) 0.79272(2) 0.01123(7) Uani 1 1 d . . . . .
Te03 Te 0.45271(2) -0.22836(6) 0.63296(2) 0.01132(7) Uani 1 1 d . . . . .
O01 O 0.43458(14) 0.6542(9) 0.8081(2) 0.0185(7) Uani 1 1 d . . . . .
O02 O 0.36407(14) 0.2283(8) 0.7179(2) 0.0158(7) Uani 1 1 d . . . . .
O03 O 0.31485(17) 0.3099(8) 0.4000(2) 0.0199(7) Uani 1 1 d . . . . .
O04 O 0.47973(13) -0.1756(8) 0.5473(2) 0.0159(6) Uani 1 1 d . . . . .
O05 O 0.27876(14) 0.7806(7) 0.2999(2) 0.0143(6) Uani 1 1 d . . . . .
O06 O 0.38227(13) -0.1568(8) 0.5742(2) 0.0177(7) Uani 1 1 d . . . . .
O07 O 0.44481(15) -0.6297(8) 0.6301(2) 0.0199(7) Uani 1 1 d . . . . .
O08 O 0.40418(15) 0.1735(8) 0.8769(2) 0.0172(7) Uani 1 1 d . . . . .
O09 O 0.22164(13) 0.6288(9) 0.3988(2) 0.0212(7) Uani 1 1 d . . . . .
 
 
_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
Pb01 O08 2.303(4) 2_656 ?
Pb01 O04 2.328(3) . ?
Pb01 O04 2.517(4) 5_656 ?
Pb01 O01 2.724(4) 2_646 ?
Pb02 O05 2.386(3) . ?
Pb02 O05 2.459(4) 4 ?
Pb02 O03 2.498(4) 1_565 ?
Pb02 O02 2.631(4) 6_565 ?
Pb03 O06 2.249(4) . ?
Pb03 O02 2.263(4) . ?
Pb03 O09 2.416(4) 7_556 ?
Te01 O03 1.872(4) . ?
Te01 O09 1.876(3) . ?
Te01 O05 1.886(4) . ?
Te02 O01 1.863(4) . ?
Te02 O08 1.878(3) . ?
Te02 O02 1.882(4) . ?
Te03 O07 1.858(4) . ?
Te03 O06 1.880(3) . ?
Te03 O04 1.886(3) . ?
 
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
O08 Pb01 O04 93.65(13) 2_656 . ?
O08 Pb01 O04 80.50(13) 2_656 5_656 ?
O04 Pb01 O04 69.72(13) . 5_656 ?
O08 Pb01 O01 70.09(12) 2_656 2_646 ?
O04 Pb01 O01 72.41(12) . 2_646 ?
O04 Pb01 O01 129.70(11) 5_656 2_646 ?
O05 Pb02 O05 77.54(10) . 4 ?
O05 Pb02 O03 75.99(13) . 1_565 ?
O05 Pb02 O03 96.90(13) 4 1_565 ?
O05 Pb02 O02 74.12(13) . 6_565 ?
O05 Pb02 O02 118.51(11) 4 6_565 ?
O03 Pb02 O02 126.16(12) 1_565 6_565 ?
O06 Pb03 O02 92.98(13) . . ?
O06 Pb03 O09 77.68(13) . 7_556 ?
O02 Pb03 O09 81.99(13) . 7_556 ?
O03 Te01 O09 99.62(19) . . ?
O03 Te01 O05 96.08(16) . . ?
O09 Te01 O05 93.14(16) . . ?
O01 Te02 O08 95.23(16) . . ?
O01 Te02 O02 99.39(15) . . ?
O08 Te02 O02 93.59(16) . . ?
O07 Te03 O06 94.23(17) . . ?
O07 Te03 O04 99.90(16) . . ?
O06 Te03 O04 94.16(15) . . ?
Te02 O01 Pb01 109.56(16) . 2_666 ?
Te02 O02 Pb03 132.59(19) . . ?
Te02 O02 Pb02 105.24(15) . 6_566 ?
Pb03 O02 Pb02 109.16(14) . 6_566 ?
Te01 O03 Pb02 109.45(16) . 1_545 ?
Te03 O04 Pb01 128.58(17) . . ?
Te03 O04 Pb01 112.94(16) . 5_656 ?
Pb01 O04 Pb01 110.28(13) . 5_656 ?
Te01 O05 Pb02 118.55(16) . . ?
Te01 O05 Pb02 108.39(16) . 4_545 ?
Pb02 O05 Pb02 115.78(14) . 4_545 ?
Te03 O06 Pb03 123.54(17) . . ?
Te02 O08 Pb01 120.93(17) . 2_656 ?
Te01 O09 Pb03 141.3(2) . 7_556 ?
 
_refine_diff_density_max    1.541
_refine_diff_density_min   -3.085
_refine_diff_density_rms    0.444



# start Validation Reply Form
_vrf_PLAT972_plumbotell_c
;
PROBLEM: Check Calcd Resid. Dens.  0.55A   From Pb01           -2.98 eA-3  
RESPONSE: crystallographic ripples near heavy atoms
;
# end Validation Reply Form
